CN102554218A - Method for preparing tungsten-copper composite powder by means of electroless copper plating - Google Patents
Method for preparing tungsten-copper composite powder by means of electroless copper plating Download PDFInfo
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- CN102554218A CN102554218A CN2011103765798A CN201110376579A CN102554218A CN 102554218 A CN102554218 A CN 102554218A CN 2011103765798 A CN2011103765798 A CN 2011103765798A CN 201110376579 A CN201110376579 A CN 201110376579A CN 102554218 A CN102554218 A CN 102554218A
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Abstract
The invention discloses a method for preparing tungsten-copper composite powder by means of electroless copper plating, which includes the steps: firstly, weighing tungsten powder by 80-95wt% of the mass of the tungsten-copper composite powder needing preparation, and calculating the needed mass of copper; secondly, adding dispersing agents into the tungsten powder, filtering out the tungsten powder after ultrasonic vibration and cleaning the tungsten powder with distilled water; thirdly, weighing copper sulfate pentahydrate by 3.89 times of the calculated mass of the copper, and dissolving the copper sulfate pentahydrate to prepare copper sulfate liquor with the concentration of 4-12g/L; and fourthly, adding the copper sulfate liquor into double complex agent liquor, directly adding NaOH (sodium hydroxide) solid into the double complex agent liquor, adjusting the pH (potential of hydrogen) value of the mixed liquor, adding stabilizing agents into the mixed liquor, heating the mixed liquor in a thermostatic water bath, adding formaldehyde and the tungsten powder into the mixed liquor, heating and stirring the mixed liquor in the thermostatic water bath until the tungsten powder turns red, cleaning lower tungsten-copper composite powder with distilled water and alcohol, and drying the mixed liquor to obtain the tungsten-copper composite powder. The method solves the problem of non-uniformity of a copper coating layer prepared by an existing tungsten-copper composite material preparation method.
Description
Technical field
The invention belongs to powder metallurgical technology, relate to a kind of method for preparing W-Cu composite powder through electroless copper.
Background technology
Tungsten-copper composite material has the advantage of tungsten and copper simultaneously, like high elevated temperature strength, high electrical and thermal conductivity, good anti-galvanic corrosion property, higher hardness, low thermal coefficient of expansion and certain plasticity etc.In addition, can also control and adjust the performance of its corresponding machinery and physics through changing its proportion of composing.This distinctive combination property is applied in electrical contact material and the electrode material tungsten-copper composite material widely.
Traditional tungsten-copper composite material preparation method is infiltration method and lqiuid phase sintering method.During melting infiltration sintering, liquid phase copper only depends on the capillarity of W skeleton hole to infiltrate, and the copper solidifying phase distributes thick and inhomogeneous.During simple liquid-phase sintering, low at a lower temperature wellability makes liquid phase copper be difficult to even distribution, and tungsten powder can seriously be assembled and grows up under the high temperature sintering condition, forms thick heterogeneous structure.So evenly coat layer of copper at tungsten powder surface, and then produce tungsten-copper composite material with the method for sintering or infiltration and can avoid tungsten to contact, strengthen the final combination property that improves tungsten-copper composite material of basal body interface comprehensively with the direct of tungsten.The cladding process of comparative maturity has at present: sol-gel process, electroless plating method etc., though it is wherein gel-sol method method is simple, easy to operate; But clad is inhomogeneous; Be difficult to control coating thickness, and need to coat material formation presoma, the scope of application is limited.The coated powder clad and the powder matrix bond of electroless plating method preparation are tightr, and coating thickness is controlled easily, and the equipment of employing is fairly simple.
Summary of the invention
The purpose of this invention is to provide and a kind ofly prepare the method for W-Cu composite powder, solved the uneven problem of copper-clad coating that exists among the existing tungsten-copper composite material preparation method through electroless copper.
The technical scheme that the present invention adopted is, a kind ofly prepares the method for W-Cu composite powder through electroless copper, and concrete operating procedure is following:
Step 1, the 80～95wt% for preparing the W-Cu composite powder quality as required takes by weighing tungsten powder, and all the other are copper, and according to the required quality of the shared cubage copper of copper;
Step 2 adds dispersant in the tungsten powder that step 1 takes by weighing, filtering out tungsten powder behind the ultrasonic concussion 10min under 40～60 ℃ of temperature, and cleaning with distilled water;
Step 3 takes by weighing cupric sulfate pentahydrate according to 3.89 times of the copper mass that calculates in the step 1, uses dissolved in distilled water, processes the copper-bath that concentration is 4～12g/L;
Step 4 is got natrium citricum and triethanolamine, uses dissolved in distilled water respectively, mixes then to form two enveloping agent solutions, and the copper-bath that then step 3 is made slowly joins under stirring condition in two enveloping agent solutions, obtains suspension;
Step 5 under stirring condition, directly joins the NaOH solid in the suspension of step 4 gained, and adjustment pH value adds stabilizing agent afterwards in 12～14 scopes, obtain mixed liquor;
Step 6, the mixed liquor that step 5 is made is heated to 40～60 ℃ in water bath with thermostatic control, add formaldehyde again, and adds the tungsten powder that step 2 filters out, and becomes muddy liquid;
Step 7 heats the muddy liquid of step 6 gained, and constantly stirs with magnetic stirring apparatus in 40 ℃～60 ℃ waters bath with thermostatic control, tungsten powder is suspended in the solution, reddens until tungsten powder, after the clarification of muddy liquid upper strata, stops heating and stirring;
Step 8; The muddy liquid of completing steps 7 after static 20 minutes, is removed the upper strata settled solution, and the lower sediment thing is W-Cu composite powder; Clean W-Cu composite powder 3 times with distilled water then; Use the alcohol wash W-Cu composite powder again 3 times, then in drying box with 80～100 ℃ temperature drying, promptly accomplish.
Characteristics of the present invention also are,
The tungsten powder particle diameter 6～8um that takes by weighing in the step 1.
Dispersant in the step 2 is PVP, and the concentration of dispersant PVP is 0.8-2g/L.
The concentration of natrium citricum is 8～20g/L in the navy blue suspension that step 4 makes, and the concentration of triethanolamine is 12～24ml/L.
Stabilizing agent in the step 5 is 2,2 '-bipyridyl, and concentration is 0.04～0.08g/L.
The formaldehyde volumetric concentration is 37%～40% in the step 6.
The invention has the beneficial effects as follows that the coordinating group through high molecular surfactant PVP contains N, O atom makes in the dispersion Cu to occur from micro-scale
2+In the enrichment phenomenon of tungsten powder surface, thereby preferentially produce reduction reaction, realize surperficial uniform deposition and coating, avoided the uneven problem of clad ultrafine tungsten powder in the part of enrichment.
Description of drawings
Fig. 1 is the SEM shape appearance figure of original tungsten powder before the electroless copper, and wherein scheming a is to amplify 500 times microscopic appearance, and figure b amplifies 3000 times microscopic appearance;
Fig. 2 is the SEM shape appearance figure of the W-Cu composite powder for preparing of the inventive method, and wherein scheming a is to amplify 500 times microscopic appearance, and figure b amplifies 3000 times microscopic appearance;
Fig. 3 is the XRD figure spectrum of the W-Cu composite powder for preparing of the inventive method.
The specific embodiment
Below in conjunction with the accompanying drawing and the specific embodiment the present invention is elaborated.
The present invention provides a kind of and prepares the method for W-Cu composite powder through electroless copper, and concrete operating procedure is following:
Step 1, the 80～95wt% for preparing the W-Cu composite powder quality as required takes by weighing tungsten powder, tungsten powder particle diameter 6～8um, all the other are copper, and according to the required quality of the shared cubage copper of copper;
Step 2 adds PVP as dispersant in the tungsten powder that step 1 takes by weighing, the concentration of dispersant PVP is 0.8-2g/L, is filtering out tungsten powder behind the ultrasonic concussion 10min under 40～60 ℃ of temperature, and is cleaning with distilled water;
Step 3 takes by weighing cupric sulfate pentahydrate according to 3.89 times of the copper mass that calculates in the step 1, uses dissolved in distilled water, processes the copper-bath that concentration is 4～12g/L;
Step 4; Get natrium citricum and triethanolamine, use dissolved in distilled water respectively, mix forming two enveloping agent solutions then; The copper-bath that then step 3 is made joins under stirring condition in two enveloping agent solutions slowly; Obtain the navy blue suspension, wherein the concentration of natrium citricum is 8～20g/L, and the concentration of triethanolamine is 12～24ml/L;
Step 5 under stirring condition, directly joins the NaOH solid in the suspension of step 4 gained; The pH value of adjustment mixed liquor adds stabilizing agent 2,2 '-bipyridyl afterwards in 12～14 scopes; 2,2 '-bipyridyl concentration is 0.04～0.08g/L, obtains mixed liquor;
Step 6, the mixed liquor that step 5 is made is heated to 40～60 ℃ in water bath with thermostatic control, add volumetric concentration again and be 37%～40% formaldehyde, and adds the tungsten powder that step 2 prepares, and becomes muddy liquid;
Step 7 heats the muddy liquid of step 6 gained, and constantly stirs with magnetic stirring apparatus in 40 ℃～60 ℃ waters bath with thermostatic control, tungsten powder is suspended in the solution, reddens until tungsten powder, after the clarification of muddy liquid upper strata, stops heating and stirring;
Step 8; With the muddy liquid of completing steps 7 after static 20 minutes; Remove the upper strata settled solution; Clean the W-Cu composite powder 3 times of lower floor's deposition then respectively with distilled water, use the alcohol wash W-Cu composite powder again 3 times, the temperature drying with 80～100 ℃ promptly obtains W-Cu composite powder in drying box then.
Embodiment 1
Preparation 5gW-10Cu composite powder is got original tungsten powder 4.5g.At first, original tungsten powder is joined in the beaker, add dispersant PVP0.5g,, filter, clean with distilled water with beaker ultrasonic concussion 10min under 40 ℃.
Get the 1.95g cupric sulfate pentahydrate, and use dissolved in distilled water, the copper-bath that is made into.Get the natrium citricum of 2g and the triethanolamine of 4ml, use dissolved in distilled water.Then copper-bath is joined in the enveloping agent solution under stirring condition slowly, obtain the navy blue suspension.Get NaOH dissolving back this moment and add in the above-mentioned navy blue suspension, the adjustment pH value is 13.And the 2-2 bipyridyl of adding 0.02g.Join tungsten powder and 5ml formaldehyde in the above-mentioned navy blue solution this moment.In 50 ℃ of waters bath with thermostatic control, heat, and constantly stir, tungsten powder is suspended in the solution with magnetic stirring apparatus.Redden to tungsten powder, after the clarification of muddy liquid upper strata, stop heating and stir.With the muddy liquid after static 10 minutes after the plating, remove upper solution, and with distilled water and alcohol wash W-Cu composite powder 3 times, 100 ℃ of dryings in drying box promptly obtain copper-coated tungsten composite powder then.
Embodiment 2
Preparation 5gW-15Cu composite powder is got original tungsten powder 4.25g.At first, original tungsten powder is joined in the beaker, add dispersant PVP0.45g,, filter, clean with distilled water with beaker ultrasonic concussion 10min under 40 ℃.
Get the 2.92g cupric sulfate pentahydrate, and use dissolved in distilled water, the copper-bath that is made into.Get the sodium potassium tartrate tetrahydrate of 3g and the triethanolamine of 6ml, use dissolved in distilled water.Then copper-bath is joined in the enveloping agent solution under stirring condition slowly, obtain the navy blue suspension.Get NaOH dissolving back this moment and add in the above-mentioned navy blue suspension, the adjustment pH value is 13.And the 2-2 bipyridyl of adding 0.03g.Join tungsten powder and 7.5ml formaldehyde in the above-mentioned navy blue solution this moment.In 50 ℃ of waters bath with thermostatic control, heat, and constantly stir, tungsten powder is suspended in the solution with magnetic stirring apparatus.Redden to tungsten powder, after the clarification of muddy liquid upper strata, stop heating and stir.With the muddy liquid after static 10 minutes after the plating, remove upper solution, and with distilled water and alcohol wash W-Cu composite powder 3 times, 100 ℃ of dryings in drying box promptly obtain copper-coated tungsten composite powder then.
Embodiment 3
Preparation 5gW-20Cu composite powder is got original tungsten powder 4g.At first, original tungsten powder is joined in the beaker, add dispersant PVP0.4g,, filter, clean with distilled water with beaker ultrasonic concussion 10min under 40 ℃.
Get the 3.89g cupric sulfate pentahydrate, and use dissolved in distilled water, the copper-bath that is made into.Get the sodium potassium tartrate tetrahydrate of 3.89g and the triethanolamine of 8ml, use dissolved in distilled water.Then copper-bath is joined in the enveloping agent solution under stirring condition slowly, obtain the navy blue suspension.Get NaOH dissolving back this moment and add in the above-mentioned navy blue suspension, the adjustment pH value is 13.And the 2-2 bipyridyl of adding 0.04g.Join tungsten powder and 10ml formaldehyde in the above-mentioned navy blue solution this moment.In 50 ℃ of waters bath with thermostatic control, heat, and constantly stir, tungsten powder is suspended in the solution with magnetic stirring apparatus.Redden to tungsten powder, after the clarification of muddy liquid upper strata, stop heating and stir.With the muddy liquid after static 10 minutes after the plating, remove upper solution, and with distilled water and alcohol wash W-Cu composite powder 3 times, 80 ℃ of dryings in drying box promptly obtain copper-coated tungsten composite powder then.
Embodiment 4
Preparation 5gW-15Cu composite powder is got original tungsten powder 4.25g.At first, original tungsten powder is joined in the beaker, add dispersant PVP0.45g,, filter, clean with distilled water with beaker ultrasonic concussion 10min under 50 ℃.
Get the 2.92g cupric sulfate pentahydrate, and use dissolved in distilled water, the copper-bath that is made into.Get the sodium potassium tartrate tetrahydrate of 3g and the triethanolamine of 6ml, use dissolved in distilled water.Then copper-bath is joined in the enveloping agent solution under stirring condition slowly, obtain the navy blue suspension.Get NaOH dissolving back this moment and add in the above-mentioned navy blue suspension, the adjustment pH value is 13.And the 2-2 bipyridyl of adding 0.03g.Join tungsten powder and 7.5ml formaldehyde in the above-mentioned navy blue solution this moment.In 60 ℃ of waters bath with thermostatic control, heat, and constantly stir, tungsten powder is suspended in the solution with magnetic stirring apparatus.Redden to tungsten powder, after the clarification of muddy liquid upper strata, stop heating and stir.With the muddy liquid after static 10 minutes after the plating, remove upper solution, and with distilled water and alcohol wash W-Cu composite powder 3 times, 100 ℃ of dryings in drying box promptly obtain copper-coated tungsten composite powder then.
Among Fig. 1 figure a and figure b be respectively before the electroless copper original tungsten powder amplify 500 times with 3000 times microscopic appearance, can find out that from scheming a original tungsten powder particles size is inhomogeneous, tangible agglomeration is arranged; Figure b can find out pure tungsten powder surface smoothing, cleaning, and particle is the polygonal shape of rule basically, and what between the particle there be whole face contacts, and the granularity of tungsten powder is at 4～8um.Figure a and figure b are respectively the microscopic appearances of 500 times of the W-Cu composite powders that carry out obtaining behind the electroless copper and 3000 times among Fig. 2; Original tungsten powder before figure a can find out adopts surface dispersant PVP not only to play peptizaiton, and has successfully carried out electroless copper; Figure b can find out that tungsten powder surface becomes coarse, is coated by many tiny particles.Avoid the direct contact between the tungsten particle like this, made things convenient for later sintering and post processing, helped improving the final performance of tungsten-copper composite material.
W-Cu composite powder to the electroless copper preparation carries out X-ray diffraction analysis, and the result is as shown in Figure 3.The data contrast of collection of illustrative plates and card base can be known, is 40.26 °, 58.27 °, the 73.20 ° characteristic diffraction peaks of locating to occur tungsten at 2 θ, respectively (110), (200) and (211) face of the body-centered cubic structure of corresponding tungsten; 2 θ are 43.16 °, 50.30 °, the 74.06 ° characteristic diffraction peaks of locating to occur copper, respectively face-centred cubic structure (111), (200) and (220) face of corresponding copper.The intensity at Cu peak is more weak with respect to the W peak among the figure, and this is because the copper layer that tungsten powder surface coats is thinner.
The present invention adopts the coated powder clad and the powder matrix bond of electroless plating method preparation tightr, and coating thickness is controlled easily, and the equipment of employing is fairly simple.Conventional electroless copper coated tungsten powder must carry out preliminary treatment and comprise alligatoring, sensitization, three steps of activation.Common sensitizer is a stannous chloride, and activator is a palladium bichloride.Possibly introduce low-melting metallic tin in the activation process, tungsten-copper alloy electrovacuum performance is had negative effect.Palladium salt is precious metal salt in addition, and cost is expensive, and is not easy to handle.So we consider the N that contains through high molecular surfactant PVP, the coordinating group of O atom makes in the dispersion Cu to occur from micro-scale
2+In the tungsten powder surface enrichment phenomenon, thereby, realize surperficial uniform deposition and coating, avoided the uneven problem of clad ultrafine tungsten powder preferentially producing reduction reaction in the part of enrichment.The present invention has not only avoided the introduction low melting point element, has practiced thrift cost simultaneously, and has reduced the time of chemical plating process, has improved operating efficiency greatly.
Claims (6)
1. one kind prepares the method for W-Cu composite powder through electroless copper, it is characterized in that concrete operating procedure is following:
Step 1, the 80～95wt% for preparing the W-Cu composite powder quality as required takes by weighing tungsten powder, and all the other are copper, and according to the required quality of the shared cubage copper of copper;
Step 2 adds dispersant in the tungsten powder that step 1 takes by weighing, filtering out tungsten powder behind the ultrasonic concussion 10min under 40～60 ℃ of temperature, and cleaning with distilled water;
Step 3 takes by weighing cupric sulfate pentahydrate according to 3.89 times of the copper mass that calculates in the step 1, uses dissolved in distilled water, processes the copper-bath that concentration is 4～12g/L;
Step 4 is got natrium citricum and triethanolamine, uses dissolved in distilled water respectively, mixes then to form two enveloping agent solutions, and the copper-bath that then step 3 is made slowly joins under stirring condition in two enveloping agent solutions, obtains suspension;
Step 5 under stirring condition, directly joins the NaOH solid in the suspension of step 4 gained, and adjustment pH value adds stabilizing agent afterwards in 12～14 scopes, obtain mixed liquor;
Step 6, the mixed liquor that step 5 is made is heated to 40～60 ℃ in water bath with thermostatic control, add formaldehyde again, and adds the tungsten powder that step 2 filters out, and becomes muddy liquid;
Step 7 heats the muddy liquid of step 6 gained, and constantly stirs with magnetic stirring apparatus in 40 ℃～60 ℃ waters bath with thermostatic control, tungsten powder is suspended in the solution, reddens until tungsten powder, after the clarification of muddy liquid upper strata, stops heating and stirring;
Step 8; The muddy liquid of completing steps 7 after static 20 minutes, is removed the upper strata settled solution, and the lower sediment thing is W-Cu composite powder; Clean W-Cu composite powder 3 times with distilled water then; Use the alcohol wash W-Cu composite powder again 3 times, then in drying box with 80～100 ℃ temperature drying, promptly accomplish.
2. method according to claim 1 is characterized in that, the tungsten powder particle diameter 6～8um that takes by weighing in the step 1.
3. method according to claim 1 is characterized in that, the dispersant in the step 2 is PVP, and the concentration of dispersant PVP is 0.8-2g/L.
4. method according to claim 1 is characterized in that, the concentration of natrium citricum is 8～20g/L in the navy blue suspension that step 4 makes, and the concentration of triethanolamine is 12～24ml/L.
5. method according to claim 1 is characterized in that, the stabilizing agent in the step 5 is 2,2 '-bipyridyl, and concentration is 0.04～0.08g/L.
6. method according to claim 1 is characterized in that, the formaldehyde volumetric concentration is 37%～40% in the step 6.
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| CN103447526A (en) * | 2013-09-11 | 2013-12-18 | 中南大学 | Preparation method of nanometer WC-Co composite powder |
| CN103572268A (en) * | 2012-07-30 | 2014-02-12 | 比亚迪股份有限公司 | Chemical copper plating liquid and chemical copper plating method |
| CN104001929A (en) * | 2014-06-20 | 2014-08-27 | 阮秀仕 | Method for manufacturing copper and tungsten alloy powder through mechanical alloying |
| CN104096837A (en) * | 2014-06-23 | 2014-10-15 | 中国石油天然气集团公司 | Tungsten copper alloy powder industrialized production method |
| CN104550943A (en) * | 2015-01-28 | 2015-04-29 | 中国科学院过程工程研究所 | Spherical copper coating tungsten composite powder, preparation method and application thereof |
| CN109093111A (en) * | 2018-09-21 | 2018-12-28 | 靖江市海源新材料科技有限公司 | A kind of preparation method of copper-tungsten |
| CN109454229A (en) * | 2019-01-07 | 2019-03-12 | 广东省材料与加工研究所 | A kind of pomegranate type tungsten alloy powder and the preparation method and application thereof |
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| CN104550943A (en) * | 2015-01-28 | 2015-04-29 | 中国科学院过程工程研究所 | Spherical copper coating tungsten composite powder, preparation method and application thereof |
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| CN109454229A (en) * | 2019-01-07 | 2019-03-12 | 广东省材料与加工研究所 | A kind of pomegranate type tungsten alloy powder and the preparation method and application thereof |
| CN109454229B (en) * | 2019-01-07 | 2019-12-10 | 广东省材料与加工研究所 | Pomegranate type tungsten alloy powder and preparation method and application thereof |
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Application publication date: 20120711 |