CN110666159A - Composite copper powder for acid degreasing process and preparation method and application thereof - Google Patents
Composite copper powder for acid degreasing process and preparation method and application thereof Download PDFInfo
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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Abstract
The invention relates to composite copper powder for an acid degreasing process, and a preparation method and application thereof, wherein the composite copper powder is of a core-shell structure, a core part is a dispersed copper-based powder material, a shell part is an acid-resistant protective material, and the mass of the shell part accounts for 30-50% of the total composite material and is prepared by adopting a chemical deposition precipitation method, CVD (chemical vapor deposition), electroplating, high-temperature vapor deposition, electrochemical deposition or electronic sputtering. Compared with the prior art, the invention has the advantages of convenient preparation and treatment, lower cost, controllable size and shape, uniform structure, strong oxidation acid resistance and the like.
Description
Technical Field
The invention relates to the technical field of material preparation treatment and application thereof, in particular to composite copper powder capable of being used in an acid degreasing treatment process and a preparation method and application thereof.
Background
The copper-based material is a material which is formed by taking a copper element as a main element, has very excellent application performance in nature and wide sources, and is widely developed and applied by people in the early days, for example, the copper-based material is prepared and used in large quantities in the spring, autumn and warring countries in China, and the wide use of the copper-based material also plays a great role in promoting the development and progress of the human society. However, copper-based materials also present problems during use, which have a very limiting effect on their widespread use in large quantities. One of the important problems is that the copper-based material has insufficient stability, such as the copper verdigris is generated in the long-term use process, mainly because the acid resistance and the oxidation resistance of the copper are not good, so that the copper-based application material with good chemical stability can be developed to effectively promote the application development of the copper-based material.
The existing technology of banburying-injection molding-acid degreasing is widely applied to the processing of various devices, compared with other technological processes, the technology has the advantages of high efficiency, strong controllability and the like, and particularly can be used for processing 3D (three-dimensional) devices which are difficult to process and manufacture by other technological processes, so that the technological process has wide application prospect and market demand. However, not all materials can be applied to the process flow, which has some specific requirements for the processed powder precursor, for example, the copper powder product on the market can not be directly applied to the process flow at present, because concentrated nitric acid steam is often used in the acid degreasing process for removing the organic resin and the binder, and the copper powder product can not be kept stable at all under the condition, can be oxidized, corroded and deteriorated, and therefore, a qualified device can not be obtained at all. Therefore, the chemical stability of the copper powder is improved through a certain treatment process, so that the copper powder can be applied to a high-efficiency acid degreasing process, and a processing device with excellent performance can be obtained, and the copper powder has important market value and significance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the composite copper powder which has a core-shell structure, is convenient to prepare and treat, has lower cost, controllable size and shape, uniform structure and strong oxidation acid resistance and can be used in the acid degreasing treatment process, and the preparation method and the application thereof.
The purpose of the invention can be realized by the following technical scheme:
the composite copper powder used in the acid degreasing process is of a core-shell structure, a core part is a dispersed copper-based powder material, a shell part is an acid-resistant protective material, and the mass of the shell part accounts for 30-50% of the total composite material. The core-shell structure refers to a composite structure formed by coating one material with another material, the coating and/or sealing can be dense and/or uniform, and the coating of the core part by the shell part can be formed by mechanisms such as chemical bond action, electrostatic action, surface deposition action, adsorption layer medium action and the like.
Furthermore, the diameter of the particle of the composite copper powder is 100nm-500 μm, the diameter of the core part is 50nm-400 μm, the thickness of the shell part is 1nm-400 μm, and the coating rate of the shell part is 90-100%. The thickness of the shell part in the composite copper powder material can be 10-30nm, 30-50nm, 50-70nm, 70-90nm, 90-110nm, 110-130nm, 130-150nm, 150-250nm, 250-350nm, 350-500nm, 500-700nm, 700-1000nm, 2000-5000nm, 5000-10000nm and 10000-40000 nm. The parameters of the shell layer growth process can be adjusted, so that the aim of adjusting the shell thickness can be fulfilled. The cladding ratio of the shell portion in the composite copper powder material is generally not less than 90%, not less than 92%, not less than 94%, not less than 96%, not less than 98%, not less than 99%, not less than 99.5%, or not less than 99.9%, and the cladding ratio generally refers to the percentage of the area of the portion of the surface of the core material covered with the shell portion material.
Further, the core material is a pure copper-based particle material and/or a copper-based alloy particle material; the shell material is an acid-resistant protective material and comprises one or more of inorganic oxide, silane coupling agent, high molecular polymer, inorganic simple substance and inorganic salt. The shell material has good stability or can be effectively passivated in a strong oxidizing and strong acid atmosphere, so that the copper-based material in the shell can be effectively coated and protected.
Further, the silane coupling agent refers to an organic silicon compound containing two groups with different chemical properties in a molecule, the high molecular polymer comprises a carbon chain polymer or a heterochain polymer, and the inorganic salt comprises one or more of carbonate, phosphate, sulfate, sulfite, silicate and aluminosilicate.
Further, the copper-based alloy includes bronze, brass or cupronickel, and the inorganic oxide includes Al2O3、SiO2、TiO2、ZrO2、CeO2、SnO2The inorganic simple substance comprises one or more of aluminum, iron, silver, carbon, silicon, gold and titanium, the silane coupling agent comprises a chloro-silane coupling agent (a silane coupling agent containing a group with a chloro end), an amino-silane coupling agent (a silane coupling agent containing a group with an amino end), a fluoro-silane coupling agent (a silane coupling agent containing a group with a fluoroalkyl end), an epoxy-silane coupling agent (a silane coupling agent containing a group with an epoxy end), a mercapto-silane coupling agent (a silane coupling agent containing a group with a mercapto end), a methoxy-silane coupling agent (a silane coupling agent containing a group with a methoxy end), an ethoxy-silane coupling agent (a silane coupling agent containing a group with an ethoxy end), a methoxy-ethoxy composite silane coupling agent (a silane coupling agent containing a group with a methoxy end and an ethoxy end), a silane coupling agent with a fluorine atom(s) and a silane coupling agent(s) with a fluorine atom(s) and a fluorine atom(s) in the molecule(s), The polymer comprises one or more of polystyrene, phenolic resin, polyacrylic acid, poly barbituric acid and polyurethane, and the inorganic salt comprises one or more of calcium sulfate, aluminum sulfate, sodium carbonate and sodium silicate.
The preparation method of the composite copper powder used for the acid degreasing process adopts one or more of chemical deposition precipitation, CVD, electroplating, high-temperature vapor deposition, electrochemical deposition and electron sputtering to coat the shell material and the core material.
Further, the chemical precipitation method is a method for precipitating a precursor of the shell part material on the surface of the core part material through chemical and/or physical action under certain conditions, and specifically comprises the following steps:
(1) copper powder is used as a precursor of a core material under the action of a catalyst;
(2) dissolving a precursor of the shell part material and a precursor of the core part material in a solvent together, and stirring for reaction to generate a brown yellow gel solution;
(3) carrying out hydrothermal treatment, centrifugation, cleaning and drying on the brown yellow gel solution to obtain a crude product;
(4) and calcining the crude product to obtain the composite copper powder which can be used in the acid degreasing treatment process.
Further, the mass ratio of the copper powder, the catalyst, the solvent and the shell material is 3-10: 10-30: 450: 3-5, the catalyst is a substance capable of releasing ammonia molecules, and comprises a mixture of ammonia water, formic acid and ammonium formate; the precursor of the shell material is a substance capable of generating inorganic oxide sol and comprises aluminum sulfate or aluminum chloride; the solvent comprises one or more of water, ethanol and isopropanol.
Further, the stirring reaction in the step (2) means that the mixture is stirred for 20-40min, then heated to 75-85 ℃, and then continuously stirred for 12-24 h; the hydrothermal temperature in the step (3) is 100-200 ℃, the time is 8-24h, the centrifugal rotation speed is 6000-10000rpm, the time is 1-10min, the washing is carried out for three times by using ethanol and then by using water, the drying temperature is 50-80 ℃, and the time is 8-24 h; the calcining gas atmosphere in the step (4) is nitrogen, the temperature is 350-450 ℃, and the time is 3-5 h. Besides the chemical deposition method, the core material can be coated by one or more of CVD, electroplating, high-temperature vapor deposition, electrochemical deposition and electron sputtering with the shell material which can resist strong-oxidizing strong-acid etching
The application of the composite copper powder which can be used in the acid degreasing treatment process is applied to the process of manufacturing application devices by adopting an injection molding-acid degreasing technical process.
Compared with the prior art, the invention has the following advantages:
(1) the core-shell structure is prepared by adopting the raw materials with low cost, and the purposes of adjustable size and uniform structure can be realized according to the proportion of precursors of the core part and the shell part;
(2) the shell structure is made of acid-resistant and strong oxidation-resistant materials, so that corresponding protection can be given to the core part;
(3) the material is used in the technological process of injection molding-acid degreasing, and has great significance for the development of the processing and manufacturing technology of copper-based application devices due to the improvement of the chemical stability of the copper powder.
Drawings
FIG. 1 is a TEM (characteristic transmission electron microscope) image of the core-shell structure composite copper powder material in example 1.
FIG. 2 is an optical photograph of the copper powder sintered to obtain a bulk after the composite copper powder material with a core-shell structure in example 1 is subjected to acid degreasing treatment.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
5g of formic acid and 15.0g of ammonium formate are added to a mixed solution of 150ml of organic alcohol and 300ml of water to be dissolved, 3g of aluminum sulfate is added after the dissolution, 3g of commercially available copper powder product is added, the stirring is continued for half an hour, and then the solution is heated to 80 ℃ at a controlled temperature and kept stirred at the temperature for 12 to 24 hours. And adding the generated brown yellow gel solution into a hydrothermal kettle, treating for 12h, centrifuging the obtained product at the rotating speed of 8000rpm for 5 min, separating to obtain a product, washing with ethanol for three times, washing with water for three times, centrifuging and washing the obtained product, drying in the air at 60 ℃ for 12h, calcining at 400 ℃ for 4h under the nitrogen atmosphere, and thus obtaining the copper powder material microsphere with the composite core-shell structure. The overall morphology of the copper powder particles is shown in FIG. 1. The prepared composite copper powder material has a middle shell layer coated with alumina, the thickness of the alumina is about 10-15nm, the surface structure of the coated composite copper powder material is almost unchanged after the coated composite copper powder material is placed in concentrated nitric acid steam for 24 hours, obvious 0.5 mm corrosion air holes are not found by observing the material through an optical microscope, the conductivity coefficient of the coated composite copper powder material can reach 90% of that of an original pure copper product through a conductivity test, and the prepared composite copper powder material is proved to have good stability.
Example 2
5g of formic acid and 15.0g of ammonium formate are added to a mixed solution of 150ml of organic alcohol and 300ml of water to be dissolved, 5g of aluminum sulfate is added after the dissolution, 3g of commercially available copper powder product is added, the stirring is continued for half an hour, and then the solution is heated to 80 ℃ at a controlled temperature and kept stirred at the temperature for 12 to 24 hours. And adding the generated brown yellow gel solution into a hydrothermal kettle, treating for 12h, centrifuging the obtained product at the rotating speed of 8000rpm for 5 min, separating to obtain a product, washing with ethanol for three times, washing with water for three times, centrifuging and washing the obtained product, drying in the air at 60 ℃ for 12h, calcining at 400 ℃ for 4h under the nitrogen atmosphere, and thus obtaining the copper powder material microsphere with the composite core-shell structure. The prepared composite copper powder material has a middle shell layer coated with alumina, the thickness of the alumina is about 20-25nm, the surface structure of the alumina is almost unchanged after the alumina is placed in concentrated nitric acid steam for 24 hours after coating, obvious corrosion pores of 0.5 mm are not found when the material is observed by an optical microscope, the conductivity coefficient of the alumina can reach 92% of that of the original pure copper product through conductivity tests, and the alumina has good stability and good stability.
Example 3
A vacuum sputtering device is adopted, a high-purity metal aluminum target is adopted, a 50-10000nm metal aluminum layer is deposited and grown on the surface of a copper powder product purchased from 10g in the market, then concentrated nitric acid steam is adopted for passivation treatment, the surface of the prepared composite copper powder material is coated with an aluminum-aluminum oxide composite material, the surface structure is almost unchanged after the composite copper powder material is coated and placed in the concentrated nitric acid steam for 24 hours, obvious 0.5 mm corrosion air holes are not found through an optical microscope, the conductivity coefficient can reach 85% of that of the original pure copper product through conductivity test, and good stability is proved to have good stability and good stability, as shown in figure 2.
Example 4
The composite copper powder is in a core-shell structure, a core part is a dispersed copper-based powder material, a shell part is an acid-resistant protective material, and the mass of the shell part accounts for 30% of the total composite material. The core-shell structure refers to a composite structure formed by coating one material with another material, the coating and/or sealing can be dense and/or uniform, and the coating of the core part by the shell part can be formed by mechanisms such as chemical bond action, electrostatic action, surface deposition action, adsorption layer medium action and the like.
The diameter of the particle of the composite copper powder is 100nm-500 μm, the diameter of the core part is 50nm-400 μm, the thickness of the shell part is 1nm-400 μm, and the coating rate of the shell part is 90%. The parameters of the shell layer growth process can be adjusted, so that the aim of adjusting the shell thickness can be fulfilled.
The core material is pure copper-based particle material, and the shell material is acid-resistant protective material, such as alumina. The shell material has good stability or can be effectively passivated in a strong oxidizing and strong acid atmosphere, so that the copper-based material in the shell can be effectively coated and protected.
The shell material is prepared by adopting a chemical precipitation method, wherein the chemical precipitation method is a method for precipitating a precursor of the shell material on the surface of the core material under certain conditions through chemical and/or physical actions, and specifically comprises the following steps:
(1) copper powder is used as a precursor of a core material under the action of a catalyst;
(2) dissolving a precursor of the shell part material and a precursor of the core part material in a solvent together, and stirring for reaction to generate a brown yellow gel solution; the mass ratio of the copper powder, the catalyst, the solvent and the shell material is 3: 10: 450: 3, the catalyst is ammonia water, and the precursor of the shell material is aluminum sulfate; the solvent is 1: 1 water and ethanol. Stirring the mixture for 20min, heating to 75-85 deg.C, and stirring for 12 hr;
(3) carrying out hydrothermal treatment, centrifugation, cleaning and drying on the brown yellow gel solution to obtain a crude product; the hydrothermal temperature is 160 ℃, the hydrothermal time is 8h, the centrifugal speed is 6000rpm, the centrifugal time is 1min, after the washing with ethanol is carried out for three times, the washing with water is carried out for three times, the drying temperature is 50 ℃, and the drying time is 8 h;
(4) and calcining the crude product to obtain the composite copper powder which can be used in the acid degreasing treatment process. The atmosphere of the calcining gas is nitrogen, the temperature is 350 ℃, and the time is 3 h.
The surface structure of the obtained composite copper powder is almost unchanged after the composite copper powder is placed in concentrated nitric acid steam for 24 hours, obvious corrosion air holes of more than 0.5 mm are not found when the material is observed by an optical microscope, and the conductivity coefficient of the composite copper powder can reach 90% of that of the original pure copper product through conductivity tests, so that the composite copper powder has good stability.
The material is applied to the process of manufacturing application devices by adopting an injection molding-acid degreasing technical process.
Example 5
The composite copper powder is in a core-shell structure, a core part is a dispersed copper-based powder material, a shell part is an acid-resistant protective material, and the mass of the shell part accounts for 50% of the total composite material. The core-shell structure refers to a composite structure formed by coating one material with another material, the coating and/or sealing can be dense and/or uniform, and the coating of the core part by the shell part can be formed by mechanisms such as chemical bond action, electrostatic action, surface deposition action, adsorption layer medium action and the like.
The diameter of the particle of the composite copper powder is 100nm-500 μm, the diameter of the core part is 50nm-400 μm, the thickness of the shell part is 1nm-400 μm, and the coating rate of the shell part is 100%. The parameters of the shell layer growth process can be adjusted, so that the aim of adjusting the shell thickness can be fulfilled.
The core material is pure copper-based particle material, and the shell material is acid-resistant protective material, such as alumina. The shell material has good stability or can be effectively passivated in a strong oxidizing and strong acid atmosphere, so that the copper-based material in the shell can be effectively coated and protected.
The shell material is prepared by adopting a chemical precipitation method, wherein the chemical precipitation method is a method for precipitating a precursor of the shell material on the surface of the core material under certain conditions through chemical and/or physical actions, and specifically comprises the following steps:
(1) copper powder is used as a precursor of a core material under the action of a catalyst;
(2) dissolving a precursor of the shell part material and a precursor of the core part material in a solvent together, and stirring for reaction to generate a brown yellow gel solution; the mass ratio of the copper powder, the catalyst, the solvent and the shell material is 10: 30: 450: 5, the catalyst is ammonia water, and the precursor of the shell material is aluminum chloride; the solvent is 1: 1 water and isopropanol. Stirring the mixture for 40min, heating to 75-85 deg.C, and stirring for 24 hr;
(3) carrying out hydrothermal treatment, centrifugation, cleaning and drying on the brown yellow gel solution to obtain a crude product; the hydrothermal temperature is 170 ℃, the time is 24 hours, the centrifugal speed is 10000rpm, the time is 10 minutes, after the washing with ethanol is carried out for three times, the washing with water is carried out for three times, the drying temperature is 80 ℃, and the time is 24 hours;
(4) and calcining the crude product to obtain the composite copper powder which can be used in the acid degreasing treatment process. The atmosphere of the calcining gas is nitrogen, the temperature is 450 ℃, and the time is 5 h.
The obtained composite copper powder is placed in concentrated nitric acid steam for 24 hours, the surface structure is almost unchanged, obvious corrosion air holes exceeding 0.5 mm are not found when the material is observed by an optical microscope, and the conductivity coefficient can reach 95% of the original pure copper product through conductivity test, so that the composite copper powder has good stability
The material is applied to the process of manufacturing application devices by adopting an injection molding-acid degreasing technical process.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. The composite copper powder for the acid degreasing process is characterized in that the composite copper powder is of a core-shell structure, a core part is made of dispersed copper-based powder materials, a shell part is made of acid-resistant protective materials, and the mass of the shell part accounts for 30-50% of the total composite copper powder.
2. The composite copper powder for use in an acid degreasing process as claimed in claim 1, wherein the diameter of the particles of the composite copper powder is 100nm-500 μm, the diameter of the core portion is 50nm-400 μm, the thickness of the shell portion is 1nm-400 μm, and the coating rate of the shell portion is 90-100%.
3. The composite copper powder for use in an acid degreasing process as recited in claim 1, wherein said core material is a pure copper-based particulate material and/or a copper-based alloy particulate material; the shell material is an acid-resistant protective material and comprises one or more of inorganic oxide, silane coupling agent, high molecular polymer, inorganic simple substance and inorganic salt.
4. The composite copper powder for use in an acid degreasing process as recited in claim 3, wherein said copper-based alloy comprises bronze, brass or cupronickel;
the inorganic oxide comprises Al2O3、SiO2、TiO2、ZrO2、CeO2、SnO2One or more of;
the silane coupling agent is an organic silicon compound containing two groups with different chemical properties in a molecule;
the high molecular polymer comprises a carbon chain polymer or a heterochain polymer;
the inorganic simple substance comprises one or more of aluminum, iron, silver, carbon, silicon, gold and titanium;
the inorganic salt comprises one or more of carbonate, phosphate, sulfate, sulfite, silicate and aluminosilicate.
5. The composite copper powder for acid degreasing treatment according to claim 3 or 4, wherein the silane coupling agent comprises one or more of a chloro-silane coupling agent, an amino-silane coupling agent, a fluoro-silane coupling agent, an epoxy-silane coupling agent, a mercapto-silane coupling agent, a methoxy-silane coupling agent, an ethoxy-silane coupling agent, a methoxyethoxy composite silane coupling agent, and an acetoxy-silane coupling agent; the high molecular polymer comprises one or more of polystyrene, phenolic resin, polyacrylic acid, polybarbituric acid and polyurethane; the inorganic salt comprises one or more of calcium sulfate, aluminum sulfate, sodium carbonate and sodium silicate.
6. The method for preparing composite copper powder for acid degreasing process as claimed in claim 1, wherein the shell material capable of resisting oxidative strong acid corrosion is used to coat the core material by one or more of chemical deposition precipitation, CVD, electroplating, high temperature vapor deposition, electrochemical deposition, and electron sputtering.
7. The method for preparing composite copper powder for acid degreasing process as claimed in claim 6, wherein the chemical precipitation method comprises the following steps:
(1) the copper-based powder material is used as a precursor of the core material under the action of a catalyst;
(2) dissolving a precursor of the shell part material and a precursor of the core part material in a solvent together, and stirring for reaction to generate a brown yellow gel solution;
(3) carrying out hydrothermal treatment, centrifugation, cleaning and drying on the brown yellow gel solution to obtain a crude product;
(4) and calcining the crude product to obtain the composite copper powder which can be used in the acid degreasing treatment process.
8. The method for preparing the composite copper powder used for the acid degreasing treatment process as claimed in claim 7, wherein the mass ratio of the copper powder, the catalyst, the solvent and the shell material is (3-10): (10-30): 450: (3-5), the catalyst is a substance capable of releasing ammonia molecules, and comprises a mixture of ammonia water, formic acid and ammonium formate; the precursor of the shell material is a substance capable of generating inorganic oxide sol and comprises aluminum sulfate or aluminum chloride; the solvent comprises one or more of water, ethanol and isopropanol.
9. The method for preparing composite copper powder for use in acid degreasing process as claimed in claim 7, wherein the stirring reaction in step (2) is that the mixture is stirred for 20-40min, then heated to 75-85 ℃, and then stirred for 12-24 h; the hydrothermal temperature in the step (3) is 100-200 ℃, the time is 8-24h, the centrifugal rotation speed is 6000-10000rpm, the time is 1-10min, the washing is carried out for three times by using ethanol and then by using water, the drying temperature is 50-80 ℃, and the time is 8-24 h; the calcining gas atmosphere in the step (4) is nitrogen, the temperature is 350-450 ℃, and the time is 3-5 h.
10. Use of the copper composite powder according to claim 1 for acid degreasing applications, wherein the material is used in the manufacture of devices using the injection-acid degreasing process.
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| CN107321975A (en) * | 2017-06-05 | 2017-11-07 | 苏州博卡金属颜料有限公司 | A kind of aqueous Cu-Zn alloy powder preparation method and aqueous copper metallic ink and coating |
| CN107858663A (en) * | 2017-11-15 | 2018-03-30 | 上海上大瑞沪微系统集成技术有限公司 | It is a kind of using CVD method directly in the method for Copper Powder Surface coated graphite alkene |
| CN110125385A (en) * | 2019-04-15 | 2019-08-16 | 中国航发北京航空材料研究院 | A kind of preparation method of the graphene Cu-base composites based on fabricated in situ |
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