CN1900332A - Method for preparing copper base composite material by chemical precipitation method to obtain composite powder - Google Patents
Method for preparing copper base composite material by chemical precipitation method to obtain composite powder Download PDFInfo
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Abstract
The process of preparing copper base composite material with composite powder prepared through chemical precipitation includes the following steps: dropping ammonium bicarbonate into mother liquid comprising copper sulfate and aluminum ammonium sulfate at 25-30 deg.c to obtain settled NH4Al(OH)2CO3-Cu2(OH)2CO3 sol, ageing for 8 hr and centrifuging to obtain NH4Al(OH)2CO3 -Cu2(OH)2CO3 gel, washing the gel with anhydrous alcohol, centrifuging to eliminate alcohol and stoving and grinding at 50deg.c to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3 precursor, igniting the precursor at 1100-1200 deg.c to obtain composite Al2O3-CuO powder, reducing the composite Al2O3-CuO powder in reducing methanol or hydrogen atmosphere at 350 deg.c for 0.5-1 hr to obtain composite Al2O3-Cu powder; cold pressing the composite Al2O3-Cu powder at 100 kN pressure to form blank, and final at 800-850 deg.c. The present invention has precisely controlled Al2O3 content for required wear resistance and conductivity.
Description
Technical Field
The invention relates to a preparation method of a nano composite material, in particular to a method for preparing a copper-based composite material by using composite powder obtained by a chemical precipitation method.
Background
The dispersion strengthening copper-based composite material is characterized in that second phase particles with good thermal stability are formed in a copper matrix in a dispersion distribution manner through a certain process, so that the strength and the high-temperature stability of the material are improved. The copper-based composite material has excellent electrical and thermal conductivity, high-temperature stability and high strength, has great application potential in the high-tech fields of electromechanics, astronavigation, microelectronics and the like, is widely applied to large-scale integrated circuit lead frames, electric welding electrodes, change-over switches, electric contacts and the like, and is a key material for the development of the modern electronic information industry.
At present, tungsten, molybdenum, graphite andsilicon carbide are often selected as reinforcing phases to be sintered into a copper-based composite material together with Cu powder through powder metallurgy, but the proportion of tungsten and molybdenum is high, and the compounding amount of silicon carbide is large. Nano Al2O3Has the characteristics of high strength, excellent thermal conductivity, small thermal expansion coefficient and good high-temperature stability, and can be used for reinforcing the copper-based material, not only can not greatly reduce the electrical conductivity of the matrix, but also can ensure the strength of the matrix due to the reinforcing effectAnd the high temperature performance is significantly improved. Al in the prior art2O3the-Cu composite powder ① adopts a mechanical alloying method, namely Cu and Al2O3Grinding the powder in high-energy ball mill for a long time to obtain composite powder, ② internal oxidation by adding unstable compound powder into alloy powder to make the components in alloy and added compound generate thermal reduction reaction to generate more stable ceramic reinforced particles, ③ nm Al2O3Powder chemical copper plating method. These methods have more or less some problems: such as mechanical alloying, cannot completely open nanoscale Al2O3The oxygen supply amount of the powder and internal oxidation method cannot be accurately controlled, and the proportion of the powder and the internal oxidation method cannot be accurately controlled by the powder chemical copper plating method.
Disclosure of Invention
The invention provides a method for preparing a copper-based composite material by using composite powder obtained by a chemical precipitation method, and nanoscale Al is obtained by using the chemical precipitation method2O3-Cu composite powder with precise control of Al2O3Al in-Cu composite powder2O3The content of the copper-based composite material is convenient for preparing copper-based composite materials with different properties, and the requirements of various working conditions are met.
The technical solution of the invention is as follows: firstly, at the temperature of 25-30 ℃, adding precipitator ammonium bicarbonate dropwise into mother liquor consisting of copper sulfate and ammonium aluminum sulfate, and coprecipitating to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Sol, NH4Al(OH)2CO3-Cu2(OH)2CO3Aging the sol at room temperature for 8 hours, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Soaking gel in anhydrous ethanol for 4 hr, centrifuging to remove alcohol to obtain gel, washing with alcohol for more than 3 times, oven drying the gel slowly at 50 deg.C, grinding, and sieving with 100 mesh and 200 mesh sieve to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Firing the precursor powder at 1100-1200 DEG CGrinding the precursor powder for 0.5-1 hour, and sieving with a 200-mesh sieve and a 400-mesh sieve to obtain the nano Al2O3-CuO composite powder; then, adding Al2O3reducing-CuO composite powder at 350 ℃ in methanol or hydrogen reducing atmosphere to obtain Al2O3-a Cu composite powder; finally, Al2O3And (4) cold-pressing the-Cu composite powder into a blank, and sintering and forming at 800-850 ℃ to obtain the copper-based composite material.
The invention relates to a method for preparing a copper-based composite material by using composite powder obtained by a chemical precipitation method, wherein the raw materials comprise copper sulfate, aluminum ammonium sulfate, ammonium bicarbonate and sulfurThe acid copper and the aluminum ammonium sulfate form mother liquor, and the ammonium bicarbonate is used as a precipitator; according to Al2O3Al in-Cu composite2O3To determine NH4Al(SO4)2And CuSO4According to NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3Is 1: 2 to determine NH4HCO3Amount of Al2O3Al in-Cu2O3Less than 5% by mass; NH (NH)4Al(OH)2CO3-Cu2(OH)2CO3The precursor powder is burnt at the high temperature of 1100-1200 ℃ for 0.5-1 hour to obtain Al2O3-a Cu composite powder; al (Al)2O3Reducing the-CuO composite powder in a reducing atmosphere of methanol or hydrogen at 350 ℃ for 0.5 to 1 hour to obtain Al2O3-a Cu composite powder; al (Al)2O3And (4) carrying out cold pressing on the-Cu composite powder under the pressure of 100kN to form a blank, and sintering at the temperature of 800-850 ℃ to obtain the copper-based composite material.
The invention relates to a method for preparing a copper-based composite material by using composite powder obtained by a chemical precipitation method, which comprises the following specific steps:
(1) firstly, preparing nano Al by a chemical precipitation method2O3-CuO composite powder;
the operating conditions are as follows: the temperature of the constant temperature water bath is set to be 25-30 ℃;
mother liquor and precipitant: according to Al2O3Al in-Cu2O3Ratiometric determination of NH4Al(SO4)2And CuSO4In accordance with NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3Is 1: 2 to determine NH4HCO3Amount of (1), Al2O3Al in-Cu2O3Less than 5% by mass;
surfactant (b): the weight of the sodium hexametaphosphate with the concentration of 0.5mg/L is two ten-thousandth of the weight of the raw material;
the method comprises the following operation steps: A. NH to be configured according to the above requirements4Al(SO4)2And CuSO4Adding the mother liquor into a reaction kettle, simultaneously adding sodium hexametaphosphate, and mechanically stirring until the mother liquor is dissolved;
B. dripping the precipitant into the mother liquid at a speed of 10ml/min, and continuously stirring for 0.5 hour after all the precipitant is dripped out to ensure the homogenization of the system and finally generate NH4Al(OH)2CO3And Cu2(OH)2CO3Sol;
C. aging the sol for 8 hours at room temperature, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Soaking the gel in absolute ethyl alcohol for 4 hours, centrifuging and dealcoholizing to obtain gel, and repeating the alcohol washing process for more than 3 times;
D. slowly drying the dealcoholized gel at 50 ℃, grinding, and sieving with 100-mesh and 200-mesh sieves to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Precursor powder;
E. calcining the precursor powder for 0.5-1 hour at 1100-1200 ℃, grinding, and sieving with a 200-mesh sieve and a 400-mesh sieve to obtain the nano Al2O3-CuO composite powder;
(2) then, reducing Al2O3Al from CuO2O3-Cu composite powder:
reducing the mixture in a reducing atmosphere of methanol or hydrogen at 350 ℃ for 0.5 to 1 hour to obtain Al2O3-a Cu composite powder.
(3) And finally, cold pressing to form a blank, and sintering at normal pressure:
mixing Al2O3Carrying out cold pressing on the Cu composite powder on a press to form a blank, and selecting the double-sided cold pressing for more than 6 times under the pressure of 100 kN; and then sintering and molding in a sintering furnace at 800-850 ℃ to obtain the copper-based composite material.
It is known to use aluminum ammonium sulfate (NH)4AlSO4·12H2O) is mother liquid, ammonium hydrogen carbonate (NH)4HCO3) As a precipitant, alumina (Al) can be obtained2O3) Powder:
copper sulfate (CuSO) is known4·5H2O) is mother liquor, ammonium hydrogen carbonate (NH)4HCO3) As a precipitant, copper oxide powder can be produced:
thus, ammonium bicarbonate (NH) is employed4HCO3) As co-precipitating agent, depending on the Al content of the composite2O3To determine NH4Al(SO4)2、CuSO4And NH4HCO3The quality of the reactant is controlled, and the agglomeration of the powder is controlled by controlling the technical parameters in the preparation process, so that the nano-grade composite powder is obtained.
Due to Al2O3The non-conductor is added, although the strength and the wear resistance can be improved, the electrical conductivity of the product is influenced to a certain extent, and the more the content of the non-conductor is, the poorer the electrical conductivity is. Therefore, according to different requirements, different Al contents can be obtained by adjusting the relative amount of the mother liquor2O3The copper-based composite material has high strength, high conductivity, good thermal property, high hardness and good wear resistance, and can be used for contact materials, spot welding electrodes, integrated circuit lead frames, aviation and other occasions requiring high strength and high wear resistance in the field of microelectronic packaging.
Detailed Description
Method for preparing copper-based composite material by using composite powder obtained by chemical precipitation methodThe method comprises the following steps: firstly, at the temperature of 25-30 ℃, in the group of copper sulfate and aluminum ammonium sulfateThe mother liquid is added with ammonium bicarbonate as precipitant and then coprecipitated to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Aging the solat room temperature for 8 hours, removing supernatant, centrifugally dewatering to obtain gel, soaking the gel in absolute ethyl alcohol for 4 hours, centrifugally dealcoholizing, repeating the alcohol washing process for more than 3 times, slowly drying the dealcoholized gel at 50 ℃, grinding, sieving by a 100-mesh sieve and a 200-mesh sieve to obtain precursor powder, calcining the precursor powder for 0.5-1 hour at 1100-1200 ℃, grinding, sieving by a 200-mesh sieve and a 400-mesh sieve to obtain the nano Al2O3-CuO composite powder; then, adding Al2O3reducing-CuO composite powder at 350 ℃ in methanol or hydrogen reducing atmosphere to obtain Al2O3-a Cu composite powder; finally, Al2O3And (4) carrying out cold pressing on Cu to form a blank, and sintering and forming at 800-850 ℃ to obtain the copper-based composite material.
The method comprises the following specific steps:
(1) firstly, preparing nano Al by a chemical precipitation method2O3-CuO composite powder:
the operating conditions are as follows: the temperature of the constant temperature water bath is set to be 25-30 ℃;
mother liquor and precipitant: according to Al2O3Al in-Cu2O3Ratiometric determination of NH4Al(SO4)2And CuSO4In accordance with NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3Is 1: 2 to determine NH4HCO3Amount of (1), Al2O3Al in-Cu2O3Less than 5% by mass;
surfactant (b): the weight of the sodium hexametaphosphate with the concentration of 0.5mg/L is two ten-thousandth of the weight of the rawmaterial;
the method comprises the following operation steps: A. NH to be configured according to the above requirements4Al(SO4)2And CuSO4Adding the mother liquor into a reaction kettle, simultaneously adding sodium hexametaphosphate, and mechanically stirring until the mother liquor is dissolved;
B. adding a precipitator NH4HCO3Dropping into the mother liquor at a speed of 10ml/minAfter the partial dripping is finished, stirring is continued for 0.5 hour to ensure the homogenization of the system and finally generate NH4Al(OH)2CO3And Cu2(OH)2CO3Sol;
C. aging the sol for 8 hours at room temperature, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Soaking the gel in absolute ethyl alcohol for 4 hours, centrifuging and dealcoholizing to obtain gel, and performing alcohol washing for more than 3 times;
D. slowly drying the gel after dealcoholization at 50 ℃, grinding and sieving with 100-mesh and 200-mesh sieves to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Precursor powder;
E. calcining the precursor powder for 0.5-1 hour at 1100-1200 ℃, grinding and sieving with 200-mesh and 400-mesh sieves to obtain the nano Al2O3-CuO composite powder;
(2) then, reducing Al2O3Al from CuO2O3-Cu composite powder:
reducing the mixture in a reducing atmosphere of methanol or hydrogen at 350 ℃ for 0.5 to 1 hour to obtain Al2O3-a Cu composite powder.
(3) And finally, cold pressing to form a blank, and sintering at normal pressure:
mixing Al2O3Carrying out cold pressing on the Cu composite powder on a press to form a blank, and selecting the double-sided cold pressing for more than 6 times under the pressure of 100 kN; and sintering and molding in a sintering furnace at 800-850 ℃ to obtain the copper-based composite material.
Example 1:
(1) firstly, preparing nano Al by adopting a chemical precipitation method2O3-CuO composite powder:
the operating conditions are as follows: the temperature of the constant temperature water bath is set at 25 ℃;
mother liquor and precipitant: by Al in copper-based composites2O3For an example of a content of 5% (mass fraction), 0.75g of NH was weighed4Al(SO4)2And 6.25g of CuSO4Adding water to prepare 200mlSolution according to NH4Al(SO4)2And NH4HCO3In a molar ratio of 1 to4 and CuSO4And NH4HCO3In a molar ratio of 1: 2, 4.47g of NH are determined4HCO3Adding water to prepare 200ml of solution; to make CuSO4·5H2O and NH4Al(SO4)2·12H2Complete reaction of O and make up for the waste, NH, during the addition4HCO3An appropriate excess was made, so 4.5g of NH were weighed4HCO3Adding water to prepare 205ml of solution;
surfactant (b): 0.2mg of sodium hexametaphosphate;
the method comprises the following operation steps: A. NH to be configured according to the above requirements4Al(SO4)2And CuSO4Adding the mother liquor into a reaction kettle, simultaneously adding sodium hexametaphosphate, and mechanically stirring until the mother liquor is dissolved;
B. adding a precipitator NH4HCO3Dripping into the mother liquor at a speed of 10ml/min, and continuing stirring for 0.5 hour after all dripping to ensure the homogenization of the system and finally generate NH4Al(OH)2CO3And Cu2(OH)2CO3Sol;
C. aging the sol for 8 hours at room temperature, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Soaking the gel in absolute ethyl alcohol for 4 hours, centrifuging and dealcoholizing to obtain gel, and performing alcohol washing for more than 3 times;
D. slowly drying the dealcoholized gel at 50 ℃, grinding, and sieving with a 100-mesh sieve to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Precursor powder;
E. calcining the precursor powder for 0.5 hour at 1100 ℃, grinding, and sieving with a 200-mesh sieve to obtain the nano Al2O3-CuO composite powder;
(2) then, reducing Al2O3Al from CuO2O3-Cu composite powder:
methanol at 350 ℃Reducing for 0.5 hour in reducing atmosphere to obtain Al2O3-a Cu composite powder.
(3) And finally, cold pressing to form a blank, and sintering at normal pressure:
mixing Al2O3Carrying out cold pressing on-Cu composite powder on a press to form a blank, wherein the pressure is selected to be100kN, cold pressing the two surfaces for more than 6 times; and then sintering and molding in a sintering furnace at 800 ℃ to obtain the high-strength medium-conductivity copper-based composite material.
Example 2:
(1) firstly, preparing nano Al by adopting a chemical precipitation method2O3-CuO composite powder:
the operating conditions are as follows: the temperature of the constant temperature water bath is set at 28 ℃;
mother liquor and precipitant: by Al in copper-based composites2O3For example, the content was 3% (mass fraction), and 0.44g of NH was weighed4Al(SO4)2And 6.25g of CuSO4Adding water to prepare 200ml of solution according to NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3In a molar ratio of 1: 2, 4.26g of NH are determined4HCO3Adding water to prepare 200ml of solution; to make CuSO4·5H2O and NH4Al(SO4)2·12H2Complete reaction of O and make up for the waste, NH, during the addition4HCO3An appropriate excess was made, so 4.3g of NH were weighed4HCO3Adding water to prepare 205ml of solution;
surfactant (b): 0.2mg of sodium hexametaphosphate;
the method comprises the following operation steps: A. NH to be configured according to the above requirements4Al(SO4)2And CuSO4Adding the mother liquor into a reaction kettle, simultaneously adding sodium hexametaphosphate, and mechanically stirring until the mother liquor is dissolved;
B. adding a precipitator NH4HCO3Dripping into the mother liquor at a speed of 10ml/min, and continuing stirring for 0.5 hour after all dripping to ensure the homogenization of the system and finally generate NH4Al(OH)2CO3And Cu2(OH)2CO3Sol;
C. aging the sol for 8 hours at room temperature, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Soaking the gel in absolute ethyl alcohol for 4 hours, centrifuging and dealcoholizing to obtain gel, and performing alcohol washing for more than 3 times;
D. slowly drying the dealcoholized precursor gel at 50 ℃, grinding,sieving with 200 mesh sieve to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Precursor powder;
E. calcining the precursor powder for 0.8 hour at 1150 ℃, grinding and sieving with a 400-mesh sieve to obtain the nano Al2O3-CuO composite powder;
(2) then, reducing Al2O3Al from CuO2O3-Cu composite powder:
reducing for 0.8 hours in hydrogen reducing atmosphere at 350 ℃ to obtain Al2O3-a Cu composite powder.
(3) And finally, cold pressing to form a blank, and sintering at normal pressure:
mixing Al2O3Carrying out cold pressing on the Cu composite powder on a press to form a blank, and selecting the double-sided cold pressing for more than 6 times under the pressure of 100 kN; and then sintering and molding in a 830 ℃ sintering furnace to obtain the high-strength high-conductivity copper-based composite material.
Example 3:
(1) firstly, preparing nano Al by adopting a chemical precipitation method2O3-CuO composite powder:
the operating conditions are as follows: the temperature of the constant temperature water bath is set at 30 ℃;
mother liquor and precipitant: by Al in copper-based composites2O3For an example of a content of 1% (mass fraction), 0.144g of NH was weighed4Al(SO4)2And 6.25g of CuSO4Adding water to prepare 200ml of solution according to NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3Is determined to be 4.1 when the molar ratio of (1: 2)g NH of4HCO3Adding water to prepare 200ml of solution; to make CuSO4·5H2O and NH4Al(SO4)2·12H2Complete reaction of O and make up for the waste, NH, during the addition4HCO3An appropriate excess was made, so 4.2g of NH were weighed4HCO3Adding water to prepare 205ml of solution;
surfactant (b): 0.2mg of sodium hexametaphosphate;
the method comprises the following operation steps: A. NH to be configured according to the above requirements4Al(SO4)2And CuSO4FemaleAdding the solution into a reaction kettle, simultaneously adding sodium hexametaphosphate, and mechanically stirring until the solution is dissolved;
B. adding a precipitator NH4HCO3Dripping into the mother liquor at a speed of 10ml/min, and continuing stirring for 0.5 hour after all dripping to ensure the homogenization of the system and finally generate NH4Al(OH)2CO3And Cu2(OH)2CO3Sol;
C. aging the sol for 8 hours at room temperature, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Soaking the gel in absolute ethyl alcohol for 4 hours, centrifuging and dealcoholizing to obtain gel, wherein the alcohol washing process needs more than 3 times;
D. slowly drying the dealcoholized precursor gel at 50 ℃, grinding and sieving by a 100-mesh sieve to obtain precursor powder;
E. calcining the precursor powder for 1 hour at 1200 ℃, grinding and sieving with a 400-mesh sieve to obtain the nano Al2O3-CuO composite powder;
(2) then, reducing Al2O3Al from CuO2O3-Cu composite powder:
reducing for 1 hour in a methanol reducing atmosphere at 350 ℃ to obtain Al2O3-a Cu composite powder.
(3) And finally, cold pressing to form a blank, and sintering at normal pressure:
mixing Al2O3Cold pressing the-Cu composite powder on a press to form a blank, and selecting pressureThe steel is 100kN, and the double faces are cold-pressed for more than 6 times; and then sintering and molding in a sintering furnace at 850 ℃ to obtain the medium-strength high-conductivity copper-based composite material.
Claims (9)
1. A method for preparing a copper-based composite material by using composite powder obtained by a chemical precipitation method is characterized by comprising the following steps: firstly, at the temperature of 25-30 ℃, adding precipitator ammonium bicarbonate dropwise into mother liquor consisting of copper sulfate and ammonium aluminum sulfate, and coprecipitating to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Sol, aging the sol for 8 hours, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Gel, washing the gel with absolute ethyl alcohol, centrifugally dealcoholizing, drying at 50 ℃ and grinding to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Precursor powder, wherein the precursor powder is burnt at the high temperature of 1100-1200 ℃ to obtain Al2O3-CuO composite powder; then, Al2O3reducing-CuO composite powder at 350 ℃ in reducing atmosphere to obtain Al2O3-a Cu composite powder; finally, Al2O3And (4) carrying out cold pressing on Cu to form a blank, and sintering and forming at 800-850 ℃.
2. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 1, wherein the method comprises the following steps: the raw materials are copper sulfate, aluminum ammonium sulfate and ammonium bicarbonate, the copper sulfate and the aluminum ammonium sulfate form mother liquor, the ammonium bicarbonate is a precipitator, and Al is used as a reference2O3Al in-Cu2O3Ratiometric determination of NH4Al(SO4)2And CuSO4In accordance with NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3Is 1: 2 to determine NH4HCO3Amount of (1), Al2O3Al in-Cu2O3Is less than 5 percent.
3. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 1, wherein the method comprises the following steps:NH4Al(OH)2CO3-Cu2(OH)2CO3and (3) firing the precursor powder at the high temperature of 1100-1200 ℃ for 0.5-1 hour.
4. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 1, wherein the method comprises the following steps: al (Al)2O3Reducing the-CuO composite powder in a methanol or hydrogen reducing atmosphere at 350 ℃ for 0.5 to 1 hour to obtain Al2O3-a Cu composite powder.
5. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 1, wherein the method comprises the following steps: al (Al)2O3And (3) carrying out cold pressing on the-Cu composite powder under the pressure of 100kN to form a blank, and then sintering at the temperature of 800-850 ℃ for 1 hour to form the final copper-based composite material.
6. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 1, wherein the method comprises the following steps: the method comprises the following specific steps:
(1) firstly, preparing nano Al by a chemical precipitation method2O3-CuO composite powder:
the operating conditions are as follows: the temperature of the constant temperature water bath is set to be 25-30 ℃;
mother liquor and precipitant: according to Al2O3Al in-Cu2O3Ratiometric determination of NH4Al(SO4)2And CuSO4In accordance with NH4Al(SO4)2And NH4HCO3In a molar ratio of 1: 4 and CuSO4And NH4HCO3Is 1: 2 to determine NH4HCO3The amount of (c); al (Al)2O3Al in-Cu2O3Less than 5% by mass;
surfactant (b): sodium hexametaphosphate, the concentration is 0.5 mg/L;
the method comprises the following operation steps: A. NH to be configured according to the above requirements4Al(SO4)2And CuSO4Adding the mother liquor into a reaction kettle, simultaneously adding sodium hexametaphosphate, and mechanically stirring until the mother liquor is dissolved;
B. adding a precipitator NH4HCO3Dripping into the mother liquor at a speed of 10ml/min, and continuing stirring for 0.5 hour after all dripping to ensure the homogenization of the system and finally generate NH4Al(OH)2CO3-Cu2(OH)2CO3Sol;
C. aging the sol for 8 hours at room temperature, removing supernatant, and centrifugally dewatering to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Gel, soaking the gel in absolute ethyl alcohol for 4 hours, centrifuging and dealcoholizing to obtain precursor gel, and repeating the alcohol washing process for more than 3 times;
D. slowly drying the gel after dealcoholization at 50 ℃, grinding and sieving with 100-mesh and 200-mesh sieves to obtain NH4Al(OH)2CO3-Cu2(OH)2CO3Precursor powder;
E. calcining the precursor powder for 0.5-1 hour at 1100-1200 ℃, grinding and sieving with 200-mesh and 400-mesh sieves to obtain the nano Al2O3-CuO composite powder;
(2) then, reducing Al2O3Al from CuO2O3-Cu composite powder:
reducing the mixture in a reducing atmosphere of methanol or hydrogen at 350 ℃ for 0.5 to 1 hour to obtain Al2O3-a Cu composite powder;
(3) and finally, cold pressing to form a blank, and sintering at normal pressure:
mixing Al2O3Carrying out cold pressing on the Cu composite powder on a press to form a blank, and selecting the double-sided cold pressing for more than 6 times under the pressure of 100 kN; and sintering and molding in a sintering furnace at 800-850 ℃ to obtain the copper-based composite material.
7. The method of claim 6The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method is characterized by comprising the following steps of: excess NH per 1L of mother liquor4HCO35-10 ml of the solution.
8. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 6, wherein the method comprises the following steps: the sintering time of the blank in the sintering furnace is determined according to the thickness, and the equivalent thickness is generally used for sintering for 10 minutes per 1 mm.
9. The method for preparing the copper-based composite material by using the composite powder obtained by the chemical precipitation method according to claim 6, wherein the method comprises the following steps: the weight of the sodium hexametaphosphate is two ten-thousandth of the weight of the raw material.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103173645A (en) * | 2013-03-25 | 2013-06-26 | 北京科技大学 | Preparation method of dispersedly strengthened aluminum-based composite material |
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| US6261336B1 (en) * | 2000-08-01 | 2001-07-17 | Rutgers, The State University Of New Jersey | Stable aqueous iron based feedstock formulation for injection molding |
| CN1141406C (en) * | 2002-05-30 | 2004-03-10 | 昆明理工大学 | Process for preparing Cu-Al2O3 composition |
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| WO2013135109A1 (en) * | 2012-03-13 | 2013-09-19 | 北京科技大学 | Method for preparing high-strength high-conductivity and dispersion-strengthened copper |
| CN103173645A (en) * | 2013-03-25 | 2013-06-26 | 北京科技大学 | Preparation method of dispersedly strengthened aluminum-based composite material |
| CN103173645B (en) * | 2013-03-25 | 2014-09-17 | 北京科技大学 | Preparation method of dispersedly strengthened aluminum-based composite material |
| CN103981381A (en) * | 2014-05-15 | 2014-08-13 | 厦门理工学院 | Method for preparing nano aluminum oxide dispersion enhanced copper-base composite material according to sol-gel method |
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| CN105350104A (en) * | 2015-12-01 | 2016-02-24 | 东华大学 | Method for preparing mesoporous zirconium phosphate supported copper oxide antibacterial polyvinyl alcohol fibers |
| CN105350104B (en) * | 2015-12-01 | 2017-10-27 | 东华大学 | A kind of preparation method of Mesoporous zirconium phosphate loaded copper oxide antibacterial polyethylene alcohol fiber |
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| CN111462939A (en) * | 2020-04-08 | 2020-07-28 | 安徽壹石通材料科技股份有限公司 | Nano-alumina-enhanced silver-based electrical contact material and preparation method thereof |
| CN114293051A (en) * | 2021-12-23 | 2022-04-08 | 北京科大京都高新技术有限公司 | Preparation method of high-temperature softening resistant high-strength high-conductivity copper-based composite material formed part |
| CN114293051B (en) * | 2021-12-23 | 2022-07-26 | 北京科大京都高新技术有限公司 | Preparation method of high-temperature softening resistant high-strength high-conductivity copper-based composite material formed part |
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