CN104759632A - Method of preparing nano-crystalline powdered alloy powder - Google Patents
Method of preparing nano-crystalline powdered alloy powder Download PDFInfo
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- CN104759632A CN104759632A CN201510128801.0A CN201510128801A CN104759632A CN 104759632 A CN104759632 A CN 104759632A CN 201510128801 A CN201510128801 A CN 201510128801A CN 104759632 A CN104759632 A CN 104759632A
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Abstract
The invention provides a method of preparing nano-crystalline powdered alloy powder, and belongs to the field of a powder metallurgy preparation technology. The method comprises the steps: preparing an oxide precursor by adopting a solution method; carrying out reductive sintering on the precursor powder in hydrogen; and obtaining pure nickel-tungsten alloy powder with fine crystal particles. According to the method provided by the invention, all raw materials are mixed by using a liquid phase, reactants can be uniformly mixed on an atom level, and the problem that the alloy powder is difficult to mix can be solved; meanwhile, the method has the characteristics of low cost and high use ratio of raw material powder; in addition, because the nano-crystalline powdered alloy powder is plied as nano-crystalline powder, and the method is higher in rigidity, wearability, corrosion resistance, resistance to high temperature oxidation and the like.
Description
Technical field
The invention belongs to advanced powder metallurgy preparing technical field, specifically provide a kind of preparation method of nickel tungsten powder.
Background technology
As a kind of traditional material nickel tungsten because have multiple superior performance, and some potential using values and receiving much attention.Tungsten nickel electrodeposited coating compact structure, heat resistance is high, can match in excellence or beauty with ceramic phase; At high temperature wear-resistant, anti-oxidant, there is good self-lubricating and decay resistance.Its performance of alloy of different nickel tungsten ratio has marked difference.When W content higher than 43 ~ 44% time, its alloy presents amorphous structure, has the performances such as excellent anti-corrosion and wear-resisting, radiation proof.When W content is less than 10%, its alloy is mainly made as base band and uses, and wherein prepares the important directions that low or nonmagnetic, strong cubic texture NiW alloy and composite baseband thereof are the research of current textured metal base band used for coating conductor.
At present, the preparation method of nickel tungsten mainly contains electro-deposition, laser formation, powder metallurgy etc.The Li Xiao spare time (application of electric deposition nickel tungsten alloy and present Research [J]. Shanghai non-ferrous metal, 2010,2:011.) using nickelous sulfate and sodium tungstate to prepare tungsten nickel for raw material electrodeposition process uses equipment simple, coating speed is fast, but the method is only suitable for preparing alloy coat and technics comparing is complicated; Laser formation method can when without the part preparing complicated shape when hard tool and mould, and the cycle is shorter, but it is confined to small lot, production equipment high in cost of production shortcoming; Prior powder metallurgy is prepared nickel tungsten and is mainly contained mechanical alloying, melting etc., and Chinese patent CN102329973A uses the method for vacuum induction melting, Ni powder and W powder is carried out mechanical mixture then mold pressing, casts alloy pig.Although NiW can fully mix by the method, need the environment of vacuum high-temperature, condition is comparatively harsh.Therefore, the synthetic method that the nickel tungsten powder that low cost, technique simply prepare different proportion still needs exploitation new.
Summary of the invention
The object of the present invention is to provide a kind of new method prepared nano-crystal nickel tungsten alloy powder and prepare.
The present invention directly adopts tungstates ammonium metatungstate, nickel nitrate and adjuvant to be raw material, has the feature of short route, low cost, and the nano-crystal nickel tungsten alloy powder designability prepared is strong, excellent performance.
Prepare a method for nano-crystal nickel tungsten alloy powder, processing step is as follows:
1, raw material: the raw material adopted has ammonium metatungstate ((NH
4)
6h
2w
12o
40), nickel nitrate (Ni (NO
3)
2), adjuvant;
2, solution preparation: selected raw material is water-soluble according to certain proportioning, mixes;
3, precursor power: the aqueous solution that step (2) obtains is heated and stirs, along with the volatilization of the aqueous solution, solution is bubbling after generation is concentrated, releases a large amount of gas, vigorous oxidation reduction reaction occurs instantaneously and generates pulverous presoma;
4, the preparation of nickel tungsten powder: the H of predecessor at 600 ~ 700 DEG C that step (3) is obtained
2reduce in atmosphere, the time is 1 ~ 2 hour, obtains pure, that crystal grain is tiny nickel tungsten powder.
The nickel nitrate wherein used in step (2) and the mol ratio of adjuvant are 0.5 ~ 5, the mol ratio of ammonium metatungstate and nickel nitrate is determined according to alloying component, the composition of finally made nanometer crystal alloy powder is: xNi-yW, ratio between x, y (mass percent) can need adjustment arbitrarily according to alloying component, is generally 0.01 ~ 99.
Advantage of the present invention is:
1, directly tungstates and nickel nitrate is adopted to be raw material, short route, low cost, simple process, quick, be applicable to large-scale production;
2, by controlling kind and the proportioning of raw material, the course of reaction of precursor power can be controlled, controlling the particle diameter of presoma, aperture and alloy powder composition;
3, liquid phase is utilized to mix each raw material, can the Homogeneous phase mixing of realization response thing on atomic level, to be evenly distributed alloy to be conducive to acquisition;
4, because nano composite powder grain diameter is tiny, surface-active is high, has certain optimization function to the following process of powder, can reduce heat treatment temperature, and improve thermal treatment rate.As shortened diffusion path in sintering process, be conducive to obtaining high-compactness, Tissue distribution is even, crystal grain is tiny alloy.
Detailed description of the invention
Embodiment 1
Nickel nitrate (Ni (NO is taken according to stoichiometry
3)
2) 0.1mol, ammonium metatungstate ((NH
4)
6h
2w
12o
40) 0.04mol, glycine (C
2h
5nO
2) 0.2mol.Material powder being dissolved in appropriate deionized water for stirring to dissolving rear constant temperature 200 DEG C heating completely, redox reaction occurring after solution evaporate to dryness and obtains predecessor tungsten oxide and nickel oxide mixed-powder.By predecessor 600 DEG C of reduction in hydrogen, be incubated 2 hours cold with stove, obtain the alloy powder that crystallite dimension is 80 ~ 120nm.
Embodiment 2
Nickel nitrate (Ni (NO is taken according to stoichiometry
3)
2) 0.1mol, ammonium metatungstate ((NH
4)
6h
2w
12o
40) 0.008mol, glycine (C
2h
5nO
2) 0.2mol.Material powder is dissolved in appropriate deionized water for stirring to be placed in Muffle furnace and to heat after dissolving completely, constant temperature 200 DEG C heating, reacts after solution evaporate to dryness and obtains predecessor tungsten oxide and nickel oxide mixed-powder.By predecessor 600 DEG C of reduction in hydrogen, be incubated 2 hours cold with stove, obtain the alloy powder that crystallite dimension is 50 ~ 100nm.
Embodiment 3
Nickel nitrate (Ni (NO is taken according to stoichiometry
3)
2) 0.1mol, ammonium metatungstate ((NH
4)
6h
2w
12o
40) 0.01mol, glycine (C
2h
5nO
2) 0.4mol.Material powder is dissolved in appropriate deionized water for stirring to be placed in Muffle furnace and to heat after dissolving completely, constant temperature 200 DEG C heating, reacts after solution evaporate to dryness and obtains predecessor tungsten oxide and nickel oxide mixed-powder.By predecessor 650 DEG C of reduction in hydrogen, be incubated 2 hours cold with stove, obtain the alloy powder that crystallite dimension is 30 ~ 100nm.
Embodiment 4
Nickel nitrate (Ni (NO is taken according to stoichiometry
3)
2) 0.1mol, ammonium metatungstate ((NH
4)
6h
2w
12o
40) 0.04mol, glycine (C
2h
5nO
2) 0.4mol.Material powder is dissolved in appropriate deionized water for stirring to be placed in Muffle furnace and to heat after dissolving completely, constant temperature 200 DEG C heating, reacts after solution evaporate to dryness and obtains predecessor tungsten oxide and nickel oxide mixed-powder.By predecessor 600 DEG C of reduction in hydrogen, be incubated 2 hours cold with stove, obtain the alloy powder that crystallite dimension is 20 ~ 50nm.。
Embodiment 5
Nickel nitrate (Ni (NO is taken according to stoichiometry
3)
2) 0.2mol, ammonium metatungstate ((NH
4)
6h
2w
12o
40) 0.05mol, urea (CO (NH
2)
2) 0.072mol.Material powder is dissolved in appropriate deionized water for stirring to be placed in Muffle furnace and to heat after dissolving completely, constant temperature 200 DEG C heating, reacts after solution evaporate to dryness and obtains predecessor tungsten oxide and nickel oxide mixed-powder.By predecessor 650 DEG C of reduction in hydrogen, be incubated 2 hours cold with stove, obtain the alloy powder that crystallite dimension is 30 ~ 80nm.
Claims (4)
1. prepare a method for nano-crystal nickel tungsten alloy powder, it is characterized in that concrete steps are as follows:
(1) raw material: the raw material adopted has ammonium metatungstate ((NH
4)
6h
2w
12o
40), nickel nitrate (Ni (NO
3)
2), adjuvant;
(2) solution preparation: selected raw material is water-soluble according to certain proportioning, mixes; The nickel nitrate used and the mol ratio of adjuvant are 0.5 ~ 5, the ratio of ammonium metatungstate and nickel nitrate is determined according to alloying component, the composition of finally made nanometer crystal alloy powder is: xNi-yW, x, y are mass percent, and ratio needs to adjust arbitrarily in 0.01 ~ 99 scope according to alloying component;
(3) precursor power: the aqueous solution that step (2) obtains is heated and stirs, along with the volatilization of the aqueous solution, solution is bubbling after generation is concentrated, releases a large amount of gas, vigorous oxidation reduction reaction occurs instantaneously and generates pulverous presoma;
(4) preparation of nickel tungsten powder: predecessor step (3) obtained is at H
2reduce in atmosphere, obtain pure, that crystal grain is tiny nickel tungsten powder.
2. a kind of method preparing nano-crystal nickel tungsten alloy powder as claimed in claim 1, is characterized in that in step, the adjuvant described in (1) is at least one in glycine, urea, thiocarbamide, citric acid.
3. a kind of method preparing nano-crystal nickel tungsten alloy powder as described in the step (4) in claim 1, the temperature of hydrogen reducing is 600 ~ 700 DEG C, and the time is 1 ~ 2 hour.
4. a kind of method preparing nano-crystal nickel tungsten alloy powder as described in the step (4) in claim 1, final prepared nickel tungsten powder is nanocrystalline, and granularity is between 20 ~ 120nm.
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Family
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Cited By (5)
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|---|---|---|---|---|
| CN106180742A (en) * | 2016-07-16 | 2016-12-07 | 北京工业大学 | A kind of preparation method of coating conductor NiW alloy base band alloy nano-powder |
| CN107790738A (en) * | 2017-10-18 | 2018-03-13 | 北京科技大学 | It is a kind of to prepare a nanometer method for W Re alloy powders |
| CN109675598A (en) * | 2019-03-04 | 2019-04-26 | 合肥工业大学 | A kind of preparation method of the nickel tungsten carbide composite nano-powder as elctro-catalyst |
| CN114260459A (en) * | 2021-12-28 | 2022-04-01 | 厦门大学 | Preparation method of temperature-sensitive nickel-based bimetal nano alloy |
| CN114888286A (en) * | 2022-05-06 | 2022-08-12 | 南京国重新金属材料研究院有限公司 | Nickel-tungsten alloy seeding block forming device and forming method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106180742A (en) * | 2016-07-16 | 2016-12-07 | 北京工业大学 | A kind of preparation method of coating conductor NiW alloy base band alloy nano-powder |
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| CN107790738A (en) * | 2017-10-18 | 2018-03-13 | 北京科技大学 | It is a kind of to prepare a nanometer method for W Re alloy powders |
| CN107790738B (en) * | 2017-10-18 | 2019-10-22 | 北京科技大学 | A method of preparing a nanometer W-Re alloy powder |
| CN109675598A (en) * | 2019-03-04 | 2019-04-26 | 合肥工业大学 | A kind of preparation method of the nickel tungsten carbide composite nano-powder as elctro-catalyst |
| CN109675598B (en) * | 2019-03-04 | 2022-03-11 | 合肥工业大学 | Preparation method of nickel tungsten carbide nano composite powder used as electrocatalyst |
| CN114260459A (en) * | 2021-12-28 | 2022-04-01 | 厦门大学 | Preparation method of temperature-sensitive nickel-based bimetal nano alloy |
| CN114888286A (en) * | 2022-05-06 | 2022-08-12 | 南京国重新金属材料研究院有限公司 | Nickel-tungsten alloy seeding block forming device and forming method thereof |
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Application publication date: 20150708 |