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US. Cl.
CPC ............ .. H01M 4/386 (2013.01); H01M 4/625
(2013,01)
POWDER
USPC
........................................................ .. 252/502
(57)
ABSTRACT
_ _
(22) Flled:
Jul 26 2013
Publication Classi?cation
(2006.01)
H01M 4/62
(2006.01)
[Graphene/Graphene fluoride 1
G ra phene/Silica/Mg
composite powder
Mixing
Heat treatment
Acidic graphene
Graphene/Silicon/MgO
solution/dispersion
composite powder
pH value testing
Graphene-doped Silicon
Hydrolysis and
POWder/
50|Uti0n
7
Adjust pH value
Drying
Gel formation
Drying
Graphene/silica nano
composite powder
Ball milling with Mg
Graphene/Silica/Mg
composite powder
Filtration, drying
and air mM
Graphene duped
Silicon nano powder
'i
[Graphene/Graphene fluoride ]
US 2015/0028263 A1
Mixing
V
Acidic graphene
solution/dispersion
pH value testing
V
Hydrolysis and
powder/
solution
Graphene/silica nano
composite solution
Adjust pH value
Drying
L Gel formation ]
V
Drying
'
Graphene/silica nano
composite powder
[ Graphene/Silica/Mg ]
composite powder
FIG. 1(a)
Graphene/Silica/Mg
composite powder
US 2015/0028263 A1
Heat treatment
V
Graphene/Silicon/MgO
composite powder
lAcid etching
Graphene-doped Silicon
nano composite solution
Filtration, drying
and air mM
- -
- - _
_ _
--\
FIG. 1(b)
powder
US 2015/0028263 A1
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"iii '
US 2015/0028263 A1
US 2015/0028263 A1
[0001]
Jan. 29,2015
No. 10/274,473 (Oct. 21, 2002); now US. Pat. No. 7,071,258
BACKGROUND
cation Ser. No. 11/982,672 (Nov. 5, 2007) now US. Pat. No.
ucts have been extremely expensive and this cost issue has
severely impeded the full-scale commercialization of Si nano
[0004]
quantities.
[0008]
US 2015/0028263 A1
[0009]
tional processes:
trolysis chamber.
[0025]
2008).
[0013]
(Apr. 19,2011).
[0015] 6. Sushil Kumar, et al., Process for the preparation
of photo luminescent nanostructured silicon thin ?lms, US
Pub. No. 2010/0285235 (Nov. 11,2010).
[0016] 7. L. W. Wu, et al., Nano powder production system,
US Pub. No. 2003/0108459 (Jun. 12, 2003).
[0017] 8. Hai-Lin Sun, et al., Method of manufacturing
silicon nano-structure, US. Pat. No. 7,888,271 (Feb. 15,
201 1).
[0018]
1 989).
[0019]
over 20000 C.) and thus has become a popular technique used
US 2015/0028263 A1
[0036]
[0031]
composite powder.
[0038] In yet another preferred embodiment, step (c) of
converting the silicon precursor includes placing the magne
sium-coated silicon precursor/graphene nano composite
powder in a sealed chamber and purging the powder to a
heating apparatus that allows the reaction between magne
sium and silicon precursor to occur therein for forming a
slightly larger.
[0032] In terms of Si nano powder production yield, pris
tine graphene is the best choice and graphene oxide (G0) the
worst. The following summarizes the order: pristine
graphene>boron-doped
graphene>nitrogen-doped
graphene>amine-functionalized
graphene>graphene
?uoride>graphene chloride>graphene bromide>graphene
[0039]
[0033]
system.
[0040] Up to step (d), the method produces a graphene
doped silicon nano powder product. The graphene compo
[0042]
US 2015/0028263 A1
[0043]
silicon powders.
[0046]
silicon powders.
Si3N4, SiC, SiH4, SiCl4, SiOz, MxSi (silicide, MILi, Ti, Ni,
Mg, Au, Ag, Al, Ca, Mo . . . ). The industrial production
Au, Ag, Al, Ni, Cu, Ti, Co, and Sn, can be selectively added to
the dispersion to obtain a metal doped silica/NGP nano com
[0051]
[0052]
results).
[0053]
US 2015/0028263 A1
Example 1
[0056]
tion, allowing the reaction to proceed for 2-24 hours and then
putting the turbid liquid to an ultrasonic bath for 1 hour. The
suspension was poured into the ?ltration system and the large
particles trapped at the bottom of the system were discarded.
DI water was used to rinse the ?ltrate three times to obtain
Example 2
Nanocomposites
[0059]
of the following metal elements: Au, Ag, Al, Cu, Ti, Ni, Co or
a combination thereof. The particle size of these preferred
metals is in the range of 10 nm to ~5 um, and when particle
size is over 1 pm in diameter, a step of high energy ball milling
could be carried out to reduce the diameter. In some preferred
embodiments, metal salts with some anions removed may
Example 3
Graphene-Doped Nano Silicon from Nano Silica
[0060] In a typical process, 10 wt. % nano silica emulsion is
prepared and ultrasonicated at an ultrasonic energy level of
paste. The paste is then dried at 120 C. and the resulting nano
US 2015/0028263 A1
Example 4
preference:
pristine
graphene>boron-doped
graphene>nitrogen-doped graphene>amine-functionalized
Example 5
described in example 1.
Graphene
[0062]
nickel powder (<100 nm) into the sol and then ultrasonicate
the resulting suspension. Then, add ammonia wate into the
suspension to form a chocolate color gel. The subsequent
procedures are similar to those described in example 1 till the
?nal nano silicon is collected. Then, a certain amount of the
and purge with a mixture of Ar/HZ, repeat the step for three
times. Then, heat the furnace to 550 C. at a rate of 5 C/min.
Keep the temperature at 550 C. for 30 min and then heat the
furnace to 950 C. at 5 C/min. Keep the temperature at 950
powders.
[0063]
[0065]
for
selecting
Si
precursor
material:
sodium
>SiF4>SiCl4>SiBr4>Sil4.
We claim:
1. A method of producing graphene-doped silicon nano
planes.
halogen compound.
US 2015/0028263 A1
tains MgFZ.
6. The method of claim 1, wherein said step (a) of preparing
a silicon precursor/graphene nano composite includes dis
persing or dissolving a silicon precursor in an acidic graphene
solution to form a hybrid suspension, removing a liquid com
composite.
9. The method of claim 1, wherein said step (a) of preparing
silicon precursor/graphene nano composite includes pre-dop
ing a metal powder selected from Au, Ag, Ti, Ni, Cu, Al or a
precursor thereof for silicon nano wire production.
contains SiOZ.
cooling system.
20. The method of claim 18 wherein said chamber contains
a thermally stable material selected from a stainless steel, a
nickel alloy, a titanium alloy, a cobalt alloy, a superalloy, or a
an Ar/H2 atmosphere.
*