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1
EXCESS HEAT IN ELECTROLYSIS EXPERIMENTS AT
ENERGETICS TECHNOLOGIES
I. Dardik, T. Zilov, H. Branover, A. El-Boher, E. Greenspan,B. Khachatorov, V. Krakov, S. Lesin, and M. Tsirlin
Energetics Technologies Ltd.
Omer, [email protected]
Presented at the11 th
International Conference on Cold Fusion, ICCF-11Marseilles, France
November 1 - 6, 2004
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CONTENTS1. Presentation objective
2. SuperWaves
used for driving the cell3. Review of glow discharge experiments
4. Description of ET electrolytic cells5. Pd Cathode and its pretreatment
6. Excess heat obtained7. Excess tritium
8. Material analysis
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3
PRESENTATION OBJECTIVES
1. Review of SuperWave
principles2. Review of Glow Discharge Experiments
3. Description of 3 ET electrolytic cell experimentsthat resulted in significant excess heat generation:
Experiment #
56
64a
64b
Cycle
4 1 2
Loading time (s)
80
5
16
Excess heat (EH) (%)
80
2500
1500Duration of EH (h)
300
17
80
Excess energy (EE) (MJ)
3.1
1.1
4.6
Specific* EH (W/g Pd)
11
71
62
Specific* EE (KeV/Pd atom)
13.5
4.8
20 (24.8)
* - pertaining to effective part of cathode ( 6 x 0.7 cm )
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Operator
Parameters
set up
Superwave
form signalgeneration usingLabView
software
Current amplifierExperimental
system
Lowcurrent
EC are driving by SuperWaves
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))](sinA1)((sinAt)[1(sin)(F 22
212
102
02 t t At ++=
)))](sinA1)((sinA1)((sinAt)[1(sin)(F 32
322
212
102
03 t t t At +++=
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Glow Discharge CellCooling WaterOutput
Cooling Water Input
+
Ground
Tungsten Wire
Palladium Layer
D+
Plasma
100 mm
20 mm
StainlessSteel Body
Conceptual Design
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Cell Assembly
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ETG-1
0
10
20
30
40
50
60
70
80
0 2 4 6 8 10 12 14
Time,h
E n e r g y
, k J
Ein Eout Ex ( Excess Energy = Eout - Ein )
Experimental Results with thin Palladium film (about1 m) on Stainless Steel Body
ETG-1
0
0.5
1
1.5
2
2.5
3
3.5
4
0 2 4 6 8 10 12
Time, h
P o w e r , W
Pin Pout
DC
WavesWaves
Shut Down
Maximum Excess Power = 3.7 x Input Power
Total Excess Energy = 6.7 x Input Energy
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Experimental Results with thick Palladium foil (100 m)
ETG-2
-20
0
20
40
60
80100
120
140
160
180
200
220
240260
280
10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52
Time,h
E
n e r g y , k J
Ein Eout Ex(Excess Energy=Eout-Ein)
ETG-2
0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
1.8
10 12 14 16 18 20 22 24 26 28 30 32 34 36 38 40 42 44 46 48 50 52
Time,h
P o w e r , W
Pin Pout
Maximum Excess Power = 0.8 x Input Power
Total Excess Energy = 0.8 x Input Energy
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Glow Discharge Experiment Cell ETG-2-18
0
0.2
0.4
0.6
0.8
1
1.2
1.4
1.6
1.8
0 20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460
Time, h
P o w e r ,
W
-150
-100
-50
0
50
100
150
C O P E
, %
Pin Pout COPE=(Pout-Pin):Pin x 100%
Excess Heat Generation during 20 days
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Energy Production from Cell ETG-2-18
0
500
1000
1500
2000
2500
0 20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460
Time,h
E n e r g y , k
J
Ein Eout Eex
Excess Energy during 20 days
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Energy Output after shutting down of GD Cel l ETG-3-22
0
1020
30
4050
60
7080
90
0 2 4 6 8Time, hr
E , k
J
Heat After Death
Thermal Energy Stored in GD Cell SS body (m*c p
* T)
Eout
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15
A AC
T4T5
Teflon
AluminaAluminum
Recombiner
Electrolyte
ET Electrolytic Cell
EC is inside a Teflon beaker that is placed inside an isoperibolic calorimeter
0.1M LiOD
in low tritium content D 2
O (230 ml)
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Cathode & Pre-treatment
50 m Pd foil, prepared by
Dr. Vittorio Violante (ENEA Frascatti, Italy)
Annealed at 870o
C in vacuum for 1h
Etched:
-
in Nitric Acid 65-67%; 1 min
-
in Aqua Regia
1:1 water solution; 1 min
Rinsed:
- D 2
O four times
-
Ethanol 95% twice-
Ethanol Absolute once
Dried:
in vacuum at ambient temperature for 24 h
6 0 m m
7 mm
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05
10152025
30354045505560657075
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
Delta T
P o w e r
Typical Calibration Curve for Electrolytic Cell Calorimeter
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Block diagramPC
Analyzing,displaying, printout
LCR
Amplifier Temperatures (5)Current,Voltage
Cathode resistance
Wave form
Current Superwave
Cell
Water bath
Temperature
Data Logger
Measured Parameters:
-
Input Current
- Input Voltage
- Wall Temperatures
T 4
and T 5
-
Resistance of cathode
for monitoring loading(four probe AC method)
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Study of Influence of Modulations on Loading
1st level of modulation Constant parametersChangeableparameters
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212nd
level of modulationChangeableparameters Constant parameters
Study of Influence of Modulations on Loading
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223rd
level of modulationChangeableparameters Constant parameters
Study of Influence of Modulations on Loading
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1st
levelof modulation
2nd
level of modulation
3rd
level of modulation
Of-line RR 0 versus time for Foil N056 (Dr.Violante)
1.
Study of Influence of Modulations on Loading
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Of-line RR 0 versus time for Foil N056 (Dr.Violante)
2.
Study of Influence of Modulations on Loading
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25Of-line RR 0 versus time for Foil N056 (Dr.Violante)
3.
Study of Influence of Modulations on Loading
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Diagram loading versus level of modulation
1.6
1.65
1.7
1.75
1.8
1.85
1 2 3 3 2 1 1 2 3 3 2 1 2 3 2 1 2 3 3
Level of modulation
C u r r e n
t d e n s i
t y , m
A / c m
2
010
20
30
40
50
60
R R 0
RR0 j
Foil N056 (Dr.Violante )
Study of Influence of Modulations on Loading
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Diagram loading versus level of modulation
1.7
1.75
1.8
1.85
1.9
1.95
2
1 2 3 3 2 1 1 2 3 3 2 1 2 3 2 1 2 3 3 3 3
Level of Modulation
R R
0
0
10
20
30
4050
60
70
80
90
100
C u r r e n
t d e n s
i t y , m
A / c m
2RR0 j
Foil N051 (Dr.Violante )
Study of Influence of Modulations on Loading
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Excess Power; Exp. # 56
Excess Power of up to ~3.5 watts; Average ~2.7 watts for ~300 h
300 h
Average Pout ~6.9 watts
Average Pinet
~3.9 watts
COPE=(Pout-Pinet):Pinet
(6.9-3.9):3.9
0.8
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Excess Energy; Exp. # 56
Excess energy of ~3.1 MJ
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Excess Power; Exp. # 64a
Pout=K T
Pinet=Iin*Vin
P dis
Excess Power of up to 34 watts; Average ~20 watts for 17 h
17 h
Average Pinet
~0.74 watts
Average Pout ~20 watts
COPE=(Pout-Pinet):Pinet
(20-0.74):0.74
25
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Temperature Evolution Exp # 64a
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Temperature Evolution, Exp. # 64a
A AC
T 4T 5
T 1
T 2
T 3
T4
T5Tbath
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T=T 4
-T5
Average Current Density = 7.09 mA/cm 2
Cell Voltage, V
Current & Voltage; EXP. # 64a
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34Loading is relatively low (~0.8)
R/Ro & Power; EXP. # 64a
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Excess Power; Exp. # 64b
Excess Power of up to 32 watts; Average ~12 watts for 80 h
COPE=(Pout-Pinet):Pinet
(12-0.72):0.72
15
Average Pout ~12 watts
Average Pinet
~0.72 watts
80 h
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36Excess energy of ~4.6 MJ
Excess Energy; Exp. # 64b
Energy production from Cell ETE-4-64, second run
0.00E+00
5.00E+05
1.00E+06
1.50E+06
2.00E+06
2.50E+06
3.00E+06
3.50E+06
4.00E+06
4.50E+06
5.00E+06
0 10 20 30 40 50 60 70 80 90 100
Time, h
E n e r g y ,
J o u
l e
Ein Eout Ex=Eout-Ein
T t E l ti E # 64b
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A AC
T 4T
5
T 1
T 2
T 3
Temperature Evolution, Exp. # 64b
T4T5
Tbath
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T, Current Density & Voltage ; EXP. # 64b
T=T 4
-T5
Average Current Density = 8.37 mA/cm 2
Cell Voltage, V
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R/Ro & Power; Exp. # 64b
Loading relatively low (~0.8)
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Excess Tritium in # 64
Tritium concentration measured at end of #64 analysis ~ 250% of
reference
~625 cm 3
of D 2
O has been added to make-up for evaporation; initial
inventory was 230 cm 3
Assuming TDO/D 2
O evaporation rate ~ 1.0 Estimated T effective concentration ~ 750%
This amount of tritium corresponds to
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Material Analysis
Diagnostics:
Auger Electron Spectrometry
Scanning Electron Microscopy-Energy Dispersive
Spectrometry SEM-EDS
Transmission Electron Microscopy (TEM) Secondary Ion Mass Spectrometry (SIMS)
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Material Analysis # 64 vs. 63; SEM-EDS
Surface of Pd foil after rolling and annealing at 870 0C:
sample #64 sample #63
f l l k d
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View of Typical Black Spot on # 64 and its composition
SEM-EDS
Element Wt % At % ____________________________ C 35.77 52.48O 26.19 28.84
Na 4.92 3.77Al 0.43 0.28Si 1.05 0.66Pt 0.39 0.04S 1.44 0.79
Cl 10.68 5.31Pd 2.55 0.42K 11.07 4.99Ca 5.52 2.43Total 100.00 100.00
_____________________________
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AES profiles of Pd, C, O and Cl
of Pd foils #63 and # 64
0 20 40 60 80
0.0
0.2
0.4
0.6
0.8
1.0
Cl-64
C-64
Pd-64
O-63
Cl-63
C-63
Pd-63
A t . p a r t s
Depth, A 0
After etching in Aqua Regia
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Sample 64. SIMS depth profiling.
0 100 200 300 400 500 600
102
103
104
105
Pd
C
Pt
CNO
S
D
H
Total
C o u n t s
Depth, A 0
Sp ti l distrib tion of selected isotopes me s red b SIMS in #64
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Spatial distribution of selected isotopes measured by SIMS in #64 a
D, b -
32S, c -
total isotopes content, d -
195Pt.Scale bar -
30 m.
ab
c d
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The dislocations in Pd foils after annealing.
#63 #643x1010 , cm -2 6x1010 , cm -2
Dislocation density
TEM
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Plastic deformation of Pd foil caused by D2 absorption.Planes of sliding (111) are visible.
Sample #64
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The area that is shown in the previous picture by an arrow.
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Sample #56
Contact area Working area
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Brittle destruction of Pt Wire Sample #64
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Summary of Material Analysis
Pd surface is covered at least with two types of impurities. The
first
one is a lubricant used at a rolling process with Pd during plasticdeformation of the metal. The second one is a result of adsorption of
air components by Pd surface.
The lubricant stains are of various sizes and configurations andpresent on surface of all samples before and after the electrolysis.
Annealing at 850 0
does not fully remove the lubricant's componentsfrom Pd surface.
The density of dislocations and the average size of grains in sample #64 are twice higher, than in the reference sample.
Nuclear reaction product can not be detected on surface zone due tohigh concentration of impurities. No He measurement has been
attempted.
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SUMMARY
Significant amount of excess heat has been generated in 3 experimentsusing 2 Pd foils.
Dardiks modified SuperWaves have been used for current drive in all thethree experiments.
The average current density was relatively low:
< 10 mA/cm 2
The maximum excess power was
2500% . This range of excess power issuitable for commercial applications (although the operating temperatureswere too low for such applications).
The maximum excess energy generated with a single Pd foil is
5.7 MJ .
This corresponds to a specific energy of
24.8 KeV
per Pd atom.
The highest average power density obtained is
~70 W/g Pd (versus 20 to 50W/g U in commercial fission reactors).
SUMMARY ( t )
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SUMMARY (cont.)
Significant increase in the tritium concentration in the electrolyte has beenobserved. However, the amount of tritium produced is negligible ascompared with the excess energy generated.
No measurement of He has been attempted.
The Pd cathode surface was contaminated by what appears to be lubricantfrom the roller used for pre-treatment as well as impurities adsorbed from
the air.