CN116162442A - Preparation method of self-sharpening agglomerated abrasive - Google Patents
Preparation method of self-sharpening agglomerated abrasive Download PDFInfo
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- CN116162442A CN116162442A CN202211673713.5A CN202211673713A CN116162442A CN 116162442 A CN116162442 A CN 116162442A CN 202211673713 A CN202211673713 A CN 202211673713A CN 116162442 A CN116162442 A CN 116162442A
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- sharpening
- self
- agglomerated abrasive
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- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 24
- 239000010432 diamond Substances 0.000 claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000001694 spray drying Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000032683 aging Effects 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 229920002472 Starch Polymers 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 239000008107 starch Substances 0.000 claims abstract description 7
- 235000019698 starch Nutrition 0.000 claims abstract description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 6
- 239000001913 cellulose Substances 0.000 claims abstract description 6
- 229920002678 cellulose Polymers 0.000 claims abstract description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 abstract description 21
- 238000000227 grinding Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000006061 abrasive grain Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 230000004075 alteration Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention relates to a preparation method of self-sharpening agglomerated abrasive, which comprises the following steps: the self-sharpening agglomerated abrasive is prepared from the following raw materials in percentage by weight: 30-50% of surface multi-edge diamond, 15-20% of water, 25-64% of ceramic binder powder and 1-5% of binder; the grain diameter of the surface multi-edge diamond is 1-100 mu m; the binder is at least one of starch, cellulose and polyvinyl alcohol; uniformly mixing the surface multi-edge diamond with a binder, ceramic bond powder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in a protective atmosphere to obtain the self-sharpening agglomerated abrasive. According to the preparation method of the self-sharpening agglomerated abrasive material, disclosed by the invention, the self-sharpening agglomerated abrasive material can be obtained by adopting the surface multi-edge diamond, water, a binder and ceramic bond powder as raw materials through uniform mixing and spray drying and high-temperature aging in a protective atmosphere, and the preparation method is relatively simple, does not need special steps, and meanwhile, the prepared agglomerated abrasive material has higher overall strength and better self-sharpening property, so that the technical problem to be solved is solved.
Description
Technical Field
The invention relates to the technical field of abrasives, in particular to a preparation method of a self-sharpening agglomerated abrasive.
Background
Machining is a main component part of equipment manufacturing industry and is embodied in the national comprehensive national force level. Along with the continuous improvement of the scientific and technical level, particularly the high-speed development of material science, engineering material categories are continuously refined and deepened. Industry chains of considerable size and length have been developed. Compared with a huge number of engineering material systems, the development of the processing materials has the phenomenon of relative hysteresis. As "industrial teeth", grinding is a basic machining method in machining, and has an irreplaceable position. Also, grinding processes are also subject to process mismatch between the abrasive material and the engineered material. In the field of abrasive article manufacturing, the abrasive article manufacturing technology is at its heart. Therefore, development of a novel abrasive is necessary.
In grinding, the abrasive directly participates in the processing of the processed part. In the case of single abrasive particles, the working condition is very bad, and both high grinding heat and heavy grinding load directly act on the abrasive particles. This places higher demands on the properties of the abrasive particles themselves. The high grinding heat not only brings thermal shock to the grinding material, but also affects the processing surface, and the excessive grinding heat can generate burn on the processing surface and has great influence on the surface integrity of the workpiece. The grinding heat is generated partly by cutting away the workpiece material with individual abrasive grains, and partly by the reduced sharpness of the abrasive grains, which is rubbed against the workpiece surface. The frictional heat caused by the reduced sharpness of the abrasive grains should be eliminated as much as possible. Therefore, when the sharpness of the abrasive is reduced, the dull abrasive can timely fall off, and the generation of friction heat can be effectively reduced. Therefore, the abrasive should possess a degree of self-sharpening.
The existing preparation method of the agglomerated abrasive in the market generally comprises the steps of mixing a metal oxide glass binder and a fine-grained diamond abrasive, granulating, sintering at high temperature, crushing and grading. The method can obtain isotropic agglomerated abrasive grains, the cutting edges of the inner layer and the outer layer of the grains are consistent, the service life is relatively long, but the preparation method is complex, the overall strength of the prepared agglomerated abrasive is still not very high, and meanwhile, the prepared agglomerated abrasive also has the technical problem of poor self-sharpening.
Disclosure of Invention
The invention aims to provide a preparation method of self-sharpening agglomerated abrasive materials, which aims to solve the technical problems that the preparation method of agglomerated particles is complex, the overall strength of the prepared agglomerated abrasive materials is still not very high, and the self-sharpening property of the prepared agglomerated abrasive materials is poor.
In order to achieve the above purpose, the technical scheme of the preparation method of the self-sharpening agglomerated abrasive material of the invention is as follows:
a method of preparing a self-sharpening agglomerated abrasive, comprising the steps of: the self-sharpening agglomerated abrasive is prepared from the following raw materials in percentage by weight: 30-50% of surface multi-edge diamond, 15-20% of water, 25-64% of ceramic binder powder and 1-5% of binder; the grain diameter of the surface multi-edge diamond is 1-100 mu m; the binder is at least one of starch, cellulose and polyvinyl alcohol;
uniformly mixing the surface multi-edge diamond with a binder, ceramic bond powder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in a protective atmosphere to obtain the self-sharpening agglomerated abrasive.
Compared with the prior art, the invention has the following advantages:
according to the preparation method of the self-sharpening agglomerated abrasive material, disclosed by the invention, the self-sharpening agglomerated abrasive material can be obtained by adopting the surface multi-edge diamond, water, a binder and ceramic bond powder as raw materials through uniform mixing and spray drying and high-temperature aging in a protective atmosphere, and the preparation method is relatively simple, does not need special steps, and meanwhile, the prepared agglomerated abrasive material has higher overall strength and better self-sharpening property, so that the technical problem to be solved is solved.
The surface multi-edge diamond is a product in the prior art, and the specific model is HFD-MC surface multi-edge diamond.
Preferably, the ceramic bond powder consists of the following components in percentage by weight: znO 6% -8% and SiO 2 31%~34%、Al 2 O 3 8%~10%、H 3 BO 3 28%~31%、Na 2 CO 3 3%~6%、Li 2 CO 3 11%~24%。
The beneficial effects are that: further improving the strength of the self-sharpening agglomerated abrasive.
Preferably, the protective atmosphere is a nitrogen atmosphere.
The beneficial effects are that: further improving the strength of the self-sharpening agglomerated abrasive.
Preferably, the inlet temperature of spray drying is 190-200 ℃ and the outlet temperature is 100-110 ℃.
The beneficial effects are that: further improving the strength of the self-sharpening agglomerated abrasive.
Preferably, the high temperature aging temperature is 400-600 ℃.
The beneficial effects are that: further improving the strength of the self-sharpening agglomerated abrasive.
Detailed Description
The embodiments of the present invention will be further described, and it should be noted that modifications and alterations can be made by those skilled in the art without departing from the principles of the present invention, and such modifications and alterations are also to be considered as protective scope of the invention.
Specific example 1 of the method of making a self-sharpening agglomerated abrasive of the present invention:
the self-sharpening agglomerated abrasive material of the embodiment is prepared from the following raw materials in percentage by weight: 30% of surface multi-edge diamond, 15% of water, 64% of ceramic binder powder and 1% of binder; the binder is starch; the ceramic bond powder consists of the following components in percentage by weight: znO 6% and SiO 2 31%、Al 2 O 3 8%、H 3 BO 3 28%、Na 2 CO 3 3%、Li 2 CO 3 24%;
Uniformly mixing the surface multi-edge diamond with a binder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in nitrogen atmosphere to obtain self-sharpening agglomerated abrasive materials; the inlet temperature of spray drying is 190 ℃, and the outlet temperature is 100 ℃; the high temperature ageing temperature was 400 ℃.
Specific example 2 of the method of making a self-sharpening agglomerated abrasive of the present invention:
the self-sharpening agglomerated abrasive material of the embodiment is prepared from the following raw materials in percentage by weight: 35% of diamond with multiple edges on the surface, 18% of water and ceramic knots45% of mixture powder and 2% of binder; the binder is starch and cellulose; the ceramic bond powder consists of the following components in percentage by weight: znO 8%, siO 2 34%、Al 2 O 3 10%、H 3 BO 3 31%、Na 2 CO 3 6%、Li 2 CO 3 11%;
Uniformly mixing the surface multi-edge diamond with a binder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in nitrogen atmosphere to obtain self-sharpening agglomerated abrasive materials; the inlet temperature of spray drying is 200 ℃ and the outlet temperature is 110 ℃; the high temperature ageing temperature was 600 ℃.
Specific example 3 of the method of making a self-sharpening agglomerated abrasive of the present invention:
the self-sharpening agglomerated abrasive material of the embodiment is prepared from the following raw materials in percentage by weight: 40% of surface multi-edge diamond, 18% of water, 39% of ceramic binder powder and 3% of binder; the binder is starch and polyvinyl alcohol; the ceramic bond powder consists of the following components in percentage by weight: znO 7%, siO 2 33%、Al 2 O 3 9%、H 3 BO 3 30%、Na 2 CO 3 5%、Li 2 CO 3 16%;
Uniformly mixing the surface multi-edge diamond with a binder and water, then spray drying to prepare a sphere, and aging the sphere at high temperature in an argon atmosphere to obtain a self-sharpening agglomerated abrasive; the inlet temperature of spray drying is 190 ℃, and the outlet temperature is 110 ℃; the high temperature ageing temperature was 500 ℃.
Specific example 4 of the method of making a self-sharpening agglomerated abrasive of the present invention:
the self-sharpening agglomerated abrasive material of the embodiment is prepared from the following raw materials in percentage by weight: 45% of surface multi-edge diamond, 19% of water, 28% of ceramic binder powder and 4% of binder; the binder is cellulose and polyvinyl alcohol; the ceramic bond powder consists of the following components in percentage by weight: znO 6% and SiO 2 31%、Al 2 O 3 8%、H 3 BO 3 28%、Na 2 CO 3 3%、Li 2 CO 3 24%;
Uniformly mixing the surface multi-edge diamond with a binder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in nitrogen atmosphere to obtain self-sharpening agglomerated abrasive materials; the inlet temperature of spray drying is 200 ℃ and the outlet temperature is 110 ℃; the high temperature ageing temperature was 600 ℃.
Specific example 5 of the method of making a self-sharpening agglomerated abrasive of the present invention:
the self-sharpening agglomerated abrasive material of the embodiment is prepared from the following raw materials in percentage by weight: 50% of diamond with multiple edges on the surface, 20% of water, 25% of ceramic binder powder and 5% of binder; the binder is starch, cellulose and polyvinyl alcohol; the ceramic bond powder consists of the following components in percentage by weight: znO 8%, siO 2 34%、Al 2 O 3 10%、H 3 BO 3 31%、Na 2 CO 3 6%、Li 2 CO 3 11%;
Uniformly mixing the surface multi-edge diamond with a binder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in nitrogen atmosphere to obtain self-sharpening agglomerated abrasive materials; the inlet temperature of spray drying is 200 ℃ and the outlet temperature is 100 ℃; the high temperature ageing temperature was 400 ℃.
Claims (5)
1. A method for preparing a self-sharpening agglomerated abrasive, comprising the steps of:
the self-sharpening agglomerated abrasive is prepared from the following raw materials in percentage by weight: 30-50% of surface multi-edge diamond, 15-20% of water, 25-64% of ceramic binder powder and 1-5% of binder; the grain diameter of the surface multi-edge diamond is 1-100 mu m; the binder is at least one of starch, cellulose and polyvinyl alcohol;
uniformly mixing the surface multi-edge diamond with a binder, ceramic bond powder and water, then spray drying to prepare spheres, and aging the spheres at high temperature in a protective atmosphere to obtain the self-sharpening agglomerated abrasive.
2. The method of preparing a self-sharpening agglomerated abrasive according to claim 1, wherein: the ceramic bond powder consists of the following components in percentage by weight: znO 6% -8% and SiO 2 31%~34%、Al 2 O 3 8%~10%、H 3 BO 3 28%~31%、Na 2 CO 3 3%~6%、Li 2 CO 3 11%~24%。
3. The method of preparing a self-sharpening agglomerated abrasive according to claim 1, wherein: the protective atmosphere is a nitrogen atmosphere.
4. The method of preparing a self-sharpening agglomerated abrasive according to claim 1, wherein: the inlet temperature of the spray drying is 190-200 ℃, and the outlet temperature of the spray drying is 100-110 ℃.
5. The method of preparing a self-sharpening agglomerated abrasive according to claim 1, wherein: the high-temperature aging temperature is 400-600 ℃.
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Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6551366B1 (en) * | 2000-11-10 | 2003-04-22 | 3M Innovative Properties Company | Spray drying methods of making agglomerate abrasive grains and abrasive articles |
CN102634319A (en) * | 2012-03-30 | 2012-08-15 | 天津大学 | Novel microcrystalline abrasive for super-hard abrasive tools and production method thereof |
CN103273434A (en) * | 2013-05-31 | 2013-09-04 | 湖南大学 | Ultrafine diamond and ceramic binding agent stacked abrasive materials and preparation method thereof |
CN103551971A (en) * | 2013-10-28 | 2014-02-05 | 博深工具股份有限公司 | Ceramic binding agent for ceramic grinding block and preparation method thereof |
CN103709993A (en) * | 2013-12-11 | 2014-04-09 | 祝世连 | Self-sharpening diamond abrasive material and preparation method thereof |
CN105196201A (en) * | 2015-09-22 | 2015-12-30 | 景德镇陶瓷学院 | Novel grinding material, novel grinding tool, preparing method of novel grinding material and preparing method of novel grinding tool |
CN105563363A (en) * | 2014-11-05 | 2016-05-11 | 江苏华东砂轮有限公司 | Method for preparing ceramic bond stacking abrasive material through centrifugal drying granulation technology |
CN105856078A (en) * | 2016-04-19 | 2016-08-17 | 南京航空航天大学 | Preparation method and use of self-sharpening sintered abrasive material |
CN107722935A (en) * | 2017-10-18 | 2018-02-23 | 绍兴自远磨具有限公司 | A kind of ball-like diamond accumulation abrasive material and its manufacture method |
CN110295361A (en) * | 2019-06-25 | 2019-10-01 | 郑州航空工业管理学院 | A kind of preparation method of multiple-cutting-edge diamond abrasive grain |
CN112059930A (en) * | 2020-09-11 | 2020-12-11 | 新乡市荣锋材料科技有限公司 | Grinding block for grinding disc for alloy material processing, preparation method of grinding block and grinding disc |
CN112659003A (en) * | 2020-12-16 | 2021-04-16 | 郑州磨料磨具磨削研究所有限公司 | Self-sharpening superhard material grinding wheel and preparation method thereof |
-
2022
- 2022-12-26 CN CN202211673713.5A patent/CN116162442A/en active Pending
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6551366B1 (en) * | 2000-11-10 | 2003-04-22 | 3M Innovative Properties Company | Spray drying methods of making agglomerate abrasive grains and abrasive articles |
CN102634319A (en) * | 2012-03-30 | 2012-08-15 | 天津大学 | Novel microcrystalline abrasive for super-hard abrasive tools and production method thereof |
CN103273434A (en) * | 2013-05-31 | 2013-09-04 | 湖南大学 | Ultrafine diamond and ceramic binding agent stacked abrasive materials and preparation method thereof |
CN103551971A (en) * | 2013-10-28 | 2014-02-05 | 博深工具股份有限公司 | Ceramic binding agent for ceramic grinding block and preparation method thereof |
CN103709993A (en) * | 2013-12-11 | 2014-04-09 | 祝世连 | Self-sharpening diamond abrasive material and preparation method thereof |
CN105563363A (en) * | 2014-11-05 | 2016-05-11 | 江苏华东砂轮有限公司 | Method for preparing ceramic bond stacking abrasive material through centrifugal drying granulation technology |
CN105196201A (en) * | 2015-09-22 | 2015-12-30 | 景德镇陶瓷学院 | Novel grinding material, novel grinding tool, preparing method of novel grinding material and preparing method of novel grinding tool |
CN105856078A (en) * | 2016-04-19 | 2016-08-17 | 南京航空航天大学 | Preparation method and use of self-sharpening sintered abrasive material |
CN107722935A (en) * | 2017-10-18 | 2018-02-23 | 绍兴自远磨具有限公司 | A kind of ball-like diamond accumulation abrasive material and its manufacture method |
CN110295361A (en) * | 2019-06-25 | 2019-10-01 | 郑州航空工业管理学院 | A kind of preparation method of multiple-cutting-edge diamond abrasive grain |
CN112059930A (en) * | 2020-09-11 | 2020-12-11 | 新乡市荣锋材料科技有限公司 | Grinding block for grinding disc for alloy material processing, preparation method of grinding block and grinding disc |
CN112659003A (en) * | 2020-12-16 | 2021-04-16 | 郑州磨料磨具磨削研究所有限公司 | Self-sharpening superhard material grinding wheel and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
陈春晖 等: "类多晶(堆积)磨料的研究现状与应用", 超硬材料工程, no. 02, pages 1 - 6 * |
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