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1 Synthesis of Superconductor Collect: Agate mortar (clean with sponge after use) Label one zip-lock bag with student ID and name (To collect the synthesized superconductors) Prepare: Plastic spatula x1 Mask (self-prepared) (2020/05/08 revised)

Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

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Page 1: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

1

Synthesis of Superconductor

Collect:

• Agate mortar (clean with sponge after use)

• Label one zip-lock bag with student ID and name

(To collect the synthesized superconductors)

Prepare:

• Plastic spatula x1

• Mask (self-prepared)

(2020/05/08 revised)

Page 2: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

2

Superconductors

Metal conductors

Conductivity decreases with

increasing temperature

Semiconductors

Conductivity increases with

increasing temperature

Superconductors

Zero resistance at transition

temperature, Tc

Temp. (K)

0

0

Conductor

Semiconductor

Superconductor

Tc

Resis

tance

Page 3: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

3

At superconducting transition temperature, Tc

– Zero resistance

– Meissner effect

Properties of Superconductor

(b) The Meissner effect

Magnet

Superconductor

Page 4: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

4

Yttrium Barium Copper Oxide

Superconductor

Chemical formula: YBa2Cu3O7-x

Crystalline structure

Tc: 95 K(Boiling point of liquid nitrogen 77 K)

Synthetic methods

–Solid-state reaction

–Sol-gel method

–Co-precipitation

Unit cell

Page 5: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

5

Procedures of Solid-State Reaction

Yttrium oxide, Y2O3

Barium Carbonate, BaCO3

Copper(II) Oxide, CuO

Grind

Press

1 ton/cm2 YBa2Cu3O7-x

superconductorAtomic ratio

Y : Ba : Cu = 1 : 2 : 3

930 oC, in air

10 h

Page 6: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

6

Calculation of Formula

To synthesize 0.004 mol YBa2Cu3O7-x

(Y : Ba : Cu = 1 : 2 : 3 )

Obtain:

Y2O3 1/2 × 0.004 × 225.82 = 0.4516 0.45 g

BaCO3 2 × 0.004 × 197.31 = 1.5785 1.58 g

CuO 3 × 0.004 × 79.55 = 0.9546 0.95 g

* The stochiometric amount of starting materials is

critical to the success of the experiment!

Page 7: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

7

Grind and Mix the Reactants

Use agate mortar (NTD 9,000~15,000)

Mix chemicals with plastic spatula first, then grind

Grind until color appears gray and homogeneous, that may

take about 10~15 min.

Collect the ground powder in a piece of weighing paper

Still contains white powder

Page 8: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

8

Pressing-Hydraulic Press and Dies

Pressure

gauge

Parts of dies

Hydraulic press

Hollow ring

Page 9: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

9

Setup and Procedures of Pressing

Place weighing

paper underneath

the die

Transfer powder

into die

Rotate the die left to

right to even up

powder

Place the dies on

center of hydraulic

plateform

Close the valve

clockwise

Release the valve

counter-

clockwise

Fix the dies in

position Apply the pressure to

1 ton/cm2 for 1 min.

Page 10: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

10

Setup and Procedures of Obtaining Pellet

• Place the dies in center of

plateform upside down

• Setup the hollow ring and

leveling surface

• Close the valve clockwise

• Pull leverage to surface the

superconductor pellet

• Release the valve

• Take out the hollow ring

Resulting sample

pellet

Place pellet on to an alumina plate

with plastic tweezers carefully

Dies with

sample

Cylinder

sample

Sample

Hollow

ring

Page 11: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

11

Sintering at 930 oC

The box furnace can hold 4 × 4 = 16 samples

Alumina plate cannot be labeled, record the position

in furnace instead

Sinter the samples at 930oC for 10 h. by raising and

lowering the temperature at a rate of 5oC/min.

Page 12: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

12

Place superconductor in petri dish

Pour in liquid nitrogen and immerse the superconductor

Place magnetic bars on superconductor pellet with plastic tweezers, compare levitation height and amount of magnetic bars

Notice that the magnetic bars are small and easily lost

Dry and warm the superconductor with a hair dryer to room temp.

Examine the Meissner Effect

- Levitation of Magnets

Page 13: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

13

Design Your Superconductors as

a Souvenir

3.5 cm

5.0 cm

Page 14: Synthesis of Superconductor - 國立臺灣大學genchem99/doc/presentation/... · 2020. 5. 11. · Superconductors Zero resistance at transition temperature, T c Temp. (K) 0 0 Conductor

14

Notice

The dies should be placed in center of platform to

prevent uneven application of pressure when

pressing

Pressure should be kept at 1 ton/cm2 for 1 min.

Clean up the dies thoroughly after each use to avoid

the powders pile up in dies and cause it to get stuck

Avoid direct contact with liquid nitrogen which may

cause frostbite

Condensed report