CN107790738B - A method of preparing a nanometer W-Re alloy powder - Google Patents
A method of preparing a nanometer W-Re alloy powder Download PDFInfo
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- CN107790738B CN107790738B CN201710968874.XA CN201710968874A CN107790738B CN 107790738 B CN107790738 B CN 107790738B CN 201710968874 A CN201710968874 A CN 201710968874A CN 107790738 B CN107790738 B CN 107790738B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
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Abstract
A nanometer method for W-Re alloy powder is prepared the present invention provides a kind of, belongs to powder metallurgy powder preparation technical field.Specifically the preparation method comprises the following steps: 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 nanoparticle then is made using hydrogen reducing.The low-temperature combustion synthesis that the present invention uses belongs to liquid phase synthesizing method, can achieve the other mixing of molecular level, and tungsten oxide, rheium oxide uniformly mix in obtained presoma, and reduzate is alloy powder, is not necessarily to subsequent specially treated.In addition the raw material of this method is simple and easy to get, and equipment is simple, and technique is quick, is appropriate for being mass produced.
Description
Technical field
The invention belongs to field of powder metallurgy, are related to the method for preparation nanometer W-Re alloy powder.
Background technique
Tungsten (W) has high-melting-point, high rigidity, good elevated temperature strength, thermally conductive, 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 element is added in W alloy can improve the recrystallization temperature of W alloy significantly, so as to improve W alloy
Mechanical behavior under high temperature, improve its maximum operation (service) temperature.The traditional preparation methods of W-Re alloy are that W powder and Re powder are first used ball
The method of mill mixes, and tungsten alloy then is made by compacting and incipient fusion sintering process, prepares not using deformation after unloading processing
The W-Re alloy material of same type.102130288 A of patent CN prepares pre-alloyed powder using the method mixed admittedly, by W powder
With rehenic acid ammonium by ball milling mixing, mixed-powder is dispersed after calcining with alcohol, the powder after dispersion by reduction, forming,
Incipient fusion sintering, swaging is made W-Re alloy wire with drawing process.102816963 A of patent CN using solid-liquid mixing (tungsten powder with
Ammonium rhenate solution) method prepare W-Re alloy powder, then will be carried out after powder reduction compacting and incipient fusion sintering prepare W-Re
Alloy.The uniformity of the W-Re alloy powder of these methods preparation is poor, and powder size is larger, and sintering activity is poor, needs very
Density needed for high sintering temperature or very long sintering time can be only achieved deformation after unloading processing.In addition, these methods are time-consuming
It is longer, it is readily incorporated impurity, complex process and energy consumption is higher.So finding a kind of side simple and quick, inexpensive, energy consumption is low
Method is used to prepare high sintering activity and the uniform W-Re powder of ingredient has important scientific meaning.
Summary of the invention
It is an object of the invention to according in the prior art or energy consumption is larger, elapsed time is longer or preparation method is numerous
Trivial disadvantage provides a kind of method of simple and quick preparation nanometer W-Re alloy powder, and the mass fraction of Re 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 aqueous solution.It will
Solution is heated to that combustion reaction occurs, and obtains fluffy precursor powder.
(2) obtained precursor powder is ground, is then restored using hydrogen and obtains a nanometer W-Re alloy powder.
Further, fuel described in step (1) is at least one of glycine, urea, EDTA, thiocarbamide.
Further, 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, 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, and being passed through for hydrogen is kept in reduction process, and hydrogen flowing quantity is greater than 0.5L/min.
Technology of the invention has advantage below:
(1) raw material is simple and easy to get, and equipment is simple, and technique is quick, can prepare a large amount of product in a short time.
(2) method of presoma is prepared using wet chemical method, each ingredient 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, are not necessarily to subsequent specially treated.
(3) due in presoma oxide particle reach nano-scale, it is short to restore required temperature and time, consume energy low,
It can be with save the cost.The nanometer W-Re alloy powder particle finally prepared is tiny, and sintering activity is high, and sintering required temperature is low, when
Between it is short.
The ingredient of W-Re alloy freely can accurately be regulated and controled by adjusting the additional amount of raw material.
Specific embodiment
Embodiment 1
By 0.01mol ammonium metatungstate, 0.0012mol rehenic acid ammonium, 0.1mol urea, 0.2mol ammonium nitrate is put into beaker simultaneously
Suitable water is added to dissolve to obtain clear solution, which is placed on electric furnace and is heated to reaction, is obtained fluffy
Precursor powder.Precursor powder is put into tube furnace and is restored, reduction temperature is 750 DEG C, hydrogen flowing quantity 1L/min, heat preservation
Time is 2.5h, and the rate of heat addition is 8 DEG C/min, cools to room temperature with the furnace after the completion of heat preservation and obtains a nanometer W-0.1wt%Re alloy
Powder.
Embodiment 2
By 0.01mol ammonium metatungstate, 0.042mol rehenic acid ammonium, 0.2mol glycine, 0.35mol ammonium nitrate is put into beaker
Suitable water is added to dissolve to obtain clear solution, solution is placed in the Muffle furnace for being previously heated to 260 DEG C, wait react hair
It is taken out after life and obtains precursor powder.Precursor powder is put into tube furnace and is restored, 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 with the furnace after the completion of heat preservation and obtains a nanometer W-
26wt%Re alloy powder.
Embodiment 3
By 0.01mol ammonium metatungstate, 0.0076mol rehenic acid ammonium, 0.12mol urea, 0.3mol ammonium nitrate is put into beaker
Suitable water is added to dissolve to obtain clear solution, solution is placed on to heat preservation in the Muffle furnace for be previously heated to 245 DEG C and is extremely fired
It burns reaction to complete, taking-up obtains precursor powder.Precursor powder is put into tube furnace and is restored, 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 heat preservation and obtains
Nanometer W-6wt%Re alloy powder.
Embodiment 4
By 0.01mol ammonium metatungstate, 0.013mol rehenic acid ammonium, 0.16mol glycine, 0.3mol ammonium nitrate is put into beaker
Suitable water is added to dissolve to obtain clear solution, which is placed on electric furnace and is heated to reaction, is obtained fluffy
Precursor powder.Precursor powder is put into tube furnace and is restored, reduction temperature is 750 DEG C, hydrogen flowing quantity 1L/min, heat preservation
Time is 2.5h, and the rate of heat addition is 8 DEG C/min, cools to room temperature with the furnace after the completion of heat preservation and obtains a nanometer W-10wt%Re alloyed powder
End.
Embodiment 5
By 0.01mol ammonium metatungstate, 0.021mol rehenic acid ammonium, 0.150mol urea, 0.05molEDTA, 0.28mol nitric acid
Ammonium, which is put into beaker, to be added suitable water and dissolves to obtain clear solution, and solution is placed on and is previously heated to 250 DEG C of Muffle
Heat preservation to combustion reaction is completed in furnace, and taking-up obtains precursor powder.Precursor powder is put into tube furnace and is restored, reduction temperature
Degree is 800 DEG C, hydrogen flowing quantity 2L/min, soaking time 2h, and the rate of heat addition is 5 DEG C/min, furnace cooling after the completion of heat preservation
A nanometer W-15wt%Re alloy powder is obtained to room temperature.
Claims (1)
1. a kind of prepare a nanometer method for W-Re alloy powder, it is characterised in that preparation step 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 aqueous solution, solution is heated to combustion reaction occurs, be obtained fluffy
Precursor powder；
2) obtained precursor powder is ground, then obtains a nanometer W-Re alloy powder using hydrogen reducing；
Ammonium metatungstate, rehenic acid ammonium, fuel and ammonium nitrate molar ratio in step (1) are 1:(0.12~4.2): (10~25):
(20~35)；
Fuel in step (1) is at least one of glycine, urea, EDTA, thiocarbamide；
Reduction temperature is 600~1000 DEG C in step (2), and heating rate is 1~10 DEG C/min, and soaking time is 1~8h, reduction
Being passed through for hydrogen is kept in the process, and hydrogen flowing quantity is greater than 0.5L/min.
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| 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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| 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 |
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