UNIVERSITY OF CENTRAL LANCASHIRE

SCHOOL OF COMPUTING, ENGINEERING AND PHYSICAL SCIENCES

COMPUTER AIDED ENGINEERING BEng (Hons)

FINAL PROJECT REPORT

Project – MP3997

A STUDY ON

HB9 - Functional Coatings for 3D Printed Parts

TUTOR

Dr Hadley Brooks

REPORT BY

Jonathan Ambrose

ACADEMIC YEAR

2014/2015

I. Declaration

I would like to declare that all of the work within this dissertation is my

own. Also, all references, quotations and support information are fully

identified and acknowledged in the reference list.

Student Name:

Student UCLAN ID:

Signed:

Date:

2

II. Acknowledgements

I would like to thank Charlotte Pickthall for being supportive and

understanding during my period at university.

A special thank you to my mother for her supportive nature and

encouragement to make me the person I am today.

With the addition consideration of all family, friends and tutors who have

provided understanding and support through thick and thin.

‘It is during our darkest moments that we must focus to see the light’

Aristotle Onassis

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III. Abstract

Physical testing results have shown that applying a metal coating to a

3D printed part improves the material properties whilst retaining the low

mass of the polymer.

Further tests and research are to be conducted to improve the two

methods of the process; Conductive Coating Solution and

Electrodeposition.

4

IV. Equation and Variable List

Faraday’s Law of Electrolysis (Electroplating Deposition Rate)

I = Electric Current, t = Time, Q = Electric Charge

W = Weight of the deposited material (g)

μ = Weight of one mole of the anode (Metal)

n = Number of electrons transferred by the ion into the solution

F = Faraday’s Constant = 96485 Coulombs

Consider electric charge = Q = I * t

Then Faraday’s law may be expressed by the following formula:

Faraday’s Law = W = I*t*μ /(n*F)

Vickers Hardness (HV) Conversion (Top) and HV Formula (Bottom)

5

V. Table List

Table 1 – 12 Orders of Magnitude

Table 2 - Polymer Solvent Reactivity Table

Table 3 - Conductive Coating Phase Risks

Table 4 - Electricity Human Damaging Table

Table 5 - Electrodeposition Phase Risks

Table 6 – Weekly Schedule of Work

Table 7 – Risk Management

6

VI. Applicable / Useful Patents, Standards and Safety

Legislations

The following are useful and applicable patents that allow for a better understanding

of the conductive coating and electrodeposition phases:

US 7235165 B2 – Safe Electroplating Solution

US 3715289 A – Brightener Composition for Acid Copper Electroplating

Baths

US 3542655 – Electrodeposition of Copper

CN 1152098 C – Graphite Conductive Coating Material

US 5476580 A – Process for Preparing a Non-conductive Substrate for

Electroplating

US 3249559 A – Conductive Coating.

The following are useful and applicable standards that allow for quality assurance of

material composition, preventing the influence of contaminants during the conductive

coating and electrodeposition phases:

BS EN 509-1:1987 – Acetone Purity Standard

BS EN 13604 – Copper Bar Purity Standard

BS EN 12166 – Copper Wire Purity Standard

ASTM B281 – 88 (2013) – Standard Practise of Preparing Copper

Electroplating Coatings

BS OHSAS 18001 – Occupational Health and Safety Management.

7

Applicable / Useful Patents, Standards and Safety Legislations

(Continued)

Before commencing work on the project, the following laws and regulations were

read and understood.

Health and Safety at Work Act (HASAWA) 1974

Control of Substances Hazardous to Health (COSHH) 2002

Personal Protective Equipment at Work Regulation 1992

Chemicals (Hazard Information and Packaging for Supply) Regulations

(CHIP) 2002

Electrical Equipment (Safety) Regulations 1994

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Contents

I. Declaration

II. Acknowledgements

III. Abstract

IV. Equation and Variable List

V. Table List

VI. Applicable, Useful Patents and Standards and Safety

Legislations

1 Summary ………………………………………………….……………..14

2 Introduction ………………………………………………………….….15

9

3 Literature Review …………………………………………………..…..16

3.1 Additive Manufacturing (3D Printing) 16

3.2 Conductive coatings 17

3.3 Electroplating 18

3.4 SEM (Scanning Electron Microscope) 19-22

3.4.1 Introduction 19-20

3.4.2 SEM Essential Equipment 20-21

3.4.3 SEM Limitations 22

3.5 Grain Growth effecting Coat Quality 23-24

3.6 Vickers Hardness Testing Machine (VHTM) 25-28

3.6.1 Introduction 25

3.6.2 VHTM Essential Equipment 26-27

3.6.3 SEM Limitations 28

3.7 Project Management 29-35

3.7.1 Introduction 29

3.7.2 Time Management 30-31

3.7.3 Risk Management 32-33

3.7.4 Resource Management 33-34

3.7.5 Experimentation Management of Project 34

3.7.6 Evaluation 35

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4 Electroplating Method ……………………………………………..36-54

4.1 Conductive Coatings 36-44

4.1.1 Materials / Resource Requirements 36-38

4.1.2 Health and safety 38-39

4.1.3 Method and Constraints 39-41

4.1.4 Observations and Risks 41-44

4.2 Electrodeposition 45-54

4.2.1 Materials / Resource Requirements 45-46

4.2.2 Health and Safety 46-47

4.2.3 Method and Constraints 48-51

4.2.4 Observations and Risks 52-54

5 Mechanical Property Testing ………………………………………...55

5.1 Hardness Tests 55-56

5.1.1 Results 55-56

5.2 Conductivity 57

5.2.1 SEM Images 57

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6 Conclusion and Recommendations ………………………………...58

6.1 Further Research Recommendations 58-61

6.1.1 Experimental / Commercial / Industrial Applications 58

6.1.2 Conductive Coating Recommendations 58-60

6.1.3 Electroplating Recommendations 61

6.2 Evolution of Experimental Sample Results 62-67

6.2.1 Initial Experimentation Results 62-65

6.2.2 Implementing Experimentation Knowledge to Final Design 65-67

6.3 External Constraints 68-69

6.3.1 Industrial Constraints 68

6.3.1.1 Manufacturing 68

6.3.2 Commercial Constraints 68

6.3.2.1 Customer Needs 69

6.3.2.2 Selling Price 69

6.3.2.3 Quality Regulation 69

6.3.2.4 Patenting 69

6.4 Conclusion 70-73

6.4.1 Conclusive Introduction 70

6.4.2 Conductive Coating Conclusion 70

6.4.3 Electrodeposition Conclusion 70

6.4.4 Post-Treatment Conclusion 71

6.4.5 Hardness Conclusion 71

6.4.6 Final Conclusion 71-72

6.4.7 Project Costing 73

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7 References …………………………………………………………..74-75

8 Appendices ……………………………………………………...…76-170

8.1 Personal Learning 76

8.2 Project Diary 77-88

8.3 Project Plan and Specification 89-94

8.4 Task Gantt Chart 95

8.5 Project Gantt Chart 96

8.6 SEM Training Manual 97-101

8.7 VHTM Training Manual 102-107

8.8 Support Data 108

8.9 Material Safety Data Sheets (MSDS) 109-170

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1 Summary

This report presents the development of functional coatings for 3D printed parts.

This was initially composed due to the need for simple and effective coating

techniques upon 3D printed parts. This is only viable for polymer printed parts;

therefore two elements were devised for successfully producing plated coatings

upon polymer parts:

Creating a uniform Conductive Coating

Electroplating Homogenously

The techniques developed were compared for value simplicity and quality of

coating, whilst considering cost, material properties and safety.

The stages of development shall include multiple techniques to which they are

applied with; the superior methods shall include evidence and data with

controlled experimental methods.

This report finds that combining conductive coating and electroplating techniques

upon the 3D printed part.

This successfully enhances the electrical conductivity, Young’s Modulus,

compressive and tensile strength and hardness from the incorporation of the

metal coating; with the additional benefit of having an increased resistance to

corrosion.

For more information on the plan and specification see appendices 8.3 project

plan and specification.

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2 Introduction

This project will be the sole work of Jonathan Ambrose under the supervision of

Dr Hadley Brooks. This report has been written to satisfy the learning outcomes

stated in module MP3997. This module is a requirement for awarding an honours

degree at the university of central Lancashire.

A head researcher of manufacturing stated” the additive manufacturing industry

has grown exponentially from a value of $200M in 2009; to 2014 with $1B worth

of systems” Gibson, I (2011). This developing manufacturing technique is

improving how products are manufactured; locally and internationally.

There is a continued need to improve this process, to expand the capabilities of

the technique whilst reducing price and increasing quality.

Additive manufacturing technology is still in its early embryonic stages and has

great potential for future development.

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3 Literature Review

3.1 Additive Manufacturing (3D Printing)

Additive manufacturing (AM) is the creation of a 3D object from a CAD model to a

solid model via an AM technique. Experts have stated that it is important to

understand that AM was not developed in isolation from other technologies. For

instance it would not be possible for AM to exist were it not for innovation in areas

like 3D graphics and Computer Aided Design software, this view was supported

by Gibson, I (2011).

This report shall investigate the Fused Deposition Modelling (FDM) technique.

FDM uses a .STL file (a CAD file which has been converted into a path to follow)

which manipulates the extruder nozzle on the FDM.

The extruder follows via Cartesian coordinates whilst extruding material;

essentially developing and building a 3D Model as supported by Dr Chua, C

(2014)

Other AM techniques offer a variety of qualities in regards to cost, material

properties, speed of print, variety of materials used, tolerance of print, less waste

etc. This flexibility AM offers has near limitless capabilities to which it has been

realised that the biggest spur for AM was not the limitless customisation, but the

economics of production.

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3.2 Conductive Coatings

A researcher stated that conductive coating is an applied material which is

electrically conductive, embedded upon a component which may or may not be

previously conductive. Davis, J (2004). The following are crucial parameters

which need to be considered and adopted when developing a conductive coating

solution and method:

Adhesion

o Quality of adhesion between conductive solution and component

which is to be coated

Conductivity

o The resistance of the post-electroplated part is at least 95% of the

anode

Hardness

o Hardness of post-coated part is hard enough to resist damage

during electrodeposition is aimed at achieving 75% of the anode

Safety of Chemicals

o The chemicals used during this phase need to have MSDS for each

to make the user aware of the risks involves with specified PPE for

each. The safest methods shall be of priority.

Research has been conducted to develop a conductive solution based on systematic

experimentation. Data from these trials has been developed and improved.

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3.3 Electroplating

Electroplating (or otherwise known as electrolysis) is the method of applying an

electrically conductive material (known as the anode) upon a conductive part

(known as the cathode).

This method uses a power supply, Anode, Cathode and a plating solution; with

multiple parameters depending on application. However in practise this works as

follows:

The Plating Solution is placed in a non-conductive container (Usually

Glass)

The power supply is set-up connecting the anode to positive (coating

material) and the cathode to negative (component being plated)

The Anode and Cathode are placed within the solution (Not Touching)

The power supply is turned on to the relevant voltage / current

Apply coating material sulphate to solution to speed up coating (e.g. if

using copper as the Anode, add copper sulphate to the solution to speed

up the coating process) Also use Faraday’s Law to calculate the

deposition rates

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3.4 SEM (Scanning Electron Microscope)

3.4.1 Introduction

“A SEM uses a focused beam of high-energy electrons to generate the

topography of the component or sample of solid specimens” stated by Egerton,

R. F. (2005). The signals which develop the information are from electron-sample

interactions which reveal information about the specimen including topography,

material composition, crystalline structure and orientation of materials which

make up the sample. In the majority of applications the data collected is from a

selected area on the surface of the part which generates a 2D / 3D image

displaying the spatial variations on a tribological scale. The SEM is used due to

the order of magnitude required to gain reliable results for this particular

application. See below for the 12 orders of magnitude.

Table 1- 12 Orders of Magnitude

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The applicable surface area range which the SEM can develop is approximately

1cm to 5 microns squared. This can be imaged in conventional SEM techniques.

Magnification can range from 20X to 30,000X, with spatial resolution of 50 to

100nm. A SEM scientist described the capability of the SEM as “capable of

generating graphical feedback showing the topography on a 3D generated graph

also showing the average peaks and troughs between designated areas”. Clarke,

A. R. (2002).

3.4.2 SEM essential equipment

The SEM needs the following essential components to be able to produce highly

accurate results and sustain component quality:

Electron source

Electron lenses

Sampling stage

Signal detectors (Electron Sample Interactions)

Output Devices to Display Data (i.e. Monitor)

Infrastructure Requirements:

o Power Supply

o Vacuum System

o Cooling System

o Vibration-Free Floor

o Room free of magnetic and electronic interference (fields)

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SEM has the following benefits; it has the ability to produce data extremely fast,

with the sample preparation time being less than 5 minutes. The data available is

in digital formatting making it highly portable. As an investigating tool the SEM is

of great importance in all fields that require specification of solid materials from

topography to composition.

An extremely useful aspect of the SEM, is its ability to also produce composition

tests to accurately produce sample material composition reading with supporting

graphs. The SEM (Inspection Machine 1) used to conduct the experiments is

shown below.

Inspection Machine 1 - SEM (Found in JB Firth Building)

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3.4.3 SEM Limitations

However, the SEM does have limitations which are the following:

Samples must be Solid

Maximum Horizontal Dimensions are around 10cm

Maximum Vertical Dimensions are around 40mm

Samples must be stable in a vacuum at 10-5 to 10-6 torr

Samples may depreciate at low pressures (Low vacuum and

Environmental SEM variations exist)

SEMs cannot detect very light elements (H, He and Li) and unable to

detect elements with atomic numbers less than 11

Electrically Conductive coatings must be applied to electrically insulating

samples for study in conventional SEMs (However Gold Powder Coating is

Available for Non-Electrically conductive samples)

For more information on the usage of the SEM and the Official UCLAN Training

manual see appendices 8.7 SEM Training Manual.

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3.5 Grain Growth effecting Coat Quality

During electroplating, the grain growth on the Cathode is directly proportionate to

the voltage applied during electrolysis; which in-turn reflects the quality of the

applied coat.

A Grain Growth researcher considered that the energy of the grain nucleus’

formation, depends on the cathode of potential voltage. A. Milchev (2002).

The following parameters need to be adjusted to accommodate for the copper

plating process on the graphite:

Maintaining Optimum PH Level

Electroplating Solution Temperature

o An electroplating researcher stated “It should be noted that

increasing the bath temperature has two contradictory effects; (i) an

increase in critical size of nucleus due to a decrease in

thermodynamic driving force of the crystallization. This leads to

lower nucleus densities, (ii) an increase in kinetic the driving force

that can lead to a higher nucleation rate” J.W.P. Schmelzer (2003):.

Electroplating Solution / Copper Sulphate Density

Voltage through Anode to Cathode

It was found that increasing the voltage beyond the limit affects growth

consistency and quality. This is due to during the electroplating phase the

voltage breaks the anode down and attaches that to the cathode. This

replaces electrons; during this process the anode is heated and therefore

expands creating bigger grain growth. The use of Faraday’s law and an

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SEM should be used to gather information of the optimum voltage for

electroplating. For this specific grade of copper used. The optimum voltage

for this experiment was found to be 1.5V / 20mm2.

Below shows how voltage during electrodeposition affects grain growth

Figure 2 –Low voltage electroplating (Left), High Voltage Electroplating (Right)

From the observation it can be seen that increased grain growth affects the

aesthetics of the part however it has not yet been tested whether this affects the

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material properties. Further research should be conducted whether it could be used

at an advantage to improve a specific area of material properties.

3.6 Vickers Hardness Testing Machine (VHTM)

3.6.1 Introduction

The Vickers Hardness Testing Machine (VHTM) is a material property testing tool

that measures the material property of hardness. This test uses a square based

pyramid diamond indenter with an angle of 136 degrees between the opposite

faces at the vertex. The Indenter presses into the sample using a user defined

force (F), the total test time is 20 seconds long; once the force is removed, the

legnths of the vertex’s are measured (d). The hardness number is given by the

following formula. See HV rating and conversion rating formula below.

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Diamond Indenter

Equation 1 - Vickers Hardness Conversion to Mega Pascal

3.6.2 VHTM Essential Equipment

The VHTM requires essential components to be able to produce highly accurate

results and sustain component quality. The following are the essential

components of the VHTM:

Diamond Indenter

Calibration Blocks and Setters

Sampling Base

Output Gauge.

Due to the basic set-up and operation of the

VHTM and no electronic source, it becomes

simple to measure the HV rating.

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VHTM Calibrating Gauge Set

The VH testing machine used to conduct material tests on the samples

developed is showns on the next page.

Hardness Testing Machine 1 – Vickers Hardness Testing Machine

27

For the methodology of using the VHTM see appendices 8.8 VHTM training Manual.

3.6.3 VHTM Limitations

Due to the simplicity of the VHTM, measurements of the indenting vertex are

inspected by the user, which introduces human error during measurement. With

the addition of calibration introducing any further error.

The indenting of the sample during the release of the load, can spring back due

to elasticity of the component which introduces further inaccuracies.

The wear and tear of the indenting tool can also affect inaccurate results,

however being diamond tipped this can be of low possibility.

Overall the limitations which appear are the inaccuracies of preparation and

usage by the user. However careful preparation and measurements are to be

carefully to ensure the highest of accuracy.

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3.7 Project Management

Project Management is key in creating an efficient and effective usage of a

project resources, deliverables and quality of products. This ensures the project

runs smoothly to which milestones are met at designated time frames.

3.7.1 Introduction

This section of the report, introduces the project management methods

implemented. The following will describe and evaluate the methods used.

‘Even if you are on the right track, you will get ran over if you just sit there’ (Covey

1996) The quote by Steven Covey tells us that no matter if you are on the right

direction, a plan needs to be made and progress needs to keep going. One of the

largest risks in this module is the possibility of failing, with this being of core

priority this has to be passed.

Progress has to be made to ensure success; this is why project management is

crucial for this instance. The following sections shall delve into more detail in time

and resource management of the project.

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3.7.2 Time Management

The managing of time is one of / if not the most crucial resource within any

project of any size. Without proper managment of the project over an available

time scale, the work done will be hard to track and maintain a momentum to

complete the course at university.

This is to be prepared and managed effectively at the start of the project to create

milestones and effectively utilize of one’s time; an effective tool for managing time

is by creating a Gantt chart.

Henry Ford who is the founder of Ford Motor Company once said ‘ Nothing is

particularly hard if you divide it into smaller jobs’; from the success of Henry Ford

this shows that any task can be completed by dividing into smaller chunks to

complete, which is therefore why the development of the Gantt chart began.

See appendix 8.4 for this projects developed Gantt chart.

Due to the amount of work to be completed during the time at the university

course a weekly project plan was developed to organize and schedule the time

resource. This can be seen in table 6 to the right.

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Table 6 – Weekly Schedule of Work

The above table shows the initial weekly schedule plan which was used as a

guide to maintain work progress between modules, to which it shows at least 20

hours allocated for the project work each week.

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3.7.3 Risk Management

Throughout any project, a degree is risk exists which could affect the overall

progress and relinquish resources. This is why at the start of a project, the risks

need to be identified early to minimize the impact on the project and develop

necessary actions to take when one does occur.

Table 7 shows the risks present from the start of this project and processes made

to reduce each risk. A traffic light system has been used to identify the level of

each risk; with green being low, indicating the impact will be low on the project;

red being the highest of risks therefore having the greatest impact on the project.

Table 7 - Risk Management

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The majority of the risks are universally the same at a project of this level. The

processes to reduce each slightly differ; however notice how losing motivation can

be of low risk to which it has been identified that the project student is a kinaesthetic

learner from the VAK test taken; this therefore creates a customized solution.

3.7.4 Resource Management

An expert in project management stated “the management of resources at their full

potential whilst extracting the knowledge and creating progress is key with any

resource” Pugh, S. (1991). The following are resources used with benefits and

limitations to both:

Time

o The benefit is that time is free and becomes better utilized to which the

more is spent.

o The limitation is that the resource may be low and repetition and

boredom can occur if used on a regular basis; reducing the utilization

of the resource.

Computer Software

o The benefit is that it allows quicker processing of information.

o The limitation is that it requires skills which may not have been learned

therefore time would have to be used to learn.

Online Information

o The benefit is that it allows a broader knowledge to be gained, it

requires heavily on the resource time but can gain a lot of knowledge

from similar projects already made.

33

o The limitations is that it may not be a valid source of information

Chemicals / Materials

o The benefit allows direct hands-on experimentation validating results

investigated.

o The limitations are it requires money and possible lead-time if ordered

in.

Computer Software

o The benefit is that it allows creation and sorting of tasks, such as gantt

chart, Microsoft word and excel, supporting interfaces with machines

etc.

o Costs money for software and time to train to learn.

3.7.5 Experimentation Management of Project

Throughout the preliminary stage of the project, current methodology of the

project was of low existence which depended on experiments and trial and error

to be heavily focused on. This created a burden on the developed Gantt chart

and its processes, however maintaining a weekly schedule and creating an

effective process of gained knowledge allowed progression to be exponential.

This developed a learning curve of knowledge allowing me to strategic set tasks

from the results gained, to increase the chance of creating concrete results to

develop a methodology.

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3.7.6 Evaluation

During the management of the project a good way to keep track of the progress

was to create a Gantt chart and define set times within the week to work. The

main problem which occurred was that all the tasks could not be defined. This

was due to lack of knowledge during preliminary stages, preventing progress to

be met.

This resulted in repetition of the testing phases to produce adequate knowledge

and effectively produce a learning curve to understand the process.

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4 Electroplating Method

4.1 Conductive Coating

4.1.1 Materials / Resource Requirements

The conductive coatings stage, consisted of multiple techniques that require use

of various equipment and materials. The following list shall consist of all

equipment used for all the methods:

Paint Brushes / Variable Brushes (Preferably Short Bristles)

Rotary Buffer / Polisher (Minimum 2000 RPM)

Polisher Pads (for Rotary Buffer)

Buffer Pads / Cloth

Glass Container (Preferably >250ml)

Atomizer / Spray Bottle (Not made from ABS, Acrylic, CPVC, PC, PVC and

PVDF)

Graphite (Powder) At least 90% Carbon*

Acetone Solution BS EN 509-1:1987*

Grey Primer AutoTek*

ABS (Solid State)

Copper Powder

*Note Materials to British Standard are Ideal but not necessary, to which poor

quality material will still perform the experiment well i.e. instead of copper rod

a 2 pence coin as the anode will still perform electroplating but poorly.

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An alternative to Acetone is Grey primer; from the experiments has shown

significant improvements in material wear resistance and cathode coverage.

Results have shown that the Grey Primer has additional solvents are including

which have shown to improve the quality of the coating.

Check table below for applicable materials which will work B – D with possible

results from A. Different solvents. If safety and speed of plating is priority,

Acetone is recommended; if quality and increased mechanical properties are

priority the use of primer is recommended. Both are to be used carefully with

safe preparation and control.

Table 2 - Polymer Solvent Reactivity Table - Prairie, E. (2009)2.

37

Key:

A = No Attack, possible slight absorption. No effect on mechanical properties.

B = Slight attack by absorption. Some swelling and a small reduction in

mechanical properties.

C = Moderate attack of appreciable absorption. Material will have limited life.

D = Material will decompose or dissolve in a short time.

‘* ‘ = No Data Available.

4.1.2 Health and Safety

Health and safety was considered for all multiple methods that require a certain

degree of preparation to avoid possible risks. The chemicals / materials used are

relatively safe to which skin contact with any of them listed; will not cause harm.

However due to being pure chemicals it is recommended to wear protective

goggles and gloves whilst handling the materials.

Also be aware of the low vapour pressure properties of Acetone and grey primer;

which is highly flammable in its liquid and vapour state. This can cause light-

headedness during inhalation; it is recommended to wear a procedure mask

during usage; however from the MSDS in Appendix 8.1 there is no evidence to

suggest carcinogenic properties exist in Acetone due to the organic nature of the

chemical.

To see the Material Safety Data Sheet of any of the chemicals listed above see

Appendix 8.1.

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The equipment used for creating the conductive coating is relatively safe with no

lethal consequence under normal use; however the only piece of equipment

which may cause harm is the rotary buffer; which is powered electronically

therefore posing the risk of electrical faults and moving parts (spinning rotary).

Under normal / safe operation of the equipment listed and correct PPE equipped,

the operation shall pose minimal risk.

Table 3 - Conductive Coating Phase Risks

4.1.3 Method and Constraints

Creating a conductive coating on an ABS part can be split into two phases;

initially embedding graphite into the ABS; secondly, aligning the graphite to

become conductive. The following 4 phases of applying the conductive coating

are as follows:

1. Firstly creation of the conductive solution; uses 1 part graphite powder to

10 parts solvent. This mixture is flexible to change as long as the solution

becomes dark. This is due to the solution evaporating during normal

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atmospheric use. (Note: Too much solvent will cause details within the

model to smoothen)

2. The solution is then applied to the component via brushing. Once the part

is fully covered leave for 5 minutes at room temperature for the solution to

evaporate in a well ventilated; area due to risk of light headiness. During

evaporation the component appears cold, this is due to the low vapour

pressure of the solution. It is recommended to wait until the component

returns to room temperature to avoid damaging the component.

WARNING: Beware of application of ACETONE near sparking tools due to

FLAMABILITY. To ensure safety; when applying, leave to dry before

setting sample upon the electroplating phase.

3. Once the part is dried, the buffing stage begins. It is recommended to use

a rotary buffer (RB) at 2000 RPM, however if that is unavailable use of a

cloth or tissue, is recommended. Rub in small circular motions until the

component appears Grey Metallic.

4. The first layer should now be complete; repeat this step 2 more times to

develop 3 layers. Once all 3 layers are complete, record the resistance

using the multimeter. Usage of the RB method should record a resistance

of around 50Ω-100Ω or using the cloth / tissue the resistance should be

around 150Ω-400Ω.

40

The resistance on the surface of the component is directly proportional to the

quality of the buffer to which the lower the resistance of the buff the better the

quality of coat.

The lower the resistance the quicker and smoother the electroplating will be so

ensure that the component is fully buffered on each layer and comprises of a

shiny grey texture.

Due to lack of resources at this current time, it is found that the quality of the

conductive coating is directly correlated to the quality of the electroplating

procedure. A superior theoretical alternative will be to buffer the post-conductive

coated part with a fine sand blast. This provides benefits of being able to reach

complex areas (which are unable to be buffered due to location), and provides a

smooth alignment of the graphite grain.

Observations and Risks

During creation of the conductive coating it has been found that during

impregnation of the graphite / solvent solution the surface of the component will

remain soft to which buffering / contact during this stage is to be avoided until the

solution has evaporated. To test the surface softness, lightly press the multimeter

probe against the component, if an indent appears, leave the component longer

to cure. DO NOT apply component near a heat source i.e. radiator due to this

may cause the graphite to separate from the polymer sample.

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Scratchable Rating:

A

: Unscratable, Very hard to remove coat

B

: Hard, Scratable but takes effort to remove

C

: Intermediate, Takes abit of pressure to remove

D

: Soft, Little pressure needed to remove

E: Easily Scratched off, No or Little pressure needed.

Conductive Coating Phase

Resistance in Ohms

(10mm^2 and 20mm^2) Scratch able Rating

1L-2RPM 550 E

1L-10RPM 280 D

3L-2RPM 50 C

3L-10RPM 30 C

1L-2RPM-ABS 800 E

1L-10RPM-ABS 750 E

3L-2RPM-ABS 500 D

3L-10RPM-ABS 450 C

42

Key:

1L : 1 Layer of Graphite / Acetone Solution

3L : 3 Layers of Graphite / Acetone Solution

2RPM : Buffered at rotary speed of 2000 RPM

10RPM : Buffered at rotary speed of 10000 RPM

ABS : 2% ABS 98% Graphite / Acetone Solution

BRPM : Lowest Resistance out of 2000 / 10000 RPM

2HR : Data Recorded after 2 hours Electroplating @ 1V

4HR : Data Recorded after 4 hours Electroplating @ 1V

OS : Electroplating using Original Solution

NS : Electroplating using New Solution

Acetone / Graphene Solution Experiment

Spray + Burn 1 Layer 3 Layers Spray 1 Layer 3 Layers

+ Gr = None 800 300 + Gr = None 1200 800

+ Gr = 10% 700 150 + Gr = 10% 1100 750

+ Gr = 30% 550 60 + Gr = 30% 1000 700

Key:

+ Gr = Added Graphite

ALL UNITS ARE IN OHMS

Burn = Burnished

43

A problem occurred during the preliminary stages of the project of that the

atomizer became clogged due to the graphite / acetone solution. An emulsifier

could be incorporated within the solution to reduce the pressure vapour within the

solution therefore allowing the solution to flow through the nozzle, reducing the

clogging. The atomizer is to be avoided due to this case.

It is found from the preliminary experimenting with the initial samples that

increasing the number of applied layers and buffering rotary speed, significantly

improves the coating quality. This reduces the overall electrical resistance

(OHM). However adding ABS into the conductive solution reduces this

improvement of the coat, it was initially theorised that this will increase the

bonding to which it may have done, but results have shown it decreases the

overall electrical resistance (OHM).

44

4.2 Electrodeposition

4.2.1 Materials / Resource Requirements

During the electroplating stage, multiple techniques require use of a range of

equipment and materials, the list following shall consist of all equipment used for

all methods:

Power Supply / DC Unit

Glass Container (Preferably >250ml)

Power Supply Clips / Crocodile Clips

Oxalic Acid

Trisodium Phosphate

Ammonium Sulphate

Water (Preferably Distilled)

Copper Sulphate

Nickel / Copper Anode

Copper Rods / Bar BS EN 13604*

Copper Wire BS EN 12166*

Hydra* Copper Brightener

*Note materials / brands and British Standards are Ideal but not necessary.

Poor quality material will still perform the experiment sufficiently i.e. instead of

45

copper rod a 2 pence coin as the anode will still perform electroplating but

poorly.

It is found that alternative electrolysis solutions exist that may improve the quality

of the coat; however from existing patents and research this solution has been

found to suffice to the needs of the project. The current solution is safe to apply

(Contains No Corrosive Chemicals) and is applicable to current resources. See

VI Applicable / Useful Patents, Standards and Safety Legislations for alternative

electroplating solutions.

4.2.2 Health and Safety

Health and safety are considered for all methods that require a certain degree of

preparation to avoid possible risks; the chemicals / materials used are relatively

safe to which skin contact with any of them listed will not cause harm. However

due to being pure chemicals it is recommended to wear protective goggles and

gloves whilst handling the materials.

Due to a majority of the chemicals listed, being used as baking products (Except

Copper Sulphate) it is relatively safe. However it is recommended to wear

protective goggles and gloves whilst handling the materials; however due to the

increased risk with ingestion or inhalation of copper sulphate it is strongly

recommended to wear protective goggles, procedure mask and gloves whilst

handling this chemical.

To see the Material Safety Data Sheet of any of the chemicals listed above see

Appendix 8.1.

46

The equipment used during electroplating are non-lethal, however the piece of

equipment that offers risk is the DC Unit. It is recommended to be aware of the

outgoing current which may cause electrocution.

See electric damaging scale to the right, to see how much current is harmful.

Table 4 - Electricity Human Damaging Table - Oli Glaser. (Sep' 2011).1

47

Table 5 - Electrodeposition Phase Risks

4.2.3 Method and Constraints

Electroplating the polymer conductive component uses methods which are

capable to be manufactured on an experimental, commercial and industrial level.

However the electroplating solution involving the following Ideal* mixture of

chemicals:

32g Oxalic Acid

10g Trisodium Phosphate

4g Ammonium Sulphate

950mL Distilled Water

5g Copper Sulphate

(1g Copper Brightener)

48

The above mixture excluding brackets is under a patent No US 7235165 B2 by

Richard Lacey. This allows experimental and scientific exploration uses, but

prevents commercial and industrial use; without patent consent. Patent No US

3715289 A by Stauffer Chemical Co uses a Brightener composition for acid

copper electroplating baths. In this instance this patent isn’t used but can be used

as a guide to improve the quality of the methods listed further in this report.

However the mixture of the chemicals mentioned above (including the bracket) is

currently not patented (Correct at April 2015); therefore it can be applied

privately, commercially and industrially without any legal consequences.

The solution used is relatively safe, however it is recommended to wear

appropriate PPE.

The following are 8 phases of the electroplating stage:

1. The cathode (+) is the component that is to be coated and the anode is the

substance of the coat. The anode for this case shall be copper bar or

ideally copper wire. (Recommendation: Copper wire shall fully surround

the Cathode with a recommended length of 3 times the circumference of

inside the container)

2. The cathode is to be connected to the negative electric flow (-) via the DC

unit and anode to the positive. (Do not turn on the power supply till all

equipment is secure and set-up).

49

3. Using the crocodile clips to connect each substance, do NOT let the clips

become submerged in the solution as this will attract the copper ions

during electroplating and influence the components coat to be uneven.

4. During total submersion of the part at 1v for 2 hours. Rotate the

component to improve the uniformity of the coating. Repeat this stage by

incrementally increasing voltage by 1v (Maximum of 5v).

(Recommendation: Between each stage ensure that the solution is stirred

due to the instability of the copper sulphate within the electroplating

solution.)

5. If all phases mentioned previously have been followed and care has been

taken on each step the copper coating shall be bright, however complex

parts may endure decolourisation upon the part; if this occurs repeat the

final submersion stage (5v for 30mins) as many times till satisfactory coat

has been performed.

6. If a copper coat is not satisfactory after phase number 5, check the

resistance of the Anode. Exposure of the anodes integrity can fall due to

material being converted into copper sulphate within the solution; or re-

buffer component and repeat. If problem persists there may be a fault with

the purity of chemicals, composition of solution or power supply failure.

7. During electroplating oxides and discolouration can occur, this is just a bi-

process of the electrodeposition phase. To overcome this copper

50

brightening agent should be used in-conjunction with the electroplating

solution; this dissolves the oxides and promotes uniformity within the

applied layers. If discolouration hasn’t occurred continue to step 8.

8. To improve the aesthetics of the coat quality, electroplate for 15 minutes

@1.5v, this produces fine copper grain growth and creating an overall

better post-electroplate look. Repeat if necessary.

9. Submerge in a solution of 10 parts water, 1 part brightener powder for 15

minutes to achieve a brightened component. See post-electroplated Yoda

below.

51

Post-Electroplated Yoda Submerged in Brightener Solution

52

4.2.4 Observations and Risks

Observations and experiments have been made with the appropriate coding’s

and results below.

Electroplating Sample Phase

Resistance in Ohms (10mm^2 and 20mm^2) Scratchable Rating

1L-BRPM-OS-2HR 80 C

1L-BRPM-OS-4HR 30 C

3L-BRPM-OS-2HR 10 C

3L-BRPM-OS-4HR 2 B

1L-BRPM-NS-2HR 60 C

1L-BRPM-NS-4HR 25 C

3L-BRPM-NS-2HR 10 C

3L-BRPM-NS-4HR >1 B

Key:

1L : 1 Layer of Graphite / Acetone Solution

3L : 3 Layers of Graphite / Acetone Solution

2RPM : Buffered at rotary speed of 2000 RPM

10RPM : Buffered at rotary speed of 10000 RPM

ABS : 2% ABS 98% Graphite / Acetone Solution

BRPM : Lowest Resistance out of 2000 / 10000 RPM

2HR : Data Recorded after 2 hours Electroplating @ 1V

4HR : Data Recorded after 4 hours Electroplating @ 1V

OS : Electroplating using Original Solution

NS : Electroplating using New Solution

53

Scratchable Rating:

A

: Unscratable, Very hard to remove coat

B

: Hard, Scratable but takes effort to remove

C

: Intermediate, Takes abit of pressure to remove

D

: Soft, Little pressure needed to remove

E: Easily Scratched off, No or Little pressure needed.

From the electroplating sample phase results. Evidence has found that the increase

in applied layers and submersion time during electrodeposition is directly

proportionate to the electrical resistance and scratch able rating. However it is shown

that using the grey primer delivers a better post-electroplated sample.

From the results above, the general trend of the solvents performance can be shown

on a graph below.

54

The trend is caused by the additional graphite content and mixture of solvents

which attribute for the application of this process. It is recommended that with

further research, the content of graphite in conjunction with a mixture of

adhesives, can improve the quality of the coatings. (See Appendices 8.3 Material

Data Safety Sheet MSDS – AUTOTEK GREY PRIMER MSDS)

The observational risks that can occur electroplating during the phase is that

exposure to high amounts of voltage can cause a degrading of a coat quality

During the submersion of the component in the electroplating solution, ensure

that the part is cleansed after submersion. This prevents a crystalline texture can

be caused due to solution drying and oxidizing on the surface. See Crystallized

Part below.

Post-Electroplated Crystalized Component

55

5 Mechanical Property Testing

5.1 Hardness Test

5.1.1 Results

The current experimental samples have been conducted upon the Vickers

Hardness Testing Machine. Below shows a table of the Hardness Vickers Rating

with the conversions into Pascal shown.

56

Evidence shows that the conductive coatings solution added on the ABS sample

provides no additional hardness, however the application of copper for 4 hours of

sample 3L-10RPM-CP has shown a total hardness of 40% (215MPa) that of the

Anode; 3L-10RPM-CP-NP has been exposed for a total of 8 hours (4 for Copper

and 4 for Nickel) has shown a total hardness of 90% (540MPa) of the hardest

anode.

57

5.2 Conductivity Test

5.2.1 SEM Images

The image to the right shows that

the acetone / graphite solution at a

magnification of 800x, with a scale

on the bottom right at 50 microns.

Notice how there are large contours

and the brightness of the sample

piece.

This is a basic indication of the electrical conductivity between samples (as long

as the brightness / contrast aren’t

adjusted on the SEM interface).

The image to the right shows that the

grey primer / graphite solution at a

magnification of 800x with a scale of

50 microns. Notice that this image

appears brighter and has less large

contours; this reflects electric

conductivity as the SEM uses electrons bouncing of a sample to develop an

image. This shows that this image should have a lower electrical resistance.

From the results shown previously, this theory appears to be correct.

6 Conclusion and Recommendations

6.1 Further Research Recommendations

58

Figure 3 - Acetone / Graphite Solution @800x Magnification on SEM

Figure 4 - Grey Primer / Graphite Solution @800x Magnification on SEM

6.1.1 Experimental / Commercial / Industrial Applications

The methods and material compositions used in both the conductive coating and

electroplating phases; are bound to no legal limitations for experimental,

commercial and industrial applications.

6.1.2 Conductive Coating Recommendations

The following are further application recommendations, which would have been

progressed to. However due to time and resource as the main constraint, this

feature has been developed to provide an insight to the planned further research.

Further advancements on the current processes, can be improved with the use of

a fine sand-blasting for the buffer phase. The parameters which will need further

research are the sand size and force per cm2. This has shown theoretical benefits

of reaching complex locations on the component, an increased homogenous of

the electro-resistance coat and more control over producing a low electrical

resistance. With the possible capability of developing an even lower resistance

rating than initially developed.

The following are the benefits of sand blasting and the theoretical material

property advancements:

59

Homogenous Post-buffer coating

o Creating a more even electroplating coating

More Control over the Post-buffer Coating

o Due to constant force of blasted particles at the same

distance allows various conductivity ratings for various sizes

and materials.

Possibility of very low electroplating resistance than from methods

used initially

o Less Voltage needed to electroplate

o Less Time to coat

An additional recommended method that could be developed, will be vacuum

bagging of the component to compress the graphite grains. Theoretically

mimicking the burnishing phase, the following are the possible benefits:

Homogenous Post-Buffer Coating

Lower Removal of Material

Possible lower resistance achieved

60

A materials / chemicals recommendation will to continue further study into a

higher applicable solution. From current studies it has shown that adding graphite

with the AutoTek grey primer has shown significant improvements than just

adding graphite to 95% pure acetone. Therefore below is the chemical list of

added materials with the majority being a mixture of butane, propane and

acetone. This provides the possibility that the mixture of solvents improves the

application. Below shows the current composition table of the AutoTek Primer

from Appendices 8.9 Material Data Safety Sheets.

During the bonding of the graphite particles, a certain percentage of added

graphite increases the connectivity until bonding is of excess; this can be

described as the percolation threshold. This is recommended to be further

61

researched to gain a broader knowledge on the optimum amounts of added

graphite.

6.1.3 Electroplating Recommendations

Further Advancements on the current process enables multiple layers of coatings

to develop multiple material characteristics. The following are ambiguous

methods applicable from multiple layers:

Multiple coats including thermal protection, electrical conductivity,

increased impact / hardness / tensile properties etc.

A battery expert stated that “In collaboration of a zinc and copper coat

submerged in an electrolyte can essentially produce a battery which can

be used for applications that may be submerged in sodium, potassium,

calcium, bicarbonate, magnesium, chloride, hydrogen phosphate and

hydrogen carbonate” A.M. Rashidi. (2010).

A circulation pump within the electrodeposition tank can be developed to

aid the sulphates bond to the cathode evenly.

There appears to be room for improvement for the electroplating solution. From

the perspective of current resources and safety, practically the current solution is

acceptable for this application.

62

6.2 Evolution of Experimental Sample Results

From the preliminary experimental samples, the lack of expertise in theoretical

and practical applications created poor results. However with increased research

in specific elements of the process, the results can be shown to be progressed

visually with SEM statistics as evidence.

6.2.1 Initial Experimentation Sample Results

Initial methods of the application have shown to be significantly improved. Below

are the preliminary results from the lack of expertise, the methods have still

shown dramatic improvements to which all the methods where re-defined and

improved.

1 Layer 2 Layer 3 Layer0

2000

4000

6000

8000

10000

12000

14000

16000

4200

3500

1200

Conductive Resistance of Coating Application

applied layers of conductive solution

Resi

stan

ce R

ating

in O

hms

63

The graph above shows the application of the initial solution (Acetone and

Graphite) and the building up of layers to which are measured at 10mm2 and

20mm2.

1 Layer 2 Layer 3 Layer0

1000

2000

3000

4000

5000

6000 5500

21001500

3200

1800

800

Results after Burnishing Each Layer

APPLIED LAYERS OF CONDUCTIVE SOLUTION

RESI

STAN

CE R

ATIN

G IN

OH

MS

The graph above shows the application of burnishing each layer between the

applications of layers for the Initial Solution.

1 2 30.0

50.0

100.0

150.0

200.0

250.0

300.0

350.0

400.0

450.0400.0

160.0

3.4

Resistance of Coating in Ohms

Hours Exposed in Electrolysis

RESI

STAN

CE R

ATIN

G IN

OH

MS

The graph above provides evidence for the amount of hours exposed in the

electroplating phase decreases the resistance of the coating in OHMS.

64

The graphs provided the foundation to develop methods from to utilize the best

method for the application to get the desired material properties; this data was at

the preliminary testing stage.

The sample pieces created during experimentation, improved through trial and

error, each method was incrementally improved. This has reached the highest

quality due to the time constraints to which future recommendations has been

logged in 6.1 Further Research

Recommendations.

Below shows a time view representation

of how visually the sample processes had

evolved which each step defined to the

right.

1. Shows the initial sample to which the

copper powder used within the

conductive solution, a problem

occurred with the quality of the copper

powder.

2. Once the conductive coating had

been of an acceptable quality, it was

set-up to electroplate to which the

voltage was too high and caused the

coat to bubble.

3. The first sample showing the

successful low quality coat of copper.

65

4. A thicker coat was achieved, to which 3 layers of conductive coating and 8v

electrodeposition @30mins was used.

5. An increase in voltage made the plating quality decrease which was the

cornerstone for low voltage.

6. After many samples of tweaking the processes, the defining time and voltage

was achieved at 1volts for 2hrs. The copper coat can be clearly seen and

distinctive.

6.2.2 Implementing Experimentation Knowledge to Final Design

Once the methods where re-worked and defined to its current levels, work on the

Yoda model begun. This was particularly complex due to the variety of the

surfaces which became a model to test the boundaries and quality of the

methods.

YODA – 3D Printed Part RAW

The image to the left shows the PLA

Yoda model in the preliminary phase or

Pre-Conductive Coating Phase.

YODA – 3D Printed Post-Conductive Coating

Phase

To the right shows the post-conductive coating

completion applied on the part, to which the

66

successful coating solution (Grey Primer Mixed with 10% Graphite + 10% Acetone)

has been applied onto the part, left to vapour off the solvent and embed the graphite.

The part was then burnished between each layer; this was repeated 3 times putting

a total of 3 layers applied. See 4.1 – Conductive Coatings for more details.

YODA – 3D Printed Post-

Electroplating Phase

The post-electroplating phase is

the effect of a total submersion and

electro-deposition of 6 hours using

the electroplating method in

section 4.2 electrodeposition.

YODA – POST-ELECTROPLATING-BRIGHTENER-SUBMERSION PHASE

The image (right) shows

the component which has

been brightened and

buffered repeatedly until a

higher level of quality was

achieved. However,

oxidisation within the

67

atmosphere created the component to become darker, tarnishing the quality of the

component over time.

To the left shows the OHM ratings of the

YODA at particular phases of the

procedure, the area of measurement was

from the top of the head to the bottom of

the component being a length of 100mm.

The results above, provide evidence that the electroplating on a complex component

has been successfully in coverage. From tests, it is safe to assume that the

component gains the material property advantages recorded from the sample

pieces.

68

1

2

3

4

5

6

6.1

6.2

6.3 External Constraints

Many constraints exist that can affect the timing and quality of a project; some can

be so critically damaging to even stop the project from developing. The two main

sectors of external constraints that exist are commercial and industrial; these shall

be discussed with actions to take to prevent them from occurring.

6.3.1 Industrial Constraints

Constraints exist industrially for this project via, any problem that can affect the

timing and quality of the project from developing; this could be from new technology

or new advancements in coating polymers; therefore making this method less

applicable.

6.3.1.1 Manufacturing

69

Manufacturing this project industrially can cause mass exploitation of the benefits

that this technology offers. It is theoretically possible to mass manufacture metal

coated polymer parts, also offering the possibility of customized mass manufactured

3D Printed Metal Coated parts; which are cost effective. The only major constraint is

the time it takes to print, cover in conductive coating and apply electrodeposition.

6.3.2 Commercial Constraints

Commercial constraints are constraints that occur, which affects the selling of the

methodological process applied to the polymer parts. To the right identifies

commercial constraints that could occur.

6.3.2.1 Customer Needs

During the start of the project, customer needs where considered from the improved

material properties these methods offers. For instance the added hardness achieved

with the assumed thermal insulating capability could achieve the propeller blade

rotary testing for a plane; this requires thermal testing’s whilst retaining essential low

weight.

6.3.2.2 Selling Price

The selling price of the method will entirely depend on the complexity of the

component coating to which it will be hard to define a costing system for the part.

6.3.2.3 Quality Regulation

Due to the technology being new, regulation of the quality of the method will have to

be defined on the materials used. A possible definition of the regulation of quality

70

could be the comparison of the Anode to the final coat, the thickness achieved

and/or material properties gained.

6.3.2.4 Patenting

A patent gives the inventor / institute the exclusive rights to whatever they have

invented. This means that they are the only people / body who are able to

manufacture or sell the rights to manufacture the idea. This could be a constraint

because it would mean that all of the researched which has been conducted wouldn’t

be able to be used d be a waste of time if a patent already exists for coating of a 3D

printed part, which isn’t the case from the delivery of this report.(April 2015)

6.3

6.4 Conclusion

6.4.1 Conclusive Introduction

Two main phases within the methodology of creating an electroplated 3D printed

model have been found. They are the conductive coating phase and the

electroplating phase; only applicable to 3D printed polymers.

6.4.2 Conductive Coating Conclusion

During the conductive coating phase, from the experimental results it has shown

that building up the coating layers whilst buffering in-between. Using grey-primer

as the solvent and increasing the acetone level, avoiding too high of a purity

gives a good quality pre-electroplating component.

6.4.3 Electrodeposition Conclusion

71

During the electroplating phase, from the experimental results it has shown that

using a low voltage induces small grain growth of the anode upon the cathode.

Adding Brightener to the electroplating solution has shown improvements in the

post-electrodeposition quality.

6.4.4 Post-Treatment Conclusion

For the Post-Electroplating after treatment, soaking in brightener has shown

significant aesthetical improvements to which increases the hardness; as shown

in evidence on the scratch able test.

6.4.5 Hardness Conclusion

The hardness of the sample pieces are directly correlated to the hardness of the

anode and the submersion time during electrodeposition. From results shown in

5.1.1 nickel has been coated upon a copper sample which has shown significant

hardness improvements.

6.4.6 Final Conclusion

72

During this project it is found that the conductive coating method is universal to a

range of polymers so being applicable to most 3D printed polymers. The

electroplating phase has been found to be applicable to nickel and copper to

which different metals will require changes in voltage. This method is applicable

to a wide range of polymers and metals. The coatings of the samples have found

to achieve a 90% hardness value of that of the anode showing significant

engineering applications for 3D printed parts.

The following possible applicable usages of the coatings are as follows:

Thermal Insulation / Conductivity

Improved Hardness / Impact Resistance

Lightweight

Improved Strength

Electrically Conductive

Improved Toughness

Chemical / Atmospheric Resistance

Experience has shown to be a tremendous benefactor to completing this

project, however the documentation of the experiences needs to be logged to

ensure other uses can continue from the author’s progression from the

recommended further research. Attached is the project diary and all other

support information to support future research.

73

6.4.7 Project Costing

Below shows the Project Costings with assumed rates of pay for engineers, with

equipment and material costings including and time on processes.

74

7 References

75

1Oli Glaser. (Sep' 2011). How much voltage is “dangerous”?. Available:

http://electronics.stackexchange.com/questions/19103/how-much-voltage-is-

dangerous. Last accessed 01/2015

2Prairie, E. (2009). Chemical Resistance. Available:

http://www.plasticsintl.com/plastics_chemical_resistence_chart.html. Last

accessed 01/2015

3Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis.

Kluwer Adacemic/Plenum Pulbishers, 689 p.

4Reimer, L. (1998) Scanning electron microscopy : physics of image formation

and microanalysis. Springer, 527 p.

5Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction

to TEM, SEM, and AEM. Springer, 202.

6Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press

(electronic resource)

7Schlesinger, M. (2010). Analysis of Electroplated Files using SEM techniques.

In: Snyder, D and Paunovic,M Modern Electroplating. Milan: Wiley. p637-642.

8J. E. Palmer, C. V. Thompson, and H. I. Smith(1987), J. Appl. Phys. 62, pg2492

9L. H. Chou (1991), Appl. Phys. Lett. 58, 2631 ~1991!.

10A. Milchev (2002): Electrocrystallization, Fundamentals of Nucleation and

Growth, Kluwer Academic Publishers, 2002, 11.

76

11J.W.P. Schmelzer (2003): Mater. Phys. Mech., 2003, 6, 21.

12A.M. Rashidi. (2010). Effect of Electroplating Parameters on Microstructure of

Nanocrystalline Nickel Coatings. Electroplating. 1 (1), p1-5.

13Knowlton, K. (2006). The 2006 California Heat Wave. Impacts on

hospitalizations and emergency department visits. (1)(5), p1

14Davis, J (2004). Copper and Copper Alloys. 3rd ed. London: Pearson. p136.

15Gibson, I (2011). Additive Manufacturing Technologies. 2nd ed. London:

Pearson. p19-23

16Chua, C (2014). 3D Printing and Additive Manufacturing. 4th ed. London: World

Scientific Publishing. p34-56.

17 Pugh, S. (1991). Total Design . Cornwall: Addison-Wesley.

18 Covey, S. (1996). Total Design Methodology. London: Pearson..

8 Appendices

8.1 Personal Learning

77

The start of the project involved the coating of 3D printed parts to which the

author had limited knowledge, therefore the beginning of the project involved a

major amount of researching to understand the processes and methods of

conductive coatings and electroplating. However from being a kinaesthetic

learner the author found this to be repetitive.

Therefore the author began studying whilst conducting research from the

knowledge gained from the journals with trial and error from experiments with

journals of electroplating as support. This enabled the author to visualize and

build upon the knowledge learnt by hand-on experiments to which progress

spurred the author to continue progress.

As the project neared the end and the addition of a new born baby, bringing the

project to the end became crucial, to which additional hours and training upon

the VHTM was conducted to finalize the improved material properties.

Successfully enough the improved material improvements and the aesthetically

improved Yoda became the icing on the cake to which the author feels major

progress has been made.

8.2 Project Diary

78

Project Meetings Scheduled with Hadley

07/11/2014

The brief meeting about the project involved the possible processes involved in the project and the following tasks to complete:

Streamline Specification and Plan to reflect meeting Enquire access to the Tribology Lab Develop sample pieces Develop knowledge of application of coatings research Develop knowledge of improved material properties

From now on research shall be made to develop a better understanding of the processes.

The following processes shall be researched to gain sound knowledge and be able to practically produce samples are:

Create Conductive Coatings which are applicable to ABS (3D printed part material)

Electroplate parameters (Material, Solution, Voltage) Chemistry knowledge of Acetone, Graphite, ABS and any relevant material

which shall also be used. Safety Knowledge of the above Materials and Chemicals

18/11/2014

From the previous research made and development of the spec and plan has progressed my report to develop a sample with a conductive surface.

During today’s meeting, we tried to apply a solution of acetone and graphite. This infused the graphite to the surface therefore creating a conductive surface, we wiped down the part with force to connect the graphite together.

This experiment worked surprisingly successfully as it seemed that the graphite was embedded into the component it gave a highly conductive surface with minimal removal during wiping down; we shall leave the ABS component to cure and check the properties afterwards

For the next meeting we shall have a brief meeting, with myself being scheduled to provide ABS sample parts and apply a graphite and copper sample with one being a mixture then the results will be initially checked via multimeter.

25/11/2014

79

During today’s meeting, we examined the conductivity of the sample piece to which was highly conductive; therefore we approached using a solution with dissolved ABS within the Acetone / Graphite. This gave a soft top coating which gave a low reading on the multimeter.

Therefore burnishing graphite was looked at to which it improves the conductivity coat due to burnishing arranged the graphite bonds.

02/12/2014

This weekly meeting involved experimenting with the 3 methods of sampling applying from 1, 2 and 3 layers of each method therefore a total of 9 samples is made. The methods are Graphite mixed with Acetone, Copper mixed with Acetone and Graphite / Copper mixed with Acetone; these were applied to give results of resistance per sample. I then took some equipment home and begun experiments of electrolysis there.

06/01/2015

During this week’s there has been a change in direction to which the previous experiments allowed us to enhance our experience in the coating and electrolysis of the test pieces. Now the experiments shall be the following

Acetone / Graphene Solution Experiment

Spray + Burn 1 Layer 3 Layers Spray1 Layer

3 Layers

+ Gr = None+ Gr = None

+ Gr = 10%+ Gr = 10%

+ Gr = 30%+ Gr = 30%

Key:

+ Gr =Added Graphite

Spray AtomizationBurn = Burnished

Therefore 12 sample pieces shall be made show the difference between burnishing and not, the percentage of graphite added and the layers made. They shall be controlled using an atomizer to completely expose the sample. The reason for unburnished is due to the effect on complex parts which will not be easily burnished.

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Updated Gantt Chart

06/01/2015

13/01/2015

20/01/2015

27/01/2015

Homo SolAp Sol on TPRec ConElec PlateRec Con 2Key:Homo Sol = Homogenize the SolutionAp Sol on TP Apply Solution on Test piecesRec Con = Record the electric conductivityElec Plate =

Electroplate sample pieces at set procedures

Rec Con 2=

Record the electric conductivity of plated sample

The updated gantt chart shall replace the original for these new experiments due to new findings.

13/01/2015

From the updated Gantt chart, the high shear homogenization of the Graphite solution was unavailable due to the homogenizer lacking the required RPM to produce graphene. Therefore is was put on at 2000 RPM for 2 hours.

This solution was then split to 3 solutions with the required percentage of ABS; 1st with 0%, 2nd with 25% and 3rd with 50%. The percentage of ABS is in regards to chemicals added to acetone therefore the 25% ABS had 75% of graphene and so on.

During the application of the mixtures, there has been a failure during electroplating which is do with the lack of conductive coating which, I suspect is a problem during atomizing where graphene is blocking the pipe.

Therefore from the results the new goals shall be to:

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Find nozzle capable of spraying solution without clogging Apply brushing solution on Find the benefits of adding ABS into solution Electroplate successfully

14/01/2015

During the failure of creating a high electrically conductive surface on the samples, the problem has been amended by buffering each layer individually then applying a new layer. This proved to be a highly positive method which produced a resistance reading of 50 ohms from a 40ml Acetone / 2g Graphite solution with no ABS.

The added content of ABS has proved to be unsuitable for this application due to buffering aligning the Graphite to increase conductivity the ABS prevents this and whilst buffering results in a paste which is easily removed from the surface therefore no ABS shall be used but buffering individual layers shall be used.

The application methods of spraying and brushing have both proved to be effective whilst buffering each layer, to which spraying produced a smoother more homogenous surface.

Gantt Chart Electrical Conductive Coating Samples

14/01/2015

15/01/2015

16/01/2015

17/01/2015

18/01/2015

Ap GrAcSCr Mix

Key:Ap GrAcS =

Apply Graphite / Acetone Solution

Cr Mix =

Create Mixtures of Graphite / Acetone

Gantt Chart Electroplating Samples

14/01/2015

15/01/2015

16/01/2015

17/01/2015

18/01/2015

Rec ROhmsElecPl

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ate

Key:Rec Rohms

Record resistance readings from conductive samples

ElecPlate

Electroplate the sample pieces

Spray + Burn 1 Layer

3 Layers Spray 1 Layer

3 Layers

+ Gr = None

+ Gr = None

+ Gr = 10%

+ Gr = 10%

+ Gr = 30%

+ Gr = 30%

These shall be started from the scheduled plan to which shall be updated within the project diary and Gantt charts.

1 Layer 2 Layer 3 Layer0

2000

4000

6000

8000

10000

12000

14000

16000

4200

3500

1200

Conductive Resistance of Coating Application

applied layers of conductive solution

Resi

stan

ce R

ating

in O

hms

19/01/2015

During the graphite application the spraying developed problems due to only the fine graphite passing through the nozzle with the larger parts becoming clogged and causing problems therefore I have resorted to applying directly via brushing and burnishing between layers.

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The electroplating has become a success by producing a sample piece entirely plated with a full coverage of 25Ω/10mm2. This was over an 8 hour period at 18v.

However, during the success of the nickel plating a sample piece, the uniformity of the application increased but due to the increased voltage a greater amount of heat was produced from crocodile clips; therefore considering faradays law, I shall reduce the voltage to 6v and add 5 grams of copper sulphate to the solution; this shall in theory speed up plating due to the copper sulphate and create a more even plate due to the lower voltage.

20/01/2015

During the process of having the voltage at 6v with the addition of copper sulphate; this proved successful with majority coverage of copper with very clear copper coat upon the sample pieces.

Therefore to improve the homogenous of the coating a rotary buffer has been purchased due to the realization that the quality of the coating is in direct correlation to the quality of the buffered graphite; in theory this shall improve the speed of coating (Due to a lower resistance from buffering) and quality of coat.

23/01/2015

The rotary buffer has arrived to which has significantly reduced the resistance of the initial conductive coating from 300 Ohms (Buffered using Tissue) to 70 Ohms (Buffered using rotary polisher) therefore the speed of plating shall significantly improve.

Just placed a rotary buffered sample piece to be electroplated and in under 5 minutes @ 10 volts it has been fully plated, however the copper plate is easily wiped off. This is due to the voltage increasing the heat of the graphite particles therefore enabling them to be removed.

I shall no commence by comparing the copper coatings to the sample pieces, but reduce the voltage.

24/01/2015

During reduction of the voltage from 10v to 1v for 10 minutes, the quality and the adhesion of the coating has improved which backs up the theory of the graphite particles being heated up and being easily removed, reducing the voltage reduces the heat therefore enabling a better coat.

26/01/2015

A successful sample piece with a high quality coating has been developed using the following method:

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1v for 30 minutes Remove sample piece, dry off and leave for 15 minutes at room temperature 1.5v for 30 minutes Remove sample piece, dry off and leave for 15 minutes at room temperature 2v for 30 minutes Sample piece should have a high quality coat after finally drying.

This method has proved better than fully exposing the sample piece for 1.5hrs due to the coating having time to cure.

This shall now be tried out on a complex part (the Owl) to check how well it coats uneven surfaces.

30/01/2015

Due to the recent success of results on the sample piece, different polymer materials and solvents to adapt the methods to become universal or slight tweaks dependent upon materials / chemicals used therefore below shows a table of 4 solvents with multiple polymers that are applicable, however due to safety and performance Acetone is the solvent which is highly recommended.

Also the complex part coating has not yet been initiated but has been prepared for electroplating exposure (Been rotary buffered to an acceptable resistance)

SEM training has been scheduled for the 2nd February in JB014 at 11am.

02/02/2015

SEM training has been completed today to which basic data on the most recent sample piece using the 3 stage submersion in the electroplating tank.

With meeting with Hadley we discussed the processes and why the copper coating was easily scratched off and we concluded that it was due to the electroplating solution due to comparing plating techniques with multiple previously made experiments.

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This showed that currently, the samples were being electroplated for 2 hours, however other groups who have completed a similar experiment expose there samples for 4 hours therefore double the exposure time shall be made and a commercial electroplating copper solution shall be used in conjunction with existing methods just a change of the solution.

03/02/2015

An Excel spreadsheet shall be developed showing the difference of resistance (10mm2 & 20mm2) in ohms, from each electroplating method previously mentioned.

07/02/2015

The conductive coating has reached its peak capability in regards to combination of electroplating solution and conductive paint. The assumed constraint is the electroplating solution which when in process of plating, produces small hydrogen bubbles on the surface which slightly disrupts the graphite layer. Therefore when the surface is scratched removes the copper, so either adjustment of the conductive paint, electroplating solution or anode.

The multiple layers of conductive coats have found to give a significantly reduced resistance but decrease the wear resistance upon plating.

13/02/2015

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Electroplating solution has been researched to which Midas Bright Electro-forming Copper Solution (Copper Sulphate Solution) has shown great promise in increasing wear resistance and maintaining the copper upon the coat.

20/02/2015

Research into multiple conductive paints that replaces, the first proposed idea is to replace acetone with lacquer or primer, following the same procedures the see if there is a better result from a different a solvent.

The Midas electroplating solution has been ordered to which experiments using this shall begin on or around the 28/02/2015.

22/02/2015/

A grey primer / graphite conductive paint has been produced, with burnishing between layers… It has been noticed at this early stage that the resistance is not as low as acetone, but still low producing a 600Ω/10mm2 , it is assumed due to the impurities within the grey primer this may help in bonding the conductive coating to the ABS sample, therefore helping the copper.

It has been placed in the safe electroplating solution @1.5 volts for 4 hours.

After 4 hours of electroplating on the primer / acetone solution the same has achieved roughly 75% coverage with a noticeable increase in copper electrodeposition. The sample shall remain electroplating for a further 4 hours to assure full coverage.

The test has shown that the grey primer / graphite solution has a decreased post-burnished resistance but from the post-plating sequence has shown an increased wear resistance than the acetone counterpart.

During burnishing there is a noticeable difference between the grey primer / graphite solution and the acetone / graphite solution, therefore, both burnished samples shall have SEM images and a composition test to notice the difference between them.

26/02/2015

The SEM machine has been booked for 05/03/2015 at 11pm to gather composition and imaging data to identify the bonding connection on a nano scale.

The grey primer / graphite solution has been deemed successful due to the significantly increased quality of copper coat and material property capabilities. The following are the materials and parameters used for the successful sample:

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Grey Primer – Autotek (MSDS supplied) Graphite Powder Burnished between layers @ 2000RPM Incremental increase in voltage from 1V to 5V over 16 Hours Incremental Rotation of Component during electroplating phase

Now that a standard procedure, that successfully works has been identified, fine tuning of this process shall commence. With 3D printed components being produced for functional applications of this process i.e. coated polymer cogs

02/03/2015

The SEM images developed have shown to be highly helpful in showing the electrically conductive properties of the sample. (See the SEM images of the two samples below) Notice on the 2 samples below that Grey Primer / Graphite Solution appears brighter than the Acetone / Graphite Solution, this isn’t due to the adjusting of the brightness but the conductivity of the sample piece, a good way to graphically represent the electrical resistance.

95%+ Acetone / Graphite Solution SEM Image @ 50 Microns (Below)

Grey Primer / Graphite Solution SEM Image @ 50 Microns (Below)

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05/03/2015

From recent research I have found, having the correct grain growth is key to developing a uniformed coat. This is to do with the solutions PH Levels, Temperature and composition. So therefore I found a paper showing 55 degrees is optimum temperature for nickel coating, so I applied this to copper and it failed, causing a slight bubbling effect within the sample. Therefore from the failed sample, I have placed an order for the copper brightener which should cause the most significant increase in quality.

10/03/2015

The Brightener has arrived to which the following electroplating solution was created:

32g Oxalic Acid 10g Trisodium Phosphate 4g Ammonium Sulphate 950mL Distilled Water 3g Copper Sulphate

This created a shiny copper coating on a grey primer sample piece within 15 minutes @ 1V.

The component was then soaked in a 200ml water / 3g Brightener Solution for 15 minutes.

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The next step shall be to create high quality copper coats

13/03/2015

The brightener solution needs to be dissolved within the solution @ 50c while stirring, therefore a litre batch shall be made. Using the formula below.

1. Copper sulfate "powder" is actually made up of very fine crystals. The recipes on the web contain instructions for mixing acid copper plating solutions using both liquid copper sulfate (CuSO4) and crystalline copper sulfate pentahydrate

(CuSO4•5H2O). Go to: Acid Copper Plating Solution .

Specifically, you want 10 to 12 oz of copper sulfate crystals per gallon of plating solution. To make up a single gallon of acid copper electrolyte, add:

o 25 oz (weight) or 1.6 cups (volume) 98% sulfuric acid to 3 quarts (12 cups) of COLD deionized. The solution will heat up VERY rapidly as you add the acid so be VERY CAREFUL!!!

o Heat the solution to 60C (140F) and slowly stir in 10 oz. of copper sulfate flakes. Stir until ALL of the crystals are dissolved.

o Add 0.63 cc of 35% HCl (hydrochloric acid) and 19 cc of Copper Gleam PCM+.

o You have added a little less copper sulfate than you actually need but the anodes, when they activate, will quickly make up the difference.

http://www.ami.ac.uk/courses/topics/0223_plate/index.html

16/03/2015

It has been found that the copper anode used initially was too high in contaminants to cause a quality coating, therefore a high quality copper anode is recommended (at least 95%).

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8.3 Project Plan and Specification

Project – MP 3997

Project: HB9 Functional Coatings for 3D Printed Parts

Tutor: Dr Hadley Brooks

Project Specification and Plan

Report By: Jonathan Ambrose

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Contents

Specification…………………………………………………………………………...…3-4

Introduction 3

Aims 3

Information 3

Theory 3

Design 3

Manufacture 3

Test 4

Risk 4

Plan…………………………………………………………………………………………...4

Main Tasks 4

Time Scale 4

Interdependency between Tasks 5

Critical Paths 5

Milestones 5

Indication of Resource Needs 5

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Specification

Introduction

The project shall be based on embedding a surface hard coating upon a 3D printed part to induce strength and durability.

This shall be done by using the theory behind applying a coating on a part by adjusting treatments on sample parts to successfully produce a part which is cheaper, stronger and more durable than it’s in use counter-part.

This studies main task is to embed the polymer part surface with a ferrous component and successfully apply a metallic coating which shall improve the parts properties substantially; whilst keeping the process simple, cheap and effective.

AimsTo achieve a surface coating upon a 3D engineered printed part, which shall have superior strength during application; compared to a mass produced counter-part.

InformationUse of hardware such as the 3D FDM(fused deposition model) printer, Acetone Bath, Electrolysis Bath and Equipment; and any other technical equipment to satisfy the needs of the project.Use of software such as SolidWorks, AutoCAD, ANSYS, FEA add-ons, MatLab; and any other technical software to satisfy the needs of the project.

TheoryThe theory behind the project is that to apply a surface coating to a 3D prototyped part. This shall be achieved using a coating method for embedding the surface with ferrous material mixed in the solution; once the ferrous material has been embedded into the part, the coatings shall begin via PVD (physical vapour deposition) or CVD (chemical vapour deposition).

DesignThe design of the component shall be that of a mass manufactured part which requires strict testing analysis; for example a propeller requires a fire test to ensure under certain conditions it remains stable, however with one or more coatings; this shall be reduced and substantially improve the components properties under usage.

ManufactureThe design shall be conceived using an appropriate CAD package and various amounts of static and thermal analysis to ensure the component performs as needed; Inspire shall be

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integrated within the model to reduce weight and stress concentrations and allow for a structurally viable component. Once the design has been verified to be feasible from data using FEA, the component can then be prototyped using an in-house 3D printer.

TestSample parts shall be tested using appropriate material property testing equipment.

FEA integrated CAD packages shall be used to verify statistically, that under thermal and static analysis it performs well within the factor of safety.

RiskThe embedding process may not embed the component evenly or may not allow the shell to be an effective shell of the component.

The component may need multiple nanocomposite coatings to provide sufficient protection and operational satisfaction; this is due to component legislation involved for passing operational tests.

Plan

Main Tasks Research Methods of surface coating and electrolysis application Research into Coating Material to apply to ABS Create sample parts using variable methods for impregnation Perform Material Testing on a solid plastic, coated and solid metal component Use FEA testing to check how component acts under force From testing results, decide whether to produce component and apply best method Compare and contrast in use component with prototype coated part

Time ScaleThe time scale of the project shall include a Gantt chart on the assigned week date. It is assumed that during the period of this project the activities within shall change and alter due to unforeseen circumstances. The following are the tasks to be completed within the scheduled instances for each report (in bold). (See Project Gantt chart)Plan and Specification – 7th November 2014Research Methods of surface coating and electrolysis applicationResearch into Coating Material to apply to ABSInterim Report – 5th December 2014Create sample parts using variable methods for impregnationPerform Material Testing on a solid plastic, coated and solid metal componentInterview – 19th January 2015Use FEA testing to check how component acts under forceFrom testing results, decide whether to produce component and apply best methodCompare and contrast in use component with prototype coated part

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Final Report – 1st May 2015

Interdependency between TasksThe tasks dependent on being achieved to move on flow in a linear way other than a complicated multi-task project.The tasks can be split into four groups:- Initial Stage- Prototype Stage- Coating Stage- Testing StageThe Initial Stage; Research, design and analysis are the first tasks to be completed before any practical procedures can take place.Then from the research, design and analysis the Prototype Stage can begin to which the component can become developed with preparation for the coatings application beginning in conjunction with the 3D printer.The Coating Stage can begin once the coating preparation and research is complete. And finally the Testing Stage can begin which compares and contrasts a similar industrial component in regards to material properties and operation usage.

Critical PathsSee Appendix for Gantt chart and Critical Path.

MilestonesThe milestones achieved shall be the following:1. Completion of relevant research on coatings, embedding and electrolysis2. Successful sample parts3. Best method of coating application achieved4. Create and coat prototype component5. Compare and Contrast via Material Properties of Prototype

Indication of Resource NeedsMultiple resources shall be used when needed; this shall be indicated when a milestone has been completed. The following are the milestones completed and the resources needed. Complete milestone 1 and gain access to the Tribological Lab for Electrolysis research Once milestone 1 is complete, the next resource will be the 3D printer to complete milestone 2. After the completion of milestone 2, the Ferrous Solution and Vapour Deposition will be needed. The coating material and application machines (electrolysis) will be needed once this is complete from the results milestone 3 can be complete. Once the best method from the results is found and the processes have been successful the prototype phase can be initiated with best method applied to this.

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Then comparison to in use component shall be made to compare material properties.

8.4 Task Gantt chart

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8.5 Project Gantt chart

8.6 SEM Training Manual

FIRSTLY…

You have to book a time slot using the booking form in the SEM room. You must have relevant COSHH forms for your samples. You must complete training before using the SEM. Contact Jim, Tamar or Hannah. Remember to dispose of your sample accordingly and tidy up once you are finished.

SAMPLE PREPERATION

ALUMINIUM STUB

SAMPLE

STICKY CARBON PAD

HOW TO USE THE SEM

1. Your sample must be dry.2. From the drawer take an aluminium stub

and attach a sticky carbon pad on top. Peel off the top layer and add your sample on top.

3. If the sample is a powder use the air duster to remove any loose particles.

4. Be careful not to overload the pad, think about what you are looking for in your sample.

5. If the sample is conducting no further preparation is needed.

6. If the sample is non-conducting the sample may need to be sputter coated with gold.

SPUTTER COATING

1. Place your aluminium stub with sample on into the sputter coater chamber. If you have several samples run them in the coater at the same time.

2. Make sure that the lid of the sputter coater chamber is properly aligned over the seals otherwise it will not start.

3. Press “Start” on the base unit. The display will countdown and the chamber will go into vacuum. A purple glow will appear during the coating.

4. When the machine has finished the chamber will vent and you will be able to lift the lid and remove your sample ready for the SEM.

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PUTTING YOUR SAMPLE IN THE SEM CHAMBER

1. The SEM must always be in vacuum when not in use. 2. The chamber must firstly be vented. “Un-Pause” the

chamber camera by clicking in the chamber camera box and clicking the “Pause” icon on the top toolbar. The green pause button will then disappear.

3. Click the “Vent” icon on the top right hand side and click “Yes” in the pop up window.

4. After a few minutes the vacuum status on the bottom right hand side will turn red and say “Vented”. You may now open the chamber door and place your stub on the stage using the gloves and tweezers provided.

5. Close the chamber and click “Pump”. Wait for the vacuum status to go from “Pumping” to “Vacuum”. This will take around 5 minutes.

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VIEWING YOUR IMAGE ON SCREEN

1. “UN-Pause” the top left box. The blue bar at the bottom of the box indicates that it is active.

2. Click on the “HV” button on the right hand side and choose a spot size using the table below. Use 20kV voltage.

3. An image will begin to appear. Make sure the magnification is at 50x to begin with. The magnification can be altered by using the + and – keys on the keyboard.

SPOT SIZE

BEST USE

1,2 Very High Resolution (small structures e.g. nano-particles)

3,4,5 Standard Imaging6,7,8 EDAX, BSE9,10 Not Used

ACTIONS MOUSE/KEYBOARDZOOM + AND – KEYS ON KEYBOARDCENTRE AREA OF INTEREST DOUBLE CLICK LEFT MOUSE BUTTON ON

SPECIFIC AREAFOCUS CLICK AND HOLD RIGHT MOUSE BUTTON

AND MOVE LEFT OR RIGHT ACCORDINGLY

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PRODUCING A GOOD QUALITY IMAGE

1. Firstly adjust the brightness/contrast. The simplest way to begin this is to use the “auto adjust” icon on the top left hand side tool bar. You can then use the brightness and contrast bars on the right hand side of the screen to make further adjustments.

2. Take into consideration your spot size (use the table to help).3. You can adjust the rate at which the image refreshes. Use the Hare + and Tortoise – icons on the top

tool bar to increase or decrease the rate. Hint: higher refresh rate = poorer quality. 4. To focus on your sample hold down the right mouse button in the active box and slowly move left or

right according to your on screen image OR5. Click on the reduced area button on the top toolbar and use step 4 within the smaller box. To apply to

the whole image click outside the smaller box.6. You will have to refocus your image every time magnification is altered.7. To navigate around your sample double click the left mouse button on areas of interest.

ASTIGMATISM (correcting changes in the beam shape)

1. Focus the image as well as possible.2. Select the reduced area icon.3. Bring the image out of focus in one direction and check for astigmatic distortion (image out of focus

unevenly).4. Do the same in the opposite direction and look for a different distortion.5. Bring the focus to the midpoint between the distortions.6. Hold down the shift key and the right mouse button and a four headed arrow will appear.7. Move this arrow slowly around the screen until the best focus is obtained.

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HOW TO SAVE YOUR IMAGE

1. Firstly pause the active box using the “Pause” icon on the top tool bar. The icon will remain orange until the final refresh is complete.

2. Once the pause icon is green click “File” and choose “Save As” from the drop down menu.3. If you have not yet created a folder with your name do so and save all your images into said folder.4. To save this onto a USB unplug the keyboard from the USB port at the back of the computer (do

not remove the mouse as it will break) and use that port. 5. Once you have copied your files onto your USB “safely remove hardware” otherwise the files may

not save on your USB.6. Don’t forget to plug the keyboard back in once you have removed your USB.

CHANGING YOUR SAMPLE

1. Reduce magnification to 50x.2. Change spot size to 5 and turn off HV.3. Pause the active box.4. Vent the chamber.5. Carefully remove your sample when the

chamber has vented.6. Insert new sample and follow instructions as

detailed previously.

ENDING YOUR SESSION

1. Reduce magnification to 50x.2. Change spot size to 5 and turn off HV.3. Pause the active box.4. Vent the chamber.5. Carefully remove your sample when the

chamber has vented6. Close the chamber door.7. DON’T FORGET click on “Pump” to put the

chamber back into vacuum.8. Select the box with the camera of the

inside of the chamber and pause it.

REMEMBER

If you are finished with your sample remove sticky pad from stub and dispose of according to your COSHH.

Return stub to plastic bag. If you need to carry out further SEM work

leave your sample stub in the sample box provided.

Do not forget to dispose once finished with. Make sure the SEM room is clean and tidy

before you leave. Any further questions contact Jim, Tamar or

Hannah.

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8.5

8.6

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8.7 VHTM Training Manual

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106

107

108

109

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8.8 Support Data

http://www.3ders.org/images/credit-suisse-3d-printing-1.png

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8.9 Material Safety Data Sheets (MSDS)

The following pages are split into individual

MSDS booklets for every material and chemical

used within the project.

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