LANR Cathode Preparation

for
Electrolysis Experiments:
A Comparison of Protocols
and
Implications
Frank Gordon
Stan Szpak
Harper Whitehouse
2014 CF/LANR Collouiu! at "#$
"ar%h 21&2'( 2014
Presentation
Summary
A )ide *ariet+ o, Co&deposition proto%ols ha*e -een .su%%ess,ull+
used
Co&deposition has al)a+s -een %redited )ith produ%in/ hi/h
loadin/ ratios
"a/neti% and/or ele%tri% 0elds !a+ to -e i!portant
Fukai su//ests that loadin/ ratios %ould -e e*en hi/her )ith
produ%tion o,
SA12s 3141
5 #!pli%ations4 Su//ests a lot !ore
e6peri!entation )ith
%o&deposition
Che!istr+ *s %urrent densit+ and pro0le *s !a/neti% 0eld *s 777
Are produ%ts 8heat( radiation9 di:erent ,or di:erent %onditions7
At )hat latti%e %on%entration does h+dro/en -e%o!e a poison7
Evolution of Co-
eposition
Fleis%h!ann & ;ons e:e%t pu-lished <;onFlH=>?
Cathode4 -ulk palladiu! 8;d9
Lon/ loadin/ ti!e o, 2&4 )eeks
@6%ess heat diA%ult to repli%ate
Szpak & Boss %o&deposition pu-lished <Szp"oS>1?
Cathode4 ele%trodeposited ;d on Cu and other !aterials
"odest loadin/ ti!e o, da+s
@6%ess heat repli%a-le
"an+ others ha*e used/are usin/ %o&deposition
Letts C Ha/elstein proto%ol pu-lished <LetHa/12?
Cathode4 ele%trodeposited ;d on Au %oated Cu
Di:erent %on%entrations o, ;d
Hi/her %urrent densit+ resultin/ in short %o&deposition ti!e
@6%ess heat reported
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$emperature vs $ime Pro%le
&' Electroanal' Chem'( )ol'*+,( pp' ,---,.+ !/00/#
*0
solution electrode
Exp / current o1
*2
*-
**
Exp ,
3$ 4 *',"C
*,
*+
cathode
*/
3$ 4 ,'5"C
,0
,2
,-
solution
,6
-/+ + /+ ,+
time !sec#
thermocouples
+ ,+ 5+ .+
time !min#
$he Electrode is 7armer than the Solution8
9:ot Spots; and 9<ini-
Explosions;
Il Nuovo Cimento( )ol //,A( pp' -22--6- !/000#
a C hot spots - & piezoele%tri%
#n,rared %a!era and polarized ,erroele%tri% ;E$ transdu%er
responses
SE< of Co-eposited
Pd= >ilm
&' Electroanal' Chem' -6+ pp,65-,0+ !,++-#
Eur Phy & Appl Phys 5+ pp,0*-*+* !,++2#
a C a,ter %o!pletion o, %o&deposition(
- C e6posed to e6ternal ele%tri% 0eld( % C e6posed to !a/neti% 0eld
Electrochemical Co-eposition
Processes
F8t19
F809
Di:usion Li!itin/
Current
Current
& i
G
H i
t829 t819
G
t8'9
t809 i(1) i(2) J(0)
J(t2)
Sta-ilization
euterium ?p-ta@e
&' Electroanal' Chem' *20 pp /,/-/,2 !/005#
td
Deuteriu! up&take durin/ %o&depositionI J% K & L!A%!&2 and
Ja K L !A%!&2( )ith %ell %urrent re*ersal at 1(2(4( and = se%ondsI
Hi/h loadin/ ratios are a%hie*ed durin/ %o&deposition
Initial Co-eposition $hermal
Aehavior
>usion $echnoloBy *. pp,*5-,5/ !/000#
endother!i% a-sorption C 0iMiA <0iMia? (
endother!i% a-sorption -alan%ed -+ e6other!i% rea%tion CaiMi-
<aMi-?(
e6other!i% rea%tion do!inates Mia <-Mi?
Calileo 9Protocol;
$he %o&deposition proto%ol de*eloped at
S;AWAR
-+ Szpak and "osier&Boss as part o, the
Galileo
;roJe%t to %on0r! nu%lear parti%le
/eneration
usin/ CR&'> as an ar%hi*al parti%le
dete%tor
;roto%ol and proJe%ts results reported in4
http4//ne)ener/+ti!esI%o!/*2/proJe%ts/t/p/200N$G;/200NGalileo;roJe%tReportIpd,
;roto%ol su!!ar+4
A platin/ phase 8appro6i!atel+ 2 )eeks9
A loadin/ phase 8appro6i!atel+ 1 )eek9
Su%%ess,ull+ de!onstrated nu%lear parti%le
tra%ks
in CR&'>
SDpa@ <osier-Aoss !SPAEAR#
Protocol
as ?sed in FLet:aB/,G
Su-strate C ;repared %opper
@le%trol+te 8su-seuentl+ diluted L0O to
redu%e
;d -uild&up9
0I'0 " LiCl
0I0L " ;dCl2
>>I>O D2F
Current pro0le
1I'( 2IP( PI' !A/%!2
Applied in steps
Additional %onditions
Qnkno)n i, !a/nets )ere used
Did not produ%ed e6%ess po)er 8heat9
<odi%ed SPAEAR <ethod in
FLet:aB/,G
Electrodes
Anode4 0I>>> ;t )ire in the ,or! o, !ulti&turn spiral %oil
Cathode4 Copper su-strate /old plated 80IL %!29
Electrolyte
0I1L " LiCl
0I0012L " ;d %on%entration 80I44 / ;dCl2 solution IL )t O solution in 10 )t O HCl9
>>I>O D2F ,ro! Aldri%h
Current pro%le
Co&deposition done at RL00 !A/%!2 8Solution %lears in a %ouple o, hours9
Applied i!!ediatel+
Additional conditions
Cell )ere %losed
Gasses re%o!-ined )ith 1/= inI alu!ina pellets %oated )ith 0ILO platinu! redu%ed
Experimental results:
e6%ess ener/+ produ%ed
Letts-:aBelstein Results
SC"NS P( 2012 pp44&L4
0&=00 !inutes4 Cali-ration )ith D2F( LiCl
=00 C 1100 !inutes4 0I44 !l ;dCl ## LO)t( 10O)t HCl
1100&end !inutes4 D2F repla%ed )ith H2F
Current at L00 !A/%!2 throu/hout
Important Events in the Search
for
Excess :eat in Pd-
Szpak and %o)orkers <Szp"oS>1? sho)ed that ele%trol+ti%
%odeposition o, ;d
and D ,ro! a solution %ontainin/ LiCl
#n an #CCF1L 8200>9 presentation "%Tu-re and %o)orkers at SR#
sho)ed that
so!e o, the %onditions that !ust -e !eet to repli%ate the
Fleis%h!ann/;ons
e6%ess ener/+ ,ro! ;d %athodes durin/ hea*+ )ater ele%trol+sis
)ere4
D/;d loadin/ 3 0I=L( perhaps 0I>L
Lon/ )aitin/ period o, 2&4 )eeks -e,ore e6%ess heat o-ser*ed
At #CCF&1N Letts and Ha/elstein spe%ulate .III a-out the
i!portan%e o,
*a%an%ies in produ%in/ the e6%ess po)er e:e%t in deuterated
palladiu!
%athodesIU <LetHa/1'?
.III <We? ,ound onl+ one para!eter that in%reased -+ '40O )ith a 1'
de/ree
in%rease in %ell te!perature C the nu!-er o, *a%an%ies in the
palladiu! %athode(
IIIU
Ehat are 9SuperaHundant )acancies; !SA)#I
Normal vs' SA) lattice
:ydroBen loaded
<Ea/Val10?
,I%I% 1a%an%+&ordered L12 stru%ture(
;d'1a%Hn !a6i!u! n K 4
"a6 loadin/ 141 "a6 loadin/ 44'
<Fukai>L?
SuperaHundant
)acancies !SA)#
<Fukai >' & 0N?
Fne o, the i!portant re%o/nitions /ained ,ro! the SA1 ,or!ation
is that
the !ost sta-le stru%ture o, "&H allo+s is in ,a%t a de,e%t
stru%ture
%ontainin/ a lar/e nu!-er o, *a%an%ies
.III in all !etals in*esti/ated -+ ion i!plantation e6peri!ents( H
ato!s are
trapped -+ *a%an%ies( up to si6 ato!s per *a%an%+( )ith rather
lar/e
-indin/ ener/ies III IU
#n !etal&h+dro/en 8"&H9 allo+s at hi/h te!perature and hi/h
h+dro/en
pressure .the latti%e para!eter o, Ni and ;d de%reased o*er
se*eral hours
until it rea%hed a li!itin/ *alue R1ILO s!allerU
$here is .the possi-ilit+ o, %reatin/ SA1s )ithout an+ e6tre!e
%onditions(
na!el+ -+ ele%trol+ti% deposition .
#n ele%trodeposition .the sta-le stru%ture should -e rea%hed
dire%tl+ as H
and " ato!s are deposited si!ultaneousl+ in%orporatin/
*a%an%ies in
appropriate proportionsU
JHservations and
Kuestions
Co&deposition has -een su%%ess,ull+ used in a )ide
*ariet+ o,
e6peri!ental proto%ols
What is the roll o, a !a/neti% and/or ele%tri% 0eld7
Can di:erent proto%ols lead to di:erent rea%tion paths7
Was the F&; e6peri!ent reall+ a %o&deposition
e6peri!ent7
Did %o&deposition o%%ur durin/ the 2&4 )eek .loadin/U period7
Were SA12s %reated in the -ulk durin/ that ti!e7
What is the roll o, SA12s7
Were ;ons and Fleis%h!ann lu%k+ )ith their proto%ol7
Co&deposition produ%es -oth hi/h sur,a%e area and
SA12sI
Are SA12s in*ol*ed in /as loadin/ o, nano&parti%les7
So far( the main thinB that ILm learninB is ho7
much I donLt @no78
Ac@no7ledBments
"it%hell S)artz et alI ,or or/anizin/ the
!eetin/
Stan Szpak( ;a! "osier&Boss and the
S;AWAR
tea!
Dennis Letts and ;eter Ha/elstein
$o e*er+one )orkin/ in the 0eld and
%ontri-utin/
to the ad*an%e!ent o, LANR