CN101745645B - Preparation method of nano-copper-nickel alloy by liquid phase method - Google Patents
Preparation method of nano-copper-nickel alloy by liquid phase method Download PDFInfo
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- CN101745645B CN101745645B CN2008102097218A CN200810209721A CN101745645B CN 101745645 B CN101745645 B CN 101745645B CN 2008102097218 A CN2008102097218 A CN 2008102097218A CN 200810209721 A CN200810209721 A CN 200810209721A CN 101745645 B CN101745645 B CN 101745645B
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Abstract
The invention relates to a preparation method of a nano-copper-nickel alloy by the liquid phase method. The commonly used preparation method of nano-alloy materials is a mechanical alloying method. The method of the invention comprises the following steps that: at a temperature of 90 DEG C, 40mL of 0.8mol / L nickel acetate / copper sulfate and 1,2 - propylene glycol solution is prepared, and 11.00g oleic acid is dissolved in 40mL of 1,2 -propylene glycol solution; 8.00g NaOH powder is dissolved in 80mL of 1,2 -propylene glycol solution, and the nickel acetate and an anhydrous copper sulfate solution are evenly mixed and then are mixed with an oleic acid solution, and are ultrasonically treated for 20min, and are heated up to 120 DEG C under the protection of nitrogen, then are added with a NaOH solution, are stirred and heated up to 181 DEG C to 182 DEG C at a rotary speed of 300r/min, and reflux for 2.5h; after the end of reaction, the solution is cooled to room temperature, and 50mL ( one fourth of the total volume ) of acetone is added to be settled and centrifugally separated; and distilled water, ethanol and acetone are respectively used to repeatedly wash until the filtrate is colorless, and black alloy powder can be obtained after the vacuum drying for 24h at a temperature of 50 DEG C. The invention is applied to the preparation of nano alloy materials.
Description
Technical field:
The present invention relates to a kind of method of preparation method of nano-copper-nickel alloy by liquid phase.
Background technology:
Nano material is because self specific function and become the commanding elevation of high-tech sector competition is day by day being brought into play the effect that can not be substituted in fields such as novel energy material, ecological environment material nd, functional coating material, high-performance electronic material and novel rare-earth materials.Wherein, the Nanoalloy material shows the character of very good uniqueness at aspects such as electricity, magnetic, corrosion stability, catalysis because its grain size and structure are different from the bulk alloy material, become the research emphasis of field of nanometer material technology in recent years.
The Nanoalloy material preparation method that generally adopts is that mechanical alloying method claims high-energy ball milling method again at present, this method is to utilize the rotation of ball mill or vibrations to make hard sphere carry out strong bump, grinding and stirring to raw material, the metal or alloy powder is pulverized be the method for nano_scale particle.This method efficient is not high, and the gained grain diameter is bigger, and skewness, elemental metals particle content height in the Nanoalloy of preparing.
Summary of the invention:
The method that the purpose of this invention is to provide a kind of preparation method of nano-copper-nickel alloy by liquid phase, the nano-copper-nickel alloy crystal fine particle size of making is even, good dispersion.
Above-mentioned purpose realizes by following technical scheme:
The method of preparation method of nano-copper-nickel alloy by liquid phase; under 90 ℃; nickel acetate/copper sulphate 1 of preparation 0.8mol/L, 2-propylene glycol solution 40mL is dissolved in 40mL 1 with 11.00g oleic acid; in the 2-propylene glycol solution; the NaOH powder of 8.00g is dissolved in 80mL1, in the 2-propylene glycol solution, nickel acetate and anhydrous slufuric acid copper solution is mixed the back mix with oleic acid solutions; ultrasonic 20min; under nitrogen protection, drip NaOH solution after being warming up to 120 ℃, be warming up to 181 ℃～182 ℃ under stirring; rotating speed is 300r/min; the 2.5h that refluxes under this temperature, reaction is cooled to room temperature after finishing; add 50mL (1/4 cumulative volume) acetone sedimentation; distilled water is used in centrifugation respectively; ethanol and acetone washing, repeated washing; colourless until filtrate, obtain the black alloy powder behind 50 ℃ of vacuum drying 24h.
The method of preparation method of nano-copper-nickel alloy by liquid phase, the mol ratio of nickel acetate/copper sulphate are 4.5: 5.5-6.5: 3.5.
This technical scheme has following beneficial effect:
1. among the present invention 1, the 2-propane diols be solvent be again reducing agent, this helps remaining bivalent metal ion and 1,2-propane diols homogeneous phase mixes.The adding of oleic acid can be in solution produces chemical action with bivalent metal ion, can control like this generation alloy particle size and prevent that the alloy particle that generates is oxidized.
2. the present invention reduces cupric and nickel salt and can prevent that the alloy particle that generates is oxidized in nitrogen protection and alkaline environment.Under high-speed stirred and on the abundant mixed base of solution, the size of the alloy particle of 181 ℃～182 ℃ reaction generations is even, good dispersion.
3. the alloy particle XRD spectra of the present invention's preparation conforms to for 09-0205 number fully with standard spectrum chart database JCPDS card, and its alloy particle is the Cu3.8Ni alloy crystal.Chemical method prepares the Cu3.8Ni alloy crystal, and document does not appear in the newspapers.
4. the present invention adopts liquid phase method, is reducing agent with the propane diols, reduction cupric and nickel salt in alkaline environment, synthetic corronil nanocrystal particulate.This alloy nano crystal is Cu3.8Ni, 100nm, sphere after testing, and size is even, good dispersion.
The specific embodiment:
Embodiment 1:
The method of preparation method of nano-copper-nickel alloy by liquid phase; under 90 ℃; nickel acetate/copper sulphate 1 of preparation 0.8mol/L, 2-propylene glycol solution 40mL is dissolved in 40mL 1 with 11.00g oleic acid; in the 2-propylene glycol solution; the NaOH powder of 8.00g is dissolved in 80mL 1, in the 2-propylene glycol solution, nickel acetate and anhydrous slufuric acid copper solution is mixed the back mix with oleic acid solutions; ultrasonic 20min; under nitrogen protection, drip NaOH solution after being warming up to 120 ℃, be warming up to 181 ℃～182 ℃ under stirring; rotating speed is 300r/min; the 2.5h that refluxes under this temperature, reaction is cooled to room temperature after finishing; add 50mL (1/4 cumulative volume) acetone sedimentation; distilled water is used in centrifugation respectively; ethanol and acetone washing, repeated washing; colourless until filtrate, obtain the black alloy powder behind 50 ℃ of vacuum drying 24h.
Embodiment 2:
The method of preparation method of nano-copper-nickel alloy by liquid phase, the mol ratio of nickel acetate/copper sulphate are 4.5: 5.5-6.5: 3.5.
Claims (2)
1. the method for a preparation method of nano-copper-nickel alloy by liquid phase; it is characterized in that: under 90 ℃; nickel acetate/copper sulphate 1 of preparation 0.8mol/L, 2-propylene glycol solution 40mL is dissolved in 40mL 1 with 11.00g oleic acid; in the 2-propylene glycol solution; the NaOH powder of 8.00g is dissolved in 80mL 1, in the 2-propylene glycol solution, nickel acetate and anhydrous slufuric acid copper solution is mixed the back mix with oleic acid solutions; ultrasonic 20min; under nitrogen protection, drip NaOH solution after being warming up to 120 ℃, be warming up to 181 ℃～182 ℃ under stirring; rotating speed is 300r/min; the 2.5h that refluxes under this temperature, reaction is cooled to room temperature after finishing; add the i.e. acetone sedimentation of 1/4 cumulative volume of 50mL; distilled water is used in centrifugation respectively; ethanol and acetone washing, repeated washing; colourless until filtrate, obtain the black alloy powder behind 50 ℃ of vacuum drying 24h.
2. the method for preparation method of nano-copper-nickel alloy by liquid phase according to claim 1, it is characterized in that: the mol ratio of nickel acetate/copper sulphate is 4.5: 5.5-6.5: 3.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2008102097218A CN101745645B (en) | 2008-12-17 | 2008-12-17 | Preparation method of nano-copper-nickel alloy by liquid phase method |
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| CN2008102097218A CN101745645B (en) | 2008-12-17 | 2008-12-17 | Preparation method of nano-copper-nickel alloy by liquid phase method |
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| CN101745645A CN101745645A (en) | 2010-06-23 |
| CN101745645B true CN101745645B (en) | 2011-05-11 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051574A (en) * | 2011-01-14 | 2011-05-11 | 上海大学 | Method for treating nano alloying surface of low-carbon steel plate |
| CN102689017A (en) * | 2012-05-25 | 2012-09-26 | 南京白云化工环境监测有限公司 | Automatic production equipment for manufacturing copper nickel nano-alloy |
| CN103302303B (en) * | 2012-12-05 | 2015-01-28 | 黑龙江大学 | Method for preparing copper-nickel solid solution powder by microwaves |
| CN103008675B (en) * | 2012-12-19 | 2016-04-20 | 国家钽铌特种金属材料工程技术研究中心 | A kind of preparation method of nickel coated copper composite powder |
| CN103170649A (en) * | 2013-04-15 | 2013-06-26 | 南京理工大学 | Preparation method of magnetic nickel nano material |
| CN110576191B (en) * | 2019-10-18 | 2022-04-26 | 济宁学院 | Method for preparing copper-nickel alloy nano material with bevel bipyramid morphology characteristics in hydrophobic phase |
| CN113977130B (en) * | 2021-11-24 | 2023-03-31 | 广东中实金属有限公司 | High-temperature-resistant soldering paste capable of being sintered at low temperature under no pressure and preparation method and use method thereof |
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2008
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Non-Patent Citations (3)
| Title |
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| Dong Chen et al..Properties of Core-Shell Ni-Au Nanoparticles Synthesized through a Redox-Transmetalation Method in Reverse Microemulsion.《Chem. Mater.》.2007,第19卷3399-3405. * |
| 张锡凤等.修饰剂对1,2-丙二醇体系中制备纳米镍的影响.《精细化工》.2006,第23卷(第4期),第328页 1.2纳米镍的制备第1-7行. * |
| 李鹏等.1，2-丙二醇液相还原法制备纳米镍粉的研究.《材料科学与工艺》.2001,第9卷(第3期),第260页1实验材料及方法第1-10行. * |
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