excess heat in electrolysis experiments at energetics...

54
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, Israel [email protected] Presented at the 11 th International Conference on Cold Fusion, ICCF-11 Marseilles, France November 1 - 6, 2004

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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 the11th International Conference on Cold Fusion, ICCF-11

Marseilles, FranceNovember 1 - 6, 2004

2

CONTENTS

1. 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

3

PRESENTATION OBJECTIVES

1. Review of SuperWave© principles2. Review of Glow Discharge Experiments3. Description of 3 ET electrolytic cell experiments

that resulted in significant excess heat generation:

Experiment # 56 64a 64b

Cycle ? 4 1 2Loading time (s) 80 5 16Excess heat (EH) (%) 80 2500 1500Duration of EH (h) 300 17 80Excess energy (EE) (MJ) 3.1 1.1 4.6Specific* EH (W/g Pd) 11 71 62Specific* EE (KeV/Pd atom) 13.5 4.8 20 (24.8)

* - pertaining to effective part of cathode ( 6 x 0.7 cm )

4

5

OperatorParameters

set up

Superwave form signal generation using LabView software

Current amplifierExperimental

system

Low current

EC are driving by SuperWaves

6

t)(sin)(F 02

00 ωAt =

))(sinAt)(1(sin)(F 12

102

01 tAt ωω +=

SuperWaves formation principles

7

))](sinA1)((sinAt)[1(sin)(F 22

212

102

02 ttAt ωωω ++=

)))](sinA1)((sinA1)((sinAt)[1(sin)(F 32

322

212

102

03 tttAt ωωωω +++=

8

Glow Discharge Cell

Cooling Water Output

Cooling Water Input

+

Ground

Tungsten Wire

Palladium Layer

D+ Plasma

100 mm

20 mm

StainlessSteel Body

Conceptual Design

9

Cell Assembly

10

ETG-1

0

10

20

30

40

50

60

70

80

0 2 4 6 8 10 12 14

Time,h

En

erg

y,k

J

Ein Eout Ex ( Excess Energy = Eout - Ein )

Experimental Results with thin Palladium film (about 1 µm) 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

Pow

er, W

Pin Pout

DC

WavesWaves

Shut Down

Maximum Excess Power = 3.7 x Input Power

Total Excess Energy = 6.7 x Input Energy

11

Experimental Results with thick Palladium foil (100 µm)

ETG-2

-20

020

40

6080

100120140

160

180200220

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

En

erg

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,hP

ow

er,

W

Pin Pout

Maximum Excess Power = 0.8 x Input Power

Total Excess Energy = 0.8 x Input Energy

12

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

Po

wer

, W

-150

-100

-50

0

50

100

150

CO

PE

, %

Pin Pout COPE=(Pout-Pin):Pin x 100%

Excess Heat Generation during 20 days

13

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

En

erg

y, k

J

Ein Eout Eex

Excess Energy during 20 days

14

Energy Output after shutting down of GD Cell ETG-3-22

0

10

20

30

40

50

60

70

80

90

0 2 4 6 8Time, hr

E, k

J“Heat After Death”

Thermal Energy Stored in GD Cell SS body (m*cp*? T)

Eout

15

A AC

T4

T5

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 D2O (230 ml)

16

Electrolytic Cell

Three cells are immersed in a constant temperature water bath of +2.50C ± 0.250C

17

Cathode & Pre-treatment

• 50 µm Pd foil, prepared by

Dr. Vittorio Violante (ENEA Frascatti, Italy)

• Annealed at 870oC in vacuum for 1h

• Etched:

- in Nitric Acid 65-67%; 1 min

- in Aqua Regia 1:1 water solution; 1 min

• Rinsed:

- D2O four times

- Ethanol 95% twice

- Ethanol Absolute once

• Dried:

in vacuum at ambient temperature for 24 h

60 m

m

7 mm

18

05

1015202530354045505560657075

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30

Delta T

Pow

er

Typical Calibration Curve for Electrolytic Cell Calorimeter

19

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

T4 and T5

- Resistance of cathode for monitoring loading (four probe AC method)

20

Study of Influence of Modulations on Loading

1st level of modulation Constant parametersChangeable parameters

212nd level of modulation

Changeable parameters Constant parameters

Study of Influence of Modulations on Loading

223rd level of modulationChangeable parameters Constant parameters

Study of Influence of Modulations on Loading

23

1st levelof modulation

2nd level ofmodulation

3rd level ofmodulation

Of-line RR0 versus time for Foil N056 (Dr.Violante)

1.

Study of Influence of Modulations on Loading

24Of-line RR0 versus time for Foil N056 (Dr.Violante)

2.

Study of Influence of Modulations on Loading

25Of-line RR0 versus time for Foil N056 (Dr.Violante)

3.

Study of Influence of Modulations on Loading

26

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

Cur

rent

den

sity

, mA

/cm

2

0

10

20

30

40

50

60

RR

0

RR0 j

Foil N056 (Dr.Violante)

Study of Influence of Modulations on Loading

27

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

RR

0

0

10

20

30

40

50

60

70

80

90

100

Cur

rent

den

sity

, mA

/cm

2

RR0 j

Foil N051 (Dr.Violante)

Study of Influence of Modulations on Loading

28

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

29

Excess Energy; Exp. # 56

Excess energy of ~3.1 MJ

30

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

31

Input Energy~0.033MJ

Output Energy

Excess Energy

Excess energy of ~1.1 MJ

Excess Energy; Exp. # 64a

32

Temperature Evolution, Exp. # 64a

A AC

T4

T5

T1

T2

T3

T4

T5Tbath

33

?T=T4-T5

Average Current Density = 7.09 mA/cm2

Cell Voltage, V

Current & Voltage; EXP. # 64a

34Loading is relatively low (~0.8)

R/Ro & Power; EXP. # 64a

35

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

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

Ene

rgy,

Jou

le

Ein Eout Ex=Eout-Ein

37

A AC

T4

T5

T1

T2

T3

Temperature Evolution, Exp. # 64b

T4

T5Tbath

38

?T, Current Density & Voltage ; EXP. # 64b

?T=T4-T5

Average Current Density = 8.37 mA/cm2

Cell Voltage, V

39

R/Ro & Power; Exp. # 64b

Loading relatively low (~0.8)

40

Excess Tritium in # 64

• Tritium concentration measured at end of #64 analysis ~ 250% of reference

• ~625 cm3 of D2O has been added to make-up for evaporation; initial

inventory was 230 cm3

• Assuming TDO/D2O evaporation rate ~ 1.0

• Estimated T effective concentration ~ 750%

• This amount of tritium corresponds to <1J – negligible as compared with the 5.7MJ excess energy generated.

41

Material Analysis

Diagnostics:

• Auger Electron Spectrometry

• Scanning Electron Microscopy-Energy Dispersive

Spectrometry SEM-EDS

• Transmission Electron Microscopy (TEM)

• Secondary Ion Mass Spectrometry (SIMS)

42

Material Analysis # 64 vs. 63; SEM-EDS

Surface of Pd foil after rolling and annealing at 8700C:

sample #64 sample #63

43

View of Typical Black Spot on # 64 and its composition

SEM-EDS

Element Wt % At %____________________________C 35.77 52.48 O 26.19 28.84 Na 4.92 3.77 Al 0.43 0.28 Si 1.05 0.66 Pt 0.39 0.04 S 1.44 0.79 Cl 10.68 5.31 Pd 2.55 0.42 K 11.07 4.99 Ca 5.52 2.43 Total 100.00 100.00_____________________________

44

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

At.

part

s

Depth, A0

After etching in Aqua Regia

45

Sample 64. SIMS depth profiling.

0 100 200 300 400 500 600

102

103

104

105

Pd

C

Pt

CNO

S

D

H

Total

Cou

nts

Depth, A0

46

Spatial distribution of selected isotopes measured by SIMS in #64a – D, b - 32S, c - total isotopes content, d - 195Pt.

Scale bar - 30 µm.

a b

c d

47

The dislocations in Pd foils after annealing.

#63 #643x1010, cm-2 6x1010, cm-2

Dislocation density

TEM

48

Plastic deformation of Pd foil caused by D2 absorption. Planes of sliding (111) are visible.

Sample #64

49

The area that is shown in the previous picture by an arrow.

50

Sample #56

Contact area Working area

51

Brittle destruction of Pt Wire Sample #64

52

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 plastic deformation 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 8500 does not fully remove the lubricant's components from 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 to high concentration of impurities. No He measurement has been attempted.

53

SUMMARY

• Significant amount of excess heat has been generated in 3 experiments using 2 Pd foils.

• Dardik’s modified SuperWaves have been used for current drive in all the three experiments.

• The average current density was relatively low: < 10 mA/cm2

• The maximum excess power was 2500%. This range of excess power is suitable for commercial applications (although the operating temperatures were 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 50 W/g U in commercial fission reactors).

54

SUMMARY (cont.)

• Significant increase in the tritium concentration in the electrolyte has been observed. However, the amount of tritium produced is negligible as compared with the excess energy generated.

• No measurement of He has been attempted.

• The Pd cathode surface was contaminated by what appears to be lubricant from the roller used for pre-treatment as well as impurities adsorbed from the air.