CN111748709A - Preparation method of ultra-coarse-grain high-strength hard alloy reclaimed material - Google Patents
Preparation method of ultra-coarse-grain high-strength hard alloy reclaimed material Download PDFInfo
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- CN111748709A CN111748709A CN202010661285.9A CN202010661285A CN111748709A CN 111748709 A CN111748709 A CN 111748709A CN 202010661285 A CN202010661285 A CN 202010661285A CN 111748709 A CN111748709 A CN 111748709A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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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
- B22F8/00—Manufacture of articles from scrap or waste metal particles
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
The application provides a preparation method of an ultra-coarse grain high-strength hard alloy reclaimed material, which comprises the following steps of: calcining, zinc melting, dry ball milling, screening, wet ball milling, preparing a mixture, granulating, press forming and sintering; the grain size of the hard alloy reclaimed material prepared by the method can reach more than 6.0 mu m through high-temperature calcination and high-temperature twice sintering, the hard alloy reclaimed material belongs to ultra-coarse grain hard alloy, and the strength of the hard alloy reclaimed material prepared by the method is remarkably improved due to the ultra-coarse grains, and the bending strength is more than or equal to 3300 MPa; thereby realizing the preparation of the ultra-coarse grain high-strength hard alloy reclaimed material by utilizing the recycled waste hard alloy.
Description
Technical Field
The invention relates to the technical field of waste hard alloy recycling, in particular to a preparation method of an ultra-coarse grain high-strength hard alloy recycled material.
Background
The hard alloy has high strength, hardness, corrosion resistance and wear resistance, is known as industrial teeth, and is widely applied to the fields of mines, machining, oil drilling, military aerospace aviation and the like. In recent years, the price of raw materials gradually rises, the energy use is more and more tense, and the recovery process of the hard alloy is promoted to be concerned by people in the industry widely. Particularly, in recent years, along with the rapid development of the hard alloy industry, the contradiction between the increasing scarcity of tungsten and cobalt resources and the increasing increase of the demand thereof is more and more prominent, and the recycling of waste hard alloys is more and more emphasized by people. According to data reports, the production of the hard alloy in the world is strong, and the recovery amount of the waste hard alloy accounts for about 35 percent of the total production amount. However, the quality problem of the reclaimed material produced after the recovery of the waste hard alloy is always very outstanding, and the problems of poor product performance stability, low strength, uneven grain size and the like of the reclaimed material generally exist.
According to the international passing specification, the grain size of 2.5-6.0 μm is coarse grain hard alloy, and the grain size of more than 6.0 μm is ultra-coarse grain hard alloy (ultra-coarse grain hard alloy). The grain size of the macrocrystalline cemented carbide depends on the grain size of the WC powder. The coarse grain hard alloy and the ultra-coarse grain hard alloy have a series of excellent performances of high hardness, wear resistance, good strength and toughness, small creep deformation, heat resistance, corrosion resistance and the like at high temperature, and are widely used for mine tools, oil drilling tools, coal mining machine cutting pick tools, shield machine cutters for tunnel engineering, stamping dies, hard surface spraying and the like.
Therefore, how to prepare the ultra-coarse grain hard alloy reclaimed material by utilizing the recycled waste hard alloy has great significance.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of an ultra-coarse grain high-strength hard alloy reclaimed material.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of an ultra-coarse grain high-strength hard alloy reclaimed material comprises the following steps in sequence:
1) and (3) calcining: calcining the waste hard alloy;
2) zinc melting: performing zinc melting treatment on the waste hard alloy calcined in the step 1);
3) dry ball milling: carrying out dry ball milling treatment on the product obtained after the zinc melting treatment in the step 2);
4) screening: screening the powder obtained after the dry ball milling treatment in the step 3) by using a 170-190 mesh screen, and taking undersize;
5) wet ball milling: carrying out wet ball milling treatment on the undersize obtained by screening in the step 4);
6) preparing a mixture: adding a forming agent into the powder obtained after the wet ball milling in the step 5), and then drying and screening the powder in sequence to obtain undersize, namely a mixture;
7) and (3) granulating: granulating the mixture obtained in the step 6) to obtain granules;
8) and (3) pressing and forming: pressing the granulated material prepared in the step 7) into a target required shape;
9) and (3) sintering: sintering the product obtained after the press forming in the step 8), wherein the primary sintering temperature is 1510-1530 ℃, furnace cooling is carried out after the primary sintering heat preservation process is finished, the temperature is increased to 1510-1530 ℃ again after the primary sintering heat preservation process is finished, secondary sintering is carried out, and the ultra-coarse grain high-strength hard alloy reclaimed material is obtained after the secondary sintering is finished.
Preferably, in the step 1), the waste hard alloy is a tungsten-cobalt hard alloy, and the grain size of tungsten carbide in the waste hard alloy is 2.4-3.2 μm; the calcining temperature is 2000-2100 ℃.
Preferably, in the step 3), in the dry ball milling, the ball-material ratio is 2:1, the diameter of the grinding ball is 6 mm-10 mm, and the dry ball milling time is 2.5 hours-3 hours.
Preferably, in the step 4), the powder obtained after the dry ball milling treatment in the step 3) is screened by using a 180-mesh screen.
Preferably, in the step 5), the wet ball milling time is 24 hours.
Preferably, in step 6), the forming agent is polyethylene glycol (PEG) or paraffin, the addition amount of the forming agent is 2 wt%, and the screen is 350 meshes.
The application provides a preparation method of an ultra-coarse grain high-strength hard alloy reclaimed material, which comprises the following steps of: calcining, zinc melting, dry ball milling, screening, wet ball milling, preparing a mixture, granulating, press forming and sintering;
the grain size of the hard alloy reclaimed material prepared by the method can reach more than 6.0 mu m and belongs to ultra-coarse grain hard alloy by high-temperature calcination and sintering at 1510-1530 ℃ which is higher than the common sintering temperature and twice sintering in front and back, and the strength of the hard alloy reclaimed material prepared by the method is remarkably improved due to the ultra-coarse grains, and the bending strength is more than or equal to 3300 MPa; thereby realizing the preparation of the ultra-coarse grain high-strength hard alloy reclaimed material by utilizing the recycled waste hard alloy.
Drawings
FIG. 1 is an SEM image of an ultra-coarse grain high strength cemented carbide reclaimed material (trade name: reclaimed YK20) prepared in example 1 of the invention;
fig. 2 is an SEM image of the virgin cemented carbide (brand name virgin YK20) in comparative example 1 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 embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The application provides a preparation method of an ultra-coarse grain high-strength hard alloy reclaimed material, which comprises the following steps of:
1) and (3) calcining: calcining the waste hard alloy;
2) zinc melting: performing zinc melting treatment on the waste hard alloy calcined in the step 1);
3) dry ball milling: carrying out dry ball milling treatment on the product obtained after the zinc melting treatment in the step 2);
4) screening: screening the powder obtained after the dry ball milling treatment in the step 3) by using a 170-190 mesh screen, and taking undersize;
5) wet ball milling: carrying out wet ball milling treatment on the undersize obtained by screening in the step 4);
6) preparing a mixture: adding a forming agent into the powder obtained after the wet ball milling in the step 5), and then drying and screening the powder in sequence to obtain undersize, namely a mixture;
7) and (3) granulating: granulating the mixture obtained in the step 6) to obtain granules;
8) and (3) pressing and forming: pressing the granulated material prepared in the step 7) into a target required shape;
9) and (3) sintering: sintering the product obtained after the press forming in the step 8), wherein the primary sintering temperature is 1510-1530 ℃, furnace cooling is carried out after the primary sintering heat preservation process is finished, the temperature is increased to 1510-1530 ℃ again after the primary sintering heat preservation process is finished, secondary sintering is carried out, and the ultra-coarse grain high-strength hard alloy reclaimed material is obtained after the secondary sintering is finished.
In one embodiment of the application, in the step 1), the waste hard alloy is a tungsten-cobalt hard alloy, and the grain size of tungsten carbide in the waste hard alloy is 2.4 μm to 3.2 μm; the calcining temperature is 2000-2100 ℃.
In one embodiment of the present application, in the step 3), in the dry ball milling, the ball-to-material ratio is 2:1, the diameter of the grinding balls is 6mm to 10mm, and the dry ball milling time is 2.5 hours to 3 hours.
In one embodiment of the present application, in step 4), the powder obtained after the dry ball milling process of step 3) is sieved by using a 180-mesh sieve.
In one embodiment of the present application, the wet ball milling time in step 5) is 24 hours.
In one embodiment of the present application, in step 6), the forming agent is polyethylene glycol PEG or paraffin, the addition amount of the forming agent is 2 wt%, and the mesh is 350 mesh.
In the application, in the step 1), firstly, calcining the waste hard alloy at 2000-2100 ℃, and fully growing tungsten carbide crystal grains in the waste hard alloy through high-temperature calcination;
in the step 9), the primary sintering temperature is 1510-1530 ℃, furnace cooling is carried out after the primary sintering heat preservation process is finished, the temperature is increased to 1510-1530 ℃ again after the primary sintering heat preservation process is cooled to 950-1050 ℃, secondary sintering is carried out, 1510-1530 ℃ higher than the common sintering temperature is adopted for sintering, and the front sintering and the back sintering are carried out twice, so that tungsten carbide crystal grains are further and fully grown.
In the application, in the step 3) of dry ball milling, the zinc-melted part on the surface layer is ensured to be crushed into powder, and the non-melted part in the alloy is not mechanically crushed into powder.
In the application, in the screening in the step 4), oversize materials are returned to the step 1), and high-temperature calcination, zinc melting treatment and dry ball milling treatment are sequentially carried out again.
In the application, a forming agent is added into the powder obtained after the wet ball milling in the step 5), and the addition amount of the forming agent is 2 wt% of the sum of the mass of the powder obtained after the wet ball milling and the mass of the forming agent.
For further understanding of the present invention, the following will explain the preparation method of an ultra-coarse grain high strength cemented carbide reclaimed material provided by the present invention in detail with reference to the following examples, and the scope of the present invention is not limited by the following examples.
Example 1
A preparation method of an ultra-coarse grain high-strength hard alloy reclaimed material for preparing a reclaimed YK20 hard alloy comprises the following steps in sequence:
1) and (3) calcining: calcining the waste hard alloy;
in the step 1), the waste hard alloy comprises the following components in percentage by mass: 10 wt% cobalt, balance tungsten carbide; the grain size of the tungsten carbide is 2.4-3.2 μm; the calcination temperature is 2100 ℃;
2) zinc melting: performing zinc melting treatment on the waste hard alloy calcined in the step 1);
3) dry ball milling: carrying out dry ball milling treatment on the product obtained after the zinc melting treatment in the step 2);
in the step 3), in the dry ball milling, the ball material ratio is 2:1, the diameter of the grinding ball is 6 mm-10 mm, and the dry milling time is 3 hours;
4) screening: screening the powder obtained after the dry ball milling treatment in the step 3) by using a 180-mesh screen, and taking undersize;
5) wet ball milling: carrying out wet ball milling treatment on the undersize obtained by screening in the step 4), wherein the wet ball milling time is 24 hours;
6) preparing a mixture: adding a forming agent into the powder obtained after the wet ball milling in the step 5), and then drying and screening the powder in sequence to obtain undersize, namely a mixture;
in the step 6), the forming agent is paraffin, the addition amount of the forming agent is 2 wt%, and the screen is 350 meshes;
7) and (3) granulating: granulating the mixture obtained in the step 6) to obtain granules;
8) and (3) pressing and forming: pressing the granulated material prepared in the step 7) into a target required shape;
9) and (3) sintering: sintering the product obtained after the press forming in the step 8), wherein the primary sintering temperature is 1520 ℃, furnace cooling is carried out after the primary sintering heat preservation process is finished, the temperature is raised to 1520 ℃ again after the primary sintering heat preservation process is finished, secondary sintering is carried out, and the ultra-coarse grain high-strength hard alloy reclaimed material is obtained after the secondary sintering is finished.
The performance data of the ultra-coarse grain high strength cemented carbide reclaimed material prepared in example 1 is shown in table 1.
TABLE 1 Performance data for the ultra-coarse grain high strength cemented carbide regrind prepared in example 1 and comparative example 1
Methods and devices not described in detail in the present invention are all the prior art and are not described in detail.
The principles and embodiments of the present invention are explained herein using specific examples, which are set forth only to help understand the method and its core ideas of the present invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (6)
1. The preparation method of the ultra-coarse grain high-strength hard alloy reclaimed material is characterized by comprising the following steps of:
1) and (3) calcining: calcining the waste hard alloy;
2) zinc melting: performing zinc melting treatment on the waste hard alloy calcined in the step 1);
3) dry ball milling: carrying out dry ball milling treatment on the product obtained after the zinc melting treatment in the step 2);
4) screening: screening the powder obtained after the dry ball milling treatment in the step 3) by using a 170-190 mesh screen, and taking undersize;
5) wet ball milling: carrying out wet ball milling treatment on the undersize obtained by screening in the step 4);
6) preparing a mixture: adding a forming agent into the powder obtained after the wet ball milling in the step 5), and then drying and screening the powder in sequence to obtain undersize, namely a mixture;
7) and (3) granulating: granulating the mixture obtained in the step 6) to obtain granules;
8) and (3) pressing and forming: pressing the granulated material prepared in the step 7) into a target required shape;
9) and (3) sintering: sintering the product obtained after the press forming in the step 8), wherein the primary sintering temperature is 1510-1530 ℃, furnace cooling is carried out after the primary sintering heat preservation process is finished, the temperature is increased to 1510-1530 ℃ again after the primary sintering heat preservation process is finished, secondary sintering is carried out, and the ultra-coarse grain high-strength hard alloy reclaimed material is obtained after the secondary sintering is finished.
2. The method for preparing the reclaimed material of the ultra-coarse grain high-strength hard alloy according to claim 1, wherein in the step 1), the waste hard alloy is a tungsten-cobalt hard alloy, and the grain size of tungsten carbide in the waste hard alloy is 2.4 to 3.2 μm; the calcining temperature is 2000-2100 ℃.
3. The method for preparing the ultra-coarse grain high strength cemented carbide reclaimed material according to claim 1, wherein in the step 3), the ball-to-material ratio is 2:1, the diameter of the grinding ball is 6mm to 10mm, and the dry ball milling time is 2.5 hours to 3 hours.
4. The method for preparing the ultra-coarse grain high strength cemented carbide reclaimed material according to claim 1, wherein in the step 4), the powder obtained after the dry ball milling treatment in the step 3) is screened by a 180-mesh screen.
5. The method for preparing the ultra-coarse grain high strength cemented carbide reclaimed material according to claim 1, wherein the wet ball milling time in the step 5) is 24 hours.
6. The method for preparing the ultra-coarse grain high strength cemented carbide reclaimed material according to claim 1, wherein in the step 6), the forming agent is polyethylene glycol (PEG) or paraffin wax, the addition amount of the forming agent is 2 wt%, and the screen mesh is 350 mesh.
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| SE9602815L (en) * | 1996-07-19 | 1998-01-20 | Sandvik Ab | Diamond-coated body and method of making it |
| CN101824574A (en) * | 2010-05-14 | 2010-09-08 | 山东硬质合金有限公司 | Method for preparing extra-coarse grained carbide alloy |
| CN102965534A (en) * | 2012-11-13 | 2013-03-13 | 中南大学 | Preparation method of hard alloy with ultra-coarse grains on surface |
| CN102990069A (en) * | 2012-12-10 | 2013-03-27 | 湖南世纪特种合金有限公司 | Method for preparing coarse-grain hard alloy cutting tooth by using waste tungsten-cobalt alloy |
| CN106636837A (en) * | 2017-01-23 | 2017-05-10 | 四川理工学院 | Preparation method of ultra-coarse grain WC-Co hard alloy |
| CN109652712A (en) * | 2017-10-12 | 2019-04-19 | 吴庆宝 | A kind of super coarse-grain WC-Co hard alloy |
-
2020
- 2020-07-10 CN CN202010661285.9A patent/CN111748709B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE9602815L (en) * | 1996-07-19 | 1998-01-20 | Sandvik Ab | Diamond-coated body and method of making it |
| CN101824574A (en) * | 2010-05-14 | 2010-09-08 | 山东硬质合金有限公司 | Method for preparing extra-coarse grained carbide alloy |
| CN102965534A (en) * | 2012-11-13 | 2013-03-13 | 中南大学 | Preparation method of hard alloy with ultra-coarse grains on surface |
| CN102990069A (en) * | 2012-12-10 | 2013-03-27 | 湖南世纪特种合金有限公司 | Method for preparing coarse-grain hard alloy cutting tooth by using waste tungsten-cobalt alloy |
| CN106636837A (en) * | 2017-01-23 | 2017-05-10 | 四川理工学院 | Preparation method of ultra-coarse grain WC-Co hard alloy |
| CN109652712A (en) * | 2017-10-12 | 2019-04-19 | 吴庆宝 | A kind of super coarse-grain WC-Co hard alloy |
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