CN107790738A - It is a kind of to prepare a nanometer method for W Re alloy powders - Google Patents
It is a kind of to prepare a nanometer method for W Re alloy powders Download PDFInfo
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- CN107790738A CN107790738A CN201710968874.XA CN201710968874A CN107790738A CN 107790738 A CN107790738 A CN 107790738A CN 201710968874 A CN201710968874 A CN 201710968874A CN 107790738 A CN107790738 A CN 107790738A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
Abstract
A nanometer method for W Re alloy powders is prepared the invention provides a kind of, belongs to powder metallurgy powder preparing technical field.Specifically preparation method is：Using ammonium metatungstate, rehenic acid ammonium, fuel, ammonium nitrate as raw material, oxide composite end is prepared using low-temperature combustion synthesis, W Re alloy nanoparticles then are made using hydrogen reducing.The low-temperature combustion synthesis that the present invention uses belongs to liquid phase synthesizing method, can reach the other mixing of molecular level, and tungsten oxide, rheium oxide uniformly mix in obtained presoma, and reduzate is alloy powder, without follow-up specially treated.The raw material of other this method is simple and easy to get, and equipment is simple, and technique is quick, is appropriate for mass producing.
Description
Technical field
The invention belongs to field of powder metallurgy, is related to the method for preparing nanometer W-Re alloy powders.
Background technology
Tungsten (W) has high-melting-point, high rigidity, good elevated temperature strength, heat conduction, electric conductivity, in defence and military, nuclear industry
And high-temperature field has and is widely applied very much.But W alloy can recrystallize at high temperature, its mechanical property of severe exacerbation, shadow
Ring its service life.Re elements are added in W alloy can significantly increase the recrystallization temperature of W alloy, so as to improve W alloy
Mechanical behavior under high temperature, improve its maximum operation (service) temperature.The traditional preparation methods of W-Re alloys are that W powder and Re powder first are used into ball
The method mixing of mill, is then made tungsten alloy, then prepare not by deformation after unloading processing by compacting and incipient fusion sintering process
The W-Re alloy materials of same type.The A of patent CN 102130288 prepare pre-alloyed powder using the method mixed admittedly, by W powder
Disperseed with rehenic acid ammonium by ball milling mixing, mixed-powder after calcining with alcohol, disperse after powder by reduction, shaping,
Incipient fusion sintering, swage is made W-Re alloy wires with drawing process.The A of patent CN 102816963 using solid-liquid mix (tungsten powder with
Ammonium rhenate solution) method prepare W-Re alloy powders, then will be carried out after powder reduction compacting and incipient fusion sintering prepare W-Re
Alloy.The uniformity of W-Re alloy powders prepared by these methods is poor, and powder size is larger, and sintering activity difference is, it is necessary to very
High sintering temperature or very long sintering time can be only achieved the density needed for deformation after unloading processing.In addition, these methods take
It is longer, it is readily incorporated impurity, complex process and power consumption is higher.So find a kind of side simple and quick, inexpensive, power consumption is low
Method is used to prepare high sintering activity and the uniform W-Re powder of composition has important scientific meaning.
The content of the invention
It is an object of the invention to according among prior art or energy consumption is larger, elapsed time is longer, or preparation method is numerous
The shortcomings that trivial, there is provided a kind of simple and quick method for preparing nanometer W-Re alloy powders, Re mass fraction is 0.1~26%.
The present invention comprises the following specific steps that：
(1) presoma is prepared using low-temperature combustion synthesis.The process that the low-temperature combustion synthesis prepares presoma is：
Ammonium metatungstate, rehenic acid ammonium, fuel, ammonium nitrate are dissolved in deionized water by certain molar ratio and are configured to the aqueous solution.Will
Solution is heated to that combustion reaction occurs, and obtains fluffy precursor powder.
(2) obtained precursor powder is ground, is then reduced using hydrogen and obtain a nanometer W-Re alloy powders.
Further, the fuel described in step (1) is at least one of glycine, urea, EDTA, thiocarbamide.
Further, the ammonium metatungstate described in step (1), rehenic acid ammonium, fuel and ammonium nitrate molar ratio are 1：(0.12
~4.2)：(10~25):(20~35).
Further, the reduction temperature described in step (2) is 600~1000 DEG C, and heating rate is 1~10 DEG C/min,
Soaking time is 1~8h, keeps being passed through for hydrogen in reduction process, hydrogen flowing quantity is more than 0.5L/min.
The technology of the present invention has following advantage：
(1) raw material is simple and easy to get, and equipment is simple, and technique is quick, can prepare substantial amounts of product in a short time.
(2) method for preparing presoma uses wet chemical method, and each composition has reached the other mixing of molecular level in the solution,
Tungsten oxide, rheium oxide uniformly mix in obtained presoma, and reduzate is alloy powder, without follow-up specially treated.
(3) due in presoma oxide particle reach nano-scale, it is short to reduce required temperature and time, and power consumption is low,
Can be with cost-effective.The nanometer W-Re alloy powder particles finally prepared are tiny, and sintering activity is high, and temperature needed for sintering is low, when
Between it is short.
The composition of W-Re alloys can freely be regulated and controled exactly by adjusting the addition of raw material.
Embodiment
Embodiment 1
0.01mol ammonium metatungstates, 0.0012mol rehenic acid ammoniums, 0.1mol urea, 0.2mol ammonium nitrate are put into beaker simultaneously
Add appropriate water and dissolve the solution clarified, the solution is placed on electric furnace and is heated to reaction, obtain fluffy
Precursor powder.Precursor powder is put into tube furnace and reduced, reduction temperature is 750 DEG C, hydrogen flowing quantity 1L/min, insulation
Time is 2.5h, and the rate of heat addition is 8 DEG C/min, cools to room temperature after the completion of insulation with the furnace and obtains a nanometer W-0.1wt%Re alloys
Powder.
Embodiment 2
0.01mol ammonium metatungstates, 0.042mol rehenic acid ammoniums, 0.2mol glycine, 0.35mol ammonium nitrate are put into beaker
Add appropriate water and dissolve the solution clarified, solution is placed on and is previously heated in 260 DEG C of Muffle furnace, question response hair
Taken out after life and obtain precursor powder.Precursor powder is put into tube furnace and reduced, reduction temperature is 750 DEG C, hydrogen flowing quantity
For 1.2L/min, soaking time 2h, the rate of heat addition is 5 DEG C/min, cools to room temperature after the completion of insulation with the furnace and obtains a nanometer W-
26wt%Re alloy powders.
Embodiment 3
0.01mol ammonium metatungstates, 0.0076mol rehenic acid ammoniums, 0.12mol urea, 0.3mol ammonium nitrate are put into beaker
Add appropriate water and dissolve the solution clarified, solution is placed on and is previously heated to insulation extremely combustion in 245 DEG C of Muffle furnace
Burn reaction to complete, taking-up obtains precursor powder.Precursor powder is put into tube furnace and reduced, reduction temperature is 800 DEG C, hydrogen
Throughput is 1.5L/min, and soaking time 4h, the rate of heat addition is 10 DEG C/min, cools to room temperature with the furnace after the completion of insulation and obtains
Nanometer W-6wt%Re alloy powders.
Embodiment 4
0.01mol ammonium metatungstates, 0.013mol rehenic acid ammoniums, 0.16mol glycine, 0.3mol ammonium nitrate are put into beaker
Add appropriate water and dissolve the solution clarified, the solution is placed on electric furnace and is heated to reaction, obtain fluffy
Precursor powder.Precursor powder is put into tube furnace and reduced, reduction temperature is 750 DEG C, hydrogen flowing quantity 1L/min, insulation
Time is 2.5h, and the rate of heat addition is 8 DEG C/min, cools to room temperature after the completion of insulation with the furnace and obtains a nanometer W-10wt%Re alloyed powders
End.
Embodiment 5
By 0.01mol ammonium metatungstates, 0.021mol rehenic acid ammoniums, 0.150mol urea, 0.05molEDTA, 0.28mol nitric acid
Ammonium, which is put into, to be added appropriate water and dissolves the solution clarified in beaker, solution is placed on and is previously heated to 250 DEG C of Muffle
Insulation to combustion reaction is completed in stove, and taking-up obtains precursor powder.Precursor powder is put into tube furnace and reduced, reduction temperature
Spend for 800 DEG C, hydrogen flowing quantity 2L/min, soaking time 2h, the rate of heat addition is 5 DEG C/min, furnace cooling after the completion of insulation
A nanometer W-15wt%Re alloy powders are obtained to room temperature.
Claims (4)
1. a kind of prepare a nanometer method for W-Re alloy powders, it is characterised in that preparation process is as follows
1) presoma is prepared using low-temperature combustion synthesis, detailed process is：Ammonium metatungstate, rehenic acid ammonium, fuel, ammonium nitrate are pressed
Certain molar ratio, which is dissolved in deionized water, is configured to the aqueous solution, solution is heated to combustion reaction occurs, obtained fluffy
Precursor powder；
2) obtained precursor powder is ground, then obtains a nanometer W-Re alloy powders using hydrogen reducing.
2. a kind of as claimed in claim 1 prepare a nanometer method for W-Re alloy powders, it is characterised in that the fuel in step (1)
For at least one of glycine, urea, EDTA, thiocarbamide.
3. a kind of as claimed in claim 1 prepare a nanometer method for W-Re alloy powders, it is characterised in that the inclined tungsten in step (1)
Sour ammonium, rehenic acid ammonium, fuel and ammonium nitrate molar ratio are 1：(0.12~4.2)：(10~25):(20~35).
4. a kind of as claimed in claim 1 prepare a nanometer method for W-Re alloy powders, it is characterised in that reduction temperature in step (2)
Spend for 600~1000 DEG C, heating rate is 1~10 DEG C/min, and soaking time is 1~8h, and the logical of hydrogen is kept in reduction process
Enter, hydrogen flowing quantity is more than 0.5L/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109351985A (en) * | 2018-10-19 | 2019-02-19 | 浙江工业大学 | A kind of method that Hydrothermal Pressure Hydrogen Reduction prepares rhenium metal powder |
| CN109773206A (en) * | 2019-03-29 | 2019-05-21 | 中国科学院金属研究所 | A kind of ultrapure superfine rhenium powder and preparation method thereof |
| CN111112641A (en) * | 2019-12-16 | 2020-05-08 | 重庆材料研究院有限公司 | Preparation method of nano molybdenum-rhenium alloy powder |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120012122A1 (en) * | 2003-10-27 | 2012-01-19 | Philip Morris Usa Inc. | Formation and deposition of sputtered nanoscale particles in cigarette manufacture |
| CN102584231A (en) * | 2011-12-23 | 2012-07-18 | 南京工业大学 | Preparation method of ion-doped double perovskite structure tungsten molybdate oxide powder |
| CN102626785A (en) * | 2012-04-27 | 2012-08-08 | 北京科技大学 | Preparation method for rare earth oxide doped tungsten powder |
| CN103008676A (en) * | 2013-01-15 | 2013-04-03 | 北京科技大学 | Method for manufacturing high-dispersion ultrafine molybdenum-based powder |
| CN103920870A (en) * | 2014-04-12 | 2014-07-16 | 北京工业大学 | Porous spherical tungsten rhenium alloy powder and preparation method thereof |
| CN104759632A (en) * | 2015-03-23 | 2015-07-08 | 北京科技大学 | Method of preparing nano-crystalline powdered alloy powder |
| CN106825599A (en) * | 2017-01-19 | 2017-06-13 | 北京科技大学 | A kind of preparation method of the WC Co nanometer powders for adding grain growth inhibitor |
| CN107008916A (en) * | 2017-04-12 | 2017-08-04 | 湖南元极新材料有限公司 | A kind of spherical nickel rhenium alloys powder and preparation method thereof, application |
-
2017
- 2017-10-18 CN CN201710968874.XA patent/CN107790738B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120012122A1 (en) * | 2003-10-27 | 2012-01-19 | Philip Morris Usa Inc. | Formation and deposition of sputtered nanoscale particles in cigarette manufacture |
| CN102584231A (en) * | 2011-12-23 | 2012-07-18 | 南京工业大学 | Preparation method of ion-doped double perovskite structure tungsten molybdate oxide powder |
| CN102626785A (en) * | 2012-04-27 | 2012-08-08 | 北京科技大学 | Preparation method for rare earth oxide doped tungsten powder |
| CN103008676A (en) * | 2013-01-15 | 2013-04-03 | 北京科技大学 | Method for manufacturing high-dispersion ultrafine molybdenum-based powder |
| CN103920870A (en) * | 2014-04-12 | 2014-07-16 | 北京工业大学 | Porous spherical tungsten rhenium alloy powder and preparation method thereof |
| CN104759632A (en) * | 2015-03-23 | 2015-07-08 | 北京科技大学 | Method of preparing nano-crystalline powdered alloy powder |
| CN106825599A (en) * | 2017-01-19 | 2017-06-13 | 北京科技大学 | A kind of preparation method of the WC Co nanometer powders for adding grain growth inhibitor |
| CN107008916A (en) * | 2017-04-12 | 2017-08-04 | 湖南元极新材料有限公司 | A kind of spherical nickel rhenium alloys powder and preparation method thereof, application |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109351985A (en) * | 2018-10-19 | 2019-02-19 | 浙江工业大学 | A kind of method that Hydrothermal Pressure Hydrogen Reduction prepares rhenium metal powder |
| CN109351985B (en) * | 2018-10-19 | 2021-08-10 | 浙江工业大学 | Method for preparing metal rhenium powder by hydrothermal hydrogen reduction |
| CN109773206A (en) * | 2019-03-29 | 2019-05-21 | 中国科学院金属研究所 | A kind of ultrapure superfine rhenium powder and preparation method thereof |
| CN111112641A (en) * | 2019-12-16 | 2020-05-08 | 重庆材料研究院有限公司 | Preparation method of nano molybdenum-rhenium alloy powder |
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