CN103964488A - Method for preparing micro or nano copper oxide powder - Google Patents
Method for preparing micro or nano copper oxide powder Download PDFInfo
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- CN103964488A CN103964488A CN201310034708.4A CN201310034708A CN103964488A CN 103964488 A CN103964488 A CN 103964488A CN 201310034708 A CN201310034708 A CN 201310034708A CN 103964488 A CN103964488 A CN 103964488A
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Abstract
The invention relates to a method for preparing a micro or nano copper oxide powder. The method is as below: fully mixing a micron copper powder obtained by spray deposition or nano a copper powder prepared by an electrolytic method (electrochemical and chemical methods) with a proper amount of 20-80 wt.% of a thermosetting or modified thermoplastic polymer powder; heating the mixture with an air circulation oven to 450-800 DEG C for full oxidization of 10 minutes to few hours according to the amount of the material, so as to prepare loose copper oxide easy to break; and grinding and sieving the copper oxide to obtain required micron or nano copper oxide powder. The copper oxide powder prepared by the invention has similar morphology to the original copper powder through scanning electron microscope observation, and micro or nano scale size. The preparation method has the advanategs of simpleness, convenient operation, simple equipment and no pollution in the production process. The purity of the prepared copper oxide powder depends on the purity of the original copper powder, so that the product has good quality (high purity, and controllable particle size and structure). The method has high production efficiency and low production cost, and is suitable for industrialized production.
Description
Technical field
The present invention relates to cupric oxide powder technology of preparing, it is a kind of thermal plastic high polymer powdered material blend that utilizes copper powder and thermoset or correctability, then carry out oxidation and polymer burning removal that high-temperature oxidation process is realized copper, thereby the cupric oxide of making short texture and easily pulverizing, through grinding the method for the cupric oxide powder of screening acquisition desired particle size.
Background technology
Cupric oxide range of application is very extensive, can be used as the tinting material of glass, enamel, ceramic industry, anti-Zou's agent of paint, and the polishing agent of opticglass, the additive of manufacture dyestuff, and organic catalysis agent carrier etc.; Also can utilize chemical reaction characteristic for the sweetening agent of artificial silk process industry and grease; In addition nanostructure cupric oxide has high-temperature superconductor, huge magnetoresistance and the material of the abnormal characteristic in three different magnetic stages, also can be used as some specific function application.China's productive technology of powdered copper oxide is mainly that the cuprous leaching method of oxidization of copper powder method, volatile salt, copper sulfate calcination method and copper salt solution add alkali synthesis method at present.Oxidization of copper powder method is to take copper ash, copper ashes to carry out oxide treatment as raw material heats in stove, removes moisture and organic impurity in raw material in this process.The oxide compound of producing, after cooling and fragmentation, then carries out secondary oxidation in oxidized still, and the crude product cupric oxide obtaining is through centrifugation, dry, then through broken oxidation repeatedly, thereby make cupric oxide powder.This method energy consumption is large, and the cupric oxide powder particle shape and the size that make are difficult to effective control.The present invention directly utilizes copper powder, fully mixes with the thermal plastic high polymer of thermoset or correctability, through high temperature direct oxidation, forms short texture and breakable cupric oxide, obtains the cupric oxide powder of required form and particle diameter through grinding screening.
Summary of the invention
The object of the invention is according to the globule size of the form of former copper powder, by simple oxidizing reaction, obtain the cupric oxide powder of required form and granularity.
The object of the invention is to be achieved through the following technical solutions.A kind of method of preparing micron or nano-cupric oxide powder, the thermal plastic high polymer powder that it is characterized in that take copper powder and thermoset or correctability is raw material, pass through in air the abundant oxidizing reaction of mixed powder, the cupric oxide porous material that makes short texture and easily pulverize, then through grinding and screening, can obtain the micron similar to former copper powder contour structures or the cupric oxide powder of nanometer.Specifically comprise the following steps: (1) powder mixes; (2) pack mould into; (3) low-temperature prewarming moulding or directly put into oxidized still heating; (4) high temperature oxidation process in; (5) cooling and grinding; (6) screening and packing.Cupric oxide powder preparation method's concrete steps are as follows:
(1) powder mixes: copper powder (can be made to the Micron-Sized Copper Powders Coated of sprayed deposit, also can be the copper powder of the nano-scale prepared by electrolysis process (comprising electrochemistry and chemical method).By the thermal plastic high polymer of copper powder and thermoset or correctability, as resol, epoxy resin or urethane etc. in accordance with the appropriate ratio, as 20-80%(weight percent) copper powder and above-mentioned polymer 80-20%(weight percent) fully mix.The mixing tank of V-structure, two motion blending tank or three-dimensional hybrid in-tank mixing 20 minutes to 2 hours.In mixed powder process, adding quantity is 20-30 grain, diameter is aluminium oxide ceramic ball or the steel ball of 10-12 millimeter, to mix, rotating speed is 20-60 rev/min, with the coarse grid that is less than the 10-12 millimeter of balls diameter, sieves to take out Ceramic Balls or steel ball, by mixed powder, insert in the plastic containers with lid, standby;
The thermoplastic macromolecule material powder of described thermoset or modification is polyurethane, resol, epoxy resin polyethylene/polypropylene, copper powder can be different shape and structure prepared by different methods, and the shape of the cupric oxide after oxidation should be similar with the primary formation of starting material copper powder.If need the cupric oxide powder of micron level spherical structure, with regard to the copper powder with spray deposition, mix and be oxidized.If need the cupric oxide powder of nanoscale, need to mix with the nanostructure copper powder of electrolysis (electrochemistry and chemistry) method with oxide treatment and make.
(2) pack mould into: get a certain amount of above-mentioned powder mixing and pack in the mould of stainless steel, high temperature steel or ceramic structure.Preparation is carried out preheating moulding or is directly carried out oxide treatment.
(3) preheating moulding or directly put into oxidized still: the mould that above-mentioned mixed powder is packed into is placed in low temperature oven to carry out preheating moulding or be directly placed in air circulating oven, carries out heat temperature raising processing.If mould is carried out to thermal pretreatment, preheating mold temperature can be chosen between 150-250 C, and is incubated 10-20 minute; Also can directly the mould with mixed powder is placed in air circulating oven and carry out preheating moulding, preheating mold temperature be about 150-250 ℃, and low-temperature prewarming molding time is 8-12 minute.The polymeric powder mixing solidifies, and after mould cooling, takes out curing material;
(4) high temperature oxidation process in: the mould after preheating moulding is further heated up, temperature is heated to carry out oxidising process in the stove of 650-850C, soaking time is roughly 0.5 hour to 2 hours.
(5) cooling and grinding: cool to the material after above-mentioned oxidation with the furnace room temperature, also can cool to the furnace after 300C, shift out air cooling to room temperature, then above-mentioned materials be taken out and ground, because the thermal plastic high polymer powder of thermoset or correctability plays loose effect in oxidising process
(6) screening and packing: the cupric oxide powder after grinding is sieved, and the order number of screening is selected to carry out with reference to the granularity of original copper powder.Because the particle diameter of particle diameter ratio raw material copper powder is large after oxidation, according to field emission scanning electron microscope analysis and statistics, find: the size (diameter) of the rear particle of oxidation has expanded 25% and even reached 75%.In other words, the diameter of oxidation rear oxidation copper particle is original 1.25 times or 1.75 times.
Implementation example
The invention provides the manufacture method of a kind of micron or nano-cupric oxide powder, the cupric oxide powder of preparing by the Micron-Sized Copper Powders Coated that spray deposition is made.The step of its preparation process is as follows successively:
(1) copper powder and above-mentioned polymer 40%(weight percent powder mixing: by the micron order of sprayed deposit 325 order copper powders, with the thermoplastic polypropylene polymeric powder of correctability, proportionally 60%(weight percent)) fully mix.The mixing in-tank mixing of V-structure 1 hour.In mixed powder process, adding quantity is 20-30 grain, and diameter is the aluminium oxide ceramic ball of 10-12 millimeter, to mix, rotating speed is 20-60 rev/min.Then use sieving to take out Ceramic Balls of coarse grid (aperture is less than the 10-12 millimeter of balls diameter), by mixed powder, insert in the plastic containers with lid, standby;
(2) pack mould into: get the above-mentioned powder mixing and pack in stainless steel peviform structure mold, and surface roughly keeps smooth, directly carry out oxide treatment.
(3) directly put into oxidized still: the above-mentioned mould that mixed powder is housed is placed in to air circulating oven, carries out heat temperature raising processing.
(4) high temperature oxidation process in: heated oxide conditional curve is: 0.5 hour, be heated to 150C, and be suitably incubated 0.5 hour from room temperature.Then within 1 hour, from 150 C, be heated to 700 C, 700 C insulation 1 hour.Air blast keeps air cycle to guarantee that copper powder is fully oxidized formation cupric oxide.The polymeric powder mixing in this process is removed oxidizing fire, forms carbonic acid gas and water and discharges.
(5) cooling and grinding: the material after above-mentioned oxidation is cooled to the furnace after 300 C, take out air cooling to room temperature.Then above-mentioned materials is taken out and to be ground, the oxidizing fire due to the thermoplastic polypropylene of correctability, makes the cupric oxide short texture forming.
(6) screening and packing: the cupric oxide of short texture is taken out and ground, then screening, the order number of screening is selected suitably to reduce with reference to granularity 325 orders of original copper powder, can adopt 150 orders or the screening of 200 objects.Through x-ray analysis, show, what fully oxidation obtained is cupric oxide powder, does not have Red copper oxide.Cupric oxide and copper particle diameter from three field emission scanning electron microscopes of Figure of description, can find out: (Fig. 1, Fig. 2), for granule-morphology and the size of oxidation rear oxidation copper, (Fig. 3) is pattern and the size of the copper after copper powder sintering and reducing.
Preparation method of the present invention is simple, easy to operate, and equipment is simple, and production process is pollution-free, good product quality (product purity is high, structure is controlled), and production efficiency is high, and production cost is low, is applicable to suitability for industrialized production.
Accompanying drawing explanation: Fig. 1 is granule-morphology and the size figure of oxidation rear oxidation copper
Fig. 2 is granule-morphology and the size figure of oxidation rear oxidation copper
Fig. 3 is pattern and the size figure of the copper after copper powder sintering and reducing.
Claims (4)
1. a method of preparing micron or nano-cupric oxide powder, it is characterized in that take that copper powder and thermoset or correctability thermal plastic high polymer powder are raw material, after abundant oxidizing reaction in air, after grinding and sieving, makes cupric oxide powder.
2. a kind of micron or method of nano-cupric oxide powder prepared according to claim 1, is characterized in that the step of preparation process comprises:
Proportioning raw materials: copper powder can adopt nano level copper powder prepared by the Micron-Sized Copper Powders Coated of spray deposition or electrolytic process (electrochemistry and chemical method) and the copper powder of other types;
Proportioning raw materials: copper powder and thermoset or correctability thermal plastic high polymer are (20-80) % according to weight ratio: (80-20) %, standby after fully mixing 30 minutes to 2 hours;
Oxidizing reaction: mixed powder is packed in stainless steel or ceramic die, be placed in air circulating oven, heated oxide, temperature can be set as 450 C to 800 C, and temperature selects to depend on that thermoset or the burning of correctability thermal plastic high polymer remove temperature;
Grind and screening: by the resulting short texture of oxidizing reaction and the easy cupric oxide of pulverizing, cooling, by grinding and sieving, obtain the cupric oxide powder of required particle diameter.
3. a kind of micron or method of nano-cupric oxide powder prepared according to claim 1, its feature is at cupric oxide constitutional features and original copper powder structural similitude.
4. glomeration structure as regular and basic in the Micron-Sized Copper Powders Coated pattern of spray deposition; Its primary structure of pattern fundamental sum of the nano level electrolytic copper copper powder that electrochemistry makes with chemical method is similar, size be still nano level or after oxidation size increase to form submicrometer structure.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591258A (en) * | 2015-02-08 | 2015-05-06 | 福建紫鑫金属材料科技有限公司 | Method for producing oxide copper powder from copper sand |
| CN112719263A (en) * | 2020-12-30 | 2021-04-30 | 北京有研粉末新材料研究院有限公司 | Method for preparing heat pipe liquid absorption core material |
| CN115488330A (en) * | 2021-06-02 | 2022-12-20 | 华晴材料股份有限公司 | Method for producing copper pellet and copper pellet |
| CN115740431A (en) * | 2022-12-21 | 2023-03-07 | 北京有研粉末新材料研究院有限公司 | Compound copper powder and preparation method and application thereof |
Citations (1)
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| CN102795885A (en) * | 2012-09-11 | 2012-11-28 | 江苏格业新材料科技有限公司 | Preparation method of aluminum oxide-zirconium oxide composite porous ceramic for high-temperature filtration |
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2013
- 2013-01-30 CN CN201310034708.4A patent/CN103964488A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102795885A (en) * | 2012-09-11 | 2012-11-28 | 江苏格业新材料科技有限公司 | Preparation method of aluminum oxide-zirconium oxide composite porous ceramic for high-temperature filtration |
Non-Patent Citations (1)
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| 刘曰利等: "一维CuO纳米针材料的直径可控制备研究", 《功能材料》, vol. 38, 31 December 2007 (2007-12-31) * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104591258A (en) * | 2015-02-08 | 2015-05-06 | 福建紫鑫金属材料科技有限公司 | Method for producing oxide copper powder from copper sand |
| CN112719263A (en) * | 2020-12-30 | 2021-04-30 | 北京有研粉末新材料研究院有限公司 | Method for preparing heat pipe liquid absorption core material |
| CN115488330A (en) * | 2021-06-02 | 2022-12-20 | 华晴材料股份有限公司 | Method for producing copper pellet and copper pellet |
| CN115488330B (en) * | 2021-06-02 | 2024-05-10 | 华晴材料股份有限公司 | Method for producing copper particles and copper particles |
| CN115740431A (en) * | 2022-12-21 | 2023-03-07 | 北京有研粉末新材料研究院有限公司 | Compound copper powder and preparation method and application thereof |
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Application publication date: 20140806 |