CN108202145B - Preparation method of nano aluminum oxide/copper composite reinforced phase - Google Patents

Preparation method of nano aluminum oxide/copper composite reinforced phase Download PDF

Info

Publication number
CN108202145B
CN108202145B CN201810020952.8A CN201810020952A CN108202145B CN 108202145 B CN108202145 B CN 108202145B CN 201810020952 A CN201810020952 A CN 201810020952A CN 108202145 B CN108202145 B CN 108202145B
Authority
CN
China
Prior art keywords
copper
salt
aluminum
alumina
mixed solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201810020952.8A
Other languages
Chinese (zh)
Other versions
CN108202145A (en
Inventor
鲍瑞
熊倪
易健宏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kunming University of Science and Technology
Original Assignee
Kunming University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kunming University of Science and Technology filed Critical Kunming University of Science and Technology
Priority to CN201810020952.8A priority Critical patent/CN108202145B/en
Publication of CN108202145A publication Critical patent/CN108202145A/en
Application granted granted Critical
Publication of CN108202145B publication Critical patent/CN108202145B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1089Alloys containing non-metals by partial reduction or decomposition of a solid metal compound

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Geology (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

本发明涉及一种纳米氧化铝/铜复合增强相的制备方法,属于粉末冶金技术和复合材料制备技术领域。本发明所述方法为配制铜盐和铝盐的混合溶液,采用喷雾热解和还原煅烧的方法获得结合紧密,均匀细小的纳米级球形氧化铝/铜复合增强相,该复合增强粉体可以有效用于增强金属基复合材料。本发明所述方法具有工序简单、操作方便、生产过程连续、产能大、生产效率高等特点,制备的氧化铝/铜复合增强相为纳米级的尺寸,并且铜和氧化铝分散均匀,其中氧化铝和铜的摩尔比例可以通过调整溶液的浓度进行调控。

Figure 201810020952

The invention relates to a preparation method of nano-alumina/copper composite reinforcing phase, belonging to the technical field of powder metallurgy technology and composite material preparation. The method of the invention is to prepare a mixed solution of copper salt and aluminum salt, and adopt the methods of spray pyrolysis and reduction calcination to obtain a tightly bound, uniform and fine nano-scale spherical alumina/copper composite reinforcing phase. The composite reinforcing powder can have Effective for reinforcing metal matrix composites. The method of the invention has the characteristics of simple procedure, convenient operation, continuous production process, large production capacity and high production efficiency, the prepared alumina/copper composite reinforcing phase is nano-scale, and copper and alumina are uniformly dispersed, wherein alumina The molar ratio of copper and copper can be adjusted by adjusting the concentration of the solution.

Figure 201810020952

Description

Preparation method of nano aluminum oxide/copper composite reinforced phase
Technical Field
The invention relates to a preparation method of a nano aluminum oxide/copper composite reinforcing phase, belonging to the technical field of powder metallurgy and composite material preparation.
Background
Copper and copper-based composite materials are widely used as functional materials because of their good electrical conductivity, thermal conductivity, corrosion resistance, and excellent manufacturability and easy recovery. However, in general, copper-based conductive and heat-conductive composite materials have high electrical conductivity and low strength, and when the strength is increased, the electrical and thermal properties are lost. In order to improve the mechanical properties, especially the thermal stability, of the material while ensuring its electrical and thermal properties, an effective method is to use dispersion reinforcements (e.g., alumina particles) to strengthen the copper matrix.
Preparation of Al at present2O3The particle dispersion strengthening copper-based composite material mainly adopts a conventional powder metallurgy method, a mechanical alloying method, a sol-gel method and an internal oxidation method. The conventional powder metallurgy method has mature process, but the nanoscale Al is difficult to prepare by the conventional method2O3Powder, not realizing Al simultaneously2O3The particles are refined and distributed uniformly. Coarse Al2O3The particles can restrict Al2O3Cu complexThe performance of the composite material is improved. The grain size obtained by the mechanical alloying method is large, the production control is difficult, the sol-gel method process is easy to control, the performance of the prepared material is good, the material is still in the test stage at present, the internal oxidation method process is complex, the technical parameter difficulty is high, and the manufacturing cost is high.
The spray thermal decomposition prepares various metal salts into precursor solution according to the stoichiometric ratio required for preparing composite powder, the precursor solution is atomized by an atomizer and then is carried into a high-temperature reaction furnace by carrier gas, a series of physical and chemical processes of solvent evaporation, solute precipitation to form solid particles, particle drying, particle thermal decomposition, sintering and forming and the like are instantly completed in the reaction furnace, and finally ultrafine powder is formed. The raw materials are mixed in a solution state, so that the components can be uniformly distributed, the process is simple, the loss of the components is less, the stoichiometric ratio can be accurately controlled, and the method is particularly suitable for preparing multi-component composite powder. The micro powder is obtained by drying liquid drops suspended in the air, the particles are generally in a regular spherical shape, the particles are less agglomerated, subsequent washing and grinding are not needed, and the high purity and high activity of the product are ensured. The whole process is completed rapidly in short seconds, so that the liquid drop has no time for component segregation in the reaction process, and the uniformity of component distribution is further ensured.
Therefore, the invention adopts a method of combining spray pyrolysis and reduction calcination to prepare the aluminum oxide/copper composite reinforced phase.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing a nano alumina/copper composite reinforcing phase by spray pyrolysis.
A preparation method of a nano aluminum oxide/copper composite reinforced phase comprises the following specific steps:
(1) preparation of mixed solution of copper salt and aluminum salt: adding weighed copper salt and aluminum salt into a container filled with deionized water, and stirring to prepare a mixed solution of the copper salt and the aluminum salt at room temperature, wherein the molar concentration of the copper salt in the mixed solution is 0.001 mol/L-saturated concentration, and the molar concentration of the aluminum salt is 0.001 mol/L-saturated concentration;
(2) spray pyrolysis of copper salt/aluminum salt mixed solution: heating the tubular furnace to a certain temperature, pouring the mixed salt solution obtained in the step (1) into an atomizer, introducing small droplets generated by atomization into the tubular furnace for spray pyrolysis reaction, and collecting to obtain aluminum oxide/cuprous oxide composite powder;
(3) reduction and calcination of alumina/cuprous oxide: and (3) filling the composite powder obtained in the step (2) into a boat, then putting into a tube furnace, and reducing and calcining in a weak reducing atmosphere to obtain the aluminum oxide/copper composite reinforced phase.
In the step (1), the copper salt is one or more of copper acetate, copper nitrate, copper sulfate and copper chloride which are mixed according to any ratio, and the aluminum salt is one or more of aluminum nitrate, aluminum sulfate and aluminum chloride which are mixed according to any ratio.
Preferably, the stirring time in the step (1) of the invention is 30-120 min, and the concentrations of the copper salt and the aluminum salt are 0.01-1.0 mol/L respectively.
The copper salt/aluminum salt mixed solution spray pyrolysis reaction in the step (2) of the invention comprises the following specific processes: pouring the copper salt/aluminum salt mixed solution into an atomizer, wherein the power of the atomizer is 25-100W/L, when the temperature of the tube furnace is raised to 600-750 ℃, starting the atomization mode of the atomizer, the copper salt/aluminum salt mixed solution is subjected to evaporation and drying together in a low-temperature region, and then the copper salt/aluminum salt solution is subjected to thermal decomposition in a high-temperature region to generate nano cuprous oxide and aluminum oxide, (wherein the high-temperature region is a heating region, and the low-temperature region is a heat conduction region).
The weak reducing atmosphere in the step (3) of the invention is as follows: the mixed gas of the inert atmosphere and hydrogen or nitric oxide is subjected to reduction calcination at 950-1250 ℃ for 0.5-4.0 h.
The invention has the beneficial effects that:
(1) the aluminum oxide/copper composite reinforced phase prepared by the method has a nanoscale size, and the copper and the aluminum oxide are uniformly dispersed, wherein the molar ratio of the aluminum oxide to the copper can be regulated and controlled by adjusting the concentration of the solution.
(2) The aluminum oxide/copper composite reinforced phase prepared by the method fully utilizes the characteristic of spray pyrolysis, the copper salt/aluminum salt mixed solution is evaporated and dried in a low-temperature area, then the copper salt/aluminum salt mixed solution is thermally decomposed in a high-temperature area to generate nano aluminum oxide/cuprous oxide, the interface of the nano aluminum oxide/cuprous oxide and the interface of the nano aluminum oxide/cuprous oxide are tightly combined, and the aluminum oxide/cuprous oxide is reduced under the hydrogen condition to obtain the nano aluminum oxide/copper composite reinforced phase, thereby being beneficial to dispersion strengthening of a copper-based composite material and obtaining a better reinforcing effect.
(3) The method for preparing the aluminum oxide/copper composite reinforced phase has simple process, the composite reinforced phase is obtained by two steps of spray pyrolysis and reduction calcination, and the production efficiency is high.
Drawings
FIG. 1 is an XRD pattern of alumina/copper of example 1.
FIG. 2 is an SEM image of an alumina/copper composite reinforcing phase of example 1.
FIG. 3 is an EDX spot scan of the alumina/copper composite reinforcement phase of example 1.
FIG. 4 is an energy spectrum 1 of the alumina/copper composite enhanced phase of example 1.
FIG. 5 is an energy spectrum 2 of the alumina/copper composite enhanced phase of example 1.
FIG. 6 is an energy spectrum 3 of the alumina/copper composite enhanced phase of example 1.
FIG. 7 is an energy spectrum 4 of the alumina/copper composite enhanced phase of example 1.
FIG. 8 is an energy spectrum 5 of the alumina/copper composite enhanced phase of example 1.
FIG. 9 is an energy spectrum 6 of the alumina/copper composite enhanced phase of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1
A preparation method of an aluminum oxide/copper composite reinforced phase comprises the following specific steps:
(1) preparing a mixed solution of copper acetate and aluminum nitrate: weighing 6.0 g of copper acetate, adding the copper acetate into a beaker filled with 3L of deionized water, then weighing 11.3g of aluminum nitrate, adding the aluminum nitrate into the beaker filled with 3L of deionized water of copper salt, and fully dissolving the aluminum nitrate by magnetic stirring for 30 min at room temperature to prepare a mixed solution of copper salt and aluminum salt; the concentration of the obtained copper salt and aluminum salt is 0.01 mol/L;
(2) spray pyrolysis of the mixed solution: pouring the mixed solution prepared in the step (1) into an atomizer, starting the atomizer in an atomization mode (the atomizer is positioned at one end of the tube furnace) when the tube furnace is heated and the temperature rises to 600 ℃, setting the power to be 75W, evaporating and drying liquid drops generated by the mixed solution of copper salt and aluminum salt through ultrasonic atomization in a low-temperature region, and then carrying out thermal decomposition on the mixed solution in a high-temperature region to obtain the aluminum oxide/cuprous oxide composite powder.
(3) Reducing the alumina/cuprous oxide composite powder; firstly, the composite powder obtained in the step (2) is loaded into a corundum boat, then the corundum boat loaded with the composite powder is placed into a corundum tube furnace, the tube furnace is vacuumized, when the vacuum degree in the tube furnace reaches 0.01 Pa, a vacuum pump is closed, high-purity argon containing 5.0 wt% of hydrogen is introduced, the temperature is raised to 950 ℃ by the heating tube furnace, and reduction is carried out for 4.0h, so that the aluminum oxide/copper composite enhanced phase is obtained.
The microstructure of the composite powder prepared in this example is shown in fig. 1-9, and SEM images show that the size of the powder is in the order of nanometers, the morphology of the powder is spherical, XRD results show that the composite powder mainly contains alumina and copper, no other impurities are present, and EDX shows that alumina is dispersed in a copper matrix very uniformly.
Example 2
A preparation method of an aluminum oxide/copper composite reinforced phase comprises the following specific steps:
(1) preparation of mixed solution of copper nitrate and aluminum nitrate: under the condition of stirring, firstly weighing 56 g of copper nitrate into a 3L deionized water beaker, then weighing 113 g of aluminum nitrate into the 3L deionized water beaker added with the copper salt, and stirring for 40 min by adopting magnetic force at room temperature to fully dissolve the aluminum nitrate to prepare a mixed solution of the copper salt and the aluminum salt. The concentrations of the obtained copper salt and aluminum salt solutions were both 0.1 mol/L.
(2) Spray pyrolysis of the mixed solution: pouring the mixed solution prepared in the step (1) into an atomizer, starting the atomization mode of the atomizer when the temperature of the tubular furnace is raised to 650 ℃, setting the power to be 150W, evaporating and drying liquid drops generated by ultrasonic atomization of the mixed solution of copper salt and aluminum salt in a low-temperature region, and then carrying out thermal decomposition on the mixed solution in a high-temperature region to obtain the aluminum oxide/cuprous oxide composite powder.
(3) Reducing the alumina/cuprous oxide composite powder; firstly, the composite powder obtained in the step (2) is loaded into a corundum boat, then the corundum boat loaded with the composite powder is placed into a corundum tube furnace, the tube furnace is vacuumized, when the vacuum degree in the tube furnace reaches 0.01 Pa, a vacuum pump is closed, high-purity nitrogen containing 5.0 wt% of hydrogen is introduced, the temperature is raised to 1050 ℃ by the heating tube furnace, and reduction is carried out for 1.0 h, so that the aluminum oxide/copper composite enhanced phase is obtained.
SEM analysis shows that the size of the powder is in nanometer order of magnitude, the morphology of the powder presents spherical characteristics, and EDX analysis shows that the aluminum oxide is dispersed in the copper matrix very uniformly.
Example 3
A preparation method of an aluminum oxide/copper composite reinforced phase comprises the following specific steps:
(1) preparation of a mixed solution of copper chloride and aluminum chloride: under the condition of stirring, firstly weighing copper chloride and then adding the copper chloride into a 3L deionized water beaker, then weighing aluminum chloride and adding the aluminum chloride into the 3L deionized water beaker added with the copper salt, and stirring the mixture at room temperature for 40 min by adopting magnetic force to fully dissolve the copper salt and the aluminum salt to prepare a mixed solution of the copper salt and the aluminum salt. The concentration of the obtained copper salt and aluminum salt solutions was 1.0 mol/L.
(2) Spray pyrolysis of the mixed solution: pouring the mixed solution prepared in the step (1) into an atomizer, starting the atomization mode of the atomizer when the temperature of the tubular furnace is raised to 650 ℃, setting the power to be 300W, evaporating and drying liquid drops generated by ultrasonic atomization of the mixed solution of copper salt and aluminum salt in a low-temperature region, and then carrying out thermal decomposition on the mixed solution in a high-temperature region to obtain the aluminum oxide/cuprous oxide composite powder.
(3) Reducing the alumina/cuprous oxide composite powder; firstly, the composite powder obtained in the step (2) is loaded into a corundum boat, then the corundum boat loaded with the composite powder is placed into a corundum tube furnace, the tube furnace is vacuumized, when the vacuum degree in the tube furnace reaches 0.01 Pa, a vacuum pump is closed, nitrogen containing 5.0 wt% of carbon monoxide is introduced, the temperature of the tube furnace is raised to 1250 ℃ and reduced for 0.5h, and the aluminum oxide/copper composite enhanced phase is obtained.
SEM analysis shows that the size of the powder is in nanometer order of magnitude, the morphology of the powder presents spherical characteristics, and EDX analysis shows that the aluminum oxide is dispersed in the copper matrix very uniformly.
Example 4
A preparation method of an aluminum oxide/copper composite reinforced phase comprises the following specific steps:
(1) preparation of a mixed solution of copper sulfate and aluminum sulfate: under the condition of stirring, firstly weighing copper sulfate and adding into a 3L deionized water beaker, then weighing 113 g of aluminum sulfate and adding into the 3L deionized water beaker added with the copper salt, and stirring for 60 min at room temperature by adopting magnetic force to fully dissolve the copper salt and the aluminum salt to prepare a mixed solution of the copper salt and the aluminum salt, wherein the concentration of the obtained copper salt and aluminum salt solution is 0.5 mol/L.
(2) Spray pyrolysis of the mixed solution: pouring the mixed solution prepared in the step (1) into an atomizer, starting the atomization mode of the atomizer when the temperature of the tubular furnace is raised to 650 ℃, setting the power to be 150W, evaporating and drying liquid drops generated by ultrasonic atomization of the mixed solution of copper salt and aluminum salt in a low-temperature region, and then carrying out thermal decomposition on the mixed solution in a high-temperature region to obtain the aluminum oxide/cuprous oxide composite powder.
(3) Reducing the alumina/cuprous oxide composite powder; firstly, the composite powder obtained in the step (2) is loaded into a corundum boat, then the corundum boat loaded with the composite powder is placed into a corundum tube furnace, the tube furnace is vacuumized, when the vacuum degree in the tube furnace reaches 0.01 Pa, a vacuum pump is closed, high-purity nitrogen containing 5.0 wt% of hydrogen is introduced, the temperature is raised to 1100 ℃ by the heating tube furnace, and reduction is carried out for 3.0 h, so that the aluminum oxide/copper composite enhanced phase is obtained.
SEM analysis shows that the size of the powder is in nanometer order of magnitude, the morphology of the powder presents spherical characteristics, and EDX analysis shows that the aluminum oxide is dispersed in the copper matrix very uniformly.
Example 5
A preparation method of an aluminum oxide/copper composite reinforced phase comprises the following specific steps:
(1) preparation of a mixed solution of copper sulfate and aluminum nitrate: under the condition of stirring, adding weighed copper nitrate into a deionized water beaker with 10L, weighing aluminum nitrate, adding into the deionized water beaker with 10L added with the copper salt, and stirring for 30 min by adopting magnetic force at room temperature to fully dissolve the copper nitrate and the aluminum salt to prepare a mixed solution of the copper salt and the aluminum salt; the concentration of the obtained copper salt and aluminum salt solution was 0.1 mol/L.
(2) Spray pyrolysis of the mixed solution: pouring the mixed solution prepared in the step (1) into an atomizer, starting the atomization mode of the atomizer when the temperature of the tubular furnace is raised to 650 ℃, setting the power to be 500W, evaporating and drying liquid drops generated by ultrasonic atomization of the mixed solution of copper salt and aluminum salt in a low-temperature region, and then carrying out thermal decomposition on the mixed solution in a high-temperature region to obtain the aluminum oxide/cuprous oxide composite powder.
(3) Reducing the alumina/cuprous oxide composite powder; firstly, the composite powder obtained in the step (2) is loaded into a corundum boat, then the corundum boat loaded with the composite powder is placed into a corundum tube furnace, the tube furnace is vacuumized, when the vacuum degree in the tube furnace reaches 0.01 Pa, a vacuum pump is closed, pure hydrogen is introduced, and the temperature is raised to 1050 ℃ by the heating tube furnace and reduced for 1.0 h to obtain the aluminum oxide/copper composite enhanced phase.
SEM analysis shows that the size of the powder is in nanometer order of magnitude, the morphology of the powder presents spherical characteristics, and EDX analysis shows that the aluminum oxide is dispersed in the copper matrix very uniformly.

Claims (4)

1.一种纳米氧化铝/铜复合增强相的制备方法,其特征在于,具体步骤如下:1. a preparation method of nano-alumina/copper composite reinforcing phase, is characterized in that, concrete steps are as follows: (1)铜盐和铝盐混合溶液的配置:将称量的铜盐和铝盐加入装有去离子水的容器中,室温条件下,通过搅拌配制成铜盐和铝盐的混合溶液,混合溶液中铜盐的摩尔浓度为0.001mol/L~饱和浓度,铝盐的摩尔浓度为0.001mol/L~饱和浓度;(1) Configuration of the mixed solution of copper salt and aluminum salt: Add the weighed copper salt and aluminum salt into a container with deionized water, and at room temperature, prepare a mixed solution of copper salt and aluminum salt by stirring, and mix. The molar concentration of copper salt in the solution is 0.001mol/L~saturated concentration, and the molar concentration of aluminum salt is 0.001mol/L~saturated concentration; (2)铜盐/铝盐混合溶液喷雾热解:将管式炉加热升温到一定的温度,将步骤(1)所得混合盐溶液倒入到雾化器中,将雾化产生的小液滴通入到管式炉中进行喷雾热分解反应,然后收集得到氧化铝/氧化亚铜复合粉末;(2) Spray pyrolysis of copper salt/aluminum salt mixed solution: heat the tube furnace to a certain temperature, pour the mixed salt solution obtained in step (1) into the atomizer, and spray the small droplets generated by atomization Passing into the tube furnace for spray thermal decomposition reaction, and then collecting the alumina/cuprous oxide composite powder; (3)氧化铝/氧化亚铜还原煅烧:将步骤(2)所得复合粉末装入舟皿中,然后放入管式炉中,在弱还原性气氛中还原煅烧获得氧化铝/铜复合增强相;(3) Reduction and calcination of alumina/cuprous oxide: put the composite powder obtained in step (2) into a boat, and then put it into a tube furnace, and reduce and calcine in a weak reducing atmosphere to obtain an alumina/copper composite reinforcement phase. ; 步骤(2)铜盐/铝盐混合溶液喷雾热解反应具体过程为:将铜盐/铝盐混合溶液倒入雾化器中,其中雾化器的功率为25~100 W/L,当管式炉温度升至600~750℃时,将雾化器开启雾化模式,铜盐/铝盐混合溶液在低温区共同经历了蒸发、干燥,随后铜盐/铝盐溶液在高温区经历热分解,生成纳米氧化亚铜和氧化铝。Step (2) The specific process of the spray pyrolysis reaction of the copper salt/aluminum salt mixed solution is as follows: pour the copper salt/aluminum salt mixed solution into the atomizer, wherein the power of the atomizer is 25~100 W/L, when the tube When the temperature of the furnace rises to 600~750℃, the atomizer is turned on to the atomization mode. The copper salt/aluminum salt mixed solution undergoes evaporation and drying together in the low temperature area, and then the copper salt/aluminum salt solution undergoes thermal decomposition in the high temperature area. , generating nano-cuprous oxide and aluminum oxide. 2.根据权利要求1所述纳米氧化铝/铜复合增强相的制备方法,其特征在于:步骤(1)中铜盐为醋酸铜、硝酸铜、硫酸铜、氯化铜中的一种或几种按任意比混合,铝盐为硝酸铝、硫酸铝,氯化铝中的一种或几种按任意比混合。2. The preparation method of the nano-alumina/copper composite reinforcing phase according to claim 1, characterized in that: in step (1), the copper salt is one or more of copper acetate, copper nitrate, copper sulfate, and copper chloride. One or more of aluminum nitrate, aluminum sulfate, and aluminum chloride are mixed according to any ratio. 3.根据权利要求1所述纳米氧化铝/铜复合增强相的制备方法,其特征在于:步骤(1)搅拌时间为30~120 min,铜盐和铝盐的浓度分别为0.01~1.0 mol/L。3. The preparation method of nano-alumina/copper composite reinforcing phase according to claim 1, characterized in that: the stirring time of step (1) is 30-120 min, and the concentrations of copper salt and aluminum salt are respectively 0.01-1.0 mol/ L. 4.根据权利要求1所述纳米氧化铝/铜复合增强相的制备方法,其特征在于:步骤(3)中弱还原气氛为:惰性气氛与氢气或者一氧化氮的混合气体,还原煅烧温度为950~1250℃,时间为0.5~4.0 h。4. The preparation method of the nano-alumina/copper composite reinforcing phase according to claim 1, wherein the weak reducing atmosphere in step (3) is: a mixed gas of an inert atmosphere and hydrogen or nitric oxide, and the reduction calcination temperature is 950~1250℃, the time is 0.5~4.0 h.
CN201810020952.8A 2018-01-10 2018-01-10 Preparation method of nano aluminum oxide/copper composite reinforced phase Active CN108202145B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810020952.8A CN108202145B (en) 2018-01-10 2018-01-10 Preparation method of nano aluminum oxide/copper composite reinforced phase

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810020952.8A CN108202145B (en) 2018-01-10 2018-01-10 Preparation method of nano aluminum oxide/copper composite reinforced phase

Publications (2)

Publication Number Publication Date
CN108202145A CN108202145A (en) 2018-06-26
CN108202145B true CN108202145B (en) 2021-12-17

Family

ID=62606125

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810020952.8A Active CN108202145B (en) 2018-01-10 2018-01-10 Preparation method of nano aluminum oxide/copper composite reinforced phase

Country Status (1)

Country Link
CN (1) CN108202145B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110184488B (en) * 2019-06-24 2020-09-18 北京科技大学 Method for preparing metal dispersion strengthened copper in short process
CN114425055B (en) * 2020-10-15 2024-04-19 武汉工程大学 Silica supported multi-metal nano-particle, preparation method and antibacterial application thereof
CN113061768B (en) * 2021-03-22 2023-08-25 中南大学 Preparation method of dispersion strengthening copper-based composite material
CN113427013B (en) * 2021-06-07 2022-11-08 中国恩菲工程技术有限公司 Preparation method of copper-based aluminum oxide nano material
CN117138784B (en) * 2023-10-30 2024-02-06 潍坊学院 High-loading and highly-dispersed Cu-based catalysts and their synthesis methods and applications

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1760043A1 (en) * 2005-09-06 2007-03-07 ETH Zürich, ETH Transfer Reducing flame spray pyrolysis method for the production of metal, non-oxidic, ceramic and reduced metal oxide powders and nano-powders
CN101168197A (en) * 2006-10-25 2008-04-30 中南大学 A kind of preparation method of superfine/nanometer tungsten-copper-nickel composite powder
CN101875134A (en) * 2009-12-23 2010-11-03 云泰硬质合金(赣州)有限公司 Method for preparing nano tungsten-copper-rare earth composite powder
CN103394702A (en) * 2013-07-17 2013-11-20 河北工程大学 Method for uniformly and efficiently manufacturing pre-alloyed powder for nano-structured oxide-dispersion-strengthened iron-based alloy
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
CN105598470A (en) * 2016-02-25 2016-05-25 昆明理工大学 Preparation method of carbon reinforced metal/metal oxide composite powder
CN106670505A (en) * 2017-01-13 2017-05-17 昆明理工大学 Method for preparing tungsten-cobalt-carbon composite powder through spray pyrolysis method
CN107362799A (en) * 2017-06-21 2017-11-21 昆明理工大学 A kind of preparation method of titanium dioxide/cuprous oxide composite photo-catalyst

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1760043A1 (en) * 2005-09-06 2007-03-07 ETH Zürich, ETH Transfer Reducing flame spray pyrolysis method for the production of metal, non-oxidic, ceramic and reduced metal oxide powders and nano-powders
CN101168197A (en) * 2006-10-25 2008-04-30 中南大学 A kind of preparation method of superfine/nanometer tungsten-copper-nickel composite powder
CN101875134A (en) * 2009-12-23 2010-11-03 云泰硬质合金(赣州)有限公司 Method for preparing nano tungsten-copper-rare earth composite powder
CN103394702A (en) * 2013-07-17 2013-11-20 河北工程大学 Method for uniformly and efficiently manufacturing pre-alloyed powder for nano-structured oxide-dispersion-strengthened iron-based alloy
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
CN105598470A (en) * 2016-02-25 2016-05-25 昆明理工大学 Preparation method of carbon reinforced metal/metal oxide composite powder
CN106670505A (en) * 2017-01-13 2017-05-17 昆明理工大学 Method for preparing tungsten-cobalt-carbon composite powder through spray pyrolysis method
CN107362799A (en) * 2017-06-21 2017-11-21 昆明理工大学 A kind of preparation method of titanium dioxide/cuprous oxide composite photo-catalyst

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Cu-Al2O3纳米复合粉末的合成;郭均高等;《国外金属热处理》;20120415;第23卷(第2期);第8-9页 *

Also Published As

Publication number Publication date
CN108202145A (en) 2018-06-26

Similar Documents

Publication Publication Date Title
CN108202145B (en) Preparation method of nano aluminum oxide/copper composite reinforced phase
CN103801705B (en) A kind of method that porous charcoal supported nano-gold belongs to oxide or nano metal material
Portehault et al. A general solution route toward metal boride nanocrystals
CN103007963B (en) Method for preparing bimetallic nanometer alloy composite material by taking graphene as carrier
CN106077695B (en) A kind of preparation method of high-copper tungsten copper nano composite powder
WO2018064960A1 (en) Method for preparing loading-type nano-metal material using microwave-assisted carbon template method
CN110265225B (en) Method for preparing nitrogen-doped three-dimensional porous carbon microsphere-supported molybdenum carbide/molybdenum nitride and iron nanoparticle composites
CN1257785C (en) Method for preparing nano-grade tungsten-based composite powder by sol-spray drying-thermal reduction
Gao et al. Novel tunable hierarchical Ni–Co hydroxide and oxide assembled from two-wheeledunits
CN103785859A (en) Method for manufacturing nanometer mesoporous material
CN108213456B (en) A kind of preparation method of cubic nanometer copper powder
CN101168197A (en) A kind of preparation method of superfine/nanometer tungsten-copper-nickel composite powder
Liu et al. Spray-drying assisted layer-structured H2TiO3 ion sieve synthesis and lithium adsorption performance
CN105329932B (en) A method for large-scale preparation of carbon-doped mixed transition metal oxide porous microspheres
CN101785982A (en) Method for preparing hollow nanospheres by a hot emulsion method
CN110976901A (en) A kind of preparation method of nano copper powder
CN105598470A (en) Preparation method of carbon reinforced metal/metal oxide composite powder
CN109422294B (en) Preparation method of size-controllable cobaltosic oxide nanoparticles
Zou et al. Controllable self-catalytic fabrication of carbon nanomaterials mediated by a nickel metal organic framework
CN106334801A (en) Method for preparing porous carbon loaded nano-metal through microwave assistance
CN103055869B (en) Porous metal nanometer granular catalyst and preparation method thereof
CN112250043A (en) Preparation method of monodisperse nano-particle material
CN103624269B (en) A kind of nano-tungsten powder and employing collosol and gel hydrogen reduction method thereof prepare the method for nano-tungsten powder
CN111620374B (en) A kind of preparation method of rod-shaped purple tungsten with large aspect ratio
CN105800587A (en) Method for preparing porous carbon-loaded nano-material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant