CN105417525B - Dendritic crystalline three-dimensional grapheme and preparation method thereof - Google Patents
Dendritic crystalline three-dimensional grapheme and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the preparation method of dendritic crystalline three-dimensional grapheme, belong to technical field of nanometer material preparation, it includes：1）In CuSO4、NiSO4、H2SO4Mixed solution in, nanometer Cu clusters or CuNi clusters are deposited in the mixed solution by working electrode of Cu pieces, obtains graphene deposition substrate；2）Nano metal cluster is put into after being cleaned repeatedly in ultra-pure water, filters out and freeze；3）Nano metal cluster after will be lyophilized is placed in vacuum drying oven, first 800 1000 degrees Celsius of progress reduction treatments under an atmosphere of hydrogen, graphene deposition processes are carried out in the mixed atmosphere of 800 1000 degrees Celsius of hydrogen and methane again, alloy substrates are removed using ammonium persulfate solution or liquor ferri trichloridi, that is, obtain dendritic crystalline graphene.The invention also discloses a series of dendritic crystalline three-dimensional graphemes obtained using this method；The dendritic crystalline three-dimensional grapheme, there is the characteristics of one end folding, other end closures, such graphene has excellent hydrogen reduction performance.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to dendritic crystalline three-dimensional grapheme and preparation method thereof.
Background technology
Grapheme material has the performances such as excellent electric conductivity, thermal conductivity and superhigh intensity.Graphite is prepared on a large scale at present
Alkene material mainly has two kinds：A kind of is the film-form two-dimensional graphene prepared by chemical vapor deposition or oxidation-reduction method；Separately
A kind of is the three-dimensional grapheme prepared by explosion method or template.Three-dimensional grapheme relative two dimensional graphene compares table with bigger
Area, it is expected to obtain extensive use in fields such as sensing, catalysis.
Current three-dimensional grapheme is the foam-like graphene with loose structure, has the graphite of similar pine-tree structure
Alkene has not been reported.In addition, the three-dimensional grapheme template such as microstructure sizes such as foam fine copper, foam pure nickel are all micron at present
Level, and this is graphene-based in obtained by nanoscale bianry alloy dendrite substrate, utilizes the special microcosmic surface knot of nanometer base material
Structure, regulate and control and realize the excellent catalytic performance of graphene.In general, graphene does not have obvious hydrogen reduction performance, only mixes
The aerobic reducing property of ability after nitrogen.
The content of the invention
Goal of the invention：It is an object of the invention to provide the preparation method of dendritic crystalline three-dimensional grapheme, preparation method letter
It is single, the nanoscale template of excellent graphene can be prepared with simple and quick acquisition；Another object of the present invention is to provide this
Dendritic crystalline three-dimensional grapheme prepared by method, the graphene can obtain good hydrogen reduction performance under the conditions of not nitrating.
Technical scheme：For achieving the above object, the present invention adopts the following technical scheme that：
The preparation method of dendritic crystalline three-dimensional grapheme, comprises the following steps：
1）In CuSO4 、NiSO4、H2SO4It is working electrode in the mixed solution using Cu pieces in the mixed solution of additive
Middle deposition nanometer Cu or CuNi cluster, obtains sedimentation products；
2）Sedimentation products are put into after being cleaned repeatedly in ultra-pure water, filter out product and freeze, the sample after being freezed；
3）Sample after will be lyophilized is placed in vacuum drying oven, first carries out reduction treatment, then the hydrogen in high temperature under an atmosphere of hydrogen
Graphene deposition processes are carried out in gas and methane blended atmosphere, then remove gold using ammonium persulfate solution or liquor ferri trichloridi
Belong to substrate, that is, obtain dendritic crystalline three-dimensional grapheme.
Step 1）In, described CuSO4Concentration be 0.1-0.3 mol/L, NiSO4Concentration is 0-2 mol/L, H2SO4It is dense
Spend for 0.5-1.5 mol/L,
Additive is the K that concentration is 0-0.5 mol/L2SO4Or (the NH that concentration is 0-0.5 mol/L4)2SO4。
Step 1）In, described working electrode is in 0.25-1.00 A/cm220-60 s are deposited under current density condition.
Step 3）In, it in gas flow ratio is Ar that described reduction treatment, which is,：H2=8：1- 4：1, temperature 800-1000
10-30 minutes are heated under conditions of degree Celsius.
Described graphene deposition processes are in Ar in gas flow ratio：H2：CH4=8：1：1 - 4：1：1, temperature is
10-20 minutes are heated under conditions of 800-1000 degrees Celsius.
Dendritic crystalline three-dimensional grapheme prepared by the preparation method of dendritic crystalline three-dimensional grapheme, the dendritic crystalline three-dimensional grapheme one
Hold folding, other end closures；The form of the dendritic crystalline three-dimensional grapheme is in a diameter of 200-500 nm, length 300-1000
A diameter of 50-300 nm are grown on nm one-level tubular graphene alkene, length is 50-600 nm two level tubulose graphene；When
When growing three-level tubulose graphene on two level tubulose graphene, a diameter of 20-100 nm of the three-level tubulose graphene, length is
20-100 nm。
Described dendritic crystalline three-dimensional grapheme is 3 ~ 10 layers.
Beneficial effect：Compared with prior art, the preparation method of dendritic crystalline three-dimensional grapheme of the invention is simple to operate, adopts
Three-dimensional grapheme with its preparation is dendritic crystalline；In addition, the disclosed three-dimensional grapheme template such as mesh such as foam fine copper, foam pure nickel
Preceding is all micro-meter scale, and this is graphene-based made in nanometer bianry alloy dendrite substrate, obtains different microstructures, from
And excellent catalytic performance can be embodied；In general, graphene does not have an obvious hydrogen reduction performance, and the dendrite that the present invention obtains
Structure graphite alkene has good hydrogen reduction performance, and maximum reduction spike potential is -0.242V, and initial reduction current potential is -0.143V.
Brief description of the drawings
Fig. 1 is dendritic crystalline three-dimensional grapheme shape appearance figure.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described further.
Fig. 1 is dendritic crystalline three-dimensional grapheme shape appearance figure.The dendrite prepared using the preparation method of dendritic crystalline three-dimensional grapheme
The form of shape three-dimensional grapheme is：The dendritic crystalline three-dimensional grapheme has the characteristics of one end folding, other end closures；The dendritic crystalline
The form of three-dimensional grapheme is in a diameter of 200-500 nm, and length is to be grown on 300-1000 nm one-level tubular graphene alkene
A diameter of 50-300 nm, length are 50-600 nm two level tubulose graphene；In the case of certain, in the two level tubular graphene
A diameter of 20-100 nm are grown on alkene, length is 20-100 nm three-level tubulose graphene.
The preparation method of dendritic crystalline three-dimensional grapheme, comprises the following steps：
1）In CuSO4 、NiSO4、H2SO4It is working electrode in the mixed solution using Cu pieces in the mixed solution of additive
Middle deposition nanometer Cu or CuNi cluster, obtains sedimentation products；
2）Sedimentation products are put into after being cleaned repeatedly in ultra-pure water, filter out product and freeze, the sample after being freezed；
3）Sample after freezing is placed in vacuum drying oven, and elder generation carries out also original place for 800-1000 degrees Celsius under an atmosphere of hydrogen
Reason, then graphene deposition processes are carried out in the mixed atmosphere of 800-1000 degrees Celsius of hydrogen and methane, then utilize persulfuric acid
Ammonium salt solution or liquor ferri trichloridi remove alloy substrates and obtain dendritic crystalline graphene.
Step 1）In, described CuSO4Concentration be 0.1-0.3 mol/L, NiSO4Concentration 0-2 mol/L, H2SO4Concentration
For 0.5-1.5 mol/L, additive is the K that concentration is 0-0.5 mol/L2SO4Or (the NH that concentration is 0-0.5 mol/L4)2SO4。
Step 1）In, described working electrode is in 0.25-1.00 A/cm220-60 s are deposited under current density condition.
Step 3）In, it in gas flow ratio is Ar that described reduction treatment, which is,：H2=8：1- 4：1, temperature 800-1000
10-30 minutes are heated under conditions of degree Celsius.Step 3）In, described graphene deposition processes be gas flow ratio be
Ar：H2：CH4=8：1：1 - 4：1：1, temperature heats 10-20 minutes under conditions of being 800-1000 degrees Celsius.
Embodiment 1
In 0.1mol/L CuSO4+ 0.5mol/L H2SO4In mixed solution, using Cu pieces as working electrode, platinum electrode is pair
Electrode, saturated calomel electrode are reference electrode, in 0.25 A/cm2Constant current conditions under deposit the s of nanometer Cu clusters 20.Institute will be deposited
Product be put into cleaned repeatedly in ultra-pure water after it is lyophilized.Sample after lyophilized is placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）=6：1
Under conditions of in 800 degrees Centigrade 20 minutes carry out reduction treatment, then in 800 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）=8：1：
Graphene deposition is carried out under conditions of 1, deposition removes Metal Substrate after 20 minutes, using ammonium persulfate solution or liquor ferri trichloridi
Bottom can obtain dendritic crystalline graphene.The dendritic crystalline graphite has a diameter of 200-400 nm, and length is 200-1000 nm one-level
Tubular graphene alkene, a large amount of a diameter of 100-200 nm are grown above, length is 100-500 nm two level tubulose graphene,
A small amount of a diameter of 20-100 nm are grown on the tubular graphene alkene of two level, length is 20-100 nm three-level tubulose graphene.
Sample is dissolved in 4-6h in 1M ammonium persulfate solutions, copper-based bottom is dipped to and is wholly absent, can obtain the tubular graphene of no substrate
Alkene.
Graphene thickness is 5-8 layers, and maximum reduction spike potential is -0.342V, and initial reduction current potential is -0.243V.
Embodiment 2
In 0.2 mol/L CuSO4+ 1.0 mol/L H2SO4+0.8mol/L NiSO4（The addition of Ni ions can change gold
Belong to nano-cluster substrate composition, heat endurance and pattern）In mixed solution, using Cu pieces as working electrode, platinum electrode is to electrode, is satisfied
It is reference electrode with calomel electrode, in 1.00 A/cm2Constant current conditions under deposit nanometer CuNi clusters 30s.Products therefrom will be deposited
It is put into lyophilized after being cleaned repeatedly in ultra-pure water.Sample after lyophilized is placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）=6：1 condition
Under in 900 degrees Centigrade 20 minutes carry out reduction treatment, then in 900 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）= 6：1：1 bar
Graphene deposition is carried out under part, deposition can obtain dendritic crystalline graphene after 20 minutes.The dendritic crystalline graphite has a diameter of 150-
200 nm, length are 200-500 nm one-level tubular graphene alkene, grown a large amount of a diameter of 50-100 nm above, and length is
50-500 nm two level tubulose graphene, a small amount of a diameter of 20-100 nm, length are grown on the tubular graphene alkene of two level
For 20-100 nm three-level tubulose graphene.Sample is dissolved in 4-6h in 1mol/L ammonium persulfate solutions, is dipped to copper-based bottom
It is wholly absent, can obtain the tubular graphene alkene of no substrate.
Graphene thickness is 5-10 layers.Maximum reduction spike potential is -0.242V, and initial reduction current potential is -0.143V.
Embodiment 3
In 0.2 mol/L CuSO4+ 1.0 mol/L H2SO4+0.5mol/L （NH4）2SO4（（NH4）2SO4Addition will
Change plane of crystal energy, change the pattern and size of nano metal cluster）In mixed solution, using Cu pieces as working electrode, platinum electrode
For to electrode, saturated calomel electrode is reference electrode, in 1.00 A/cm2Constant current conditions under deposit the s of nanometer Cu clusters 30.Will be heavy
Product products therefrom, which is put into ultra-pure water, cleans repeatedly rear freeze.Sample after lyophilized is placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）
=6：Under conditions of 1 reduction treatment is carried out in 900 degrees Centigrade within 20 minutes, then in 900 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）=
6：1：Graphene deposition is carried out under conditions of 1, deposition can obtain dendritic crystalline graphene after 20 minutes.The dendritic crystalline graphite has straight
Footpath is 150-200 nm, and length is 200-500 nm one-level tubular graphene alkene, grown a large amount of a diameter of 50-100 above
Nm, length are 50-500 nm two level tubulose graphene, and a small amount of a diameter of 20-100 is grown on the tubular graphene alkene of two level
Nm, length are 20-100 nm three-level tubulose graphene.Sample is dissolved in 4-6h in 1mol/L ammonium persulfate solutions, is dipped to
Copper-based bottom is wholly absent, and can obtain the tubular graphene alkene of no substrate.
Graphene thickness is 5-10 layers.Maximum reduction spike potential is -0.162V, and initial reduction current potential is -0.2V.
Embodiment 4
In 0.3mol/L CuSO4+ 1.5mol/L H2SO4+0.5mol/L K2SO4（K2SO4Addition will change crystal table
Face energy, change the pattern and size of nano metal cluster）In mixed solution, using Cu pieces as working electrode, platinum electrode is to electrode, is satisfied
It is reference electrode with calomel electrode, in 0.25 A/cm2Constant current conditions under deposit nanometer Cu clusters 30s.Deposition products therefrom is put
Enter lyophilized after being cleaned repeatedly in ultra-pure water.Sample after lyophilized is placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）=6：Under conditions of 1
Reduction treatment is carried out in 900 degrees Centigrade within 20 minutes, then in 900 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）= 6：1：1 condition
Lower progress graphene deposition, deposition can obtain dendritic crystalline graphene after 20 minutes.The dendritic crystalline graphite has a large amount of a diameter of
200-400 nm, length are 200-1000 nm one-level tubular graphene alkene, grown a diameter of 100-200 nm, length above
For 100-500 nm two level tubulose graphene, a small amount of a diameter of 20-100 nm are grown on the tubular graphene alkene of two level, it is long
Spend the three-level tubulose graphene for 20-100 nm.Sample is dissolved in 4-6h in 1mol/L ammonium persulfate solutions, is dipped to copper-based
Bottom is wholly absent, and can obtain the tubular graphene alkene of no substrate.
Graphene thickness is 5-10 layers.Maximum reduction spike potential is -0.362V, and initial reduction current potential is -0.26V.
Embodiment 5
In 0.2 mol/L CuSO4+ 1.0 mol/L H2SO4+0.1 mol/L (NH4)2SO4+2mol/L NiSO4Mixing
In solution, using Cu pieces as working electrode, platinum electrode is that saturated calomel electrode is reference electrode, in 1.0 A/cm to electrode2Perseverance
Nanometer CuNi clusters 20s is deposited under the conditions of stream.Deposition products therefrom is put into lyophilized after being cleaned repeatedly in ultra-pure water.Sample after lyophilized
Product are placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）=8：Under conditions of 1 reduction treatment is carried out in 900 degrees Centigrade within 10 minutes,
Again in 1000 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）= 8：1：Graphene deposition is carried out under conditions of 1, deposition can obtain after 20 minutes
To dendritic crystalline graphene.The dendritic crystalline graphite has a large amount of a diameter of 200-400 nm, and length is 200-1000 nm one-level pipe
Shape graphene, grown a diameter of 100-200 nm above, and length is 100-500 nm two level tubulose graphene.Sample is molten
The 4-6h in 1mol/L ammonium persulfate solutions, it is dipped to copper-based bottom and is wholly absent, can obtain the tubular graphene alkene of no substrate.It is high
The molten mistake of three-level dendrite that temperature will cause nano metal cluster.
Graphene thickness is 5-10 layers, and maximum reduction spike potential is -0.252V, and initial reduction current potential is -0.123V.
Embodiment 6
In 0.2 mol/L CuSO4+ 1.0 mol/L H2SO4+0.1 mol/L (NH4)2SO4+0.9mol/L NiSO4It is mixed
Close in solution, using Cu pieces as working electrode, platinum electrode is that saturated calomel electrode is reference electrode, in 1.0 A/cm to electrode2's
The s of nanometer Cu clusters 60 is deposited under constant current conditions.Deposition products therefrom is put into lyophilized after being cleaned repeatedly in ultra-pure water.After lyophilized
Sample is placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）=4：Under conditions of 1 also original place is carried out within 30 minutes in 800 degrees Centigrade
Reason, then in 900 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）= 4：1：Graphene deposition is carried out under conditions of 1, deposition can after 10 minutes
Obtain dendritic crystalline graphene.The dendritic crystalline graphite has a large amount of a diameter of 200-400 nm, and length is 200-1000 nm one-level
Tubular graphene alkene, a diameter of 100-200 nm is grown above, length is 100-500 nm two level tubulose graphene, in two level
Tubular graphene alkene on grown a small amount of a diameter of 20-50 nm, length is 20-50 nm three-level tubulose graphene.By sample
4-6h in 1M ammonium persulfate solutions is dissolved in, copper-based bottom is dipped to and is wholly absent, can obtain the tubular graphene alkene of no substrate.
Graphene thickness is 3-6 layers.Maximum reduction spike potential is -0.222V, and initial reduction current potential is -0.133V.
Embodiment 7
In 0.2 mol/L CuSO4+ 1.0 mol/L H2SO4In mixed solution, using Cu pieces as working electrode, platinum electrode is
To electrode, saturated calomel electrode is reference electrode, in 1.00 A/cm2Constant current conditions under deposit the s of nanometer Cu clusters 30.Will deposition
Products therefrom, which is put into ultra-pure water, cleans repeatedly rear freeze.Sample after lyophilized is placed in vacuum drying oven, in Ar：H2（Flow-rate ratio）=
6：Under conditions of 1 reduction treatment is carried out in 900 degrees Centigrade within 20 minutes, then in 900 degrees Celsius of Ar：H2：CH4（Flow-rate ratio）=
6：1：Graphene deposition is carried out under conditions of 1, deposition can obtain dendritic crystalline graphene after 20 minutes.The dendritic crystalline graphite has straight
Footpath is 200-400 nm, and length is 200-1000 nm one-level tubular graphene alkene, grown a large amount of a diameter of 100-200 above
Nm, length are 100-500 nm two level tubulose graphene, and a small amount of a diameter of 20- is grown on the tubular graphene alkene of two level
100 nm, length are 20-100 nm three-level tubulose graphene.Sample is dissolved in 4-6h in 1M ammonium persulfate solutions, is dipped to
Copper-based bottom is wholly absent, and can obtain the tubular graphene alkene of no substrate.
Graphene thickness is 5-10 layers.Maximum reduction spike potential is -0.32V, and initial reduction current potential is -0.123V.
From examples detailed above as can be seen that the regulation by electric depositing solution composition and concentration can control metal nanometre cluster
Composition, pattern and size, metal nanometre cluster pattern and size are further adjusted by graphene deposition process parameters, and to graphite
Alkene thickness and powder injection molding, so as to adjust its hydrogen reduction performance.
Claims (4)
1. the preparation method of dendritic crystalline three-dimensional grapheme, it is characterised in that comprise the following steps：
1) in CuSO4、NiSO4、H2SO4Mixed solution in, nanometer Cu is deposited in the mixed solution by working electrode of Cu pieces
Or CuNi clusters, obtain sedimentation products；
2) sedimentation products are put into after being cleaned repeatedly in ultra-pure water, filter out product and freeze, the sample after being freezed；
3) will it is lyophilized after sample be placed in vacuum drying oven, first carry out reduction treatment under an atmosphere of hydrogen, then high temperature hydrogen and
Graphene deposition processes are carried out in methane blended atmosphere, then remove Metal Substrate using ammonium persulfate solution or liquor ferri trichloridi
Bottom, that is, obtain dendritic crystalline three-dimensional grapheme；In step 1), described CuSO4Concentration be 0.1-0.3mol/L, NiSO4Concentration is
0-2mol/L, H2SO4Concentration is 0.5-1.5mol/L, K2SO4Concentration is 0-0.5mol/L, (NH4)2SO4Concentration is 0-0.5mol/
L；In step 1), described working electrode is in 0.25-1.00A/cm220-60s is deposited under current density condition.
2. the preparation method of dendritic crystalline three-dimensional grapheme according to claim 1, it is characterised in that：It is described in step 3)
Reduction treatment be in gas flow ratio be Ar：H2=8：1-4：1, temperature heats 10- under conditions of being 800-1000 degrees Celsius
30 minutes.
3. the preparation method of dendritic crystalline three-dimensional grapheme according to claim 1, it is characterised in that：Described graphene sinks
Product processing is in Ar in gas flow ratio：H2：CH4=8：1：1-4：1：1, temperature adds under conditions of being 800-1000 degrees Celsius
Hot 10-20 minutes.
4. the dendritic crystalline prepared using the preparation method of the dendritic crystalline three-dimensional grapheme described in any one in claims 1 to 3
Three-dimensional grapheme, it is characterised in that：Dendritic crystalline three-dimensional grapheme one end folding, other end closures；The dendritic crystalline three-dimensional graphite
The form of alkene is in a diameter of 200-500nm, and length is that grown a diameter of 50- on 300-1000nm one-level tubular graphene alkene
300nm, length are 50-600nm two level tubulose graphene；When the growth three-level tubulose graphene on two level tubulose graphene
When, the three-level tubulose graphene a diameter of 20-100nm, length 20-100nm.
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| A new type of porous graphite foams and their integrated composites with oxide/polymer core/shell nanowires for supercapacitors: structural design, fabrication, and full supercapacitor demonstrations;Xinhui Xia et al;《Nano letters》;20140218;第14卷(第3期);结果与讨论部分1-2段及支撑材料方法与材料部分 * |
| 改良电沉积法制备硝酸根高敏传感铜簇;崔志强等;《功能材料》;20150915;第46卷(第17期);实验部分2.1及图2 * |
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