CN100427247C - Method for preparing copper powder - Google Patents
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- CN100427247C CN100427247C CNB2006100201646A CN200610020164A CN100427247C CN 100427247 C CN100427247 C CN 100427247C CN B2006100201646 A CNB2006100201646 A CN B2006100201646A CN 200610020164 A CN200610020164 A CN 200610020164A CN 100427247 C CN100427247 C CN 100427247C
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Abstract
The present invention relates to a method for preparing metal copper powder, which belongs to the technical field of metal material. Firstly, initial copper powder is prepared by using a granulation method, a liquid phase electrochemical method or a liquid phase reducer method. Secondly, a predecessor is prepared (comprising a system composed of the prepared initial copper powder, an electrolyte, a few reducer and water). Thirdly, the predecessor is put in the environment of alkaline and a mild reducing agent, and hydrothermal treatment is implemented to the predecessor under the condition of 120 to 300 DEG C for 30 minutes to 48 hours. Finally, centrifugal separation is implemented to the predecessor, is cleaned by deionized water and anhydrous alcohol containing benzortiazoel and is dried in a vacuum condition so as to obtain the metal copper powder with good dispersibility, high sphericity and strong oxidation resistance. Compared with metal copper powder prepared by the granulation method, the liquid phase electrochemical method or the liquid phase reducer method, the metal copper powder prepared by the present invention has the advantages of even grain size distribution, high sphericity and good oxidation resistance. The metal copper powder prepared by the present invention is as good as metal copper powder prepared by a vapor phase method, and the cost of the metal copper powder prepared by the present invention is greatly reduced.
Description
Technical field
A kind of method for preparing copper powder belongs to the metal material technical field, is specifically related to the technology of preparing of copper powder.
Background technology
Copper powder is meant that metallic copper simple substance powder is the metal powder material of main component.Copper powder is the important raw and processed materials of powder metallurgy, be mainly used in copper base friction material, electrical carbon product, oiliness bearing, contact alloy, chip capacitor, chemical industry or sintering machinery part etc., in industry such as aviation, automobile, national defence, military affairs, electronics, be with a wide range of applications.In general, the metallic particles sphericity is high more, and then specific area is more little, is present in the quantity few more (being that active atomic is few more) of the atom on surface, and then the antioxygenic property of metallic particles is good more; On the other hand, the metallic particles particle diameter is more little, and its surface area is also big more, and its antioxygenic property is also poor more.
Usually the method for preparing copper powder and copper alloy powder has vapor phase method, liquid phase method and mechanical crushing method etc.Vapor phase method prepares copper powder and is meant and under vacuum condition the metallic copper organic compound is decomposed to form copper atom that copper atom condenses becomes copper powder again.Vapor phase method prepares in the process of copper powder, because capillary effect, than the copper powder that is easier to make form of spherical particles, and prepared copper powder particle size distribution range is narrower, particle diameter is controlled, oxidation resistance is higher, but because vapor phase method equipment requires height, reaction need condition be carried out under certain vacuum condition, so it costs an arm and a leg.Liquid phase method is mainly to be to adopt reducing agent that metal copper ion is reduced to metallic copper simple substance.Although this method price is low, the metallic particles particle diameter of preparation is very little, and the particle diameter skewness, and specific area is huge, and oxidation resistance is relatively poor.Mechanical crushing method is that mechanical means such as employing ball milling are pulverized bulky grain and are granule with previously prepared powder just, the metal-powder pattern systematicness extreme difference of this method preparation, and grain diameter is big.
Because vapor phase method prepares copper powder equipment requirement height, cost an arm and a leg, and the prepared copper powder pattern systematicness extreme difference of mechanical crushing method, and grain diameter is big, can not adapt to the requirement of industrial applications, so liquid phase method prepares the emphasis that copper powder becomes present research.
When liquid phase method prepares copper powder, can adopt reducing agent and electrochemical method.Electrochemical process prepares copper powder by the method in cathodic reduction and is dendroid, and is different, and its pollution is big, and powder property is poor, and granularity is generally at (about 40～120 μ m).Adopting reducing agent to prepare copper powder is the emphasis of studying at present, and the reducing agent kind of use is a lot.U.S. Pat 5741347 adopts hydrazine as reducing agent, prepares copper powder under alkali condition; It is that reducing agent prepares superfine cupper powder that Chinese patent CN1188700A adopts sodium dithionite.The copper powder of these method preparations is because particle diameter is little, and size distribution is big, and antioxygenic property is very poor.
Summary of the invention
Purpose of the present invention is exactly, particle diameter poor for the powder property of the copper powder that the overcomes liquid phase method preparation shortcomings such as wide and antioxygenic property difference that distribute, and prepares the copper powder that particle size distribution range is narrow, sphericity is high and antioxygenic property is good.
Detailed technology scheme of the present invention is:
A kind of method for preparing copper powder, specific embodiment is characterized in that as shown in Figure 1 it comprises the steps:
1. preparation initial copper powder.Initial copper powder can adopt mechanical crushing method, liquid phase electrochemical process or the preparation of liquid-phase reduction agent method.
2. preparation predecessor.Initial copper powder is put into water, to 11-14, add the reducing agent that is equivalent to initial copper powder 0.5-10% quality and prepare predecessor with the pH value of NaOH, potassium hydroxide or ammoniacal liquor regulator solution.
3. hydrothermal treatment consists and post processing.Predecessor is transferred in the pyroreaction still, is warming up to 120～300 ℃, and handled 30 minutes～48 hours under the water vapor pressure under the corresponding temperature, the water circulation is cooled to below 50 ℃ then, and the liquid-solid system after handling is carried out centrifugation; Centrifugation gained solid product cleaned to pH value of solution with pure water be neutral and do not have electrolyte substantially, can obtain the copper powder that particle size distribution range is narrow, sphericity is high, oxidation resistance is strong after under vacuum condition, drying at last.
According to the prepared copper powder of above step, color and luster is purplish red, and particle size range to micron dimension, can be preserved not oxidized for a long time (its oxidizing temperature can reach about 230 ℃) in sub-micron under the normal temperature environment.
If adopt the liquid phase electrochemical process to prepare initial copper powder, concrete grammar can be in the step 1.: at first mantoquita is dissolved in the deionized water, adds sulfuric acid and surfactant, make the electrolyte of copper powder; Be anode with the copper coin then, inert metal plates such as copper coin or stainless steel are negative electrode, at 2.5-200A/dm
2Carry out electrolysis under the current density, prepare the electrolysis initial copper powder.
Be equipped with initial copper powder as if employing liquid-phase reduction agent legal system in the step 1., concrete grammar can be: at first mantoquita is dissolved in the deionized water, and extremely alkaline with the pH value of NaOH, potassium hydroxide or ammoniacal liquor regulator solution, add surfactant as dispersant, stir, form suspension; Suspension is warmed up to 50～90 ℃ then, stirs adding reducing agent down, need in the course of reaction to add alkaline matter to keep the pH value of reaction system; When reaction system has only a small amount of gas generation, add an amount of reducing agent again, continue to stir also ageing 5～120 minutes, after initial copper powder is prepared in centrifugation.
When adopting liquid phase electrochemical process or liquid-phase reduction agent legal system to be equipped with initial copper powder, used mantoquita can be inorganic mantoquita or organic copper salts such as copper formate, copper acetate such as copper chloride, copper bromide, copper sulphate.
When preparing predecessor in the step 2., can add an amount of surfactant as dispersant, to obtain finely dispersed predecessor.
In the last handling process of the described hydrothermal treatment consists of step 3., the solid product of centrifugation gained is after the pure water washing, the available absolute ethyl alcohol dehydration that contains 0.5% left and right sides benzotriazole, vacuum drying under 60～160 ℃/650～760mmHg then promptly gets the end product copper powder.The purpose of using benzotriazole is that the surface that is allowed to condition at copper powder forms layer protecting film, with the antioxygenic property of further raising copper powder.Through containing the absolute ethyl alcohol processed of 0.5% left and right sides benzotriazole, and after vacuum drying under 60～160 ℃/650～760mmHg the copper powder of gained, its oxidizing temperature can be increased to about 260 ℃.
Used reducing agent can be sodium hypophosphite, sodium dithionate, glycerine, hydrazine and hydrazine compound, formaldehyde and senior aldehydes, boron hydride, vitamin C etc. in the said process; Used surfactant can be JFC type surfactant, OP-10, polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA), polyethylene glycol, neopelex, gelatin etc.
Hydro-thermal method is meant the predecessor of a definite form (as the slip that has prepared, powder that drying was handled or solution etc.), be placed in the autoclave, under the certain high temperature condition of high voltage, carry out hydro-thermal reaction, obtain the powdery pulp of crystallization, through post processings such as separation, washing, dryings, prepare required powder method then.Usually utilize the copper powder of liquid phase electrochemical process or liquid-phase reduction agent method preparation,, have a large amount of lattice defects, make to be difficult to the very easily oxidation of prepared copper powder to obtain highly purified copper powder because degree of crystallinity is poor.And hydro-thermal reaction is to carry out in material high degree of dispersion, good fluidity and the very uniform thin environment that distributes, thus can obtain well-crystallized's powder, thus improve the antioxygenic property of copper powder; In addition, adopt hydro-thermal method can reduce the aggregate formation of powder and the introducing of impurity, make powder have good good dispersion and the high characteristics of purity, its particle diameter substep is also more even.
Also need to prove, predecessor in the pyroreaction still reaction temperature and certain relation was arranged between the reaction time, if reaction temperature is higher, the then required reaction time is shorter; If reaction temperature is lower, the then required reaction time is longer.In addition, the reaction time is long more, and the particle diameter of prepared copper powder is big more; Otherwise the particle diameter of prepared copper powder is more little.
Essence of the present invention is: at first adopt liquid phase method electrochemical process or liquid-phase reduction agent legal system to be equipped with initial copper powder, prepare predecessor (comprising the system that the initial copper powder that prepared, electrolyte, a small amount of reducing agent and water are formed) then, then predecessor is placed the environment of alkalescence and weak reductant, carry out hydrothermal treatment consists, in the hydrothermal treatment consists process, the copper powder size in the predecessor is narrowed down gradually, surface topography shifts to spheroidization gradually, reduced the quantity of surface atom like this, the copper powder oxidation resistance of preparation obviously increases.
The invention has the beneficial effects as follows: 1, compare with the prepared copper powder of mechanical crushing method, liquid phase electrochemical process or liquid-phase reduction agent method, the prepared copper powder particle diameter of the present invention distributes more evenly, sphericity is higher and antioxygenic property is better; 2, prepared copper powder performance is not second to the prepared copper powder of employing vapor phase method, but cost reduces greatly.
Description of drawings
Fig. 1 is the preparation method's of an a kind of copper powder of the present invention process flow diagram.
Fig. 2 adopts liquid-phase reduction agent method to make ESEM (SEM) photo of the copper powder of preparation, and as can be seen, liquid-phase reduction agent method is made the copper powder particle diameter skewness of preparation from photo, and sphericity is relatively poor.
Fig. 3 adopts liquid-phase reduction agent method to make the initial copper powder of preparation and ESEM (SEM) photo of the copper powder after hydrothermal treatment consists, and as can be seen, the copper powder particle diameter after hydrothermal treatment consists distributes very evenly from photo, and sphericity is higher.
The specific embodiment
The specific embodiment one: copper sulphate 20g is dissolved in the deionized water, adds sulfuric acid 180g, sodium chloride 15mg is made into 1l solution, is anode with the fine copper, and polishing stainless steel is a negative electrode, and cathode-current density is 12A/dm
2, at room temperature electrolysis 20min prepares initial copper powder, and copper powder is transferred in another container, adds the 100ml deionized water, and regulating the pH value with NaOH is 13.5, adds the 5ml hydrazine, stirs, and obtains the predecessor of electrolytic copper powder.Predecessor is placed autoclave, be warming up to 180 ℃, reaction 12h, recirculated water cools off fast, uses washed with de-ionized water four times after the centrifugation, then with the ethanol solution dehydration that contains benzotriazole 0.5g/l three times, vacuum drying under 60～160 ℃/650～760mmHg promptly obtains mauve copper powder, and particle diameter mainly is distributed in 5～15 μ m, sphericity is higher, and oxidation resistance doubles above than the copper powder without hydrothermal treatment consists.
The specific embodiment two: the 0.5mol/1 copper-bath 500mL for preparing is placed reactor, and constant temperature is in 80 ℃; NaOH with 5.0mol/L stirs adjusting pH value to 14 down, makes suspension.Stir and drip formaldehyde down in suspension, and maintain more than 13 with the pH value of NaOH control solution, the adding of formaldehyde is till the bubbles volume that reacts generation seldom.Continue to drip a small amount of formaldehyde, stir and continue reaction 10min down, make the initial stage copper powder, be transferred to (the visual volume ratio of copper powder and mother liquor is 1: 4～10) in another container with copper powder with a certain amount of mother liquor, regulating pH with NaOH is 13.5～14, add the formaldehyde of 3ml, stir, obtain the predecessor of reducing agent method preparation.Predecessor is transferred in the autoclave, be warming up to 200 ℃, reaction 120min, recirculated water cools off fast, uses washed with de-ionized water four times after the centrifugation, then with the ethanol solution dehydration that contains benzotriazole 0.5g/l three times, vacuum drying under 60～160 ℃/650～760mmHg promptly obtains copper powder rosy, and particle diameter mainly is distributed in 0.2-0.3 μ m, sphericity increases substantially, and oxidation resistance is than high more than four times without the copper powder of hydrothermal treatment consists.SEM figure before and after handling is shown in Fig. 2,3.
Claims (8)
1, a kind of method for preparing copper powder is characterized in that it comprises the steps:
1). preparation initial copper powder, initial copper powder adopt mechanical crushing method, liquid phase electrochemical process or the preparation of liquid-phase reduction agent method;
2). the preparation predecessor, initial copper powder is put into water, to 11-14, adding is equivalent to the reducing agent of initial copper powder 0.5-10% quality and prepares predecessor with the pH value of NaOH, potassium hydroxide or ammoniacal liquor regulator solution;
3). hydrothermal treatment consists and post processing, predecessor is transferred in the pyroreaction still, is warming up to 120～300 ℃, and under the water vapor pressure under the corresponding temperature, handled 30 minutes～48 hours, the water circulation is cooled to below 50 ℃ then, and the liquid-solid system after handling is carried out centrifugation; Centrifugation gained solid product cleaned to pH value of solution with pure water be neutral and do not have electrolyte substantially, can obtain the copper powder that particle size distribution range is narrow, sphericity is high, oxidation resistance is strong after under vacuum condition, drying at last.
2, a kind of method for preparing copper powder according to claim 1, it is characterized in that adopt the liquid phase electrochemical process to prepare initial copper powder in the step 1., concrete grammar is: at first mantoquita is dissolved in the deionized water, add sulfuric acid and surfactant, make the electrolyte of copper powder; Be anode with the copper coin then, copper coin or corrosion resistant plate are negative electrode, at 2.5-200A/dm
2Carry out electrolysis under the current density, prepare the electrolysis initial copper powder.
3, a kind of method for preparing copper powder according to claim 1, it is characterized in that, adopt liquid-phase reduction agent legal system to be equipped with initial copper powder in the step 1), concrete grammar is: at first mantoquita is dissolved in the deionized water, pH value with NaOH, potassium hydroxide or ammoniacal liquor regulator solution is extremely alkaline, add surfactant as dispersant, stir, form suspension; Suspension is warmed up to 50～90 ℃ then, stirs adding reducing agent down, need in the course of reaction to add alkaline matter to keep the pH value of reaction system; When reaction system has only a small amount of gas generation, add reducing agent again, continue to stir also ageing 5～120 minutes, after initial copper powder is prepared in centrifugation.
4, according to claim 2 or 3 described a kind of methods that prepare copper powder, it is characterized in that, when adopting liquid phase electrochemical process or liquid-phase reduction agent legal system to be equipped with initial copper powder, used mantoquita is copper formate, the copper acetate in copper chloride, copper bromide, copper sulphate or the organic copper salt in the inorganic mantoquita.
5, a kind of method for preparing copper powder according to claim 1 is characterized in that step 2) in preparation during predecessor, add surfactant as dispersant, to obtain finely dispersed predecessor.
6, a kind of method for preparing copper powder according to claim 1, it is characterized in that, in the last handling process of the described hydrothermal treatment consists of step 3), the solid product of centrifugation gained is after the pure water washing, with the absolute ethyl alcohol dehydration that contains benzotriazole 0.5g/l, vacuum drying under 60～160 ℃/650～760mmHg then promptly gets the end product copper powder.
7, according to claim 1,2 or 3 described a kind of methods that prepare copper powder, it is characterized in that described reducing agent is sodium hypophosphite, sodium dithionate, glycerine, hydrazine and hydrazine compound, formaldehyde and senior aldehydes, boron hydride, vitamin C.
8, according to claim 2 or 3 described a kind of methods that prepare copper powder, it is characterized in that described surfactant is JFC type surfactant, OP-10, polyvinylpyrrolidone, polyvinyl alcohol, polyethylene glycol, neopelex, gelatin.
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| WO2009060803A1 (en) * | 2007-11-05 | 2009-05-14 | Sumitomo Metal Mining Co., Ltd. | Copper fine particle, method for producing the same, and copper fine particle dispersion |
| CN101992300A (en) * | 2010-11-04 | 2011-03-30 | 江苏大方金属粉末有限公司 | Preparation method for sintered copper powder material of heat pipe |
| CN102151823B (en) * | 2011-01-26 | 2013-02-27 | 宁波广博纳米新材料股份有限公司 | Antioxidation method of nano copper powder |
| CN103949653B (en) * | 2014-04-02 | 2015-10-28 | 西安交通大学 | A kind of product separation of supercritical water thermal synthesis system and organic ligand recovery system |
| CN104475722A (en) * | 2014-11-12 | 2015-04-01 | 有研粉末新材料（北京）有限公司 | Low-lead, low-apparent-density high-branch-shaped electrolytic copper powder and preparation method thereof |
| CN110116218B (en) * | 2019-05-29 | 2022-06-17 | 西安工程大学 | Preparation method of high-purity narrow-particle-size-distribution copper powder |
| CN110144604B (en) * | 2019-06-17 | 2020-06-09 | 阳谷祥光铜业有限公司 | Preparation process of electrodeposited copper powder |
| CN112021334B (en) * | 2020-09-10 | 2021-06-29 | 中国有色桂林矿产地质研究院有限公司 | Porous copper powder carrier-loaded silver-based antibacterial material and preparation method thereof |
| CN112692305B (en) * | 2021-03-23 | 2021-06-29 | 陕西斯瑞新材料股份有限公司 | Preparation method of batch type 3D printed CuCr composite contact |
| CN113523269B (en) * | 2021-06-08 | 2023-06-16 | 五邑大学 | Copper powder and preparation method and application thereof |
| CN113832500A (en) * | 2021-10-20 | 2021-12-24 | 昆明高聚科技有限公司 | Preparation method of electronic-grade high-purity low-apparent-density dendritic copper powder |
| CN116673479A (en) * | 2023-04-27 | 2023-09-01 | 安徽旭晶粉体新材料科技有限公司 | Preparation method for synthesizing cuprous chloride from pure copper powder and chlorine gas |
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