CN103466611A - Method for preparing graphene load nano silver-nickel alloy composite powder materials - Google Patents
Method for preparing graphene load nano silver-nickel alloy composite powder materials Download PDFInfo
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Abstract
The invention relates to a method for preparing graphene load nano silver-nickel alloy composite powder materials. The method aims to solve the problems that graphene load nano silver-nickel alloy composite materials prepared in the prior art are nonuniform in scattering and poor in chemical stability. The method comprises the first step of intercalation and expansion, the second step of stripping and the third step of the preparation of the graphene load nano silver-nickel alloy composite powder materials. Oxidized graphene is prepared through an oxidation-reduction method, then the oxidized graphene, silver ions and nickel ions are mixed and restored through reducing agents to obtain the graphene nano silver-nickel alloy composite materials, the method is simple and fast, any surface dressing agent does not need to be added, and alloy particles on the surface of the graphene are uniform in distribution and stable in chemical performance. The method is used for preparing the graphene load nano silver-nickel alloy composite powder materials.
Description
Technical field
The present invention relates to the preparation method of graphene-supported nanometer silver nickelalloy matrix material.
Background technology
Graphene is a kind of carbonaceous novel material of the tightly packed one-tenth individual layer of carbon atom bi-dimensional cellular shape crystalline network, and the thickness of this graphite crystal film only has 0.335nm, is regarded as " in universe the thinnest material ", has huge application potential.Graphene is as Nano filling, and Nano filling that may be more traditional than other is more outstanding, because it has high specific surface area, thermal conductivity and electroconductibility, electromagnetic shielding ability, snappiness, transparency and low thermal expansivity.Simultaneously, the Nanoalloy material also is subject to primary study due to himself specific function and the good character that shows at aspects such as electricity, catalysis, corrosion stabilities.Nano composite material both can possess each species specificity of nano material, also can possess premium properties complementary between inorganics and organism, combining the plurality of advantages of metal, matrix material and nano material, is the extremely valuable new function material in the world today.
The preparation of Graphene mainly contains physical method and chemical process.It is raw material that physical method normally be take cheap graphite or expanded graphite, by the direct stripping method of micromechanics stripping method, liquid phase or gas phase, prepares Graphene, and this method raw material is easy to get, simple to operate, synthetic Graphene purity is high, defect is few, but time-consuming, productive rate is low, is unsuitable for scale operation.And laboratory mainly prepares Graphene by chemical process, constantly explore and improve through people, oxidation-reduction method is the method for tool potentiality and the synthesizing graphite alkene of development prospect and material thereof at present.
At present, the graphene-supported nanometer silver nickelalloy matrix material that prepared by prior art exists and disperses problem inhomogeneous, poor chemical stability.
Summary of the invention
The present invention will solve graphene-supported nanometer silver nickelalloy matrix material prepared by prior art and exist and disperse problem inhomogeneous, poor chemical stability, and the preparation method of graphene-supported nanometer silver nickelalloy composite powder material is provided.
The preparation method of graphene-supported nanometer silver nickelalloy composite powder material, specifically carry out according to following steps:
One, Graphite Powder 99 is mixed with the vitriol oil, the ice-water bath of then putting into temperature and be 0 ℃～4 ℃ stirs 30min, obtains mixing solutions, and wherein, the quality of Graphite Powder 99 is 1g～1.5g, and the volume of the vitriol oil is 50mL;
Two, under the ice-water bath condition that is 0 ℃～4 ℃ in temperature, SODIUMNITRATE and potassium permanganate are joined in the mixing solutions that step 1 obtains successively, stir 2h, then under normal temperature condition, stir 1h, then be to react 10h under 35 ℃ of water bath condition in temperature, then add distilled water, add again hydrogen peroxide to mixing solutions to be golden yellow, then add dilute sulphuric acid, carry out after cooling centrifugal, put into again the semi-permeable membranes dialysis and process to neutral, then the ultrasonic dissolution concentration colloidal sol that is 0.01g/mL; Wherein the quality of SODIUMNITRATE is 1.5g, and the quality of potassium permanganate is 10g, and the volume of distilled water is 400mL～500mL, and the volume of dilute sulphuric acid is 10mL;
Three, silver nitrate solution is mixed with nickel sulfate solution, the colloidal sol that adds again step 2 to obtain mixes, supersound process 1h, then add NaOH solution under agitation condition, then add hydrazine hydrate solution, under the ice-water bath condition that is 70 ℃ in temperature again, controlling stirring velocity is 300r/min reaction 30min, obtains product, carry out drying by after the product washing, putting into vacuum drying oven, obtain graphene-supported nanometer silver nickelalloy composite powder material through grinding, wherein, AgNO in silver nitrate solution
3quality be 0.8g～1.2g, distilled water volume is 25mL, NiSO in nickel sulfate solution
46H
2the volume that the quality of O is 3g～4g, distilled water is 10mL, and the volume of the colloidal sol that step 2 obtains is 35mL, and the volume of NaOH solution is 15mL, and the volume of hydrazine hydrate solution is 10mL.
The present invention adopts oxidation-reduction method to prepare graphene oxide exactly, again Graphene is mixed with silver ions and nickel ion by the reductive agent reduction and obtain graphene nano silver-nickel matrix material, this method is simple, quick, need not add any coating materials, Graphene surface alloy particle distribution is even, stable chemical performance.
The invention has the beneficial effects as follows:
1, this method is simple, quick, does not need to add any coating materials;
2, utilize reduction method to make to load on the Nanoalloy particle on Graphene, good dispersion, size uniform, particle diameter is less;
3, hydrazine hydrate is that reductive agent can generate nitrogen to protect the Nanoalloy particle not oxidized, without side reaction;
4, utilize the method for graphene oxide reduction can make to be connected with chemical bond between Graphene after reduction and Nanoalloy particle, its chemical property is also more stable;
Even 5 have no the relevant report for preparing graphene-supported nanometer silver nickelalloy composite powder material by reduction method.
The present invention is for the preparation of graphene-supported nanometer silver nickelalloy composite powder material.
The accompanying drawing explanation
The XRD figure of the graphene-supported nanometer silver nickelalloy composite powder material that Fig. 1 is embodiment mono-preparation;
The SEM figure of the graphene-supported nanometer silver nickelalloy composite powder material that Fig. 2 is embodiment mono-preparation.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of the graphene-supported nanometer silver nickelalloy of present embodiment composite powder material, specifically carry out according to following steps:
One, Graphite Powder 99 is mixed with the vitriol oil, the ice-water bath of then putting into temperature and be 0 ℃～4 ℃ stirs 30min, obtains mixing solutions, and wherein, the quality of Graphite Powder 99 is 1g～1.5g, and the volume of the vitriol oil is 50mL;
Two, under the ice-water bath condition that is 0 ℃～4 ℃ in temperature, SODIUMNITRATE and potassium permanganate are joined in the mixing solutions that step 1 obtains successively, stir 2h, then under normal temperature condition, stir 1h, then be to react 10h under 35 ℃ of water bath condition in temperature, then add distilled water, add again hydrogen peroxide to mixing solutions to be golden yellow, then add dilute sulphuric acid, carry out after cooling centrifugal, put into again the semi-permeable membranes dialysis and process to neutral, then the ultrasonic dissolution concentration colloidal sol that is 0.01g/mL; Wherein the quality of SODIUMNITRATE is 1.5g, and the quality of potassium permanganate is 10g, and the volume of distilled water is 400mL～500mL, and the volume of dilute sulphuric acid is 10mL;
Three, silver nitrate solution is mixed with nickel sulfate solution, the colloidal sol that adds again step 2 to obtain mixes, supersound process 1h, then add NaOH solution under agitation condition, then add hydrazine hydrate solution, under the ice-water bath condition that is 70 ℃ in temperature again, controlling stirring velocity is 300r/min reaction 30min, obtains product, carry out drying by after the product washing, putting into vacuum drying oven, obtain graphene-supported nanometer silver nickelalloy composite powder material through grinding, wherein, AgNO in silver nitrate solution
3quality be 0.8g～1.2g, distilled water volume is 25mL, NiSO in nickel sulfate solution
46H
2the volume that the quality of O is 3g～4g, distilled water is 10mL, and the volume of the colloidal sol that step 2 obtains is 35mL, and the volume of NaOH solution is 15mL, and the volume of hydrazine hydrate solution is 10mL.
Embodiment two: present embodiment is different from embodiment one: in step 1, the quality of Graphite Powder 99 is 1.2g.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one: in step 2, the mass concentration of dilute sulphuric acid is 30%.Other is identical with embodiment one.
Embodiment four: present embodiment is different from embodiment one: in step 2, the volume of distilled water is 420mL～480mL.Other is identical with embodiment one.
Embodiment five: present embodiment is different from embodiment one: in step 3, the temperature of vacuum drying oven is 40 ℃.Other is identical with embodiment one.
Embodiment six: present embodiment is different from embodiment one: AgNO in silver nitrate solution in step 3
3quality be 1.0g.Other is identical with embodiment one.
Embodiment seven: present embodiment is different from embodiment one: NiSO in nickel sulfate solution in step 3
46H
2the quality of O is 3.2g～3.8g.Other is identical with embodiment one.
Embodiment eight: present embodiment is different from embodiment one: in step 3, the concentration of NaOH solution is 0.5mol/L.Other is identical with embodiment one.
Embodiment nine: present embodiment is different from embodiment one: in step 3, the mass concentration of hydrazine hydrate solution is 80%.Other is identical with embodiment one.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment mono-:
The preparation method of the graphene-supported nanometer silver nickelalloy of the present embodiment composite powder material, specifically carry out according to following steps:
One, Graphite Powder 99 is mixed with the vitriol oil, the ice-water bath of then putting into temperature and be 0 ℃～4 ℃ stirs 30min, obtains mixing solutions, and wherein, the quality of Graphite Powder 99 is 1.2g, and the volume of the vitriol oil is 50mL;
Two, under the ice-water bath condition that is 0 ℃～4 ℃ in temperature, SODIUMNITRATE and potassium permanganate are joined in the mixing solutions that step 1 obtains successively, stir 2h, then under normal temperature condition, stir 1h, then be to react 10h under 35 ℃ of water bath condition in temperature, then add distilled water, add again hydrogen peroxide to mixing solutions to be golden yellow, then add dilute sulphuric acid, carry out after cooling centrifugal, put into again the semi-permeable membranes dialysis and process to neutral, then the ultrasonic dissolution concentration colloidal sol that is 0.01g/mL; Wherein the quality of SODIUMNITRATE is 1.5g, and the mass concentration of dilute sulphuric acid is 30%, and the quality of potassium permanganate is 10g, and the volume of distilled water is 450mL, and the volume of dilute sulphuric acid is 10mL;
Three, silver nitrate solution is mixed with nickel sulfate solution, the colloidal sol that adds again step 2 to obtain mixes, supersound process 1h, add again NaOH solution under agitation condition, then add hydrazine hydrate solution, under the ice-water bath condition that is 70 ℃ in temperature again, controlling stirring velocity is 300r/min reaction 30min, obtain product, carry out drying by after the product washing, putting into the vacuum drying oven that temperature is 40 ℃, obtain graphene-supported nanometer silver nickelalloy composite powder material through grinding, wherein, AgNO in silver nitrate solution
3quality be 1.0g, distilled water volume is 25mL, NiSO in nickel sulfate solution
46H
2the volume that the quality of O is 3.5g, distilled water is 10mL, and the volume of the colloidal sol that step 2 obtains is 35mL, and the volume of NaOH solution is that 15mL, concentration are 0.5mol/L, and the volume of hydrazine hydrate solution is that 10mL, mass concentration are 80%.
The XRD figure of graphene-supported nanometer silver nickelalloy composite powder material prepared by the present embodiment as shown in Figure 1; The SEM figure of graphene-supported nanometer silver nickelalloy composite powder material prepared by the present embodiment as shown in Figure 2.
Claims (9)
1. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material is characterized in that specifically according to following steps, carrying out the preparation method of graphene-supported nanometer silver nickelalloy composite powder material:
One, Graphite Powder 99 is mixed with the vitriol oil, the ice-water bath of then putting into temperature and be 0 ℃～4 ℃ stirs 30min, obtains mixing solutions, and wherein, the quality of Graphite Powder 99 is 1g～1.5g, and the volume of the vitriol oil is 50mL;
Two, under the ice-water bath condition that is 0 ℃～4 ℃ in temperature, SODIUMNITRATE and potassium permanganate are joined in the mixing solutions that step 1 obtains successively, stir 2h, then under normal temperature condition, stir 1h, then be to react 10h under 35 ℃ of water bath condition in temperature, then add distilled water, add again hydrogen peroxide to mixing solutions to be golden yellow, then add dilute sulphuric acid, carry out after cooling centrifugal, put into again the semi-permeable membranes dialysis and process to neutral, then the ultrasonic dissolution concentration colloidal sol that is 0.01g/mL; Wherein the quality of SODIUMNITRATE is 1.5g, and the quality of potassium permanganate is 10g, and the volume of distilled water is 400mL～500mL, and the volume of dilute sulphuric acid is 10mL;
Three, silver nitrate solution is mixed with nickel sulfate solution, the colloidal sol that adds again step 2 to obtain mixes, supersound process 1h, then add NaOH solution under agitation condition, then add hydrazine hydrate solution, under the ice-water bath condition that is 70 ℃ in temperature again, controlling stirring velocity is 300r/min reaction 30min, obtains product, carry out drying by after the product washing, putting into vacuum drying oven, obtain graphene-supported nanometer silver nickelalloy composite powder material through grinding, wherein, AgNO in silver nitrate solution
3quality be 0.8g～1.2g, distilled water volume is 25mL, NiSO in nickel sulfate solution
46H
2the volume that the quality of O is 3g～4g, distilled water is 10mL, and the volume of the colloidal sol that step 2 obtains is 35mL, and the volume of NaOH solution is 15mL, and the volume of hydrazine hydrate solution is 10mL.
2. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, the quality that it is characterized in that Graphite Powder 99 in step 1 is 1.2g.
3. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, the mass concentration that it is characterized in that dilute sulphuric acid in step 2 is 30%.
4. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, the volume that it is characterized in that distilled water in step 2 is 420mL～480mL.
5. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, the temperature that it is characterized in that vacuum drying oven in step 3 is 40 ℃.
6. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, is characterized in that in step 3 AgNO in silver nitrate solution
3quality be 1.0g.
7. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, is characterized in that in step 3 NiSO in nickel sulfate solution
46H
2the quality of O is 3.2g～3.8g.
8. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, the concentration that it is characterized in that NaOH solution in step 3 is 0.5mol/L.
9. the preparation method of graphene-supported nanometer silver nickelalloy composite powder material according to claim 1, the mass concentration that it is characterized in that hydrazine hydrate solution in step 3 is 80%.
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| CN103920497A (en) * | 2014-04-02 | 2014-07-16 | 北京化工大学 | Preparation method of graphene-loaded ultrathin metal sheet with atomic-scale thickness |
| CN105047243A (en) * | 2015-06-08 | 2015-11-11 | 黑龙江大学 | Preparation method of polyaniline-clad graphene nanometer silver-nickel alloy |
| CN105081310A (en) * | 2015-08-31 | 2015-11-25 | 哈尔滨理工大学 | Method for preparing grapheme reinforced aluminum matrix composite material |
| CN105203619A (en) * | 2015-10-30 | 2015-12-30 | 黑龙江大学 | Method for detecting p-nitrophenol with graphene/nano silver-nickel alloy as electrode |
| CN105779801A (en) * | 2016-04-08 | 2016-07-20 | 上海和伍复合材料有限公司 | Graphene enhanced silver nickel electric contact composite material and preparation method thereof |
| CN106363190A (en) * | 2016-09-18 | 2017-02-01 | 东莞市中合金科技有限公司 | Silver-nickel-graphene alloy material and preparation method thereof |
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| CN103920497A (en) * | 2014-04-02 | 2014-07-16 | 北京化工大学 | Preparation method of graphene-loaded ultrathin metal sheet with atomic-scale thickness |
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| CN105203619A (en) * | 2015-10-30 | 2015-12-30 | 黑龙江大学 | Method for detecting p-nitrophenol with graphene/nano silver-nickel alloy as electrode |
| CN105779801A (en) * | 2016-04-08 | 2016-07-20 | 上海和伍复合材料有限公司 | Graphene enhanced silver nickel electric contact composite material and preparation method thereof |
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| CN111099583A (en) * | 2018-10-26 | 2020-05-05 | 南京化学工业园环保产业协同创新有限公司 | Efficient composite synthesis method of graphene and nano-silver |
| CN111099583B (en) * | 2018-10-26 | 2022-04-29 | 南京化学工业园环保产业协同创新有限公司 | Efficient composite synthesis method of graphene and nano-silver |
| CN110814358A (en) * | 2019-11-15 | 2020-02-21 | 桂林电子科技大学 | Preparation method and application of Ag-Cu nano alloy with blood sugar detection characteristic |
| CN110814358B (en) * | 2019-11-15 | 2022-08-30 | 桂林电子科技大学 | Preparation method and application of Ag-Cu nano alloy with blood sugar detection characteristic |
| CN113394419A (en) * | 2021-07-08 | 2021-09-14 | 深圳职业技术学院 | Synthesis method of noble metal electrocatalyst for proton exchange membrane fuel cell |
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