CN107900373A - Ultra-fine W Cu composite powders and preparation method thereof - Google Patents

Ultra-fine W Cu composite powders and preparation method thereof Download PDF

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Publication number
CN107900373A
CN107900373A CN201711288859.7A CN201711288859A CN107900373A CN 107900373 A CN107900373 A CN 107900373A CN 201711288859 A CN201711288859 A CN 201711288859A CN 107900373 A CN107900373 A CN 107900373A
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fine
ultra
tungstate
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composite powders
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CN107900373B (en
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黄泽辉
邓登飞
李倩
叶艳君
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Chongyi Zhangyuan Tungsten Co Ltd
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Chongyi Zhangyuan Tungsten Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • B22F1/0007

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Abstract

The invention discloses a kind of ultra-fine W Cu composite powders and preparation method thereof, this method includes:(1) mantoquita, zinc salt and sodium tungstate solution are mixed, to obtain mixed solution;(2) mixed solution is sent and is stirred, reacts into autoclave, so as to liquid after being reacted;(3) liquid after the reaction is filtered and cleaning treatment, to obtain copper tungstate Zinc Tungstate composite powder presoma and filtered fluid;(4) processing is dried in the copper tungstate Zinc Tungstate composite powder presoma, so as to composite powder presoma after being dried;(5) composite powder presoma after the drying is subjected to reduction treatment in a hydrogen atmosphere, to obtain ultra-fine W Cu composite powders.The ultra-fine W Cu composite powders that purity is high, crystallite dimension is small and W Cu component ratios are controllable can be made using this method, while the technique is simple, it can be achieved that mass production, has a good application prospect.

Description

Ultra-fine W-Cu composite powders and preparation method thereof
Technical field
The invention belongs to composite metal powder preparation field, specifically, the present invention relates to ultra-fine W-Cu composite powders and Its preparation method.
Background technology
Tungsten has the performances such as high-melting-point, high density, resistance fusion welding, electrical erosion resistance, elevated temperature strength be good, the thermal conductivity and electricity of copper Conductance is high, ductility is good, easy to process, and part prepared by the two alloying can have the performance of tungsten and copper concurrently, be widely used in Military project material and electronic material.But since tungsten, copper powders are mutually insoluble, contact angle is big, the two can be only formed pseudo-alloy, adopts The W-Cu composite material consistency prepared with traditional powder metallurgy and infiltration method is poor, has been difficult to meet wanting for modern material Ask.The existing method for preparing ultra-fine W-Cu composite powders both at home and abroad, otherwise the long contaminating metal element of Ball-milling Time, and gained powder End is easy to agglomerating caking, and wall sticking phenomenon is serious;The precursor powder prepared is had a great influence by reaction temperature and reaction time, Reduction control is more difficult;Complex technical process, it is difficult to which mass generates.
Therefore, the existing technology for preparing ultra-fine W-Cu composite powders is further improved.
The content of the invention
It is contemplated that solve at least some of the technical problems in related technologies.For this reason, the present invention One purpose is to propose a kind of ultra-fine W-Cu composite powders and preparation method thereof.Purity height, crystal grain can be made using this method The ultra-fine W-Cu composite powders that size is small and W-Cu component ratios are controllable, while the technique is simple, it can be achieved that producing in enormous quantities, tool There is good application prospect.
The technical solution of the applicant is that inventor has found to complete based on following:At present, ultra-fine W-Cu is prepared both at home and abroad The method of composite powder mainly has mechanical alloying method, high temperature reduction method, atomization drying method and sol-gel process, chemical precipitation Method etc..Mechanical alloying method is to stir evenly two kinds of elemental metalpowders of W, Cu, in high energy ball mill carry out ball milling make W, Cu powder is uniformly mixed, and forms nanocrystalline W-Cu solid solution, and it is larger that the major defect of this method will reach grain size The Ball-milling Time that powder needs is very long, this just inevitably brings impurity metallic elements, and gained powder is easy to agglomerating caking, Wall sticking phenomenon is serious.Atomization drying method is that ammonium metatungstate and copper nitrate are made into mixed solution, the W- obtained after atomization drying Cu presomas are roasted, then product is reduced under hydrogen, that is, obtain W-Cu composite powders, using made from atomization drying method W-Cu composite powder particles are tiny and uniform, are not easily introduced impurity, but the precursor powder reduction control prepared is relatively difficult, by Reaction temperature and reaction time have a great influence.Sol-gel process is to be readily able to metallic compound (inorganic salts or the metal alcohol of hydrolysis Salt) react in certain solvent with water or other materials, gel is formed, is made after the processing such as drying/calcining and reduction W-Cu composite powders, W-Cu composite powders purity made from this method is high, and particle diameter distribution is uniform, but technical process is complex, difficult Generated with mass.Present inventor by trying to explore to the preparation process of existing ultra-fine W-Cu composite powders, The defects of aiming to solve the problem that in the prior art, is desirably to obtain with that purity is high, crystallite dimension is small and W-Cu component ratios are controllable is super Thin W-Cu composite powders.
For this reason, in one aspect of the invention, the present invention proposes a kind of method for preparing ultra-fine W-Cu composite powders, root According to the embodiment of the present invention, this method includes:
(1) mantoquita, zinc salt and sodium tungstate solution are mixed, to obtain mixed solution;
(2) mixed solution is sent and is stirred, reacts into autoclave, so as to liquid after being reacted;
(3) liquid after the reaction is filtered and cleaning treatment, to obtain copper tungstate-Zinc Tungstate composite powder forerunner Body and filtered fluid;
(4) processing is dried in the copper tungstate-Zinc Tungstate composite powder presoma, so as to composite powder after being dried Last presoma;
(5) composite powder presoma after the drying is subjected to reduction treatment in a hydrogen atmosphere, to obtain ultra-fine W- Cu composite powders.
The method for preparing ultra-fine W-Cu composite powders according to embodiments of the present invention is by by mantoquita and zinc salt and sodium tungstate Reaction, obtains copper tungstate-Zinc Tungstate composite powder presoma, then can be by the characteristic of hydrogen reducing, by forerunner using tungstates Body, which is placed under hydrogen atmosphere, carries out reduction reaction, and controls reduction temperature between simple substance zinc and elemental copper volatilization temperature, Easy to which the simple substance zinc that reduce generation can gasify and smoothly discharge, ultra-fine W-Cu composite powders are thus obtained.And because of presoma Crystallite dimension it is tiny and be evenly distributed, so presoma is not susceptible to abnormal grain growth phenomenon in hydrogen reduction, So as to which the ultra-fine W-Cu composite powders obtained can be maintained at submicron order crystallite dimension.Thus, it can be made pure using this method The ultra-fine W-Cu composite powders that degree is high, crystallite dimension is small and W-Cu component ratios are controllable, while the technique is simple, it can be achieved that large quantities of Amount production, has a good application prospect.
In addition, the method according to the above embodiment of the present invention for preparing ultra-fine W-Cu composite powders can also be with following attached The technical characteristic added:
In some embodiments of the invention, it is in step (1), the mantoquita and the zinc salt, the sodium tungstate is molten Liquid according to Cu2+And Zn2+The sum of molal quantity and Na2WO4Molal quantity is 1~2:1 is mixed.Thus, be conducive to improve ultra-fine The grade of W-Cu composite powders.
In some embodiments of the invention, in step (2), the mixing speed is 200-500r/min.Thus, may be used Further improve the grade of ultra-fine W-Cu composite powders.
In some embodiments of the invention, in step (2), the pressure in the autoclave is 0.3- 1.5MPa.Thus, it can further improve the grade of ultra-fine W-Cu composite powders.
In some embodiments of the invention, in step (2), the reaction temperature is 100-180 degrees Celsius, during reaction Between be 1-5h.Thus, it can further improve the grade of ultra-fine W-Cu composite powders.
In some embodiments of the invention, in step (5), the temperature of the reduction treatment is Celsius for 700-1000 Degree, time 1-3h.Thus, it can further improve the grade of ultra-fine W-Cu composite powders.
In another aspect of the invention, the present invention proposes a kind of ultra-fine W-Cu composite powders.It is real according to the present invention Example is applied, which be prepared using the above-mentioned method for preparing ultra-fine W-Cu composite powders.Thus, it can obtain purity The ultra-fine W-Cu composite powders high, crystallite dimension is small and W-Cu component ratios are controllable.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination accompanying drawings below to embodiment Substantially and it is readily appreciated that, wherein:
Fig. 1 is the method flow schematic diagram according to an embodiment of the invention for preparing ultra-fine W-Cu composite powders;
Fig. 2 is the SEM photographs of copper tungstate-Zinc Tungstate composite powder presoma after drying according to an embodiment of the invention Piece;
Fig. 3 is the XRD diagram of copper tungstate-Zinc Tungstate composite powder presoma after drying according to an embodiment of the invention Spectrum;
Fig. 4 is the SEM photograph of ultra-fine W-20wt.%Cu composite powders according to an embodiment of the invention;
Fig. 5 is the XRD spectrum of ultra-fine W-20wt.%Cu composite powders according to an embodiment of the invention.
Embodiment
The embodiment of the present invention is described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end Same or similar label represents same or similar element or has the function of same or like element.Below with reference to attached The embodiment of figure description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.
In one aspect of the invention, the present invention proposes a kind of method for preparing ultra-fine W-Cu composite powders, according to this The embodiment of invention, with reference to figure 1, this method includes:
S100:Mantoquita and sodium tungstate solution are mixed
In the step, mantoquita, zinc salt and sodium tungstate solution are mixed, to obtain mixed solution.Need what is illustrated It is that the particular type of mantoquita and zinc salt is not particularly restricted, those skilled in the art can be selected according to actual needs Select, for example, mantoquita can be CuSO4·5H2O, zinc salt can be Zn (NO3)2·6H2O.Specifically, the zinc salt and wolframic acid that add Sodium reaction generation Zinc Tungstate precipitation, the reduzate of Zinc Tungstate in a hydrogen atmosphere is tungsten powder, wherein zinc gas in reduction process Change volatilization discharge, the content of W in W-Cu composite powders can be improved by improving the addition of zinc salt.
According to still a further embodiment, can be by mantoquita and zinc salt, sodium tungstate solution according to Cu2+And Zn2+Mole The sum of number and Na2WO4Molal quantity is 1~2:1 is mixed.Specifically, can be according in the ultra-fine W-Cu composite powders of final products The value of W/Cu determines the relative amounts of mantoquita and zinc salt, is achieved in the control to W and Cu component ratios.Specifically, such as by n (Cu2+)+n(Zn2+)/n(Na2WO4)=1/1, when zinc salt addition is zero, i.e. n (Zn2+)=0, n (Cu2+)/n(Na2WO4)=1/ When 1, gained presoma component is copper tungstate one-component, is through reducing obtained ultra-fine W-Cu composite powders Cu contents 25.82%, this is the attainable maximum level of Cu components in made ultra-fine W-Cu composite powders.Keeping n (Cu2+)+n(Zn2 +)/n(Na2WO4)=1/1, and in the case of improving zinc salt addition, the Cu contents in the ultra-fine W-Cu composite powders of gained are less than 25.82%.Such as need that W-20wt.%Cu is made, then the relative amounts of mantoquita and zinc salt are n (Cu2+)/n(Zn2+)=0.723/ 0.277。
S200:Mixed solution is sent and is stirred, reacts into autoclave
In the step, mixed solution is sent and is stirred, reacts into autoclave, so as to liquid after being reacted.Tool Body, mixed solution contains mantoquita, zinc salt and sodium tungstate, then in autoclave, in the copper ion and zinc salt in mantoquita Zinc ion is reacted with sodium tungstate, respectively obtains copper tungstate and Zinc Tungstate precipitation, and the related chemistry reaction equation being related to is as follows:
Cu2++WO4 2-=CuWO4
Zn2++WO4 2-=ZnWO4
According to one embodiment of present invention, mixing speed is not particularly restricted, and those skilled in the art can root Made choice according to actual needs, a specific embodiment according to the present invention, mixing speed can be 200-500r/min.Invention People has found that the stir speed (S.S.) is substantially better than the rate of deposition that other conditions improve liquid after reaction.
According to still a further embodiment, the pressure in autoclave is not particularly restricted, the skill of this area Art personnel can make choice according to actual needs, a specific embodiment according to the present invention, the pressure in autoclave Can be 0.3-1.5MPa.
According to still another embodiment of the invention, the condition of reaction is not particularly restricted, and those skilled in the art can To be made choice according to actual needs, a specific embodiment according to the present invention, reaction temperature can be that 100-180 is Celsius Degree, the reaction time can be 1-5h.Inventor has found, if reaction temperature is excessive, has WO3Generation, will if reaction temperature is too low Rate of deposition is caused to decline.Thus, it can ensure tungsten precipitation under the conditions of being somebody's turn to do completely and product production is more uniform.
S300:Liquid after reaction is filtered and cleaning treatment
In the step, after reaction liquid at the same time containing copper tungstate precipitation and Zinc Tungstate precipitation, by liquid after reaction carry out filtering and Cleaning treatment, obtains copper tungstate-Zinc Tungstate composite powder presoma and filtered fluid.Inventor has found, is obtained by hydro-thermal reaction Composite powder presoma crystallite dimension it is tiny and be evenly distributed.
S400:Processing is dried in copper tungstate-Zinc Tungstate composite powder presoma
In the step, processing is dried in the above-mentioned copper tungstate-Zinc Tungstate composite powder presoma that obtains, to be done Composite powder presoma after dry.Thus, the moisture in copper tungstate-Zinc Tungstate composite powder presoma is advantageously reduced, after raising The reduction efficiency of composite powder presoma after continuous drying, and reduce reduction energy consumption.A specific embodiment according to the present invention, will After the drying that copper tungstate-Zinc Tungstate composite powder presoma is dried to obtain composite powder presoma SEM photograph as shown in Fig. 2, Its XRD spectrum is as shown in Figure 3.
S500:Composite powder presoma carries out reduction treatment after in a hydrogen atmosphere will be dry
In the step, composite powder presoma after drying obtained above is subjected to reduction treatment in a hydrogen atmosphere, with Just ultra-fine W-Cu composite powders are obtained.Specifically, composite powder presoma contains copper tungstate and Zinc Tungstate at the same time after dry, wherein Copper tungstate and Zinc Tungstate react with hydrogen respectively, by the temperature for controlling reduction treatment so that react the zinc gasification of gained Volatilization discharge, and copper leaves in solid-state, and because composite powder presoma crystallite dimension is tiny after drying and is evenly distributed, so its Abnormal grain growth phenomenon is not susceptible in above-mentioned reduction process, the ultra-fine W-Cu that can obtain submicron order crystallite dimension is compound Powder.The related chemistry reaction equation being related to is:
CuWO4(s)+4H2(g)=Cu (s)+W (s)+4H2O↑
ZnWO4(s)+4H2(g)=Zn (g) ↑+W (s)+4H2O↑
According to one embodiment of present invention, the condition of reduction treatment is not particularly restricted, and those skilled in the art can To be made choice according to actual needs, a specific embodiment according to the present invention, the temperature of reduction treatment can be 700- 1000 degrees Celsius, the time can be 1-3h.Inventor has found that, if reduction temperature is excessive, overlong time, can make production die size It is larger, and if reduction temperature is too low, the time is too short, be unfavorable for zinc gasification volatilization.Thus, use the reduction treatment condition can be with Ensure that the ultra-fine W-Cu composite powders of gained have higher grade and value.
The method for preparing ultra-fine W-Cu composite powders according to embodiments of the present invention is by by mantoquita and zinc salt and sodium tungstate Reaction, obtains copper tungstate-Zinc Tungstate composite powder presoma, then can be by the characteristic of hydrogen reducing, by forerunner using tungstates Body, which is placed under hydrogen atmosphere, carries out reduction reaction, and controls reduction temperature between simple substance zinc and elemental copper volatilization temperature, Easy to which the simple substance zinc that reduce generation can gasify and smoothly discharge, ultra-fine W-Cu composite powders are thus obtained.And because of presoma Crystallite dimension it is tiny and be evenly distributed, so presoma is not susceptible to abnormal grain growth phenomenon in hydrogen reduction, So as to which the ultra-fine W-Cu composite powders obtained can be maintained at submicron order crystallite dimension.Thus, it can be made pure using this method The ultra-fine W-Cu composite powders that degree is high, crystallite dimension is small and W-Cu component ratios are controllable, while the technique is simple, it can be achieved that large quantities of Amount production, has a good application prospect.
As described above, the method for preparing ultra-fine W-Cu composite powders according to embodiments of the present invention can have selected from following At least one advantage:
1) present invention process flow is simple, and impurity is not easily introduced in reaction process, and the W-Cu that can prepare high-purity is answered Close powder.
2) copper tungstate-Zinc Tungstate composite powder presoma crystallite dimension that the present invention is obtained by hydro-thermal reaction is tiny and divides Cloth is uniform, therefore presoma is not susceptible to abnormal grain growth phenomenon, the W-Cu composite powders of acquisition in hydrogen reduction It can keep the crystallite dimension of submicron order.
In another aspect of the invention, the present invention proposes a kind of ultra-fine W-Cu composite powders.It is real according to the present invention Example is applied, which be prepared using the above-mentioned method for preparing ultra-fine W-Cu composite powders.Thus, it can obtain purity The ultra-fine W-Cu composite powders high, crystallite dimension is small and W-Cu component ratios are controllable.It is it should be noted that above-mentioned super for preparing The described feature and advantage of method of thin W-Cu composite powders are equally applicable to the ultra-fine W-Cu composite powders, no longer superfluous herein State.
Below with reference to specific embodiment, present invention is described, it is necessary to which explanation, these embodiments are only to describe Property, without limiting the invention in any way.
Embodiment 1
Take Na2WO4·2H2O 99.59g, CuSO4·5H2O 54.16g, Zn (NO3)2·6H2O 24.72g, addition go from Sub- water 300mL is made into mixed solution, is placed in autoclave and is reacted, and reaction temperature is 170 DEG C, and reaction time 4h, is stirred Speed 400r/min is mixed, by the sample filtering after reaction, cleaning, drying, after being dried before copper tungstate-Zinc Tungstate composite powder Drive body.Presoma is placed in atmosphere furnace and is reduced in a hydrogen atmosphere, reduction temperature is 900 DEG C, and recovery time 2h, obtains ultra-fine W-20wt.%Cu composite powders, its SEM photograph is as shown in figure 4, XRD spectrum is as shown in Figure 5.
Embodiment 2
Take Na2WO4·2H2O 99.59g, CuSO4·5H2O 24.12g, Zn (NO3)2·6H2O 61.07g, addition go from Sub- water 300mL is made into mixed solution, is placed in autoclave and is reacted, and reaction temperature is 180 DEG C, and reaction time 3h, is stirred Speed 400r/min is mixed, by the sample filtering after reaction, cleaning, drying, after being dried before copper tungstate-Zinc Tungstate composite powder Drive body.Presoma is placed in atmosphere furnace and is reduced in a hydrogen atmosphere, reduction temperature is 1000 DEG C, and recovery time 1h, is surpassed Thin W-10wt.%Cu composite powders.
Comparative example
Take Na2WO4·2H2O 99.59g, CuSO4·5H2O 75.38g, add deionized water 300mL and are made into mixed solution, It is placed in autoclave and is reacted, reaction temperature is 160 DEG C, reaction time 5h, mixing speed 400r/min, after reaction Sample filtering, cleaning, drying, copper tungstate powder precursor after being dried.Presoma is placed in atmosphere furnace in hydrogen gas Reduced under atmosphere, reduction temperature is 800 DEG C, recovery time 3h, obtains ultra-fine W-25.82wt.%Cu composite powders.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description Point is contained at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms is not It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office Combined in an appropriate manner in one or more embodiments or example.In addition, without conflicting with each other, the skill of this area Art personnel can be tied the different embodiments or example described in this specification and different embodiments or exemplary feature Close and combine.
Although the embodiment of the present invention has been shown and described above, it is to be understood that above-described embodiment is example Property, it is impossible to limitation of the present invention is interpreted as, those of ordinary skill in the art within the scope of the invention can be to above-mentioned Embodiment is changed, changes, replacing and modification.

Claims (7)

  1. A kind of 1. method for preparing ultra-fine W-Cu composite powders, it is characterised in that including:
    (1) mantoquita, zinc salt and sodium tungstate solution are mixed, to obtain mixed solution;
    (2) mixed solution is sent and is stirred, reacts into autoclave, so as to liquid after being reacted;
    (3) liquid after the reaction is filtered and cleaning treatment, so as to obtain copper tungstate-Zinc Tungstate composite powder presoma and Filtered fluid;
    (4) processing is dried in the copper tungstate-Zinc Tungstate composite powder presoma, before composite powder after being dried Drive body;
    (5) composite powder presoma after the drying is subjected to reduction treatment in a hydrogen atmosphere, is answered to obtain ultra-fine W-Cu Close powder.
  2. 2. according to the method described in claim 1, it is characterized in that, in step (1), by the mantoquita and the zinc salt, institute State sodium tungstate solution according to Cu2+And Zn2+The sum of molal quantity and Na2WO4Molal quantity is 1~2:1 is mixed.
  3. 3. according to the method described in claim 1, it is characterized in that, in step (2), the mixing speed is 200-500r/ min。
  4. 4. the method according to claim 1 or 3, it is characterised in that in step (2), the pressure in the autoclave Power is 0.3-1.5MPa.
  5. 5. according to the method described in claim 4, it is characterized in that, in step (2), the reaction temperature is taken the photograph for 100-180 Family name's degree, reaction time 1-5h.
  6. 6. according to the method described in claim 1, it is characterized in that, in step (5), the temperature of the reduction treatment is 700- 1000 degrees Celsius, time 1-3h.
  7. 7. a kind of ultra-fine W-Cu composite powders, it is characterised in that the composite powder is using any one of claim 1-6 What the method for preparing ultra-fine W-Cu composite powders was prepared.
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CN110252326A (en) * 2019-06-18 2019-09-20 华南理工大学 A kind of copper tungstate@zinc oxide composite photocatalyst and the preparation method and application thereof
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CN108772569A (en) * 2018-06-25 2018-11-09 天津大学 A kind of hydrothermal preparing process of superfine nano tungsten powder
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