CN113441709A - Forming agent suitable for spray granulation of high-specific-weight tungsten alloy powder and preparation method and application thereof - Google Patents
Forming agent suitable for spray granulation of high-specific-weight tungsten alloy powder and preparation method and application thereof Download PDFInfo
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- CN113441709A CN113441709A CN202110447943.9A CN202110447943A CN113441709A CN 113441709 A CN113441709 A CN 113441709A CN 202110447943 A CN202110447943 A CN 202110447943A CN 113441709 A CN113441709 A CN 113441709A
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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
- 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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention relates to a powder metallurgy process, and provides a forming agent suitable for spray granulation of high-specific gravity tungsten alloy powder, aiming at the problem that a simple forming agent cannot realize a spray granulation process, which comprises the following components: polyvinyl alcohol, polyethylene glycol, stearic acid, propylene glycol block polyether and sodium polycarboxylate, and the solvent is distilled water. The invention also provides a preparation method and application of the forming agent. In the spray granulation process of the high specific gravity tungsten alloy, the forming agent has the advantages of simple and controllable powder performance, and excellent powder flowability, loose loading ratio and pressing performance.
Description
Technical Field
The invention relates to a powder metallurgy process, in particular to a forming agent suitable for spray granulation of high-specific-gravity tungsten alloy powder, and a preparation method and application thereof.
Background
The high-specific gravity tungsten alloy material generally comprises tungsten, iron, cobalt, nickel, copper and other elements, is generally produced by using a powder metallurgy method, and has the characteristics of high production efficiency, good powder fluidity, good powder batch stability and the like, wherein the powder is required to be granulated before forming, the quality of granulation directly influences the forming of products, the spray granulation process is suitable for the granulation of mass products, and the spray granulation process has high requirements on forming agents, is unsuitable for forming agents, seriously influences the spray granulation process and the powder stability, slightly influences the quality of formed products, and completely discards powder for heavy people.
The forming agents selected in the domestic high-specific gravity industry at present are basically divided into two types: paraffin and rubber also use cellulose forming agents, and regarding the front-end granulating process, most manufacturers select to use the traditional sieve-wiping granulating at present because the investment cost of the sieve-wiping granulating equipment is low and the technical threshold is low relatively, so that the sieve-wiping granulating equipment is suitable for small-scale multi-brand production, on the other hand, the spray granulating technology is mainly considered to be not popularized and has high technical difficulty, the most important thing is the selection of the forming agents because the traditional granulating mode has simple forming agent components, the spray granulating needs to solve a plurality of problems, and the simple 2-3 components cannot realize the spray granulating process. Accordingly, an ideal solution is needed. Patent CN111421140A discloses a method for improving fluidity of sprayed powder particles of a hard alloy mixture, which uses fatty acid diethanolamide, oleamide and paraffin wax as a medium, and adopts alcohol, after spray granulation, the loose packing density is 3.9, and the fluidity is 23 s. Through the improvement of the formula, the loose packed density can reach more than 4.0, the fluidity can reach within 14S, and the powder performance is better.
Disclosure of Invention
The invention aims to overcome the problem that a simple forming agent cannot realize a spray granulation process, and provides the forming agent suitable for spray granulation of the high specific gravity tungsten alloy powder and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: polyvinyl alcohol, polyethylene glycol, stearic acid, propylene glycol block polyether and sodium polycarboxylate, and the solvent is water.
The polyvinyl alcohol (PVA) is mainly used for helping the material to be molded and improving the problem of poor moldability of the paraffin wax molding agent, but the polyvinyl alcohol has higher hardness at normal temperature, the subsequent granulation difficulty of the material is increased, the powder is too hard, and the appearance of a pressed and sintered product is poor, so that a certain amount of polyethylene glycol (PEG6000) is added to improve the plasticity of the powder and reduce the hardness of the powder after granulation. The use of PVA and PEG in different proportions enables the powder to have moldability, improve the plastic deformation capability and reduce the molding pressure. Stearic Acid (SA) mainly has the function of improving the lubricity of powder so that the powder is not easy to generate mucosa in the subsequent forming process, and the SA is also a forming agent and has the function of the forming agent. The propylene glycol block polyether is used as a defoaming agent and is one of key reagents of the invention, if the slurry is not subjected to defoaming treatment in spray granulation, the sprayed powder has poor fluidity, low loose package, more hollow powder and difficult molding, and the propylene glycol block polyether can well eliminate foam generated by stirring PVA and PEG. The sodium polycarboxylate is used as a dispersing agent, so that the materials are fully mixed, the viscosity of slurry is reduced, the spraying process is smoother, and the stability of sprayed powder is obviously improved.
Preferably, the molding agent comprises the following components in parts by weight: 45-65 parts of polyvinyl alcohol, 15-35 parts of polyethylene glycol, 2-8 parts of stearic acid, 2-8 parts of propylene glycol block polyether and 2-8 parts of sodium polycarboxylate. More preferably, the forming agent is prepared as an aqueous forming agent solution having a mass concentration of 10 to 15%, and particularly, the effect of a mass concentration of 12% is most excellent.
The invention also provides a preparation method of the forming agent, which comprises the following steps: pouring polyvinyl alcohol and polyethylene glycol powder into water, adding stearic acid, propylene glycol block polyether and sodium polycarboxylate to stir and dissolve after the two kinds of powder are completely dissolved in the water.
Preferably, the polyvinyl alcohol and the polyethylene glycol powder are poured into water, heated to 90-95 ℃ under the condition of stirring, and kept warm for 30-60 minutes.
The invention also provides an application of the forming agent, which comprises the steps of filling powder of each component of the high specific gravity tungsten alloy into a ball mill, pouring the forming agent aqueous solution, and adding the alloy balls; starting up the ball mill; after the ball milling is finished, discharging the slurry, and performing spray granulation and drying; sieving to obtain spray-granulated powder.
Preferably, the addition amount of the water solution of the forming agent is 12-20% of the mass of each component powder of the high specific gravity tungsten alloy. More preferably, the addition amount of the alloy balls is 40-100% of the mass of each component powder of the high specific gravity tungsten alloy.
Preferably, the ball milling time is 3 to 9 hours.
Therefore, the beneficial effects of the invention are as follows: according to the invention, by screening the formula of the forming agent, the apparent density and the fluidity of the tungsten alloy powder are greatly improved, the spray granulation process is facilitated, and the quality of the finished product is excellent; polyvinyl alcohol in the forming agent helps the material to be formed, polyethylene glycol is used for solving the problem of hardness increase caused by polyvinyl alcohol, stearic acid improves the powder lubricity, and propylene glycol block polyether is used as a defoaming agent for solving the problems of poor powder fluidity, low loose filling, more hollow powder and difficult forming of powder sprayed by slurry in the spray granulation process; the sodium polycarboxylate is used as a dispersing agent, so that the materials can be fully mixed.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: 45 parts of polyvinyl alcohol (PVA), 35 parts of polyethylene glycol (PEG6000), 7 parts of Stearic Acid (SA), 6 parts of propylene glycol block polyether and 7 parts of sodium polycarboxylate, wherein a solvent is distilled water, and a forming agent aqueous solution with the mass concentration of 12% is prepared.
The preparation method of the forming agent comprises the following steps:
1) weighing polyvinyl alcohol (PVA), polyethylene glycol (PEG6000), Stearic Acid (SA), propylene glycol block polyether, sodium polycarboxylate and distilled water according to a proportion;
2) pouring polyvinyl alcohol (PVA) and polyethylene glycol (PEG6000) powder into a container containing distilled water, placing the container in a water bath, heating to 90 ℃, preserving heat for 60 minutes and stirring to completely dissolve the two kinds of powder in the distilled water;
3) adding Stearic Acid (SA), propylene glycol block polyether and sodium polycarboxylate, stirring until all components are dissolved, and preparing the forming agent aqueous solution with the mass concentration of 12%.
The forming agent is used for spray granulation of high specific gravity tungsten alloy powder, and the specific steps are as follows:
1) the method comprises the following steps of (1) mixing powder of each component of the high specific gravity tungsten alloy (the mass ratio of each component is respectively: w96, Ni2, Co1, Fe0.5 and Cu0.5) are put into a ball mill, the forming agent aqueous solution is poured, the addition amount of the forming agent aqueous solution is 12 percent of the mass of each component powder of the high specific gravity tungsten alloy, and then alloy balls are added, the addition amount of the alloy balls is 40 percent of the mass of each component powder of the high specific gravity tungsten alloy;
2) starting the machine to perform ball milling for 3 hours after the feeding is finished, discharging slurry after the ball milling is finished, performing spray granulation drying on the slurry by using a spray tower, and sieving the powder after the spray granulation is finished to obtain a finished spray granulation powder product for pressing.
Example 2
A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: 55 parts of polyvinyl alcohol (PVA), 27 parts of polyethylene glycol (PEG6000), 6 parts of Stearic Acid (SA), 6 parts of propylene glycol block polyether and 6 parts of sodium polycarboxylate, wherein a solvent is distilled water, and a forming agent aqueous solution with the mass concentration of 12% is prepared.
The preparation method of the forming agent comprises the following steps:
1) weighing polyvinyl alcohol (PVA), polyethylene glycol (PEG6000), Stearic Acid (SA), propylene glycol block polyether, sodium polycarboxylate and distilled water according to a proportion;
2) pouring polyvinyl alcohol (PVA) and polyethylene glycol (PEG6000) powder into a container containing distilled water, placing the container in a water bath, heating to 95 ℃, preserving heat for 30 minutes and stirring to completely dissolve the two kinds of powder in the distilled water;
3) adding Stearic Acid (SA), propylene glycol block polyether and sodium polycarboxylate, stirring until all components are dissolved, and preparing the forming agent aqueous solution with the mass concentration of 12%.
The forming agent is used for spray granulation of high specific gravity tungsten alloy powder, and the specific steps are as follows:
1) the method comprises the following steps of (1) mixing powder of each component of the high specific gravity tungsten alloy (the mass ratio of each component is respectively: w96, Ni2, Co1, Fe0.5 and Cu0.5) are put into a ball mill, the forming agent aqueous solution is poured, the addition amount of the forming agent solution is 20 percent of the mass of each component powder of the high specific gravity tungsten alloy, and then alloy balls are added, the addition amount of the alloy balls is 100 percent of the mass of each component powder of the high specific gravity tungsten alloy;
2) starting the machine for ball milling for 9 hours after the feeding is finished, discharging the slurry after the ball milling is finished, spraying, granulating and drying the slurry in a spraying tower, and sieving the sprayed powder to obtain a finished product of the spraying and granulating powder for pressing.
Example 3
A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: according to the weight parts, 65 parts of polyvinyl alcohol (PVA), 17 parts of polyethylene glycol (PEG6000), 6 parts of Stearic Acid (SA), 6 parts of propylene glycol block polyether and 6 parts of sodium polycarboxylate are used, and a forming agent aqueous solution with the mass concentration of 12% is prepared by using distilled water as a solvent.
The preparation method of the forming agent comprises the following steps:
1) weighing polyvinyl alcohol (PVA), polyethylene glycol (PEG6000), Stearic Acid (SA), propylene glycol block polyether, sodium polycarboxylate and distilled water according to a proportion;
2) pouring polyvinyl alcohol (PVA) and polyethylene glycol (PEG6000) powder into a container containing distilled water, placing the container in a water bath, heating to 92 ℃, preserving heat for 40 minutes and stirring to completely dissolve the two kinds of powder in the distilled water;
3) adding Stearic Acid (SA), propylene glycol block polyether and sodium polycarboxylate, stirring until all components are dissolved, and preparing the forming agent aqueous solution with the mass concentration of 12%.
The forming agent is used for spray granulation of high specific gravity tungsten alloy powder, and the specific steps are as follows:
1) the method comprises the following steps of (1) mixing powder of each component of the high specific gravity tungsten alloy (the mass ratio of each component is respectively: w96, Ni2, Co1, Fe0.5 and Cu0.5) are put into a ball mill, the forming agent aqueous solution is poured, the addition of the forming agent solution is 15 percent of the mass of each component powder of the high specific gravity tungsten alloy, and then alloy balls are added, the addition of the alloy balls is 60 percent of the mass of each component powder of the high specific gravity tungsten alloy;
2) starting the machine for ball milling for 5 hours after the feeding is finished, discharging the slurry after the ball milling is finished, spraying, granulating and drying the slurry in a spraying tower, and sieving the sprayed powder to obtain a finished product of the spraying and granulating powder for pressing.
Comparative example 1
A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: 60 parts of polyvinyl alcohol (PVA), 24 parts of polyethylene glycol (PEG6000), 8 parts of propylene glycol block polyether and 8 parts of sodium polycarboxylate, wherein a solvent is distilled water, and a forming agent aqueous solution with the mass concentration of 12% is prepared.
The preparation method of the forming agent comprises the following steps:
1) weighing polyvinyl alcohol (PVA), polyethylene glycol (PEG6000), propylene glycol block polyether, sodium polycarboxylate and distilled water according to a proportion;
2) pouring polyvinyl alcohol (PVA) and polyethylene glycol (PEG6000) powder into a container containing distilled water, placing the container in a water bath, heating to 92 ℃, preserving heat for 40 minutes and stirring to completely dissolve the two kinds of powder in the distilled water;
3) adding propylene glycol block polyether and sodium polycarboxylate, stirring until the propylene glycol block polyether and the sodium polycarboxylate are completely dissolved, and preparing the forming agent aqueous solution with the mass concentration of 12%.
The forming agent is used for spray granulation of high specific gravity tungsten alloy powder, and the specific steps are as follows:
1) the method comprises the following steps of (1) mixing powder of each component of the high specific gravity tungsten alloy (the mass ratio of each component is respectively: w96, Ni2, Co1, Fe0.5 and Cu0.5) are put into a ball mill, the forming agent aqueous solution is poured, the addition of the forming agent solution is 15 percent of the mass of each component powder of the high specific gravity tungsten alloy, and then alloy balls are added, the addition of the alloy balls is 60 percent of the mass of each component powder of the high specific gravity tungsten alloy;
2) starting the machine for ball milling for 5 hours after the feeding is finished, discharging the slurry after the ball milling is finished, spraying, granulating and drying the slurry in a spraying tower, and sieving the sprayed powder to obtain a finished product of the spraying and granulating powder for pressing.
Comparative example 2
A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: 60 parts of polyvinyl alcohol (PVA), 24 parts of polyethylene glycol (PEG6000), 8 parts of Stearic Acid (SA) and 8 parts of sodium polycarboxylate, wherein a solvent is distilled water, and a forming agent aqueous solution with the mass concentration of 12% is prepared.
The preparation method of the forming agent comprises the following steps:
1) weighing polyvinyl alcohol (PVA), polyethylene glycol (PEG6000), Stearic Acid (SA), sodium polycarboxylate and distilled water according to a proportion;
2) pouring polyvinyl alcohol (PVA) and polyethylene glycol (PEG6000) powder into a container containing distilled water, placing the container in a water bath, heating to 92 ℃, preserving heat for 40 minutes and stirring to completely dissolve the two kinds of powder in the distilled water;
3) adding Stearic Acid (SA) and sodium polycarboxylate, stirring until all components are dissolved, and preparing the forming agent aqueous solution with the mass concentration of 12%.
The forming agent is used for spray granulation of high specific gravity tungsten alloy powder, and the specific steps are as follows:
1) the method comprises the following steps of (1) mixing powder of each component of the high specific gravity tungsten alloy (the mass ratio of each component is respectively: w96, Ni2, Co1, Fe0.5 and Cu0.5) are put into a ball mill, the forming agent aqueous solution is poured, the addition of the forming agent solution is 15 percent of the mass of each component powder of the high specific gravity tungsten alloy, and then alloy balls are added, the addition of the alloy balls is 60 percent of the mass of each component powder of the high specific gravity tungsten alloy;
2) starting the machine for ball milling for 5 hours after the feeding is finished, discharging the slurry after the ball milling is finished, spraying, granulating and drying the slurry in a spraying tower, and sieving the sprayed powder to obtain a finished product of the spraying and granulating powder for pressing.
Comparative example 3
A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder comprises the following components: 60 parts of polyvinyl alcohol (PVA), 24 parts of polyethylene glycol (PEG6000), 8 parts of Stearic Acid (SA) and 8 parts of propylene glycol block polyether, wherein a solvent is distilled water, and a forming agent aqueous solution with the mass concentration of 12% is prepared.
The preparation method of the forming agent comprises the following steps:
1) weighing polyvinyl alcohol (PVA), polyethylene glycol (PEG6000), Stearic Acid (SA), propylene glycol block polyether and distilled water according to a proportion;
2) pouring polyvinyl alcohol (PVA) and polyethylene glycol (PEG6000) powder into a container containing distilled water, placing the container in a water bath, heating to 92 ℃, preserving heat for 40 minutes and stirring to completely dissolve the two kinds of powder in the distilled water;
3) adding Stearic Acid (SA) and propylene glycol block polyether, stirring until the stearic acid and the propylene glycol block polyether are completely dissolved, and preparing the forming agent aqueous solution with the mass concentration of 12%.
The forming agent is used for spray granulation of high specific gravity tungsten alloy powder, and the specific steps are as follows:
1) the method comprises the following steps of (1) mixing powder of each component of the high specific gravity tungsten alloy (the mass ratio of each component is respectively: w96, Ni2, Co1, Fe0.5 and Cu0.5) are put into a ball mill, the forming agent aqueous solution is poured, the addition of the forming agent solution is 15 percent of the mass of each component powder of the high specific gravity tungsten alloy, and then alloy balls are added, the addition of the alloy balls is 60 percent of the mass of each component powder of the high specific gravity tungsten alloy;
2) starting the machine for ball milling for 5 hours after the feeding is finished, discharging the slurry after the ball milling is finished, spraying, granulating and drying the slurry in a spraying tower, and sieving the sprayed powder to obtain a finished product of the spraying and granulating powder for pressing.
Performance testing
The powder products prepared in the above examples and comparative examples are all 965B, and the performance test results are shown in the following table:
from the examples 1-3, it can be seen that the forming agent of the invention can make the loose packing density of the tungsten alloy powder reach 4.2 or more, the fluidity can reach within 14.2S, and the powder performance is excellent; in addition, the PVA and PEG used for forming of the invention can be found to have small influence on the product performance due to trace change. However, SA, propylene glycol block polyether and sodium polycarboxylate play a key role in spray granulation of powder: as can be seen from comparative example 1, the effect of SA on prevention of mucosa was significant; the addition of the propylene glycol block polyether greatly improves the apparent density and the fluidity of the powder, and the comparative example 2 lacks the component, so that the apparent density of the powder is too low, and the product is difficult to form; and the addition of the sodium polycarboxylate obviously improves the consistency of the slurry, so that the powder particles are uniform, and the lack of the component in the comparative example 3 causes poor powder uniformity and influences the filling stability of the powder in the forming process. The components are matched with each other, so that the apparent density and the fluidity of the tungsten alloy powder are greatly improved, the spray granulation process is facilitated, and the quality of a finished product is excellent.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A forming agent suitable for spray granulation of high specific gravity tungsten alloy powder is characterized by comprising the following components: polyvinyl alcohol, polyethylene glycol, stearic acid, propylene glycol block polyether and sodium polycarboxylate, and the solvent is water.
2. The forming agent suitable for spray granulation of the high specific gravity tungsten alloy powder as claimed in claim 1, wherein the forming agent comprises the following components in parts by weight: 45-65 parts of polyvinyl alcohol, 15-35 parts of polyethylene glycol, 2-8 parts of stearic acid, 2-8 parts of propylene glycol block polyether and 2-8 parts of sodium polycarboxylate.
3. The forming agent suitable for the spray granulation of the high specific gravity tungsten alloy powder according to claim 1 or 2, wherein the forming agent is configured into a forming agent water solution with the mass concentration of 10-15%.
4. A method for preparing the molding agent according to any one of claims 1 to 3, comprising the steps of: pouring polyvinyl alcohol and polyethylene glycol powder into water, adding stearic acid, propylene glycol block polyether and sodium polycarboxylate to stir and dissolve after the two kinds of powder are completely dissolved in the water.
5. The method for preparing the molding agent according to claim 4, wherein the polyvinyl alcohol and the polyethylene glycol powder are poured into water, heated to 90-95 ℃ under stirring, and kept warm for 30-60 minutes.
6. Use of a forming agent according to any of claims 1-3, characterized in that the powder of each component of the high specific gravity tungsten alloy is charged into a ball mill, the forming agent aqueous solution is poured, and the alloy balls are added; starting up the ball mill; after the ball milling is finished, discharging the slurry, and performing spray granulation and drying; sieving to obtain spray-granulated powder.
7. The application of the forming agent as claimed in claim 6, wherein the addition amount of the aqueous solution of the forming agent is 12-20% of the mass of each component powder of the high specific gravity tungsten alloy.
8. The use of the forming agent according to claim 6, wherein the addition amount of the alloy balls is 40-100% of the mass of each component powder of the high specific gravity tungsten alloy.
9. The use of a forming agent according to claim 6, 7 or 8, wherein the ball milling time is 3 to 9 hours.
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CN1157051A (en) * | 1995-06-26 | 1997-08-13 | 住友特殊金属株式会社 | Process for producing sintered earth magnet |
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