CN104451222A - Preparation method of nano W-Cu composite block material - Google Patents
Preparation method of nano W-Cu composite block material Download PDFInfo
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- CN104451222A CN104451222A CN201410841512.0A CN201410841512A CN104451222A CN 104451222 A CN104451222 A CN 104451222A CN 201410841512 A CN201410841512 A CN 201410841512A CN 104451222 A CN104451222 A CN 104451222A
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Abstract
The invention discloses a preparation method of a nano W-Cu composite block material. The preparation method comprises the following steps: adding a pre-mixed solution prepared by organic monomers, a cross-linking agent and distilled water as well as tungsten trioxide and copper oxide powder, and a dispersing agent into the pre-mixed solution, thereby preparing slurry; performing ball-milling on the slurry, thereby obtaining injection molding slurry; adding an initiator and a catalyst into the mould injection molding slurry, injecting into the mould, drying, thereby obtaining a gel preform body; heating and roasting the gel preform body; reducing roasted products in the presence of hydrogen gas, thereby obtaining nano W-Cu composite preform body; performing in-situ heating and sintering on the composite preform body, thereby obtaining an ultra-fine grain W-Cu composite block material. After mixing, the preparation method is simple and controllable in process, free of complex equipment, low in cost, high in production efficiency, capable of realizing near net shaping and suitable for industrial volume production. The W-Cu composite block material prepared by the preparation method disclosed by the invention has relative density up to 97%, uniform and fine W particles, a thermal expansion coefficient of 6.8*10<-6>/K to 7.6*10<-6>/K, and vickers hardness number not smaller than 328HV.
Description
Technical field
The present invention relates to a kind of preparation method of high-dispersion nano W-Cu composite block material, belong to powder metallurgy preparing technical field.
Background technology
W-Cu matrix material has that good hot strength, anti-electric-arc are ablative, the feature such as high rigidity, low-expansion coefficient, electric-conductivity heat-conductivity high, can be used as electrical contact material, electrode materials, electrical heating alloys, heat sink or electronic package material, be widely used in the fields such as machinery, electrotechnical, electronic, aerospace, instrument, information and military project.But W-Cu matrix material is typical pseudoalloy, W, Cu are immiscible, time powder sintered, wettability is poor, and prior powder metallurgy method cannot be obtained at all, and density is high, the W-Cu matrix material of composition homogeneous microstructure, high comprehensive performance, cannot meet the more high performance requirements of modern technologies.But be raw material according to W-Cu composite powder that is ultra-fine or nanometer, effectively can solve the problems such as W, Cu densified sintering product is poor, composition tissue odds.
The method preparing nanograined W-Cu powder at present mainly contains: mechanical alloying, co-precipitation, sol-gel, spraying dry etc.These methods have its obvious defect, thus restrict its industrial application.Though mechanical alloying method processing unit is simple, is easy to introduce impurity, powder lack of homogeneity, Ball-milling Time are long; The powder constituents prepared of the wet chemical methods such as sol-gel, liquid-phase reduction and coprecipitation method is even, but complex process and being difficult to controls, powder dispersity is poor, cost is expensive, be difficult to realize mass industrial production; And there is problems such as needing special spraying equipment, investment is large, cost is high, gained powder dispersity is poor in spraying dry rule.
On the other hand, even if adopt nanograined W-Cu powder to be raw material, because its surface-area is large, poor fluidity, easily to reunite, traditional drawing method often cannot play the advantage of nanometer powder completely when shaping nanometer powder, make the W-Cu composite property prepared still not reach requirement.Traditional ceramic process combines with polymer chemistry by gel casting technology dexterously, is a kind of novel near-net-shape technology.Organic monomer and linking agent polymerization reaction take place under certain condition, the three-dimensional net structure formed is wrapped in equally distributed powder particle, thus avoids the reunion of nanometer powder thus cause the shortcoming of tissue odds and over-all properties difference.This manufacturing process has been successfully applied among pottery and metal-powder field, but because tungsten powder density great Yi causes layering when being applied to W-Cu powder, is thus badly in need of improving.
Summary of the invention
The object of the invention is to overcome the deficiency of prior art and provide that a kind of processing unit is simple, cost is low, be easy to realize the near clean shaping preparation method of the nanograined W-Cu composite block material produced in enormous quantities.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, comprises the following steps:
The first step: high concentration slurry is prepared
After organic monomer and linking agent 20 ~ 100:1 mixing by volume, adding distil water is mixed with the premixed liquid that mass concentration is 10 ~ 35wt%;
By the tungsten copper mass ratio of design, take tungstic oxide and cupric oxide powder respectively, the powder taken is added in premixed liquid, add the dispersion agent accounting for powder quality 1 ~ 2.5wt.% simultaneously, be mixed with slurry;
Second step: prepared by injection molding slurry
The first step gained slurry is carried out one-level ball milling and secondary ball milling successively;
During one-level ball milling, the solid volume fraction controlling slurry is 70 ~ 65vol.%, ratio of grinding media to material 8:1 ~ 10:1, and drum's speed of rotation 250 ~ 400r/min, carries out secondary ball milling after ball milling 4 ~ 10h; Ratio of grinding media to material is the mass ratio of ball milling ball and powder;
During secondary ball milling, add premixed liquid, regulate solid volume fraction to the 50 ~ 52vol.% of slurry and pH value to 8 ~ 10 of material of sizing mixing, drum's speed of rotation 100 ~ 150r/min, Ball-milling Time 0.5 ~ 1h, the effect of secondary ball milling is that slurry is mixed further, obtains injection molding slurry;
3rd step: casting and solidification
In second step gained injection molding slurry, add initiator and catalyzer, after being uniformly mixed, inject curing mold, leave standstill in 50 ~ 80 DEG C, completely after solidification, in 100 ~ 110 DEG C of dryings, obtain gel base;
4th step: calcination is reduced
Gel base is heated under air atmosphere 500 ~ 600 DEG C of insulations, after getting rid of the organism in base substrate, continues to be warming up to 700 ~ 800 DEG C and carry out calcination; Calcinate, in a hydrogen atmosphere in 650 ~ 750 DEG C of reduction, obtains high homodisperse nanograined W-Cu composite body;
5th step: in-situ sintering
After reduction terminates, continue original position and be warming up to 1150 ~ 1280 DEG C of sintering, obtain the Ultra-fine Grained W-Cu composite block material of high, the homogeneous microstructure of densification.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in premixed liquid, organic monomer is acrylamide (AM) or Methacrylamide (MAM); Linking agent is N, N ,-methylene-bisacrylamide (MBAM) or diallyl tartrate diamide (DATDA).
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, described tungstic oxide and cupric oxide powder are commercial powder product, and the granularity of tungstic oxide is 10-100 μm; The granularity of cupric oxide powder is 10-100 μm.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, described dispersion agent is polyethylene pyrrole network alkane ketone or ammonium citrate.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in the 3rd step, after adding initiator and catalyzer, the polyreaction of trigger monomer and linking agent, generates the gelinite with three-dimensional net structure.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, the addition of described initiator and catalyzer accounts for 0.1 ~ 4wt.% of stock quality; Described initiator is ammonium persulphate (APS), and described catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine (TEMED).
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in the 4th step, gel base is 1-2 hour 500 ~ 600 DEG C of binder removal times, and 700 ~ 800 DEG C of calcination times are 1 ~ 2h, and 650 ~ 750 DEG C of hydrogen atmosphere recovery times are 1 ~ 2h.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in the 4th step, after calcining reduction, directly grinds that the W-Cu nanocomposite powder granularity obtained is 200 ~ 400nm, grain fineness number is 30 ~ 35nm; Composition homogeneous microstructure, good dispersity, narrow particle size distribution.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in the 5th step, the sintered heat insulating time is 1.5 ~ 2h.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in the 5th step, sinters density >=97% of the nanograined W-Cu composite block material obtained, grain fineness number 500 ~ 900nm; Gained block materials is Ultra-fine Grained, and composition homogeneous microstructure, density is high.
The preparation method of a kind of nanograined W-Cu composite block material of the present invention, in W-Cu nanocomposite powder or block materials, the mass ratio of W and Cu is: W:Cu=90:10 ~ 70:30.
The invention has the advantages that:
1, high density wet-grinding technology and relative device is adopted, and the solid volume fraction controlling slurry is at 70 ~ 65vol.%, make to be refined to about 200nm in the raw material powder short period of time, greatly Ball-milling Time can be shortened than tradition dry grinding or ma process, improve the uniformity coefficient of powder size and composition, reduce energy consumption, decrease the introducing of impurity simultaneously; In addition, the lattice distortion that mechanical milling process is introduced can reduce calcination temperature, impels mesophase spherule CuWO
4formation, this makes follow-up reduction temperature reduce, and can be reduced to 650 DEG C.
2, gel injection method is adopted, be in making the raw material powder relative loose of super-refinement after solidification among a three-dimensional polymer mesh structure, the growing up and reunite of the nanograined W-Cu powder that can effectively avoid the formation of during low-temperature reduction, thus make that the W-Cu composite powder granularity of preparation is tiny, narrow particle size distribution, Composition and structure evenly, good dispersity.Directly can obtain that the densification of arbitrary shape is high according to original position intensification sintering process, the Ultra-fine Grained W-Cu block materials of homogeneous microstructure or goods.
3, adopt Tungsten oxide 99.999 and cupric oxide to be raw material, two-phase is fragility, and grinding efficiency is higher, and powder fragmentation speed, is conducive to ball milling thinning process; When carrying out gel casting, use oxide compound can effectively avoid directly adopting metal-powder for raw material and the demixing phenomenon that exists in slurry and injection molded process, greatly improve the homogeneity of structure of W-Cu matrix material; W-Cu composite block material prepared by the present invention, relative density arrives more than 97%, W particle and is less than 1.2 μ, and evenly tiny, Cu phase is that continuous print reticulated structure is evenly distributed in around W phase, and thermal expansivity is 6.8 × 10
-6/ K to 7.6 × 10
-6between/K, vickers hardness number>=328HV.
4, the inventive method technique is simple, controlled, and without the need to complex apparatus, cost is low, and production efficiency is high, can realize near-net-shape, be applicable to industrial volume production.
Accompanying drawing explanation
Figure 1 shows that process flow sheet of the present invention.
After Figure 2 shows that the wet-milling of the embodiment of the present invention 2 middle and high concentration, powder SEM schemes.
Figure 3 shows that the cross-section morphology SEM of W-Cu composite block material prepared by the present invention schemes.
As can be seen from accompanying drawing 2: powder is evenly tiny, spherical in class, without obvious agglomeration.
As can be seen from accompanying drawing 3: W-Cu composite block material compact structure, W uniform particles is tiny, and the mean sizes of W particle is about 870nm, and Cu phase is that continuous print reticulated structure is evenly distributed in around W phase.
Embodiment
Embodiment 1
Acrylamide (AM) and N, N ,-methylene-bisacrylamide (MBAM) by volume 20:1 phase mixes, and adds distilled water and be mixed with the premixed liquid that concentration is 25wt.%; Tungstic oxide (24.79 μm) and cupric oxide powder (16.56 μm) is taken in W-10wt.%Cu ratio, the powder taken is added in premixed liquid, add the dispersion agent accounting for powder quality 2wt.% simultaneously, be mixed with the slurry of 68vol.%, Ball-milling Time 6h under the condition of ratio of grinding media to material 10:1, rotating speed 400r/min; Add premixed liquid, the solid volume fraction of material of sizing mixing is 50vol.%, adds the pH to 10 that ammoniacal liquor regulates slurry, with rotating speed 100r/min ball milling 1h; Add ammonium persulphate (APS) initiator and N, N, N, N-Tetramethyl Ethylene Diamine (TEMED) catalyzer of 0.8wt.%, the even also injection molding of rapid stirring, leaves standstill 5min and gel solidification occurs at 70 DEG C of temperature; Gel base, in 110 DEG C of dry 0.5h, is warming up to 540 DEG C of insulation 1h binder removals, and then rises to 800 DEG C of calcination 1h; Burning forging product is in a hydrogen atmosphere in 750 DEG C of reduction 1.5h, and namely obtain high dispersive even W-Cu composite body, powder average particle size is 260nm; After reduction, adopt original position to be warming up to 1200 DEG C of sintering 1.5h immediately, obtain high-compactness, homodisperse ultra-fine W-Cu composite block material; The relative density of sintered compact is that the mean sizes of 97.2%, W particle is about 870nm, and evenly tiny, Cu phase is that continuous print reticulated structure is evenly distributed in (see accompanying drawing 3) around W phase; Thermal expansivity is about 7.4 × 10
-6/ K, vickers hardness number reaches 392HV.
Embodiment 2
By Methacrylamide (MAM) and N, N ,-methylene-bisacrylamide (MBAM) 10:1 mixing by volume, adds distilled water and is mixed with the premixed liquid that concentration is 18wt.%; By tungsten and copper mass than for 75:25 is by the tungsten trioxide powder that takes and cupric oxide powder, add in premixed liquid, add the dispersion agent ammonium citrate accounting for powder quality 1.5wt.% simultaneously, be mixed with the slurry of 70vol.%, Ball-milling Time 10h under the condition of ratio of grinding media to material 10:1, rotating speed 400r/min; Again add premixed liquid, make the solid volume fraction of slurry be 55vol.%, regulate the pH to 10 of slurry, with rotating speed 100r/min ball milling 1h; Add ammonium persulphate (APS) initiator and N, N, N, N-Tetramethyl Ethylene Diamine (TEMED) catalyzer of 0.8wt.%, the even also injection molding of rapid stirring, leaves standstill 5min and gel solidification occurs at 70 DEG C of temperature; Gel base, in 110 DEG C of dry 0.5h, is warming up to 600 DEG C of insulation 1h and gets rid of organism, then rise to 800 DEG C of calcination 1h; Burning forging product, in a hydrogen atmosphere in 700 DEG C of reductase 12 h, obtains high dispersive even W-Cu composite body; Original position sinters 2h at being warming up to 1150 DEG C, obtains the complicated shape W-Cu composite block material of high-compactness; The relative density of sintered compact is 97.9%, and average radial shrinking percentage is 12.98%, thermal expansivity about 6.9 × 10
-6/ K, vickers hardness number reaches 347HV.
Claims (10)
1. a preparation method for nanograined W-Cu composite block material, comprises the following steps:
The first step: high concentration slurry is prepared
After organic monomer and linking agent 20 ~ 100:1 mixing by volume, adding distil water is mixed with the premixed liquid that mass concentration is 10 ~ 35wt%;
By the tungsten copper mass ratio of design, take tungstic oxide and cupric oxide powder respectively, the powder taken is added in premixed liquid, add the dispersion agent accounting for powder quality 1 ~ 2.5wt.% simultaneously, be mixed with slurry;
Second step: prepared by injection molding slurry
The first step gained slurry is carried out one-level ball milling and secondary ball milling successively;
During one-level ball milling, the solid volume fraction controlling slurry is 70 ~ 65vol.%, ratio of grinding media to material 8:1 ~ 10:1, and drum's speed of rotation 250 ~ 400r/min, carries out secondary ball milling after ball milling 4 ~ 10h;
During secondary ball milling, add premixed liquid, regulate solid volume fraction to the 50 ~ 52vol.% of slurry and pH value to 8 ~ 10 of material of sizing mixing, drum's speed of rotation 100 ~ 150r/min, Ball-milling Time 0.5 ~ 1h, obtain injection molding slurry;
3rd step: casting and solidification
In second step gained injection molding slurry, add initiator and catalyzer, after being uniformly mixed, inject curing mold, leave standstill in 50 ~ 80 DEG C, completely after solidification, in 100 ~ 110 DEG C of dryings, obtain gel base;
4th step: calcination is reduced
Gel base is heated under air atmosphere 500 ~ 600 DEG C of insulations, after getting rid of the organism in base substrate, continues to be warming up to 700 ~ 800 DEG C and carry out calcination; Calcinate in 650 ~ 750 DEG C of reduction, obtains nanograined W-Cu composite body in a hydrogen atmosphere;
5th step: in-situ sintering
After reduction terminates, continue original position and be warming up to 1150 ~ 1280 DEG C of sintering, obtain W-Cu composite block material.
2. the preparation method of a kind of nanograined W-Cu composite block material according to claim 1, is characterized in that: in premixed liquid, and organic monomer is acrylamide or Methacrylamide; Linking agent is N, N ,-methylene-bisacrylamide or diallyl tartrate diamide.
3. the preparation method of a kind of nanograined W-Cu composite block material according to claim 1, is characterized in that: the granularity of described tungstic oxide is 10-100 μm; The granularity of cupric oxide powder is 10-100 μm.
4. the preparation method of a kind of nanograined W-Cu composite block material according to claim 1, is characterized in that: described dispersion agent is polyethylene pyrrole network alkane ketone or ammonium citrate.
5. the preparation method of a kind of nanograined W-Cu composite block material according to claim 1, is characterized in that: in the 3rd step, after adding initiator and catalyzer, the polyreaction of trigger monomer and linking agent, generates the gelinite with three-dimensional net structure.
6. the preparation method of a kind of nanograined W-Cu composite block material according to claim 5, is characterized in that: the addition of described initiator and catalyzer accounts for 0.1 ~ 4wt.% of stock quality; Described initiator is ammonium persulphate, and described catalyzer is N, N, N, N-Tetramethyl Ethylene Diamine.
7. the preparation method of a kind of nanograined W-Cu composite block material according to claim 1, it is characterized in that: in the 4th step, gel base is 1-2 hour 500 ~ 600 DEG C of binder removal times, and 700 ~ 800 DEG C of calcination times are 1 ~ 2h, and 650 ~ 750 DEG C of hydrogen atmosphere recovery times are 1 ~ 2h.
8. the preparation method of a kind of nanograined W-Cu composite block material according to claim 1-7 any one, is characterized in that: in the 5th step, and the sintered heat insulating time is 1.5 ~ 2h.
9. the preparation method of a kind of nanograined W-Cu composite block material according to claim 8, is characterized in that: in nanograined W-Cu composite block material, the mass ratio of W and Cu is: W:Cu=90:10 ~ 70:30.
10. the preparation method of a kind of nanograined W-Cu composite block material according to claim 9, is characterized in that: in the 5th step, sinters density >=97% of the nanograined W-Cu composite block material obtained, grain fineness number 500 ~ 900nm.
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Cited By (3)
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CN108356287A (en) * | 2018-01-22 | 2018-08-03 | 北京科技大学 | A method of catalysis gel prepares tungsten dispersed and strengthened copper-based composite material |
CN113664202A (en) * | 2021-08-25 | 2021-11-19 | 蔡精敏 | Process for preparing tungsten-copper composite material blank with complex shape |
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