CN113102751B - Method for coating copper on surface of sodium chloride particle - Google Patents
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- CN113102751B CN113102751B CN202110408637.4A CN202110408637A CN113102751B CN 113102751 B CN113102751 B CN 113102751B CN 202110408637 A CN202110408637 A CN 202110408637A CN 113102751 B CN113102751 B CN 113102751B
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- B22F1/17—Metallic particles coated with metal
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- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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Abstract
The invention discloses a method for coating copper on the surface of sodium chloride particles, belonging to the technical field of surface treatment of particle materials. Firstly, a proper amount of Cu (NO) is added 3 ) 2 Dissolving in acetone solution to obtain Cu (NO) 3 ) 2 In acetone solution, and then placing sodium chloride particles into Cu (NO) 3 ) 2 Stirring in acetone solution and ultrasonic vibrating to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in acetone solution, and then baking at low temperature to volatilize acetone to obtain coated Cu (NO) 3 ) 2 ·3H 2 O sodium chloride particles, heating at high temperature to make Cu (NO) on the surface of the sodium chloride particles 3 ) 2 ·3H 2 Decomposing O into CuO, heating the CuO in a reducing atmosphere, preserving heat for a period of time, and reducing the CuO into a Cu simple substance to obtain the sodium chloride particles with the surfaces coated with Cu. The surface treatment technology of the copper-coated sodium chloride particles has the characteristics of simple process and low cost, and can realize industrial production.
Description
Technical Field
The invention relates to a method for coating copper on the surface of sodium chloride particles, belonging to the technical field of surface treatment of particle materials.
Background
The through-hole foamed aluminum has good mechanical and sound absorption properties, and the mechanical and sound absorption properties are greatly improved along with the reduction of the aperture under the condition of certain porosity.
Infiltration casting is the mainstream preparation method of the through-hole foamed aluminum, and the used precursor material is sodium chloride particles. At present, through-hole porous aluminum with the aperture of more than 1mm can be prepared, but through-hole foamed aluminum with the aperture of less than 1mm, particularly foamed aluminum with a large-size through-hole structure, cannot be stably realized, because sodium chloride particles, aluminum and aluminum alloy melts are not wetted, so that the melts are difficult to permeate into gaps among the sodium chloride particles with the diameter of less than 1 mm. The copper metallized surface modification of the sodium chloride particles can improve the wettability of the sodium chloride particles with aluminum and aluminum alloy melts and improve the seepage performance of the melts, thereby making the preparation of the foamed aluminum with a micro-pore structure and a large size possible.
The method for coating the particle surface mainly comprises chemical plating, electroplating, vapor deposition and the like. The chemical plating is to form a metal plating layer by selectively reducing and depositing metal ions in a solution on the surface of a catalytically active object with a reducing agent without passing an external current. Electroplating is a process of depositing and covering a layer of metal film on the surface of an object to be plated by the action of electricity by utilizing the principle of electrolysis. Vapor deposition is the generation of a vapor of the material to be deposited in a vacuum, which is then condensed onto a substrate material to produce the desired film layer.
Because sodium chloride is easily dissolved in water, the conventional chemical plating and electroplating methods which relate to aqueous solutions cannot realize copper metallization on the surface of the copper chloride; the vapor deposition method has the defects of high cost, incapability of processing sodium chloride particles in a large scale and the like.
Disclosure of Invention
The invention aims to provide a technical method for coating copper on the surface of sodium chloride particles, which specifically comprises the following steps:
(1) adding Cu (NO) 3 ) 2 Dissolving in acetone to obtain Cu (NO) 3 ) 2 In an acetone solution of (2), placing sodium chloride particles in Cu (NO) 3 ) 2 Stirring in acetone solution, and ultrasonic vibrating to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in acetone solution.
(2) Mixing NaCl-Cu (NO) 3 ) 2 Baking acetone solution at low temperature to volatilize acetone to obtain Cu (NO) coated product 3 ) 2 ·3H 2 Sodium chloride particles of O.
(3) Coating the Cu (NO) prepared in the step (2) 3 ) 2 ·3H 2 Heating the sodium chloride particles of O to make Cu (NO) on the surfaces of the sodium chloride particles 3 ) 2 ·3H 2 And decomposing O into CuO to obtain the CuO-coated sodium chloride particles.
(4) Sodium chloride particles coated with CuO are added into H 2 Heating and preserving heat in the atmosphere to reduce CuO into simple substance Cu, thereby obtaining the sodium chloride particles with the surfaces coated with Cu.
Preferably, the Cu (NO) of the present invention 3 ) 2 Cu (NO) in acetone solution 3 ) 2 The amount of (2) is (20-110) g/100 g.
Preferably, the sodium chloride particles in step (1) of the present invention have a particle size of 0.05-1mm, and the sodium chloride particles are mixed with Cu (NO) 3 ) 2 The mass ratio of the acetone solution is 0.5:1-2:1, and the ultrasonic vibration time is 30-60 minutes.
Preferably, the low-temperature baking conditions in step (2) of the present invention are: baking at 50 deg.C for 30-120 min.
Preferably, the heating conditions in step (3) of the present invention are: keeping the temperature at 300 ℃ and 450 ℃ for 1-3 hours.
Preferably, the reduction temperature of CuO in the step (4) of the invention is 400-.
The sodium chloride particles of the invention are commercial industrial salts or sea salts.
The principle of the invention is as follows:
(1) the selection principle of the acetone organic solvent is as follows: in the aspect of solvent selection, since NaCl is a water-soluble salt, the solubility in water is very high, the melting point is low, and the sodium chloride particle surface is difficult to coat in the presence of water, and only the sodium chloride particle surface is treated in an organic solvent which does not dissolve NaCl. In addition, because copper and aluminum melt are mutually wet, surface coating of copper is a reasonable way for surface modification of sodium chloride particles, and an organic solvent capable of dissolving copper salt needs to be selected. In summary, acetone is an organic solvent that can dissolve NaCl but copper salts, and thus acetone is selected as the organic solvent of the present invention.
(2) The principle of copper cladding on the surface of sodium chloride particles is as follows: adding proper amount of Cu (NO) 3 ) 2 Dissolving in acetone solution to obtain Cu (NO) 3 ) 2 In acetone solution, and then placing sodium chloride particles into Cu (NO) 3 ) 2 Stirring in acetone solution and ultrasonic vibrating to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in an acetone solution; then drying at low temperature of 50 ℃ to volatilize acetone, and screening to obtain the coated Cu (NO) 3 ) 2 ·3H 2 Sodium chloride particles of O; heating at high temperature to make Cu (NO) 3 ) 2 ·3H 2 Decomposing O to obtain CuO; CuO is heated in a reducing atmosphere and is changed into a Cu simple substance after being kept warm for a period of time.
Volatilization of acetone solvent: acetone (CH) 3 COCH 3 ) Is an organic solvent which is colorless liquid at normal temperature, is easy to dissolve in water, has a melting point of-94.9 ℃ and a boiling point of 56.53 ℃, can volatilize at a lower temperature, and enables Cu (NO) to be volatilized 3 ) 2 Supersaturated precipitation, and Cu (NO) precipitated due to the large specific surface area of sodium chloride particles 3 ) 2 Can be deposited on the surface of sodium chloride particles to realize Cu (NO) 3 ) 2 ·3H 2 And (3) coating the sodium chloride particles by O.
Cu(NO 3 ) 2 ·3H 2 Thermal decomposition of O Cu (NO) 3 ) 2 ·3H 2 Melting O at 118 deg.C, removing crystal water at 203 deg.C, and converting into HNO 3 And Cu (NO) 3 ) 2 ·3Cu(OH) 2 And the CuO is completely decomposed into a final product CuO at about 310 ℃, and the reaction is as follows:
Cu(NO 3 ) 2 ·3H 2 O→1/4Cu(NO 3 ) 2 ·3Cu(OH) 2 +2/3H 2 O+3/2 HNO 3 （1）
1/4Cu(NO 3 ) 2 ·3Cu(OH) 2 +3/2 HNO 3 →1/2O 2 +3/2H 2 O+CuO +2NO 2 （2）
and (3) total reaction: cu (NO) 3 ) 2 ·3H 2 O→CuO↓+2NO 2 ↑+1/2O 2 ↑+3H 2 O（3）
Experiments prove that the Cu (NO) can be ensured by keeping the temperature of 300-450 ℃ for 1-3 hours 3 ) 2 ·3H 2 O decomposes to CuO.
(3) Reduction of CuO
The reaction that occurs when hydrogen reduces copper oxide is:
CuO（s） + H 2 （g）→H 2 O （g）+ Cu （4）
according to thermodynamic calculation, within the temperature range of 25-527 ℃, the Gibbs free energy change values of the copper oxide reduced by the hydrogen in the formula (4) are all negative, which indicates that the reaction can spontaneously proceed; through experiments, the reduction temperature of 400-500 ℃ for reducing CuO into copper is obtained, and the reduction time is 2-4 hours.
The invention has the advantages of
Aiming at the problem of difficulty in preparing porous aluminum with a micro-pore structure through hole, the invention adopts a copper-clad treatment technology for the surface of micro sodium chloride particles based on an acetone solvent; has the following advantages:
（1）Cu(NO 3 ) 2 mixing acetone solution with sodium chloride particles, baking at low temperature, heating for decomposition, and reacting with H 2 The sodium chloride particles with copper coated on the surface are obtained by reduction, the problem that the water-soluble sodium chloride particles are coated with copper is solved, the process is simple and easy to operate, and the sodium chloride particles have deeper and wider application in future development.
(2) The technology of coating copper on the surface of sodium chloride particles with the diameter of less than 1mm can prepare the high-porosity small-aperture through-hole porous aluminum, enriches the methods for preparing the through-hole porous aluminum and provides a certain basis for realizing industrialized and continuous production.
Drawings
FIG. 1 is a process flow chart of copper coating on the surface of sodium chloride particles.
Detailed Description
The invention will be described in more detail with reference to the following figures and examples, without limiting the scope of the invention.
Example 1
A method for coating copper on the surface of sodium chloride particles is characterized by comprising the following steps:
（1）Cu(NO 3 ) 2 preparing an acetone solution: according to Cu (NO) 3 ) 2 Mixing with acetone solution with concentration of 20g/100g, and adding Cu (NO) 3 ) 2 Adding into acetone, and stirring to make Cu (NO) 3 ) 2 Dissolving in acetone to obtain Cu (NO) 3 ) 2 Of (2) in acetone.
(2) Mixing sodium chloride particles: adding sodium chloride particles according to the following weight percentage: cu (NO) 3 ) 2 Acetone solution mass =0.5, and commercial industrial salt having a particle size of 0.05mm is added to Cu (NO) obtained in step (2) 3 ) 2 Stirring in acetone solution, and ultrasonic vibrating for 60 min to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in acetone solution.
(3) Baking and volatilizing acetone: NaCl-Cu (NO) obtained in the step (2) 3 ) 2 Baking the acetone solution at 50 deg.C for 30 min to volatilize acetone to obtain Cu (NO) coated solution 3 ) 2 ·3H 2 Sodium chloride particles of O.
（4）Cu(NO 3 ) 2 Heating and decomposing: coating the Cu (NO) prepared in the step (3) 3 ) 2 ·3H 2 Heating the sodium chloride particles of O to 300 ℃ and preserving the heat for 3 hours to ensure that Cu (NO) on the surfaces of the sodium chloride particles 3 ) 2 ·3H 2 The O is decomposed and converted into CuO, and the sodium chloride particles coated with the CuO are obtained.
(5) And (3) CuO reduction: h, mixing the sodium chloride particles coated with CuO obtained in the step (4) 2 Heating to 400 ℃ in the atmosphere, and preserving the heat for 4 hours to reduce CuO into simple substance Cu, thereby obtaining copper-coated sodium chloride particles with the thickness of the copper-coated layer of 5 microns.
Example 2
A method for coating copper on the surface of sodium chloride particles is characterized by comprising the following steps:
（1）Cu(NO 3 ) 2 preparing an acetone solution: according to Cu (NO) 3 ) 2 Mixing with acetone solution with concentration of 50g/100g, adding Cu (NO) 3 ) 2 Adding into acetone, and stirring to make Cu (NO) 3 ) 2 Dissolving in acetone to obtain Cu (NO) 3 ) 2 Of (2) in acetone.
(2) The sodium chloride particles are mixed evenly: adding the following components in percentage by weight according to the addition amount of sodium chloride particles: cu (NO) 3 ) 2 Acetone solution mass =1, and commercial industrial salt with a particle size of 0.2mm is added to Cu (NO) obtained in step (2) 3 ) 2 Stirring in acetone solution, and ultrasonic vibrating for 50 min to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in acetone solution.
(3) Baking and volatilizing acetone: NaCl-Cu (NO) obtained in the step (2) 3 ) 2 Baking the acetone solution at 50 deg.C for 60 min to volatilize acetone to obtain Cu (NO) coated solution 3 ) 2 ·3H 2 Sodium chloride particles of O.
（4）Cu(NO 3 ) 2 Heating and decomposing: coating the Cu (NO) prepared in the step (3) 3 ) 2 ·3H 2 Heating the sodium chloride particles of O to 350 ℃, and keeping the temperature for 2 hours to ensure that Cu (NO) on the surfaces of the sodium chloride particles 3 ) 2 ·3H 2 And decomposing O into CuO to obtain the CuO-coated sodium chloride particles.
(5) And (3) CuO reduction: h, mixing the sodium chloride particles coated with CuO obtained in the step (4) 2 Heating to 430 ℃ in the atmosphere, and preserving the heat for 3 hours to reduce CuO into simple substance Cu, thereby obtaining copper-coated sodium chloride particles with the thickness of a copper-coated layer of 10 microns.
Example 3
A method for coating copper on the surface of sodium chloride particles is characterized by comprising the following steps:
（1）Cu(NO 3 ) 2 preparing an acetone solution: according to Cu (NO) 3 ) 2 Mixing with acetone solution with concentration of 80g/100g, and adding Cu (NO) 3 ) 2 Adding into acetone, and stirring to make Cu (NO) 3 ) 2 Dissolving in acetone to obtain Cu (NO) 3 ) 2 In acetone.
(2) The sodium chloride particles are mixed evenly: adding the following components in percentage by weight according to the addition amount of sodium chloride particles: cu (NO) 3 ) 2 Acetone solution mass =1.5, and commercial industrial salt having a particle size of 0.6mm is added to Cu (NO) obtained in step (2) 3 ) 2 Stirring in acetone solution, and ultrasonic vibrating for 40 min to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in acetone solution.
(3) Baking and volatilizing acetone: NaCl-Cu (NO) obtained in the step (2) 3 ) 2 Baking the acetone solution at 50 deg.C for 90 min to volatilize acetone to obtain Cu (NO) coated solution 3 ) 2 ·3H 2 Sodium chloride particles of O.
(4) Cu (NO3)2 thermal decomposition: coating the Cu (NO) prepared in the step (3) 3 ) 2 ·3H 2 Heating the sodium chloride particles of O to 400 ℃ and preserving the heat for 1.5 hours to ensure that Cu (NO) on the surfaces of the sodium chloride particles 3 ) 2 ·3H 2 The O is decomposed and converted into CuO, and the sodium chloride particles coated with the CuO are obtained.
(5) And (3) CuO reduction: adding the CuO-coated sodium chloride particles obtained in the step (4) into H 2 Heating to 470 ℃ in the atmosphere, and preserving the heat for 2.5 hours to reduce CuO into simple substance Cu, thereby obtaining copper-coated sodium chloride particles with the thickness of a copper-coated layer of 15 microns.
Example 4
A method for coating copper on the surface of sodium chloride particles is characterized by comprising the following steps:
（1）Cu(NO 3 ) 2 preparing an acetone solution: according to Cu (NO) 3 ) 2 Preparing the acetone solution with the concentration of 110g/100g, and adding Cu (NO) 3 ) 2 Adding into acetone, and stirring to make Cu (NO) 3 ) 2 Dissolving in acetone to obtain Cu (NO) 3 ) 2 In acetone.
(2) Mixing sodium chloride particles: adding the following components in percentage by weight according to the addition amount of sodium chloride particles: cu (NO) 3 ) 2 The mass of acetone solution =2, and the grain diameter is adjusted1mm of commercial industrial salt was put into Cu (NO) obtained in step (2) 3 ) 2 Stirring in acetone solution, and ultrasonic vibrating for 30 min to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in acetone solution.
(3) Baking and volatilizing acetone: NaCl-Cu (NO) obtained in the step (2) 3 ) 2 Baking the acetone solution at 50 deg.C for 120 min to volatilize acetone to obtain Cu (NO) coated solution 3 ) 2 ·3H 2 Sodium chloride particles of O.
（4）Cu(NO 3 ) 2 Heating and decomposing: coating the Cu (NO) prepared in the step (3) 3 ) 2 ·3H 2 Heating the sodium chloride particles of O to 450 ℃ and preserving the heat for 1 hour to ensure that Cu (NO) on the surfaces of the sodium chloride particles 3 ) 2 ·3H 2 The O is decomposed and converted into CuO, and the sodium chloride particles coated with the CuO are obtained.
(5) And (3) CuO reduction: adding the CuO-coated sodium chloride particles obtained in the step (4) into H 2 Heating to 500 ℃ in the atmosphere, and preserving the heat for 2 hours to reduce CuO into simple substance Cu, thereby obtaining copper-coated sodium chloride particles with the thickness of the copper-coated layer being 20 microns.
NaCl does not dissolve in propanol, but Cu (NO) in the examples of the invention 3 ) 2 Has high solubility in propanol, and can dissolve Cu (NO) by using propanol as solvent 3 ) 2 Adding NaCl, heating to volatilize propanol, and heating to high temperature to volatilize Cu (NO) 3 ) 2 Decomposing the sodium chloride into CuO, and reducing the CuO into simple substance Cu in reducing atmosphere to finally obtain copper-coated sodium chloride particles; by adopting the copper-coated sodium chloride particles treated by the method as the seepage precursor, as the wetting angle of copper and aluminum melt at the seepage temperature is less than 90 degrees and the wettability is good, the aluminum melt can smoothly permeate into gaps of superfine sodium chloride particles, and the preparation problem of the porous aluminum with the through hole with the superfine aperture (less than 1 mm) is solved.
Claims (6)
1. A method for coating copper on the surface of sodium chloride particles is characterized by comprising the following steps:
(1) adding Cu (NO) 3 ) 2 Dissolving in acetone to obtain Cu (NO) 3 ) 2 By adding sodium chloride particles to Cu (NO) 3 ) 2 Stirring in acetone solution, and ultrasonic vibrating to make sodium chloride particles in Cu (NO) 3 ) 2 Fully soaking in an acetone solution;
(2) mixing NaCl-Cu (NO) 3 ) 2 Baking acetone solution at low temperature to volatilize acetone to obtain Cu (NO) coated product 3 ) 2 ·3H 2 Sodium chloride particles of O;
(3) coating the Cu (NO) prepared in the step (2) 3 ) 2 ·3H 2 Heating the sodium chloride particles of O to make Cu (NO) on the surfaces of the sodium chloride particles 3 ) 2 ·3H 2 Decomposing O into CuO to obtain CuO-coated sodium chloride particles;
(4) sodium chloride particles coated with CuO are put in H 2 Heating and preserving heat in the atmosphere to reduce CuO into simple substance Cu, thereby obtaining the sodium chloride particles with the surfaces coated with Cu.
2. The method of claim 1, wherein the sodium chloride particles are coated with copper on the surface, and wherein: cu (NO) 3 ) 2 Cu (NO) in acetone solution 3 ) 2 The amount of (2) added is (20-110) g/100 g.
3. The method of coating copper on the surface of sodium chloride particles according to claim 1, wherein: the sodium chloride particles in the step (1) have the particle size of 0.05-1mm, and are mixed with Cu (NO) 3 ) 2 The mass ratio of the acetone solution is 0.5:1-2:1, and the ultrasonic vibration time is 30-60 minutes.
4. The method of coating copper on the surface of sodium chloride particles according to claim 1, wherein: the low-temperature baking conditions in the step (2) are as follows: baking at 50 deg.C for 30-120 min.
5. The method of claim 1, wherein the sodium chloride particles are coated with copper on the surface, and wherein: the heating conditions in the step (3) are as follows: keeping the temperature at 300-450 ℃ for 1-3 hours.
6. The method of claim 1, wherein the sodium chloride particles are coated with copper on the surface, and wherein: in the step (4), the reduction temperature of CuO is 400-500 ℃, the reduction time is 2-4 hours, and the thickness of the obtained copper cladding is 5-20 micrometers.
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