CN114682781A - Method for manufacturing short-fiber coral-shaped copper powder - Google Patents
Method for manufacturing short-fiber coral-shaped copper powder Download PDFInfo
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- CN114682781A CN114682781A CN202210338577.8A CN202210338577A CN114682781A CN 114682781 A CN114682781 A CN 114682781A CN 202210338577 A CN202210338577 A CN 202210338577A CN 114682781 A CN114682781 A CN 114682781A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
- B22F3/1121—Making porous workpieces or articles by using decomposable, meltable or sublimatable fillers
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Abstract
The invention provides a method for preparing short-fiber coral-shaped copper powder, which comprises the steps of granulating, calcining and reducing a mixed powder material to obtain the short-fiber coral-shaped copper powder; the mixture copper powder comprises pure copper powder, a water-soluble pore-forming agent and a binder, wherein the adding proportion of the water-soluble pore-forming agent is 0-30% of the mass of the pure copper powder, and the adding amount of the binder is 5-15% of the mass of the pure copper powder; the grain diameter D90 of the pure copper powder is less than 10 mu m, and the apparent density is more than 3.5g/cm3(ii) a The water-soluble pore-forming agent is at least one of sodium chloride and potassium carbonate; the binder is ethyl cellulose solution or soluble starchAny one of the solutions. According to the invention, by adding the pore-forming agent and granulating, the copper powder is in a short fiber coral-shaped microscopic shape, and the loose ratio of the copper powder reaches 0.7g/cm3‑1.0g/cm3。
Description
Technical Field
The invention relates to the field of new materials, in particular to a method for manufacturing short-fiber coral-shaped copper powder.
Background
In recent years, electronic devices are rapidly developed towards miniaturization, integration and high performance, the heat flux is higher and higher, the performance of the electronic devices is restricted by heat dissipation capacity, and the problem of heat dissipation of the electronic devices with high heat flux becomes a problem of close attention of the current industry. The micro heat pipe or the ultrathin soaking plate is used as an efficient phase change heat transfer device, has the advantages of small volume, strong heat conduction capability and high stability, and is widely applied to cooling and heat dissipation of electronic devices. Due to size limitations, micro heat pipes used in electronic devices must be both thin and light and have good thermal performance, which has prompted the development of ultra-thin heat pipes or vapor chambers. The liquid absorption core structure is an important parameter for determining the performance of the heat pipe, generally, the liquid absorption core is made of a copper net or water atomization copper powder, a thinner copper net and thinner copper powder are required to be used under the condition of ultra-thinning development of the heat pipe or the vapor chamber, and the porosity of a capillary core made of the thin copper net and the thinner copper powder is sharply reduced, so that the heat dissipation power of the heat pipe or the vapor chamber is limited.
Copper powder is an important basic functional material in the field of heat dissipation of electronic products, and the copper powder with complex and changeable microscopic morphology can be used for manufacturing a better capillary pore structure so as to improve the heat exchange efficiency of the heat dissipation product. The loose ratio of the dendritic electrolytic copper powder can reach 1.0g/cm3-2.0g/cm3But can not be used for manufacturing high-power heat dissipation products due to poor trace element control and fine particle size distribution. At present, water atomized copper powder is widely used for manufacturing capillary cores of heat dissipation products, but the loose ratio of the water atomized copper powder is more than 1.5g/cm3In this way, further improvement of the performance of the heat dissipation product is restricted.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art, and provides a method for manufacturing short-fiber coral-shaped copper powder.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for preparing short-fiber coral-shaped copper powder comprises granulating, calcining and reducing the mixed powder material to obtain short-fiber coral-shaped copper powder;
the mixed powder material comprises pure copper powder, a water-soluble pore-forming agent and a binder, wherein the adding proportion of the water-soluble pore-forming agent is 0-30% of the mass of the pure copper powder, and the adding amount of the binder is 5-15% of the mass of the pure copper powder;
the grain diameter D90 of the pure copper powder is less than 10 mu m, and the apparent density is more than 3.5g/cm3；
The water-soluble pore-forming agent is at least one of sodium chloride and potassium carbonate;
the binder is any one of ethyl cellulose solution or soluble starch solution;
and uniformly mixing the copper powder and the water-soluble pore-forming agent, adding a binder into the mixture, and mixing the mixed powder into a semi-dry paste for the subsequent granulation process.
Further, in the granulation process, a swing type granulator is used for granulating semi-dried pasty copper powder, the particle size of the obtained copper powder is 40-200 meshes, and the copper powder falls on an electric auxiliary thermal vibration chute to be dried and then is collected in a container.
Further, the temperature on the electric auxiliary heating vibration chute is 50-400 ℃.
Further, in the calcination process, the calcination temperature is 200-500 ℃, and the calcination time is 30-60 min.
Further, the reduction process is specifically as follows: in an inert gas environment, hydrogen is used as reducing gas to finish annealing reduction treatment;
in the annealing reduction treatment process, the annealing reduction temperature is 200-400 ℃, the hydrogen proportion is not more than 10 percent, and the annealing reduction time is 60-120 min.
Further, before annealing reduction, the calcined copper powder is washed by water to remove the pore-forming agent, and the content of the pore-forming agent in the washed copper powder is within 50 ppm.
Furthermore, the micro-morphology of the short fiber coral-shaped copper powder is coral-shaped short fiber, the diameter of the copper powder is 15-70 mu m, the length of the copper powder is 10-500 mu m, and the apparent density of the copper powder is 0.7-1.0g/cm3。
Further, the porosity of the capillary core structure made of the copper powder is between 70% and 90%.
Compared with the prior art, the invention has the beneficial effects that: atomized copper powder is taken as a raw material, a pore-forming agent is added into the atomized copper powder and the atomized copper powder is granulated, so that the final copper powder product presents a short fiber coral-shaped microscopic morphology, and the loose ratio of the copper powder reaches 0.7g/cm3-1.0g/cm3The capillary core made of the copper powder has an excellent pore structure, the porosity can reach 90 percent at most, and the water absorption flux is more than 3mg/mm2And s. The product of the invention is used for replacing the traditional granular copper powder in the ultrathin heat pipe or the soaking plate, on one hand, the consumption of the copper powder can be reduced to save the material cost, on the other hand, the capillary core manufactured by the short-fiber coral-shaped copper powder product of the invention has an extremely high porosity structure, and the copper absorption amount of the capillary core is far higher than that of the traditional structure (the copper absorption amount of the traditional granular copper powder capillary core structure is less than 2 mg/mm)2S) to improve the power of the heat radiator such as the ultrathin heat pipe or the vapor chamber.
Drawings
The disclosure of the present invention is illustrated with reference to the accompanying drawings. It is to be understood that the drawings are designed solely for the purposes of illustration and not as a definition of the limits of the invention. In the drawings, like reference numerals are used to refer to like parts. Wherein:
figure 1 schematically shows a schematic representation of the appearance of copper powder after granulation.
Fig. 2 schematically shows a microscopic view of the final copper powder product.
Detailed Description
It is easily understood that according to the technical solution of the present invention, a person skilled in the art can propose various alternative structures and implementation ways without changing the spirit of the present invention. Therefore, the following detailed description and the accompanying drawings are merely illustrative of the technical aspects of the present invention, and should not be construed as all of the present invention or as limitations or limitations on the technical aspects of the present invention.
A method for preparing fibrous coral-shaped copper powder comprises the following steps:
1) adding pore-forming agent and binder into pure copper powder, and making the material into semi-dry paste
Atomized pure copper powder is used as raw material, and the particle size of the copper powder is D90<10um, the loose packed density is more than 3.5g/cm3Adding 0-30 wt% of water-soluble pore-forming agent and mixing uniformly, wherein the water-soluble pore-forming agent can be at least one of sodium chloride and potassium carbonate; adding 5-18 wt% of binder into the mixture to make the mixed powder into semi-dry paste, wherein the binder can be one of ethyl cellulose solution or soluble starch solution, and the binder is preferably ethyl cellulose solution.
2) Granulating
And (3) granulating the semi-dry pasty copper powder by using a swing type granulator, wherein the sieve of the swing type granulator can be 40 meshes, 50 meshes, 80 meshes, 100 meshes, 120 meshes, 150 meshes and 200 meshes, and copper powder with different particle size ranges can be prepared by selecting different sieves. Copper powder prepared by the swing type granulator directly falls on the electric auxiliary thermal vibration chute, the temperature of the electric auxiliary thermal vibration chute is controllable to be 50-400 ℃, the copper powder can be quickly dried through the cooperation of temperature and vibration, and the granulated copper powder is collected in a container below after being quickly dried after passing through the chute.
3) Calcination of
And calcining the granulated copper powder at 200-500 deg.c for 30-60min to eliminate adhesive and other matter from the copper powder.
4) Washing with water
And washing the calcined copper powder with water to remove pore-forming agents such as sodium chloride, potassium carbonate and the like. After twice soaking and washing and three times rinsing, pore-forming agents such as sodium chloride, potassium carbonate and the like are completely removed.
5) Reduction of
And (3) carrying out annealing reduction treatment on the washed copper powder, wherein the annealing reduction temperature is 200-400 ℃, inert gas is used as protective gas, preferably nitrogen, hydrogen is used as reducing gas, the proportion of the hydrogen is not more than 10%, and the annealing reduction time is 60-120 minutes. The copper powder particles obtained under the annealing reduction condition with low temperature and low hydrogen proportion are not easy to be adhered, and the oxygen content of the copper powder is less than 0.2 percent.
The method comprises the following specific implementation steps:
(1) adding pore-forming agent and binder into copper powder, and making the material into semi-dry paste
Atomized pure copper powder is used as a raw material, the particle size of the copper powder is less than 10um, and the apparent density is more than 3.5g/cm3The copper content is more than 99.95 percent. Adding 0-30% of potassium carbonate, sodium chloride and other pore-forming agents, fully and uniformly mixing with the copper powder, and adjusting the addition amount of the pore-forming agents to regulate and control the porosity value of the final product. The ethyl cellulose ethanol solution with the concentration of 1 percent or the soluble starch solution with the concentration of 1 percent is used as a binder, the adding amount is about 5 to 15 percent, and the copper powder product is in a semi-dry paste shape after being fully stirred.
The results of examples 1-7 show that the addition amount of the two pore-forming agents and the porosity of the final product are consistent, and the porosity of the final product can be accurately controlled by the addition amount of the pore-forming agents.
TABLE 1
The method comprises the steps of adding a binder solution into a mixture of copper powder and a pore-forming agent to prepare a semi-dry paste, and evaluating the state of the semi-dry paste through a shaping mold, wherein the state of the semi-dry paste is collapse, loose and not capable of shaping, and the two states of the paste are not beneficial to granulation of a later-stage swing granulator. The results of examples 8-14 show that the binder solution was added at a rate of about 5% to about 15% based on the shaped mold test, depending on the bulk density of the copper powder pore former mixture.
The test method of the shaping mold comprises the following steps: 2 copper bottomless semi-cylindrical molds with the diameter of 2cm and the height of 4 cm. Assembling 2 semi-cylindrical copper molds into a cylinder, placing the cylinder on a vibrating table, taking a certain amount of mixed copper powder product added with a binder to fill the mold, starting the vibrating table, supplementing mixed copper powder until the whole cylinder mold is filled, removing the 2 copper semi-cylindrical molds after stopping the vibrating table, observing the state of the mixed copper powder and recording.
(2) Granulating
And granulating the semi-dry pasty copper powder material by using a swing granulator, and preparing the copper powder with different particle size ranges by selecting different filter screens. According to the market terminal demand condition, the filter screen of the swing type granulator can be 40 meshes, 50 meshes, 80 meshes, 100 meshes, 120 meshes, 150 meshes and 200 meshes. Examples 15-22 illustrate the use of different mesh sizes to produce copper powders of different particle sizes. The copper powder prepared by the swing type granulator directly falls on a self-made electric auxiliary heating vibration chute, the temperature of the electric auxiliary heating vibration chute can be controlled to be 50-400 ℃, the granulated copper powder passes through the chute, is rapidly dried and then is collected in a container below, and the appearance is shown in figure 1.
(3) Removing the binder by calcination
And calcining the washed copper powder at 200-500 deg.c to eliminate adhesive. During the calcination process, the binder is evaporated or decomposed to burn off residual trace carbon-containing products, and the removal condition of the binder is determined by detecting the carbon content. Meanwhile, copper powder is oxidized in the calcining process, and the excessive oxidation degree is unfavorable for the subsequent reduction annealing treatment of the copper powder, so that the sintering connection among copper powder particles is easily caused. By way of examples 23-30, we prefer calcination conditions of 400 ℃ for 60 minutes.
(4) Washing to remove pore-forming agent
The pore-forming agents sodium chloride and potassium carbonate are easy to dissolve in water, and components of the pore-forming agents are removed by soaking, washing and rinsing the granulated copper powder. In actual operation, the content of the pore-forming agent in the copper powder is reduced to be within 50ppm after two times of soaking and water washing and three times of rinsing.
(5) Reducing the washed copper powder
The calcined copper powder is subjected to annealing reduction treatment to remove oxygen elements, the copper oxide layer releases heat in the annealing reduction process, sintering connection among copper powder particles can be caused by excessively high reduction speed or high reduction temperature, the annealing reduction temperature, the hydrogen proportion in a furnace and other conditions are controlled to control the reduction speed of the copper oxide layer, and therefore the bonding condition among the copper powder particles is weakened. Examples 31-39 show that under the different annealing reduction conditions tested, the preferred annealing reduction conditions were 400 ℃ for 20 minutes with a 10% hydrogen fraction.
By adding pore-forming agent and granulating, the final copper powder product has short fiber coral-shaped microscopic morphology as shown in FIG. 2, and the loose ratio of copper powder is 0.7g/cm3-1.0g/cm3The capillary core made of the copper powder has an excellent pore structure, the porosity can reach 90 percent at most, and the water absorption flux is more than 3mg/mm2And s. The product of the invention is used for replacing the traditional granular copper powder in the ultrathin heat pipe or the soaking plate, on one hand, the consumption of the copper powder can be reduced to save the material cost, on the other hand, the capillary core manufactured by the short-fiber coral-shaped copper powder product of the invention has an extremely high porosity structure, and the copper absorption amount of the capillary core is far higher than that of the traditional structure (the copper absorption amount of the traditional granular copper powder capillary core structure is less than 2 mg/mm)2S) to improve the power of the heat radiator such as the ultrathin heat pipe or the vapor chamber.
The technical scope of the present invention is not limited to the above description, and those skilled in the art can make various changes and modifications to the above-described embodiments without departing from the technical spirit of the present invention, and such changes and modifications should fall within the protective scope of the present invention.
Claims (8)
1. A method for preparing short-fiber coral-shaped copper powder is characterized in that the short-fiber coral-shaped copper powder is obtained by granulating, calcining and reducing mixed powder materials;
the mixed powder material comprises pure copper powder, a water-soluble pore-forming agent and a binder, wherein the adding proportion of the water-soluble pore-forming agent is 0-30% of the mass of the pure copper powder, and the adding amount of the binder is 5-15% of the mass of the pure copper powder;
the grain diameter D90 of the pure copper powder is less than 10 mu m, and the apparent density is more than 3.5g/cm3；
The water-soluble pore-forming agent is at least one of sodium chloride and potassium carbonate;
the binder is any one of ethyl cellulose solution or soluble starch solution;
after copper powder and a water-soluble pore-forming agent are uniformly mixed, a binder is added into the mixture, and the mixed powder is mixed into a semi-dry paste for a subsequent granulation process.
2. The method for preparing short fiber coral-shaped copper powder according to claim 1, wherein in the granulation process, a semi-dried paste copper powder is granulated by using a swing granulator, the particle size of the obtained copper powder is 40-200 meshes, and the copper powder falls on an electric assisted thermal vibration chute, is dried and is collected in a container.
3. The method for manufacturing short-fiber coral-shaped copper powder according to claim 2, wherein the temperature on the electrically-assisted thermal vibration chute is 50 to 400 ℃.
4. The method for preparing short fiber-shaped coral-shaped copper powder according to claim 2, wherein in the calcination process, the calcination temperature is 200-500 ℃ and the calcination time is 30-60 min.
5. The method for producing short-fiber coral-shaped copper powder according to claim 4, wherein the reduction process is specifically as follows: in an inert gas environment, hydrogen is used as reducing gas to finish annealing reduction treatment;
in the annealing reduction treatment process, the annealing reduction temperature is 200-400 ℃, the hydrogen proportion is not more than 10 percent, and the annealing reduction time is 60-120 min.
6. The method for preparing short-fiber coral-shaped copper powder as claimed in claim 5, wherein the calcined copper powder is washed with water to remove the pore-forming agent before the annealing reduction, and the pore-forming agent content in the washed copper powder is within 50 ppm.
7. Short fiber coral-shaped copper powder produced by the method for producing short fiber coral-shaped copper powder according to any one of claims 1 to 6, wherein the microscopic morphology of the copper powder is coral-shaped short fibers having a diameter of 15 to 70 μm, a length of 10 to 500 μm, and a bulk density of 0.7 to 1.0g/cm3。
8. The short fiber coral-shaped copper powder of claim 7, wherein the porosity of the wick structure made of the copper powder is between 70% and 90%.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030044301A1 (en) * | 2001-08-16 | 2003-03-06 | Louis-Philippe Lefebvre | Method of making open cell material |
| CN102489706A (en) * | 2011-12-05 | 2012-06-13 | 山东大学 | Method for preparing pore diameter controllable porous capillary core |
| CN102618745A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Preparation method of copper porous material |
| CN103215470A (en) * | 2013-05-03 | 2013-07-24 | 中南大学 | Preparation method of open-pore copper foam with controllable pore structure parameter |
| CN103526064A (en) * | 2013-10-11 | 2014-01-22 | 昆明理工大学 | Preparation method for foamy copper |
| WO2018041032A1 (en) * | 2016-08-31 | 2018-03-08 | 昆山德泰新材料科技有限公司 | Copper foam powder and manufacturing method thereof |
| CN111185725A (en) * | 2020-01-10 | 2020-05-22 | 中国矿业大学 | Gradient-aperture porous copper liquid absorption core for loop heat pipe and preparation method thereof |
| CN111504105A (en) * | 2020-04-30 | 2020-08-07 | 北京工业大学 | Liquid absorption core for heat pipe or vapor chamber formed by multiple phase pore-forming agent and manufacturing method thereof |
-
2022
- 2022-04-01 CN CN202210338577.8A patent/CN114682781B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030044301A1 (en) * | 2001-08-16 | 2003-03-06 | Louis-Philippe Lefebvre | Method of making open cell material |
| CN102489706A (en) * | 2011-12-05 | 2012-06-13 | 山东大学 | Method for preparing pore diameter controllable porous capillary core |
| CN102618745A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Preparation method of copper porous material |
| CN103215470A (en) * | 2013-05-03 | 2013-07-24 | 中南大学 | Preparation method of open-pore copper foam with controllable pore structure parameter |
| CN103526064A (en) * | 2013-10-11 | 2014-01-22 | 昆明理工大学 | Preparation method for foamy copper |
| WO2018041032A1 (en) * | 2016-08-31 | 2018-03-08 | 昆山德泰新材料科技有限公司 | Copper foam powder and manufacturing method thereof |
| CN111185725A (en) * | 2020-01-10 | 2020-05-22 | 中国矿业大学 | Gradient-aperture porous copper liquid absorption core for loop heat pipe and preparation method thereof |
| CN111504105A (en) * | 2020-04-30 | 2020-08-07 | 北京工业大学 | Liquid absorption core for heat pipe or vapor chamber formed by multiple phase pore-forming agent and manufacturing method thereof |
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