CN103540786A - Preparation method of graphene/copper-nickel nano composite material - Google Patents
Preparation method of graphene/copper-nickel nano composite material Download PDFInfo
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- CN103540786A CN103540786A CN201310528409.6A CN201310528409A CN103540786A CN 103540786 A CN103540786 A CN 103540786A CN 201310528409 A CN201310528409 A CN 201310528409A CN 103540786 A CN103540786 A CN 103540786A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 60
- 229910000570 Cupronickel Inorganic materials 0.000 title claims abstract description 35
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 25
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 150000002815 nickel Chemical class 0.000 claims abstract description 14
- 150000001879 copper Chemical class 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims abstract description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 5
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 16
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000012756 surface treatment agent Substances 0.000 claims description 6
- 239000002086 nanomaterial Substances 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 4
- 239000003637 basic solution Substances 0.000 claims description 4
- 239000004567 concrete Substances 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 239000008204 material by function Substances 0.000 abstract description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 abstract 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
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Abstract
The invention belongs to the technical field of nano inorganic functional materials, and relates to a preparation method of a graphene/copper-nickel nano composite material. The preparation method comprises the following steps: first, placing graphene oxide in deionized water for ultrasonic centrifugation to obtain a graphene suspension; then, dissolving sodium hydroxide in deionized water to prepare alkaline liquor; then, respectively dissolving copper salt and nickel salt in deionized water, stirring till copper salt and nickel salt are fully dissolved, and preparing copper salt and nickel salt liquor; placing the prepared alkaline liquor, and copper salt and nickel salt liquor in a flask to uniformly stir, and adding ethanediamine, hydrazine hydrate and a surface treating agent to stir, and then adding into the graphene suspension for reaction; cleaning, centrifugalizing and drying products obtained by reaction for 2-3 hours to obtain the graphene/copper-nickel nano composite material. The graphene/copper-nickel nano composite material is simple in preparation process, convenient to operate, low in cost, environment-friendly and easy for production on a large scale.
Description
Technical field:
The invention belongs to nano inorganic functional materials preparing technical field, the preparation method who relates to a kind of Graphene/copper nickel nano composite material, both made full use of the premium properties of Graphene, and again in conjunction with the electro permanent magnetic of copper nickel metallic substance, made this matrix material there is absorption of electromagnetic wave performance.
Background technology:
Along with scientific and technical development, various electronic products are day by day universal in daily life, consequent electromagnetic radiation and electromagnetic pollution are extensively present in people's surroundings, greatly affected people's life, therefore in the urgent need to preparing the electromagnetic wave absorbent material (abbreviation absorbing material) of excellent property, to reduce electromagnetic pollution; Simultaneously, absorbing material will play a significant role in the military trial of strength in countries in the world, in modern war, stealthyization of weaponry can be broken existing attacking and defending general layout, improves viability and the fighting efficiency of weapon, for example, when multi-section radar or communication equipment are used simultaneously, between each equipment, can produce signal and disturb, in equipment surface, apply electromagnetic wave absorbent material and can reduce interference, improve the performance of each equipment.Therefore the absorbing material that processability is good is aspect civilian or Military Application aspect all has great importance.
In recent years, Graphene had caused scientist's extensive concern because of its unique performance, and the two dimensional crystal structure that single-layer graphene is comprised of six-ring, is a kind of semi-conductor that there is no energy gap, has higher electronic mobility (2 * 10
5cm
2/ V), large specific surface area (2600m
2/ g) and high physical strength (130GPa), therefore Graphene has potential application prospect in nano electron device, gas sensor and prepare composite, aspect electromagnetic absorption, compare with other carbon materials, as carbon nanotube and carbon black, Graphene has larger specific surface area, thereby larger hertzian wave contact area is provided, and is conducive to electromagnetic absorption.At present less at the application report in absorption of electromagnetic wave field about Graphene, and complicated process of preparation, process is loaded down with trivial details.
Summary of the invention:
The object of the invention is to overcome the shortcoming that prior art exists, seeking design provides a kind of preparation method of Graphene/copper nickel composite function nano material, adopt one-step synthesis to reduce cupric ion and nickel ion simultaneously and prepare Graphene/copper nickel nano composite material, both made full use of the premium properties of Graphene, tied again the electro permanent magnetic of copper nickel metallic substance, made this matrix material there is unique absorption of electromagnetic wave performance.
To achieve these goals, concrete preparation process of the present invention is:
(1), adopt existing Hummers method to prepare graphene oxide;
(2), first graphene oxide is placed in to deionized water, ultrasonic 12 hours, and after centrifugal 4 minutes, get supernatant liquid under 8000rpm condition, obtain the graphene suspension that graphene oxide concentration is 0.05g/L～5g/L;
(3), sodium hydroxide being dissolved in to deionized water for stirring to solution clarifies and is cooled to room temperature preparation to obtain pH be 10～13 basic solution again; Then mantoquita and nickel salt are dissolved in respectively to deionized water for stirring to dissolving completely, it is 0.1～1mol/L copper salt solution and nickel salt solution that preparation obtains concentration;
(4) ratio that basic solution, copper salt solution and the nickel salt solution, step (3) preparation being obtained is 30:0.1:0.3 according to volume ratio is placed in flask and stirs, in flask, adding 0.1～1mL weight percent concentration is that 99% quadrol, 0.02～0.5mL weight percent concentration are the graphene suspension that adds step (2) to obtain after 80% hydrazine hydrate and surface treatment agent stir again, continue to stir, under 50～95 ℃ of temperature condition, react 0.5～12h, wherein the mol ratio of surface treatment agent and nickel salt is 3～50:1;
(5), washed with de-ionized water 3-5 time for product that step (4) reaction is obtained, under the condition of 8000 revs/min after centrifugal 5 minutes, put into the baking oven of 60～80 ℃ and be dried and after 2～3 hours, prepare Graphene/copper nickel nano composite material.
The mantoquita the present invention relates to is cupric nitrate or cupric chloride; Nickel salt is nickelous nitrate or nickelous chloride; Surface treatment agent is one or more the combination in urea, hexadecylamine, sodium lauryl sulphate, cetyl trimethylammonium bromide (CTAB), hexamethylenetetramine, polyvinylpyrrolidone (PVP), polyoxyethylene glycol.
The pattern of the copper nickel nano material in Graphene/copper nickel nano composite material prepared by the present invention is linear or spherical, and wherein the diameter of linear copper nickel nanometer is 2～500nm, and length is 5nm～100 μ m; The diameter of spherical copper nickel nanometer is 2nm～1 μ m.
The present invention compared with prior art, by Graphene/copper nickel nano composite material one-step synthesis, reaches object quick, energy-conservation, simple to operate, both can reduce preparation cost, can obtain again the Graphene composite functional material of Load Balanced, good dispersity; Its preparation technology is simple, easy to operate, and cost is low, and environmental friendliness is easy to scale operation.
Accompanying drawing explanation:
Fig. 1 is scanning electronic microscope (SEM) picture of Graphene/copper nickel nano composite material of the embodiment of the present invention 1 preparation.
Fig. 2 is to be X-ray diffraction (XRD) the test curve schematic diagram of Graphene/copper nickel nano composite material of the embodiment of the present invention 1 preparation.
Fig. 3 is the absorbing property test result curve synoptic diagram of Graphene/copper nickel nano composite material of the embodiment of the present invention 1 preparation.
Fig. 4 is scanning electronic microscope (SEM) picture of Graphene/copper nickel nano composite material of the embodiment of the present invention 2 preparations.
Fig. 5 is the absorbing property test result curve synoptic diagram of Graphene/copper nickel nano composite material of the embodiment of the present invention 2 preparations.
Embodiment:
Below by embodiment, be also described further by reference to the accompanying drawings.
Embodiment 1:
The present embodiment be take Xiao Suan Tong ﹑ Xiao Suan Nie ﹑ graphene oxide and is prepared Graphene/copper nickel nano composite material as raw material, and wherein, the pattern of copper nickel nano material is linear; Its concrete preparation process is:
(1), adopt traditional Hummers method to prepare graphene oxide;
(2), 20mg graphene oxide is placed in to 100mL deionized water, ultrasonic 12h, the centrifugal 4min of 8000rpm, get supernatant liquid, supernatant liquid is dispersed individual layer or multilayer graphene oxide preferably, the Graphene of bottom is dried and weighed, and the concentration that draws graphene oxide in supernatant liquid is 0.4g/L;
(3), take 70g sodium hydroxide and be dissolved in deionized water for stirring to solution and clarify, be cooled to room temperature, be mixed with the strong alkali solution that concentration is 7mol/L; Take again 0.6g nitrate trihydrate copper and 0.73g six water nickelous nitrates are dissolved in respectively in deionized water, be stirred to completely and dissolve, be mixed with copper nitrate solution and the 0.5mol/L nickel nitrate solution of 0.5mol/L;
(4), getting 60mL sodium hydroxide solution is put in there-necked flask, getting 0.2mL copper nitrate solution, 0.6mL nickel nitrate solution, 0.6mL quadrol (99wt%) and 0.05mL hydrazine hydrate (80wt%) is put in flask and stirs respectively again, then by concentration, be that 0.4g/L graphene oxide 60mL pours in flask and stirs, being incubated 2h after being warming up to 80 ℃ reacts;
(5), by washed with de-ionized water 3-5 time for the product that obtains, after centrifugation, be positioned in 70 ℃ of baking ovens and be dried 3h, obtain Graphene/copper nickel nano composite powder of black.
Embodiment 2:
The present embodiment be take Xiao Suan Tong ﹑ Xiao Suan Nie ﹑ graphene oxide and is prepared Graphene/copper nickel nano composite material as raw material, and wherein, copper nickel appearance of nano material is spherical; Its concrete preparation process is:
(1), adopt traditional Hummers method to prepare graphene oxide;
(2), 20mg graphene oxide is placed in to 100mL deionized water, ultrasonic 12h, the centrifugal 4min of 8000rpm, get supernatant liquid, supernatant liquid is dispersed individual layer or multilayer graphene oxide preferably, the Graphene of bottom is dried and weighed, and the concentration that calculates graphene oxide in supernatant liquid is 0.4g/L;
(3), take 70g sodium hydroxide and be dissolved in deionized water for stirring to solution and clarify, be cooled to room temperature, preparation becomes the strong alkali solution that concentration is 7mol/L; Take again 0.604g nitrate trihydrate copper and 0.727g six water nickelous nitrates and be dissolved in respectively deionized water for stirring to dissolving completely, be mixed with copper nitrate solution and the 0.5mol/L nickel nitrate solution of 0.5mol/L;
(4), get 60mL sodium hydroxide solution and be put in there-necked flask, 0.2mL copper nitrate solution, 0.6mL nickel nitrate solution, 0.6mL quadrol (99wt%), 0.05mL hydrazine hydrate (80wt%) and 0.43g urea are put in flask and are stirred respectively; By concentration, be that 0.4g/L graphene oxide 60mL pours in flask and stirs again, being incubated 6h after being warming up to 70 ℃ reacts;
(5), by washed with de-ionized water 3-5 time for the product that obtains, after centrifugation, be positioned in 70 ℃ of baking ovens and be dried 3h, obtain Graphene/copper nickel nano composite powder of black.
Claims (3)
1. a preparation method for Graphene/copper nickel nano composite material, is characterized in that concrete preparation process is:
(1), adopt existing Hummers method to prepare graphene oxide;
(2), first graphene oxide is placed in to deionized water, ultrasonic 12 hours, and after centrifugal 4 minutes, get supernatant liquid under 8000rpm condition, obtain the graphene suspension that graphene oxide concentration is 0.05g/L～5g/L;
(3), sodium hydroxide being dissolved in to deionized water for stirring to solution clarifies and is cooled to room temperature preparation to obtain pH be 10～13 basic solution again; Then mantoquita and nickel salt are dissolved in respectively to deionized water for stirring to dissolving completely, it is 0.1～1mol/L copper salt solution and nickel salt solution that preparation obtains concentration;
(4) ratio that basic solution, copper salt solution and the nickel salt solution, step (3) preparation being obtained is 30:0.1:0.3 according to volume ratio is placed in flask and stirs, in flask, adding respectively 0.1～1mL weight percent concentration is that 99% quadrol, 0.02～0.5mL weight percent concentration are the graphene suspension that adds step (2) to obtain after 80% hydrazine hydrate and surface treatment agent stir again, continue to stir, under 50～95 ℃ of temperature condition, react 0.5～12h, wherein the mol ratio of added surface treatment agent and nickel salt is 3～50:1;
(5), washed with de-ionized water 3-5 time for product that step (4) reaction is obtained, under the condition of 8000 revs/min after centrifugal 5 minutes, put into the baking oven of 60～80 ℃ and be dried and after 2～3 hours, prepare Graphene/copper nickel nano composite material.
2. the preparation method of Graphene/copper nickel nano composite material according to claim 1, is characterized in that the mantoquita relating to is cupric nitrate or cupric chloride; Nickel salt is nickelous nitrate or nickelous chloride; Surface treatment agent is one or more the combination in urea, hexadecylamine, sodium lauryl sulphate, cetyl trimethylammonium bromide, hexamethylenetetramine, polyvinylpyrrolidone and polyoxyethylene glycol.
3. the preparation method of Graphene/copper nickel nano composite material according to claim 1, the pattern of the copper nickel nano material in the Graphene/copper nickel nano composite material that it is characterized in that preparing is linear or spherical, wherein the diameter of linear copper nickel nanometer is 2～500nm, and length is 5nm～100 μ m; The diameter of spherical copper nickel nanometer is 2nm～1 μ m.
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| CN104475753A (en) * | 2014-12-29 | 2015-04-01 | 黑龙江大学 | Method for preparing nano Cu3.8 Ni alloy loaded on graphene by liquid phase reduction method |
| CN104569097A (en) * | 2014-12-17 | 2015-04-29 | 浙江理工大学 | Preparation method of copper nanowire graphene composite-modified electrode, as well as applications thereof |
| CN105695788A (en) * | 2016-04-08 | 2016-06-22 | 上海和伍复合材料有限公司 | Graphene strengthening nickel base composite material and preparing method thereof |
| CN105728743A (en) * | 2016-03-16 | 2016-07-06 | 临沂大学 | Preparation method of composite wave absorbing material |
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| CN104569097A (en) * | 2014-12-17 | 2015-04-29 | 浙江理工大学 | Preparation method of copper nanowire graphene composite-modified electrode, as well as applications thereof |
| CN104569097B (en) * | 2014-12-17 | 2018-01-12 | 浙江理工大学 | The preparation method and applications of copper nano-wire graphene complex modified electrode |
| CN104475753B (en) * | 2014-12-29 | 2016-06-29 | 黑龙江大学 | Liquid phase reduction prepares graphene-supported nanometer of Cu3.8The method of Ni alloy |
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