CN106540711A - A kind of method that green prepares Ag-ZnO grapheme foam nickel material - Google Patents
A kind of method that green prepares Ag-ZnO grapheme foam nickel material Download PDFInfo
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- CN106540711A CN106540711A CN201610937856.0A CN201610937856A CN106540711A CN 106540711 A CN106540711 A CN 106540711A CN 201610937856 A CN201610937856 A CN 201610937856A CN 106540711 A CN106540711 A CN 106540711A
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- arginine
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- silver
- graphene
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 39
- 239000006260 foam Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title abstract description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000011787 zinc oxide Substances 0.000 claims abstract description 31
- 239000000243 solution Substances 0.000 claims abstract description 26
- 239000002131 composite material Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000758 substrate Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001338 self-assembly Methods 0.000 claims abstract description 8
- 238000007654 immersion Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 5
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- 238000009413 insulation Methods 0.000 claims abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 14
- 229930064664 L-arginine Natural products 0.000 claims description 13
- 235000014852 L-arginine Nutrition 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- ODKSFYDXXFIFQN-BYPYZUCNSA-N L-arginine Chemical compound OC(=O)[C@@H](N)CCCN=C(N)N ODKSFYDXXFIFQN-BYPYZUCNSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- CDICEJAYYHXMTJ-FHNDMYTFSA-N N[C@@H](CCCNC(N)=N)C(=O)O.[N+](=O)([O-])[O-].[Ag+] Chemical compound N[C@@H](CCCNC(N)=N)C(=O)O.[N+](=O)([O-])[O-].[Ag+] CDICEJAYYHXMTJ-FHNDMYTFSA-N 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- -1 graphite alkene Chemical class 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003086 colorant Substances 0.000 claims 1
- 229910021389 graphene Inorganic materials 0.000 abstract description 20
- 239000004475 Arginine Substances 0.000 abstract 3
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 abstract 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract 2
- 239000011592 zinc chloride Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 239000002135 nanosheet Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 229910001923 silver oxide Inorganic materials 0.000 description 3
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000002079 cooperative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000004531 microgranule Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical compound CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 125000002059 L-arginyl group Chemical group O=C([*])[C@](N([H])[H])([H])C([H])([H])C([H])([H])C([H])([H])N([H])C(=N[H])N([H])[H] 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8953—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- B01J35/33—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
Abstract
The invention provides a kind of method that green prepares Ag-ZnO grapheme foam nickel material.Mainly comprise the following steps that：1. a layer graphene is grown on nickel foam substrate with chemical vapour deposition technique (CVD), prepare three-dimensional graphene foam Ni substrate；2. by ZnCl2It is dissolved in deionized water with ammonia and is sufficiently stirred for, and mixed solution is transferred in ptfe autoclave, in the three-dimensional graphene foam Ni substrate immersion solution prepared, reactor is positioned in drying baker in 100 DEG C of 150 DEG C of 1 3hrs of insulation；3. silver nitrate and L arginine are made into silver-colored arginine solution with certain molar concentration rate, then Zinc Oxide grapheme foam nickel composite is immersed in silver-colored arginine solution, 12 18hrs of self assembly takes out, deionized water is directly placed in ascorbic acid solution after being cleaned by ultrasonic, take out after 20 50mins and rinse, it is dried, obtains stay-in-grade Ag-ZnO grapheme foam nickel composite material.
Description
Technical field
The present invention relates to prepare silver-ZnO nanometer sheet-Graphene-foam nickel composite material, belong to materials chemistry preparation
Technical field.
Background technology
With Graphene as carrier, with metal-oxide or active substance metallic particles composition composite, both are utilized
Cooperative effect cause composite that there is the performances such as excellent catalysis, electrochemical sensing and gas sensing.Have been carried out at present
The preparation of graphite thiazolinyl composite.Wherein the composite of Graphene and Zinc Oxide is in electrochemical sensor, gas
There has been application well in sensor and antibacterial field.Research finds, on the basis of Zinc Oxide/graphene composite material, then
Modification Nano silver grain, its composite effect are better than simple Zinc Oxide/graphene composite material.At present, to silver/zinc oxide/stone
The preparation of black alkene composite, major part are rested on to Nano silver grain/zinc oxide nano rod/two-dimensional graphene film composite material
In the research of material, the research to silver/zinc oxide nanometer sheet/three-dimensional graphene composite material is rarely reported.Additionally, to nano grain of silver
The preparation of son/zinc oxide nano rod/two-dimensional graphene film composite material, has used substantial amounts of poisonous hazardous chemical on raw material
Reagent, mainly uses the silver ion that irradiation method reduction is attached on zinc oxide nano rod so that the Yin Na of acquisition in technique
Rice corpuscles are all wayward in size and distribution.The silver ion that can be reduced simultaneously is little, and the combination of nano oxidized rod
Also it is insecure so that Nano silver grain is easy to loss in the application, causes the drop that declines of performance.Additionally, utilize in this method
Chemical reagent L-Arginine, which primarily serves the effect of bridging agent as the important component part in protein, and concentrating at present should
For biomedical sector, the application in materials chemistry technology of preparing is extremely rare, its as green bridging agent urgently by
Use well.And in response to the demand of environmental protection, green prepares the composite with good electrochemical properties
Method be also urgently found.
The content of the invention
Technical problem：It is an object of the invention to provide one kind prepares silver-ZnO nanometer sheet-Graphene/nickel foam being combined
Hydro-thermal method and local reduction way are combined by the method for material, the method, prepare homoepitaxial in stone with simple hydro-thermal reaction
The Zinc oxide nano sheet on black alkene/foam nickel base surface, and with Zinc oxide nano sheet as platform, using poisonous material L-Arginine
Go out size and distribution all uniform spherical silver in Zinc oxide nano sheet surface reduction as bridging agent and reducing agent with ascorbic acid
Microgranule.This method low cost, simple to operate, efficiency high, can stablize prepare in a large number.
Technical scheme：A kind of silver-ZnO nanometer sheet-Graphene-foam nickel composite material of preparing of the present invention
Method, comprises the following steps：
A. the preparation of Graphene-nickel foam：Nickel foam is adopted for substrate, substrate cleans 10- with EtOH Sonicate first
15mins, then deionized water be cleaned by ultrasonic 10-15mins, with the debris of this nickel surface that defoams；Treat that nickel foam is dried
After be put into evacuation in tube furnace, be passed through argon 100-200sccm and hydrogen 100-200sccm, with 10 DEG C -20 DEG C/mins's
Speed is warming up to 800 DEG C -1200 DEG C, and the 20-30mins that anneals at this temperature；CH is passed through during growth Graphene410-20sccm
And H2100-200sccm, disconnects CH after growth 10-15min4, and fast cooling, wait stove to take out sample after being cooled to room temperature；
B. the preparation of Zinc oxide nano sheet-Graphene-nickel foam：Take the ZnCl of 0.05-1.00mol2It is dissolved in deionized water
In be sufficiently stirred for after, add ammonia stirring, with white precipitate produce, white mixed solution is obtained after stirring；Subsequently
White mixed solution is transferred in ptfe autoclave, by the foamy graphite prepared alkene-nickel immersion solution, is reacted
Kettle is positioned over 100 DEG C of -140 DEG C of insulation 1-3hrs of vacuum drying oven, and question response kettle is cooled to room temperature, sample is taken out and is rinsed, does
It is dry；
C. the configuration of silver nitrate-arginine mixed liquor：The molar concentration rate of silver nitrate and L-Arginine is 5:1-5:4, match somebody with somebody
The L-Arginine solution that concentration is 8-10mmol/L is put, and with the sodium hydroxide solution that mass concentration is 20%, its pH value is adjusted for 9-
11；It is reconfigured at the silver nitrate solution that concentration is 20-25mmol/L；Then L-Arginine solution is added drop-wise in silver nitrate solution,
With a small amount of white precipitate, 5-10mins is stirred for；
D. self assembly:In silver nitrate-arginine that Zinc oxide nano sheet-foamy graphite alkene/nickel immersion is newly configured, lucifuge
Stand 10-18hrs；
E. in-situ reducing silver particles：The sample of self assembly 12-18hrs is taken out, deionized water is cleaned by ultrasonic 10-20s
Afterwards, sample is directly placed in the ascorbic acid solution that concentration is 100-200mmol/L, takes out after 30-60min and rinse, drying.
Beneficial effect：Using the present invention, on the one hand can be existed with the graphene-based active metal particles composite of effectively solving
Do not fall off during in application process, metallic is exposed to applied environment as far as possible so that affecting its performance and used life
Problem；On the other hand the synthesis of Graphene, Zinc Oxide and silver-colored microgranule three's performance is also achieved, which is given full play to each excellent
Electricity, catalysis and sense etc. performance cooperative effect.In addition, in the preparation of composite, we select not removing skeleton
Foamy graphite alkene/nickel be substrate, this is done because：First, this two-dimensional material macro strength of Graphene is low, is removing base
Situations such as behind bottom easily there is Collapse Deformation or even rupture in Graphene；Second, for removing the shifting process of substrate to operator's
Technology and skill requirement are all very high, and process is lengthy and jumbled, are unfavorable for realizing producing in enormous quantities；3rd, during substrate is removed
Some toxic chemicals can be used, not only bad for Environmental security, impurity also can be introduced in Graphene；4th, remove substrate
Graphene is very light afterwards, and with hydrophobic characteristic, so still need in follow-up test and application process plus substrate, this
Sample causes technique more loaded down with trivial details, and cost of manufacture is improved；5th, retain foam nickel skeleton Graphene is not lost as silver/oxygen
Change the advantage of zinc nanometer sheet carrier, this is in merely by the use of nickel foam as the contrast test of substrate just as can be seen that only utilizing
Simple nickel foam can not prepare the complex of satisfactory texture, and it is relevant that this may have fold with graphenic surface.It is heavier
What is wanted is to make use of L-Arginine in experiment, as a kind of common aminoacid, its molecular structure, CHARGE DISTRIBUTION and is formed many
The ability of deuterium bond so that it can be combined with the molecule with negative charge, and this is advantageous for its self assembly with n-type semiconductor
On the Zinc oxide nano sheet of characteristic；L-Arginine has good associativity with metal ion simultaneously, is particularly combined with silver ion
Property is more preferable.Graphene is achieved that so, the effective and stable combination of Zinc Oxide and silver-colored three, and by silver nitrate-essence
The regulation and control of propylhomoserin solution concentration can realize the regulation and control to silver particles size.In the method, by hydro-thermal method and local reduction way
Combine, process is simple is easy to operate, not high to technical requirements, it is easy to accomplish, environmental pollution is little, is silver/zinc oxide nanometer
The preparation of piece-Graphene-foam nickel composite material provides a kind of effective ways.
Description of the drawings
Fig. 1 is silver-ZnO nanometer sheet-Graphene-foam nickel composite preparation principle figure.
Fig. 2 is Zinc oxide nano sheet-Graphene-foam nickel composite.
Fig. 3 is silver-ZnO nanometer sheet-Graphene-foam nickel composite.
Specific embodiment
A. the preparation of Graphene-nickel foam：Nickel foam is adopted for substrate（Surface density is 200～400g1m-2, thickness is 1-
5mm, size are 2-10cm2）, substrate cleans 10-15mins first with EtOH Sonicate, and then deionized water is cleaned by ultrasonic 10-
15mins, with the debris of this nickel surface that defoams.Evacuation in tube furnace is put into after nickel foam drying, Ar is passed through（100-
200sccm）And H2（100-200sccm）, 800 DEG C -1200 DEG C are warming up to the speed of 10 DEG C -20 DEG C/mins, and in this temperature
Lower annealing 20-30mins.CH is passed through during growth Graphene4（10-20sccm）And H2(100-200sccm) after, growing 10-15min
Disconnect CH4, and 20-30min fast coolings, wait stove to take out sample after being cooled to room temperature；
B. the preparation of Zinc oxide nano sheet-Graphene-nickel foam：Take the ZnCl of 0.05-1.00mol2It is dissolved in 20-50ml to go
After being sufficiently stirred in ionized water, the stirring of 2-5ml ammonia is added, is produced with white precipitate, white is obtained after stirring mixed
Close solution；Subsequently white mixed solution is transferred in the ptfe autoclave of 50ml, by the Graphene/foam prepared
In nickel immersion solution, reactor is positioned over 100 DEG C of -140 DEG C of insulation 1-3hrs of vacuum drying oven, and question response kettle is cooled to room temperature,
Sample is taken out and is rinsed, be dried；
C. the configuration of silver nitrate-arginine mixed liquor：The molar concentration rate of silver nitrate and L-Arginine is 5:1-5:4, match somebody with somebody
Put the L-Arginine solution of 10-40ml（Concentration is 8-10mmol/L）, add a certain amount of sodium hydroxide（Mass concentration is 20%）It is molten
Liquid, adjusts its pH value for 9-11；It is reconfigured at 30ml silver nitrate solutions（Concentration is 20-25mmol/L）；Then it is L-Arginine is molten
Drop is added in silver nitrate solution, with a small amount of white precipitate, is stirred for 5-10mins；
D. self assembly:In silver nitrate-arginine that Zinc oxide nano sheet-foamy graphite alkene-nickel immersion is newly configured, lucifuge
Stand 12-18hrs；
E. in-situ reducing silver particles：The sample of self assembly 12-18hrs is taken out, deionized water is cleaned by ultrasonic 10-20s
Afterwards, sample is directly placed into the ascorbic acid solution of 20-60ml（Concentration is 100-200mmol/L）In, take out after 30-60min
Rinse, drying.
The preferred forms of the present invention are the foregoing is only, protection scope of the present invention with above-mentioned embodiment is not
Limit, as long as the equivalence changes made according to content of the present invention by those skilled in the art, remembers in should all including claims
In the protection domain of load.
Claims (1)
1. a kind of method that green prepares silver-ZnO nanometer sheet-Graphene-foam nickel composite material, it is characterised in that the party
Method is comprised the following steps：
A. the preparation of Graphene-nickel foam：Nickel foam is adopted for substrate, substrate cleans 10-15 mins first with EtOH Sonicate,
Then deionized water is cleaned by ultrasonic 10-15 mins, with the debris of this nickel surface that defoams；It is put into after nickel foam drying
Evacuation in tube furnace, is passed through argon 100-200sccm and hydrogen 100-200sccm, with the speed liter of 10 DEG C -20 DEG C/mins
Temperature is to 800 DEG C -1200 DEG C, and the 20-30 mins that anneal at this temperature；CH is passed through during growth Graphene410-20sccm and H2
100-200sccm, disconnects CH after growth 10-15min4, and fast cooling, wait stove to take out sample after being cooled to room temperature；
B. the preparation of Zinc oxide nano sheet-Graphene-nickel foam：Take the ZnCl of 0.05-1.00mol2Fill in being dissolved in deionized water
After dividing stirring, ammonia stirring is added, is produced with white precipitate, after stirring, is obtained white mixed solution；Subsequently will be white
Mixture of colours solution is transferred in ptfe autoclave, and by the foamy graphite prepared alkene-nickel immersion solution, reactor is put
100 DEG C of -140 DEG C of insulation 1-3hrs of vacuum drying oven are placed in, question response kettle is cooled to room temperature, sample is taken out and is rinsed, is dried；
C. the configuration of silver nitrate-arginine mixed liquor：The molar concentration rate of silver nitrate and L-Arginine is 5:1-5:4, configure dense
The L-Arginine solution for 8-10mmol/L is spent, and with the sodium hydroxide solution that mass concentration is 20%, its pH value is adjusted for 9-11；
It is reconfigured at the silver nitrate solution that concentration is 20-25mmol/L；Then L-Arginine solution is added drop-wise in silver nitrate solution, it is adjoint
A small amount of white precipitate, is stirred for 5-10mins；
D. self assembly:By in the silver nitrate-arginine of Zinc oxide nano sheet-foamy graphite alkene/new configuration of nickel immersion, lucifuge stands
10-18hrs；
E. in-situ reducing silver particles：The sample of self assembly 12-18hrs is taken out, after deionized water is cleaned by ultrasonic 10-20s, will
Sample is directly placed in the ascorbic acid solution that concentration is 100-200mmol/L, takes out and rinse after 30-60min, drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610937856.0A CN106540711A (en) | 2016-10-25 | 2016-10-25 | A kind of method that green prepares Ag-ZnO grapheme foam nickel material |
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|---|---|---|---|
| CN201610937856.0A CN106540711A (en) | 2016-10-25 | 2016-10-25 | A kind of method that green prepares Ag-ZnO grapheme foam nickel material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245597A (en) * | 2017-05-31 | 2017-10-13 | 东南大学 | A kind of method of quick preparation silver nanoparticle purpose square graphite alkene foam nickel composite material |
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| CN107644744A (en) * | 2017-08-08 | 2018-01-30 | 东南大学 | A kind of method for preparing flower-shaped copper nano-cluster grapheme foam nickel material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107245597A (en) * | 2017-05-31 | 2017-10-13 | 东南大学 | A kind of method of quick preparation silver nanoparticle purpose square graphite alkene foam nickel composite material |
| CN107245597B (en) * | 2017-05-31 | 2019-03-12 | 东南大学 | A kind of method of quick preparation silver nanoparticle side-graphene-foam nickel composite material |
| CN107354336A (en) * | 2017-07-14 | 2017-11-17 | 东南大学 | A kind of preparation method of golden redox graphene foam nickel composite material |
| CN107354336B (en) * | 2017-07-14 | 2019-02-05 | 东南大学 | A kind of preparation method of gold-redox graphene-foam nickel composite material |
| CN107644744A (en) * | 2017-08-08 | 2018-01-30 | 东南大学 | A kind of method for preparing flower-shaped copper nano-cluster grapheme foam nickel material |
| CN107644744B (en) * | 2017-08-08 | 2019-07-12 | 东南大学 | A method of preparing flower-shaped copper nano-cluster-graphene-foam nickel material |
| CN107570174A (en) * | 2017-09-30 | 2018-01-12 | 大连理工大学 | A kind of preparation method and application of efficient stable nickel foam base optic catalytic material |
| CN107570174B (en) * | 2017-09-30 | 2020-01-10 | 大连理工大学 | Preparation method and application of efficient and stable foam nickel-based photocatalytic material |
| CN113173616A (en) * | 2021-04-25 | 2021-07-27 | 中国海洋大学 | Three-dimensional integrated photo-thermal conversion material and preparation method thereof |
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