CN113492211A - Preparation method of high-uniformity metal powder with controllable particle size - Google Patents
Preparation method of high-uniformity metal powder with controllable particle size Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 104
- 239000002245 particle Substances 0.000 title claims abstract description 88
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 41
- 239000002184 metal Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 53
- 238000009826 distribution Methods 0.000 claims description 50
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 50
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 17
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 description 9
- 230000002776 aggregation Effects 0.000 description 9
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- WUUZKBJEUBFVMV-UHFFFAOYSA-N copper molybdenum Chemical compound [Cu].[Mo] WUUZKBJEUBFVMV-UHFFFAOYSA-N 0.000 description 2
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- 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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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Abstract
The invention belongs to the field of powder metallurgy, and particularly relates to a preparation method of high-uniformity metal powder with controllable granularity. The method adopts the vertical fluidized bed type crushing and grading, each particle has the same motion state in the crushing and grading process, the product granularity is adjustable, and the metal powder with a plurality of granularity sections can be obtained at one time. The metal powder obtained by the method has good uniformity and high production efficiency, and compared with the prior art, the method has the advantages that the production efficiency is greatly improved, and the powder with a plurality of granularity sections can be obtained.
Description
Technical Field
The invention belongs to the field of powder metallurgy, and particularly relates to a preparation method of high-uniformity metal powder with controllable granularity.
Background
Tungsten and molybdenum have the characteristics of high melting point, good corrosion resistance, high-temperature strength, good ablation resistance, low thermal expansion coefficient and the like, and have remarkable advantages when being applied in a high-temperature environment, and typical materials are tungsten copper infiltrated composite materials and molybdenum copper infiltrated composite materials. At present, the tungsten copper-infiltrated composite material and the molybdenum copper-infiltrated composite material are widely applied in the fields of aerospace, electronics, metallurgical industry and the like, such as anti-gas-erosion parts of a gas rudder, a nozzle throat insert, a guard plate, a connecting plate and the like of a solid rocket engine, and arc-erosion-resistant materials in the electronic field and the like.
With the development of science and technology, new generation equipment puts a strict demand on high precision, which puts higher demands on uniformity and consistency of materials. The uniformity and consistency of the tungsten copper infiltrated composite material and the molybdenum copper infiltrated composite material are fundamentally solved, and one of the keys is the uniformity and consistency of the tungsten framework and the molybdenum framework. In order to obtain good tungsten skeleton and molybdenum skeleton, the particle size and uniformity and consistency of particle size distribution of the tungsten powder and molybdenum powder are preconditions. The current commercially available tungsten powder and molybdenum powder have wide particle size distribution range and agglomeration, and are difficult to meet the requirements.
At present, the powder feeding rate in the prior art is 1-20 kg/h, the maximum amount of tungsten powder or molybdenum powder treated according to 8 hours in a working day is only 160kg, and the production efficiency is too low.
Therefore, the research and development of the preparation method of the tungsten powder and the molybdenum powder with high uniformity and controllable granularity is of great significance.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of metal powder with high uniformity and controllable particle size, wherein the metal powder is tungsten powder or molybdenum powder, and the method comprises the following steps:
1) putting the metal powder raw material into a vacuum oven, and carrying out vacuum drying;
2) taking the dried metal powder raw material out of the vacuum oven, performing vertical fluidized bed type crushing and grading treatment, setting the range of each process parameter, wherein the pressure of an airtight pressure gauge is 0.05-0.3MPa, and the air volume of secondary air distribution is 400-1100 m-3The powder feeding speed of the feeder is 30-160kg/h, the speed value of the classifier is 140-.
Further, in the step 1), the temperature of the vacuum drying is 100--2Pa。
Further, in the step 2), the process parameters are as follows: the pressure of the airtight pressure gauge is 0.1-0.25MPa, and the air quantity of the secondary air distribution is 500-3The powder feeding speed of the feeder is 40-150kg/h, and the speed value of the classifier is 150-1200 r/min.
Further, in the step 1), the temperature of the vacuum drying is 100 ℃, 150 ℃ or 200 ℃, and the heat preservation time is 90min, 105min or 120 min.
Further, in the step 2), the process parameters are as follows: the pressure of the airtight pressure gauge is 0.1MPa, 0.15MPa, 0.2MPa or 0.25MPa, and the air volume of the secondary air distribution is 500m3/h、600m3/h、800m3H or 1000m3The powder feeding speed of the feeder is 40kg/h, 50kg/h, 100kg/h or 150kg/h, and the speed value of the classifier is 150r/min, 600r/min, 800r/min or 1200 r/min.
Further, the step 2) specifically comprises the following steps:
2-1) carrying out vertical fluidized bed type crushing and grading treatment, and setting each process parameter;
2-2) taking the dried metal powder raw material out of the vacuum oven, feeding the metal powder raw material into a feeding cylinder, covering the feeding cylinder with a cover, and waiting for starting;
2-3) sequentially starting each power supply according to the following sequence: starting a classifier; adjusting a grader speed adjusting table; starting the induced draft fan; fourthly, starting the blower; starting the feeder;
2-4) starting to work after all the powder conveying devices are started, determining whether the grading motor, the pressure gauge, the electric control cabinet indicator lamp and the rotating speed display are normal or not in the process, and determining whether the powder conveying of the transparent pipeline is finished or not; after the conveying is finished, the equipment runs for a period of time, the power supply is turned off, and the turn-off sequence of each power supply is opposite to the turn-on sequence in the step 2-3);
2-5) knocking the receiving hopper after the equipment stops to enable all powder in the receiving hopper to enter each receiving cylinder, then closing each receiving cylinder control valve, and taking out the powder to finish the whole preparation process.
Further, in the step 2-2), the time interval from taking out the metal powder raw material to feeding the metal powder raw material into the feeding cylinder is within 30 min.
Further, in the step 2-4), the running time of the equipment after the conveying is finished is 5-10 min.
The invention has the beneficial effects that:
the metal powder purchased in the market at present has wide particle size distribution range and agglomeration, and the particle size distribution span of the metal powder is very large, so that the requirement of new generation equipment on the particle size uniformity of the metal powder cannot be met, and the uniformity of the metal powder needs to be improved by processing the powder. The invention provides a preparation method of high-uniformity metal powder with controllable granularity. The metal powder obtained by the method has good uniformity and high production efficiency, and compared with the existing production efficiency, the production efficiency of the method can be improved by more than 7 times, and the powder with a plurality of granularity sections can be obtained. The method adopts a vertical fluidized bed type crushing and grading treatment mode, each particle has the same motion state in the crushing and grading process, the product granularity is adjustable, and the metal powder with a plurality of granularity sections can be obtained at one time.
In particular, the advantages of the invention are:
1. the fluidized bed crushing cavity is adopted, only compressed air flows through the nozzle, metal powder is crushed by mutual collision, and crushing abrasion is extremely small.
2. The vertical classifier is adopted, so that the classification can be better controlled through a flow field, the abrasion during classification is greatly eliminated, and the purity of the metal powder is ensured.
3. The combination of the induced draft fan and the secondary air blast is adopted, and the secondary air can be introduced, so that the ascending force of the metal powder in the air flow is enhanced.
4. And a special sealing measure is adopted, so that compressed air is not consumed, and large particles are prevented from leaking.
5. A plurality of graders are connected in series, so that the crushing efficiency is improved, and the graders can be divided into different particle size sections according to requirements, and the requirement of narrow particle size distribution is greatly met.
6. The powder feeding speed of the invention is 30-160kg/h, and the maximum amount of tungsten powder or molybdenum powder treated according to 8 hours in a working day is 1280 kg. Compared with the prior art, the production efficiency and the production capacity of the invention can be greatly improved, and the method has the advantages of more uniform distribution of the metal powder, controllable particle size distribution and the like.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of the raw tungsten powder used in the examples of the present invention;
FIG. 2 is a graph showing the particle size distribution of the raw tungsten powder used in the examples of the present invention;
FIG. 3 is a scanning electron micrograph of the tungsten powder obtained in example 1;
FIG. 4 is a graph showing the particle size distribution of the tungsten powder obtained in example 1;
FIG. 5 is a scanning electron micrograph of the tungsten powder obtained in example 2;
FIG. 6 is a graph showing the particle size distribution of the tungsten powder obtained in example 2;
FIG. 7 is a scanning electron micrograph of tungsten powder obtained in example 3 of the present invention;
FIG. 8 is a graph showing the particle size distribution of tungsten powder obtained in example 3 of the present invention;
FIG. 9 is a scanning electron micrograph of the original molybdenum powder used in the examples of the present invention;
FIG. 10 is a graph of the particle size distribution of the raw molybdenum powder used in the examples of the present invention;
FIG. 11 is a scanning electron micrograph of molybdenum powder obtained in example 4 of the present invention;
FIG. 12 is a graph showing the particle size distribution of molybdenum powder obtained in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The technical scheme of the invention has the following process principle: the invention relates to a method for preparing tungsten powder or molybdenum powder with high uniformity and controllable granularity by adopting a vertical fluidized bed type crushing and grading method. The method is that compressed air is used to accelerate into supersonic speed airflow and then the airflow is injected into a crushing area to make tungsten powder or molybdenum powder fluidized, and the accelerated particles are collided and crushed. Each particle has the same state of motion. The crushed tungsten powder or molybdenum powder is conveyed to a grading area by ascending airflow, and the powder meeting the requirement of the granularity is separated by a grader. The grading zones are connected in series by a multi-stage grader, and powder with a plurality of grain size sections can be obtained at one time.
Example 1
(1) Putting commercially available raw material tungsten powder into a vacuum oven for vacuum drying, wherein the drying temperature is 100 ℃, the heat preservation time is 120min, and the vacuum degree is 10-2Pa。
(2) Adopts a vertical fluidized bed type to crush and separatePerforming stage treatment, namely firstly setting each process parameter, adjusting the air quantity of a draught fan and adjusting an airtight pressure gauge to enable the inlet pressure to be 0.1 MPa; adjusting the valve of the blower to control the air quantity of the secondary air distribution to be 600m3H; adjusting a feeder to set, and adjusting the powder feeding rate to be 50 kg/h; the classifier speed adjustment value was set to 1200 r/min.
(3) And taking the dried tungsten powder out of the vacuum oven, sending the tungsten powder into a feeding cylinder (the time interval from taking out the tungsten powder to sending the tungsten powder into the feeding cylinder is not more than 30 minutes), covering the feeding cylinder with a cover, and waiting for starting.
(4) The various instruments were started up in sequence as follows: starting a classifier; adjusting a grader speed adjusting table; starting the induced draft fan; fourthly, starting the blower; the feeder is started.
(5) And after all the powder conveying devices are started, the powder conveying devices start to work, whether the grading motors, the pressure gauges, the electric control cabinet indicator lamps and the rotating speed display are normal or not is determined through observation in the process, and whether the powder conveying of the transparent pipeline is finished or not is determined through observation. And (5) running for 5min after the conveying is finished, and turning off the power supply of each instrument, wherein the turn-off sequence of the power supply of each instrument is opposite to the turn-on sequence of the step (4).
(6) And after the equipment is stopped, knocking the receiving hopper by using a rubber hammer to enable all the powder in the receiving hopper to enter each receiving cylinder, closing each receiving cylinder control valve, and taking out the powder to finish the whole preparation process.
Fig. 1 shows a scanning electron microscope image of the used original tungsten powder, and it can be seen from fig. 1 that the original tungsten powder particles have obvious agglomeration phenomenon and uneven particle size distribution. FIG. 2 shows the particle size distribution curve of the raw tungsten powder used, and it can be seen from FIG. 2 that the particle size distribution curve is not a regular normal distribution curve, and the curve has irregular bulges at the coarse particle size distribution, which indicates that the powder in the coarse particle size section has more powder than in the fine particle size section, and the particle size distribution is not uniform, and in addition, from the test data, the D10 particle size of the powder is 11.470 μm, the D90 is 52.422 μm, and the particle size range of D10-D90 reaches 40.952 μm.
FIG. 3 is a scanning electron microscope image of the tungsten powder obtained by the above method, and it can be seen from FIG. 3 that the tungsten powder particles obtained by the method of the present invention are all distributed dispersedly, no agglomeration among particles exists, the particle size difference is not large, and the particle size distribution of the powder is uniform.
FIG. 4 is a particle size distribution curve of the tungsten powder obtained by the above method, and it can be seen from FIG. 4 that the particle size distribution curve of the tungsten powder obtained by the method of the present invention is a regular normal distribution curve, the D10 particle size of the powder is 2.635 μm, D90 is 9.331 μm, and the particle size range of D10-D90 is narrowed to 6.696 μm. The average particle size of the test powder was 3.12. mu.m.
Example 2
(1) Putting commercially available raw material tungsten powder into a vacuum oven for vacuum drying, wherein the drying temperature is 200 ℃, the heat preservation time is 90min, and the vacuum degree is 10-2Pa。
(2) Adopting vertical fluidized bed type crushing and grading treatment, firstly setting various process parameters, adjusting the air quantity of a draught fan and adjusting a hermetic seal pressure gauge to enable the inlet pressure to be 0.2 MPa; adjusting the valve of the blower to control the air quantity of the secondary air distribution to be 1000m3H; adjusting a feeder to set, and adjusting the powder feeding rate to 150 kg/h; the classifier speed adjustment value was set to 150 r/min.
(3) And taking the dried tungsten powder out of the vacuum oven, sending the tungsten powder into a feeding cylinder (the time interval from taking out the tungsten powder to sending the tungsten powder into the feeding cylinder is not more than 30 minutes), covering the feeding cylinder with a cover, and waiting for starting.
(4) The various instruments were started up in sequence as follows: starting a classifier; adjusting a grader speed adjusting table; starting the induced draft fan; fourthly, starting the blower; the feeder is started.
(5) And after all the powder conveying devices are started, the powder conveying devices start to work, whether the grading motors, the pressure gauges, the electric control cabinet indicator lamps and the rotating speed display are normal or not is determined through observation in the process, and whether the powder conveying of the transparent pipeline is finished or not is determined through observation. And (5) running for 5min after the conveying is finished, and turning off the power supply of each instrument, wherein the turn-off sequence of the power supply of each instrument is opposite to the turn-on sequence of the step (4).
(6) And (3) knocking the receiving hopper by using a rubber hammer after the equipment is stopped, so that all the powder in the receiving hopper enters each receiving cylinder, closing each receiving cylinder control valve, taking out the powder, and finishing the preparation process.
FIG. 5 is a scanning electron microscope image of the tungsten powder obtained by the above method, and it can be seen from FIG. 5 that the tungsten powder particles obtained by the method of the present invention are all dispersed and distributed, no agglomeration among particles occurs, the particle size difference is not large, and the particle size distribution is uniform. As can be seen by comparing fig. 5 with fig. 2, the particle size of the powder particles obtained in example 2 is significantly larger than that of the particles obtained in example 1.
FIG. 6 is a particle size distribution curve of the tungsten powder obtained in example 2, and it can be seen from FIG. 6 that the tungsten powder obtained by the method of the present invention has a particle size distribution curve of a regular normal distribution curve, D10 particle size of 7.826 μm, D90 of 23.400 μm, and D10-D90 particle size range narrowed to 15.574 μm. The average particle size of the test powder was 7.63. mu.m.
Example 3
(1) Putting commercially available raw material tungsten powder into a vacuum oven for vacuum drying, wherein the drying temperature is 150 ℃, the heat preservation time is 105min, and the vacuum degree is 10-2Pa。
(2) Adopting vertical fluidized bed type crushing and grading treatment, firstly setting various process parameters, adjusting the air quantity of a draught fan and adjusting a hermetic seal pressure gauge to enable the inlet pressure to be 0.15 MPa; adjusting a valve of a blower to control the air volume of secondary air distribution to be 800m3H; adjusting a feeder to set, and adjusting the powder feeding rate to be 100 kg/h; the classifier speed adjustment value was set to 600 r/min.
(3) And taking the dried tungsten powder out of the vacuum oven, conveying the tungsten powder into a feeding cylinder (the time interval from the powder taking-out to the powder feeding into the feeding cylinder is not more than 30 minutes), covering the feeding cylinder with a cover, and waiting for starting.
(4) The various instruments were started up in sequence as follows: starting a classifier; adjusting a grader speed adjusting table; starting the induced draft fan; fourthly, starting the blower; the feeder is started.
(5) And after all the powder conveying devices are started, the powder conveying devices start to work, whether the grading motors, the pressure gauges, the electric control cabinet indicator lamps and the rotating speed display are normal or not is determined through observation in the process, and whether the powder conveying of the transparent pipeline is finished or not is determined through observation. And (5) running for 5min after the conveying is finished, and turning off the power supply of each instrument, wherein the turn-off sequence of the power supply of each instrument is opposite to the turn-on sequence of the step (4).
(6) And (3) knocking the receiving hopper by using a rubber hammer after the equipment is stopped, so that all the powder in the receiving hopper enters each receiving cylinder, closing each receiving cylinder control valve, taking out the powder, and finishing the preparation process.
FIG. 7 is a scanning electron microscope image of the tungsten powder obtained in example 3 of the present invention, and it can be seen from FIG. 7 that the tungsten powder particles obtained by the method of the present invention are all distributed dispersedly, no agglomeration between particles occurs, the particle size difference is not large, and the particle size distribution of the powder is uniform. In comparison with fig. 3 and 5, the particles of the powder of fig. 7 (obtained in example 3) are larger than those of fig. 3 (obtained in example 1), but slightly smaller than those of fig. 5 (obtained in example 2).
FIG. 8 is a particle size distribution curve of the tungsten powder obtained in example 3, and it is understood from FIG. 8 that the tungsten powder obtained by the method of the present invention has a particle size distribution curve of a regular normal distribution curve, D10 particle size of 5.923 μm, D90 particle size of 15.824 μm, and D10-D90 particle size range narrowed to 9.901 μm and controlled to 10 μm or less. The average particle size of the test powder was 6.02. mu.m.
Example 4
(1) Putting commercial raw material molybdenum powder into a vacuum oven for vacuum drying, wherein the drying temperature is 100 ℃, the heat preservation time is 120min, and the vacuum degree is 10-2Pa。
(2) Adopting vertical fluidized bed type crushing and grading treatment, firstly setting various process parameters, adjusting the air quantity of a draught fan and adjusting a hermetic seal pressure gauge to enable the inlet pressure to be 0.25 MPa; adjusting the valve of the blower to control the air quantity of the secondary air distribution to be 500m3H; adjusting a feeder to adjust the powder feeding rate to 40 kg/h; the classifier speed adjustment value was set to 800 r/min.
(3) And taking the dried molybdenum powder out of the vacuum oven, sending the molybdenum powder into a feeding cylinder (the time interval from the molybdenum powder taking out to the molybdenum powder feeding into the feeding cylinder is not more than 30 minutes), covering the feeding cylinder with a cover, and waiting for starting.
(4) The various instruments were started up in sequence as follows: starting a classifier; adjusting a grader speed adjusting table; starting the induced draft fan; fourthly, starting the blower; the feeder is started.
(5) And after all the powder conveying devices are started, the powder conveying devices start to work, whether the grading motors, the pressure gauges, the electric control cabinet indicator lamps and the rotating speed display are normal or not is determined through observation in the process, and whether the powder conveying of the transparent pipeline is finished or not is determined through observation. And (5) running for 5min after the conveying is finished, and turning off the power supply of each instrument, wherein the turn-off sequence of the power supply of each instrument is opposite to the turn-on sequence of the step (4).
(6) And after the equipment is stopped, knocking the receiving hopper by using a rubber hammer to enable all the powder in the receiving hopper to enter each receiving cylinder, closing each receiving cylinder control valve, and taking out the powder to finish the whole preparation process.
FIG. 9 shows a scanning electron micrograph of the used original molybdenum powder, and it can be seen from FIG. 9 that the original molybdenum powder particles have a significant agglomeration phenomenon and a non-uniform particle size distribution. FIG. 10 shows the particle size distribution curve of the original molybdenum powder used, and it can be seen from FIG. 10 that the powder is relatively rich in the fine particle size fraction and the particle size distribution is not uniform, and further, from the test data, the powder has a D10 particle size of 8.326 μm, a D90 of 36.523 μm, and a D10-D90 particle size range of 28.197 μm.
FIG. 11 is a scanning electron microscope image of the molybdenum powder obtained by the above method, and it can be seen from FIG. 11 that the particles of the molybdenum powder obtained by the method of the present invention are all distributed dispersedly, no agglomeration among the particles exists, the particle size difference is not large, and the particle size distribution of the powder is uniform.
FIG. 12 is a particle size distribution curve of the molybdenum powder obtained by the above method, and it can be seen from FIG. 12 that the particle size distribution curve of the molybdenum powder obtained by the method of the present invention is a regular normal distribution curve, the D10 particle size of the powder is 2.654 μm, the D90 particle size is 9.952 μm, and the particle size range of D10-D90 is narrowed to 7.298 μm. The average particle size of the test powder was 3.17. mu.m.
The particle size distribution of the commercial metal powder raw material is wide and has agglomeration, the particle size distribution width of D10-D90 is as high as more than 40 mu m, and the preparation method can control the particle size distribution width of D10-D90 of the metal powder within 16 mu m.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of metal powder with high uniformity and controllable particle size is characterized in that the metal powder is tungsten powder or molybdenum powder, and the method comprises the following steps:
1) putting the metal powder raw material into a vacuum oven, and carrying out vacuum drying;
2) taking the dried metal powder raw material out of the vacuum oven, performing vertical fluidized bed type crushing and grading treatment, setting the range of each process parameter, wherein the pressure of an airtight pressure gauge is 0.05-0.3MPa, and the air volume of secondary air distribution is 400-1100 m-3The powder feeding speed of the feeder is 30-160kg/h, the speed value of the classifier is 140-.
2. The method as claimed in claim 1, wherein the temperature of the vacuum drying is 100-200 ℃, the time of the vacuum drying is 90-120min, and the vacuum degree is 10 in the step 1)-2Pa。
3. The method for preparing metal powder with high uniformity and controllable particle size according to claim 1, wherein in the step 2), the process parameters are as follows: the pressure of the airtight pressure gauge is 0.1-0.25MPa, and the air quantity of the secondary air distribution is 500-3The powder feeding speed of the feeder is 40-150kg/h, and the speed value of the classifier is 150-1200 r/min.
4. The method for preparing metal powder with high uniformity and controllable particle size according to claim 2, wherein in the step 1), the temperature for vacuum drying is 100 ℃, 150 ℃ or 200 ℃, and the holding time is 90min, 105min or 120 min.
5. The method for preparing metal powder with high uniformity and controllable particle size according to claim 3, wherein in the step 2), the process parameters are as follows: the pressure of the airtight pressure gauge is 0.1MPa, 0.15MPa, 0.2MPa or 0.25MPa, and the air volume of the secondary air distribution is 500m3/h、600m3/h、800m3H or 1000m3The powder feeding speed of the feeder is 40kg/h, 50kg/h, 100kg/h or 150kg/h, and the speed value of the classifier is 150r/min, 600r/min, 800r/min or 1200 r/min.
6. The method for preparing metal powder with high uniformity and controllable particle size according to claim 3, wherein the step 2) specifically comprises the following steps:
2-1) carrying out vertical fluidized bed type crushing and grading treatment, and setting each process parameter;
2-2) taking the dried metal powder raw material out of the vacuum oven, feeding the metal powder raw material into a feeding cylinder, covering the feeding cylinder with a cover, and waiting for starting;
2-3) sequentially starting each power supply according to the following sequence: starting a classifier; adjusting a grader speed adjusting table; starting the induced draft fan; fourthly, starting the blower; starting the feeder;
2-4) starting to work after all the powder conveying devices are started, determining whether the grading motor, the pressure gauge, the electric control cabinet indicator lamp and the rotating speed display are normal or not in the process, and determining whether the powder conveying of the transparent pipeline is finished or not; after the conveying is finished, the equipment runs for a period of time, the power supply is turned off, and the turn-off sequence of each power supply is opposite to the turn-on sequence in the step 2-3);
2-5) knocking the receiving hopper after the equipment stops to enable all powder in the receiving hopper to enter each receiving cylinder, then closing each receiving cylinder control valve, and taking out the powder to finish the whole preparation process.
7. The method for preparing metal powder with high uniformity and controllable particle size according to claim 6, wherein in the step 2-2), the time interval from taking out the metal powder raw material to feeding the metal powder raw material into the feeding cylinder is within 30 min.
8. The method for preparing metal powder with high uniformity and controllable particle size according to claim 6, wherein in the step 2-4), the time for equipment operation after the conveying is finished is 5-10 min.
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