CN112705715A - Method for preparing Mo-Cu mixed powder by spray drying granulation - Google Patents
Method for preparing Mo-Cu mixed powder by spray drying granulation Download PDFInfo
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- CN112705715A CN112705715A CN202011317396.4A CN202011317396A CN112705715A CN 112705715 A CN112705715 A CN 112705715A CN 202011317396 A CN202011317396 A CN 202011317396A CN 112705715 A CN112705715 A CN 112705715A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/026—Spray drying of solutions or suspensions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
Abstract
The invention discloses a method for obtaining Mo-Cu mixed powder by spray drying granulation, which comprises the following steps: 1) weighing and mixing Mo powder and Cu powder; 2) spray drying and granulating; 3) and (3) annealing and reducing the Mo-Cu mixed powder obtained by spray drying and granulation. The Mo-Cu mixed powder obtained by the spray drying granulator has the advantages of high balling rate, high sphericity, good powder fluidity, uniform distribution of Mo and Cu in particles, low oxygen content, less impurities and the like, and can be used for preparing the alloy and effectively improve the uniformity, comprehensive mechanical property and electric conductivity of the internal structure of the alloy. The preparation method is simple, the process is easy to control, and the preparation method can be used for a small amount of preparation for experiments and can also be used for mass production to form an industrial chain.
Description
Technical Field
The invention belongs to the field of powder materials, and particularly relates to a preparation method of Mo-Cu mixed powder.
Background
The Mo-Cu alloy integrates the advantages of Cu and Mo, and has the advantages of high strength, excellent high temperature resistance, high arc ablation resistance, good electric and heat conductivity, corrosion resistance, fine structure, small thermal expansion and the like. Nowadays, Mo-Cu alloy is widely applied to the fields of manufacturing military or civil high-power microelectronic devices and energy sources, environmental protection, marine petrochemical industry and aerospace aviation.
With the good operation of development situation of the macroscopic economic environment and the industrial and scientific research fields in China, the demand of Mo-Cu alloy on the market is more and more increased. At present, the Mo-Cu alloy is mainly applied by three methods 1) that a large-volume Mo-Cu alloy is directly purchased, and a finished Mo-Cu alloy is mechanically processed to obtain a required part or shape, and the method has the defects of complex processing steps, low utilization rate, high cost and the like. 2) The Mo-Cu alloy powder is adopted for preparing parts or processing the surfaces of the required parts, the utilization rate of the means is high, and the cost can be effectively saved, but the current method for preparing the Mo-Cu alloy powder generally has the defects of poor material uniformity, more closed gaps, density generally lower than 98 percent or complex process, low production efficiency, difficulty in batch production, high production cost and the like. 3) The Mo-Cu mixed powder is adopted for preparing parts or processing the surfaces of the required parts, the method has wide powder source, low cost and easy operation, but Mo and Cu are easy to agglomerate and delaminate during processing due to large mass difference, low intersolubility and the like of Mo and Cu, so that the processed finished products cannot meet the requirements on strength, conductivity and performance uniformity.
Disclosure of Invention
Based on the problems in the prior art, the invention provides a preparation method of Mo-Cu mixed powder with excellent performance, so as to solve the technical problem that the Mo and Cu are easy to agglomerate and delaminate due to large mass difference, low intersolubility and the like of Mo and Cu, and the properties of a finished product prepared from the Mo and Cu mixed powder cannot meet the application requirements in strength, conductivity and the like.
In order to achieve the above purpose, the invention adopts the following technical scheme.
The invention provides a method for preparing Mo-Cu mixed powder by a spray drying granulation method. The method specifically comprises the following steps:
(1) mixing Mo powder and Cu powder: adding Mo powder and Cu powder into NAFION solution with the concentration of 5%, and stirring at a high speed to mix and fluidize the Mo powder and the Cu powder to obtain uniform Mo-Cu mixed powder slurry; wherein the high-speed stirring speed is 200-1000 r/min; preferably, the Mo powder and the Cu powder are both ultrafine powders, the average powder diameter is about 100nm, the mobility of the Mo powder and the Cu powder is ensured, and the uniformity of the Mo and the Cu in the mixed slurry is improved.
More specifically, the ratio of the total mass of the Mo powder and the Cu powder to the NAFION solution is 500 g/200 mL to 500 g/400 mL, and the most preferable ratio is 500g of the total mass of the Mo powder and the Cu powder: 200mL of NAFION solution can effectively ensure the balling rate and the balling degree and avoid the blockage of a spray head, a feeding pipe or a hose of a peristaltic pump of a spray drying granulator due to the problems of excessive viscosity, high density and the like of metal slurry at the concentration. And further, the mass ratio of the Mo powder to the Cu powder is 7: 3-2: 8.
(2) Spray drying and granulating: and (3) carrying out spray drying granulation on the Mo-Cu mixed powder slurry obtained in the step (1) to obtain a Mo-Cu mixed powder primary product. And in the spray drying and granulating process, the air inlet temperature of the spray drying and granulating machine is 200-300 ℃, the air volume of a fan is 50-100L/min, the pressure of a drying chamber is 0.16-0.3 Mpa, the temperature of the drying chamber is kept for 15-30 min after reaching the air inlet temperature, the drying chamber and a material receiving tank of the spray drying and granulating machine are fully dried, then feeding is started, the Mo-Cu mixed powder slurry is fed into the spray drying and granulating machine through a peristaltic pump, the rotating speed of the peristaltic pump is 20-50 r/min, and the Mo-Cu mixed powder slurry is kept to be continuously stirred at a high speed in the feeding process.
(3) Reduction annealing: reducing and annealing the Mo-Cu mixed powder primary product obtained in the step (2) in a hydrogen atmosphere, and removing an Mo-Cu mixed powder oxide layer and residual moisture formed in spray drying granulation; wherein the reduction annealing temperature is 200-250 ℃, the temperature rise time is 2 hours, and the heat preservation time is 4-8 hours.
The invention has the beneficial effects that:
(1) the Mo-Cu mixed powder obtained by the spray drying granulator has the advantages of high balling rate, high sphericity, good powder fluidity, uniform distribution of Mo and Cu in the granules, low oxygen content, less impurities and the like.
(2) The Mo-Cu mixed powder obtained by the method has high practicability and wide application range, and can be widely applied to the fields of electronics, electricity, energy, environmental protection, marine petrochemical industry and aerospace aviation.
(3) The Mo-Cu mixed powder obtained by the invention can be used for manufacturing large-volume Mo-Cu alloy, and can effectively improve the uniformity, comprehensive mechanical property, electric conductivity, heat resistance and the like of the internal structure of the alloy. The method can also be used for processing the surface of a part, can effectively avoid layering and agglomeration caused by the quality difference of Mo and Cu, poor intersolubility and the like, and improves the uniformity of the structure, the comprehensive mechanical property, the conductivity, the heat resistance and the like.
(4) According to the invention, through the improvement of the process and the equipment, the occurrence rate of the blocking condition in the experimental process is greatly reduced, and the efficiency of preparing the Mo-Cu mixed powder is improved. The improvements of the present invention are equally applicable to other materials which tend to cause blockages in spray-dried granulation.
(5) The method for obtaining the Mo-Cu mixed powder by the spray drying granulator has the advantages of simple and feasible production process, high yield, stable performance of finished products, low cost, less waste, energy conservation and environmental protection, and can be used for preparing a small amount of Mo-Cu mixed powder for experiment and producing the Mo-Cu mixed powder in a large batch to form an industrial chain.
Drawings
FIG. 1 is a metallographic photograph of a Mo-Cu mixed powder obtained in example.
FIG. 2 is an electron micrograph of the Mo-Cu mixed powder obtained in example.
FIG. 3 shows the results of the laser particle size distribution test of the Mo-Cu mixed powder prepared in the examples.
FIG. 4 is a schematic diagram showing the position of a beaker-peristaltic pump-spray drying granulator containing slurry when the Mo-Cu mixed powder is subjected to spray drying granulation in the example.
FIG. 5 shows the SEM test results of the Mo-Cu mixed powder prepared in the examples. Wherein (a) the selected region is tested by energy spectrum, (b) is a distribution diagram of copper element, and (c) is a distribution diagram of molybdenum element.
Wherein 1 is a spray drying granulator, 11 is a feed inlet of the spray drying granulator, 12 is an air inlet of the spray drying granulator, 2 is a slurry beaker, 3 is a peristaltic pump, and 4 is a feed pipeline.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the accompanying drawings, and it should be noted that the detailed description is only for describing the present invention, and should not be construed as limiting the present invention.
The equipment used in the following examples of the invention included a beaker, analytical balance, magnetic stirrer, high speed stirrer, peristaltic pump, spray drying granulator.
The materials used in the following examples of the present invention include Mo powder, Cu powder, NAFION solution with a concentration of 5%.
In some preferred schemes, the beaker is a transparent plastic beaker, so that the state of the slurry can be observed while the beaker is prevented from being damaged by a high-speed stirrer.
In some preferred schemes, the stirring rod of the high-speed stirrer is made of Teflon material, which is convenient for cleaning and preventing reaction.
In some preferred embodiments, the ratio of the Mo-Cu mixed powder to the NAFION solution is between 500g:200mL to 500g:400mL, such as 500gMo-Cu mixed powder: 200mL of NAFION solution; 500g Mo-Cu mixed powder 250m NAFION solution; 500gMo-Cu mixed powder 300mL of an AFION solution; 500gMo-Cu mixed powder 350ml of an AFION solution; 500gMo-Cu mixed powder, 400mLNAFION solution and the like, and most preferably 500gMo-Cu mixed powder, 200mLNAFION solution, can be used for effectively ensuring the balling rate and the balling degree and avoiding the blockage of a spray head, a feeding pipe or a peristaltic pump hose of a spray drying granulator due to the problems of excessive viscosity, high density and the like of metal slurry.
In some preferred embodiments, a spray dryer granulator having a drying chamber diameter of 800mm or more is used, most preferably a drying chamber diameter of 800 mm.
In the spray drying granulation process, metal powder slurry is conveyed from a beaker to a feed inlet of a spray drying granulator through a peristaltic pump, hot air enters an air inlet of the spray drying granulator, and the slurry is subjected to spray drying granulation in a drying chamber of the spray drying granulator, as shown in figure 4. In some preferred schemes, the position of a beaker for containing slurry, a peristaltic pump and a spray drying granulator is adjusted as shown in figure 4, in height, the position of the beaker for containing slurry is higher than the position of the peristaltic pump, the position of the peristaltic pump is higher than the position of a feed inlet of the spray drying granulator, and the length of each feed pipeline for conveying the slurry among the beaker for containing slurry, the peristaltic pump and the spray drying granulator is shortened as much as possible, so that the blockage of spray heads, feed pipelines or peristaltic pump hoses of the spray drying granulator and the like caused by deposition and agglomeration of metal powder in the pipelines due to the fact that the metal slurry is too heavy can be effectively avoided.
In some preferred schemes, the peristaltic pump roller adopts a six-wheel roller, and the six-wheel roller can effectively improve the stability and uniformity of feeding of the peristaltic pump compared with a three-wheel roller or a four-wheel roller.
The following is a specific example of a method for preparing a Mo-Cu mixed powder by spray drying granulation using the apparatus and materials described above and performed as follows:
(1) weighing 1000g of Mo powder and Cu powder with the average diameter of about 100nm by using an analytical balance, wherein the specific ratio of Mo to Cu can be flexibly changed according to the specific requirements of the required Mo-Cu alloy powder, for example, the mass ratio of Mo to Cu is 7: and 3, weighing 700g of Mo powder and 300g of copper powder, putting the weighed Mo powder, Cu powder and 5% NAFION solution into a plastic beaker with the capacity of 1L, adjusting the rotating speed of a high-speed stirrer to be 200r/min, putting a stirring rod into the plastic beaker, adjusting the position, starting the high-speed stirrer, stirring the Mo-Cu mixed powder and the NAFION solution into uniform slurry for standby, and continuously stirring during standby.
(2) Checking each component of the spray drying granulator to ensure normal work, closing a furnace door of the spray drying granulator, and setting parameters of the spray drying granulator as follows: the method comprises the steps of starting a spray drying granulator at an air inlet temperature of 200 ℃, an air volume of a fan of 50, a pressure of an air compressor of 0.16Mpa and a rotating speed of a peristaltic pump of 20r/min, keeping the temperature of a drying chamber at 200 ℃ for 15 min-30 min, ensuring that the drying chamber and a material receiving tank are fully dried, then starting feeding, and keeping a high-speed stirrer to continuously stir slurry of Mo-Cu mixed powder and NAFION solution in the feeding process. And after the slurry spray drying granulation is finished, adding deionized water into the beaker for continuing spray drying granulation for a period of time, closing the equipment after the hose of the peristaltic pump, the feeding pipe and the spray head of the spray drying granulator are ensured to have no slurry residue, taking down the material collecting tank after the drying chamber is cooled, and collecting Mo-Cu mixed powder particles for later use.
(3) Putting the Mo-Cu mixed powder particles collected in the step (2) into a corundum crucible, putting the crucible filled with the Mo-Cu mixed powder particles into a tubular furnace, connecting each component of the tubular furnace, checking that each component of the tubular furnace can normally work, opening a hydrogen cylinder, and after the components are continuously used for a period of time, ensuring that the hydrogen concentration in the tubular furnace reaches a safety standard, and adjusting the experimental parameters of the tubular furnace to be: heating at 200 ℃, heating for 2h, keeping the temperature for 4h, cooling in the furnace, keeping the hydrogen atmosphere in the cooling process, closing a hydrogen cylinder after the experiment is finished and the tube furnace is completely cooled, taking out the crucible containing the Mo-Cu mixed powder particles, and collecting the powder particles to obtain the reduced Mo-Cu mixed powder particle finished product.
The process parameters listed in the embodiment are one of the preferred schemes of the present invention, and the process parameters can be adjusted within the range listed in the content of the present invention through trial and error by the inventors, so as to achieve the purpose of the present invention.
The Mo-Cu mixed powder obtained was subjected to a test. Referring to FIG. 1, a metallographic photograph, FIG. 2 an electron micrograph and FIG. 3 a laser particle size distribution test result of the Mo-Cu mixed powder obtained in this example, it can be seen that the particle size distribution of the Mo-Cu mixed powder is shown. As can be seen from FIGS. 1 to 3, the prepared Mo-Cu mixed powder has high balling rate and uniform particle size distribution; the powder flowability of the powder reaches the level of 10 g/s. FIG. 5 shows the SEM spectra of Mo-Cu mixed powder prepared in example, wherein (a) is selected region of energy spectrum test, (b) is Cu distribution diagram, and (c) is Mo distribution diagram. Further verified from the electron microscope composition analysis results: the Mo and the Cu in the particles are uniformly distributed, and impurities are few, so that the technical problem that the subsequent product has poor conductivity and the like due to the common easy agglomeration and layering of the Mo and the Cu in the mixed powder is solved.
Claims (7)
1. A method for preparing Mo-Cu mixed powder by spray drying granulation is characterized by comprising the following steps:
1) mixing Mo powder and Cu powder: mixing the NAFION solution with Mo powder and Cu powder; the proportion of the total mass of the Mo powder and the Cu powder to the NAFION solution is
200mL to 500 mL, and the mass ratio of the Mo powder to the Cu powder is 7: 3-2: 8; stirring at a high speed to mix and fluidize Mo powder and Cu powder to obtain Mo-Cu mixed powder slurry;
2) spray drying and granulating: conveying the Mo-Cu mixed powder slurry obtained in the step 1) from a slurry beaker to a feed inlet of a spray drying granulator through a peristaltic pump, simultaneously feeding hot air into an air inlet of the spray drying granulator, and finishing spray drying granulation of the slurry in a drying chamber of the spray drying granulator to obtain a Mo-Cu mixed powder primary product; wherein the temperature of the hot air entering is 200-300 ℃, the air volume of the fan is 50-100L/min, and the pressure of the drying chamber is 0.16-0.3 Mpa;
3) reduction annealing: reducing and annealing the Mo-Cu mixed powder primary product obtained in the step 2) in a hydrogen atmosphere; the annealing temperature is 200-250 ℃, the temperature rising time is 2 hours, and the heat preservation time is 4-8 hours.
2. The method for preparing Mo-Cu mixed powder by spray drying granulation according to claim 1, wherein: the concentration of the NAFION solution in the step 1) is 5 percent.
3. The method for preparing Mo-Cu mixed powder by spray drying granulation according to claim 1, wherein: the rotating speed of the high-speed stirring in the step 1) is 200-1000 r/min.
4. The method for preparing Mo-Cu mixed powder by spray drying granulation according to claim 1, wherein: the average powder diameter of the added Mo powder and Cu powder in the step 1) is 100 nm; the proportion of the total mass of the Mo powder and the Cu powder to the NAFION solution is 500g:200 mL.
5. The method for preparing Mo-Cu mixed powder by spray drying granulation according to claim 1, wherein: the placement positions of the slurry beaker, the peristaltic pump and the spray drying granulator in the step 2) are as follows: the position of the slurry beaker is higher than that of the peristaltic pump, and the position of the peristaltic pump is higher than that of the feed inlet of the spray drying granulator.
6. The method for preparing Mo-Cu mixed powder by spray drying granulation according to claim 1, wherein: and 2) keeping the temperature of the drying chamber in the step 2) for 15-30 min after the temperature of the drying chamber reaches the hot air temperature, and then sending the Mo-Cu mixed powder slurry into a drying chamber of a spray drying granulator.
7. The method for preparing Mo-Cu mixed powder by spray drying granulation according to claim 1, wherein: and 2) feeding the Mo-Cu mixed powder slurry into a peristaltic pump of a drying chamber of a spray drying granulator at a rotating speed of 20-50 r/min, and keeping stirring at a high speed in the feeding process.
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