CN107030857B - Method for forming blank of ceramic micro-bead - Google Patents
Method for forming blank of ceramic micro-bead Download PDFInfo
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- CN107030857B CN107030857B CN201710358133.XA CN201710358133A CN107030857B CN 107030857 B CN107030857 B CN 107030857B CN 201710358133 A CN201710358133 A CN 201710358133A CN 107030857 B CN107030857 B CN 107030857B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000011325 microbead Substances 0.000 title claims description 15
- 239000004005 microsphere Substances 0.000 claims abstract description 31
- 238000010304 firing Methods 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 10
- 229910002027 silica gel Inorganic materials 0.000 claims description 10
- 239000000741 silica gel Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000009718 spray deposition Methods 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910001570 bauxite Inorganic materials 0.000 claims description 2
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims 1
- 238000011105 stabilization Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 19
- 239000003960 organic solvent Substances 0.000 abstract description 8
- 238000005299 abrasion Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 3
- 230000006835 compression Effects 0.000 abstract 1
- 238000007906 compression Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- 238000009694 cold isostatic pressing Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000005056 compaction Methods 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000011265 semifinished product Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/481—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing silicon, e.g. zircon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention relates to a method for forming a blank of ceramic microspheres, belonging to the technical field of special ceramics. The blank forming method comprises the steps of performing ceramic powder to obtain a microsphere blank, immersing the microsphere blank into an organic solvent for wrapping, placing the coated microsphere blank into a cold isostatic press cylinder for isostatic pressing, and finally performing low-temperature firing and high-temperature sintering to obtain a ceramic microsphere product. The invention solves the problems of high production cost, low production efficiency and difficult molding of small-micro-sized products in the production process of high-quality ceramic microspheres, has the characteristics of simple molding method, high production efficiency, good product performance and high practical popularization value, and the micron-sized ceramic microsphere blank prepared by the molding method can improve the production efficiency by 40 percent, the compression strength of the blank can reach 55-150MPa, and the volume density of the product can be improved by more than 5 percent and the self-abrasion consumption is reduced by more than 30 percent after high-temperature sintering in different modes and at different temperatures.
Description
Technical Field
The invention relates to a method for forming a blank of ceramic microspheres, belonging to the technical field of special ceramics.
Background
In recent 20 years, isostatic pressing technology has been widely applied to the fields of ceramic manufacturing, tool manufacturing, plastics, high-voltage electromagnetic porcelain bottles, high-performance materials, military industry and the like, and in the special industrial ceramic industry, the cold isostatic pressing technology is more widely popularized and applied in a large area. The cold isostatic pressing technology is that at normal temperature, flexible materials such as rubber, plastic or resin are used as materials of a sheath mold, liquid is used as a pressure transmission medium, and the cold isostatic pressing technology is mainly used for forming powder materials and providing blanks for further sintering or hot isostatic pressing procedures. The blank forming method of the ceramic microspheres utilizes the cold isostatic pressing technology, thereby ensuring the uniformity of the density of the blank of the ceramic microspheres and improving the physical properties of the finished product such as volume density, hardness, wear resistance and the like.
At present, in the field of production of high-quality ceramic microbeads (with the grain diameter of 0.1-3mm), flexible materials are used as sheathing die materials, so that the problems of high production cost and low labor production efficiency exist, and in the cold isostatic pressing process, liquid leakage (water, oil) and liquid seepage (water, oil) phenomena caused by aging and damage of the die materials due to repeated use often occur, so that production stop is needed in the production process, and equipment is overhauled or even overhauled. Therefore, it is necessary to research a technical method of auxiliary molding material to replace flexible materials such as rubber, plastic or resin as sheathing mold material to solve various defects of ceramic microbeads in the cold isostatic pressing process.
Disclosure of Invention
The invention aims to provide a method for forming a blank of ceramic microspheres, which solves the problems of high production cost, low production efficiency and difficult forming of small-micro-size products in the production process of high-quality ceramic microspheres and has the characteristics of simple forming method, high production efficiency, good product performance and high practical popularization value.
The blank forming method of the ceramic microspheres comprises the steps of performing ceramic powder to obtain a microsphere blank, immersing the microsphere blank into an organic solvent for wrapping, placing the coated microsphere blank into a cold isostatic press cylinder for isostatic pressing, and finally carrying out low-temperature firing and high-temperature sintering to obtain a ceramic microsphere product.
Wherein:
the ceramic powder material is any one or more of micron-sized powder such as aluminum oxide, zirconium silicate, silicon carbide, silicon nitride, silicon oxide, bauxite and the like.
The organic solvent is liquid silica gel, and the temperature of the organic solvent is 120 ℃.
The preforming process is any one of rolling forming, injection forming, spray forming and throwing forming.
The particle size of the microsphere blank is 0.1-3 mm.
The coating is realized by immersing the preformed microsphere blank in an organic solvent in batches in a hydrophilic coating mode, a layer of film with uniform thickness is formed on the surface of the blank, the film has the functions of bearing and isolating liquid and can prevent the blank from directly contacting with pressure conduction liquid, and the organic solution also has the characteristic of being not hydrophilic with metal materials.
The isostatic compaction is to pour the microsphere blank wrapped with the organic solvent into a stainless steel barrel for isostatic compaction, then put the stainless steel barrel into a cold isostatic press cylinder, and perform isostatic compaction on the microsphere blank according to the isostatic compaction production process set by common production under the pressure of 70-260 MPa.
The low-temperature firing is to perform heat preservation firing on the microsphere blank which is subjected to isostatic pressing in an industrial kiln at the temperature of 100-300 ℃ so as to remove the organic thin film layer coated on the surface of the microsphere blank.
The high-temperature sintering is to sinter the ceramic microsphere products according to the original sintering temperature and the microsphere blanks prepared from different raw materials.
The invention has the following beneficial effects:
the invention solves the technical problems that the ceramic microspheres (with the particle size of 0.1-3mm) are difficult to be subjected to cold isostatic pressing and various technical problems exist in the cold isostatic pressing process, and greatly improves the cold isostatic pressing production efficiency of small and micro-sized products in industrial production.
Drawings
FIG. 1 is a schematic diagram of a coating process in the present invention;
FIG. 2 is a schematic view of a coated microbead sphere blank according to the present invention.
In the figure: 1. a microsphere green body; 2. a microbead sphere blank coated by an organic solvent; 3. a stainless steel inner cylinder; 4. a stainless steel outer cylinder; 5. an organic solvent; 6. and (3) an organic coating layer.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
Taking 20Kg of alumina ceramic micro-bead ball blank (the content is 92%) with the particle size of 3mm after rolling, heating liquid silica gel to 120 ℃, keeping the temperature stable, then pouring the 20Kg of micro-bead ball blank into the liquid silica gel, simultaneously starting a stirring device, taking out the ball blank coated with organic matters after 10min by using a tool, and airing and fixing a film after 5 min; and (3) performing secondary pressure forming on the treated ball blank by using a cold isostatic press, wherein the forming pressure is 90MPa, so that a qualified semi-finished product can be obtained, and the product is manufactured after low-temperature firing to remove organic matters and high-temperature firing.
Through detection, the product performance indexes obtained in the embodiment are as follows: the bulk density is 3.76g/cm3The bending strength is 500MPa, and the self-abrasion is less than or equal to 0.15 g/Kg.h.
Example 2
Taking 10Kg of zirconia ceramic micro-bead ball blank with the particle size of 0.2mm after spray forming, heating liquid silica gel to 260 ℃ and keeping the temperature stable, then pouring 10Kg of micro-bead ball blank into the liquid silica gel, simultaneously starting a stirring device, taking out the ball blank coated with organic matters after 10min by using a tool, and airing and fixing the film after 5 min; and (3) performing secondary pressure forming on the treated ball blank by using a cold isostatic press, wherein the forming pressure is 150MPa, so that a qualified semi-finished product can be obtained, and the product is manufactured after low-temperature firing to remove organic matters and high-temperature firing.
Through detection, the product performance indexes obtained in the embodiment are as follows: the bulk density is 6.75g/cm3The bending strength is 1500MPa, and the self-abrasion is less than or equal to 6 ppm/Kg.h.
Example 3
Taking 5Kg of silica ceramic microsphere blank with the particle size of 0.3mm, which is subjected to injection molding, heating liquid silica gel to 260 ℃ and keeping the temperature stable, then pouring the 5Kg of microsphere blank into the liquid silica gel, simultaneously starting a stirring device, taking out the microsphere blank coated with the organic matters by using a tool after 10min, and airing and fixing the film after 5 min; and (3) performing secondary pressure forming on the treated ball blank by using a cold isostatic press, wherein the forming pressure is 170MPa, so that a qualified semi-finished product can be obtained, and the product is manufactured after low-temperature firing to remove organic matters and high-temperature firing.
Through detection, the product performance indexes obtained in the embodiment are as follows: the bulk density is 3.26g/cm3The flexural strength was 1000MPa and the Hardness (HV) was 1800 MPa.
Claims (2)
1. A method for forming a blank of ceramic microspheres is characterized by comprising the following steps:
performing ceramic powder to obtain a micro-bead ball blank, wherein the diameter of the micro-bead ball blank is 0.1-3mm, keeping the temperature of liquid silica gel at 120 ℃ for stabilization, then immersing the micro-bead ball blank into the liquid silica gel for wrapping, simultaneously starting a stirring device for stirring, stirring for a period of time, taking out the ball blank wrapped with the liquid silica gel by using a tool, airing, fixing a film, then placing the ball blank into a cold isostatic press cylinder for isostatic pressing, wherein the pressure during isostatic pressing is 70-260MPa, and finally performing low-temperature firing and high-temperature sintering, wherein the temperature during low-temperature firing is 100-300 ℃ to obtain a ceramic micro-bead ball product;
wherein, the ceramic powder material is any one or more of alumina, zirconia, zirconium silicate, silicon carbide, silicon nitride, silicon oxide or bauxite.
2. The method for forming a green body of ceramic microbeads according to claim 1, wherein: the preforming step is any one of roll forming, injection forming, spray forming and throwing forming.
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| CN110540409B (en) * | 2018-05-29 | 2022-02-01 | 山东工业陶瓷研究设计院有限公司 | Powder of alumina ceramic part and preparation method thereof |
| CN111251521B (en) * | 2018-12-03 | 2022-07-22 | 沈欣 | Method for preparing liquid bead pill |
| CN111233486B (en) * | 2020-02-24 | 2023-05-05 | 长裕控股集团股份有限公司 | Preparation method of ceramic microbeads |
| CN112851368B (en) * | 2021-01-27 | 2022-06-07 | 湖南柯盛新材料有限公司 | Method for preparing coated wear-resistant ceramic microspheres by non-impregnation method and wear-resistant ceramic microspheres |
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| CN101439967A (en) * | 2008-12-26 | 2009-05-27 | 武汉理工大学 | Preparation of high compactness stannic oxide ceramic |
| CN102603305A (en) * | 2012-03-03 | 2012-07-25 | 赣州虔东稀土集团股份有限公司 | Forming method and device of ceramic micro-bead green body |
| CN102875157A (en) * | 2012-11-07 | 2013-01-16 | 毕鹏云 | Preparation method of aluminum oxide ceramics |
| CN103319173A (en) * | 2013-06-29 | 2013-09-25 | 广东东方锆业科技股份有限公司 | Method for preparing zirconia ceramic microbead in rolling molding mode |
| CN103920436A (en) * | 2014-05-04 | 2014-07-16 | 辽宁石油化工大学 | Modified hollow microsphere and application thereof |
| JP2017047553A (en) * | 2015-08-31 | 2017-03-09 | 住友金属鉱山株式会社 | Cylindrical molding die, cylindrical ceramic molded body and method for producing the same |
| CN105936594A (en) * | 2016-04-09 | 2016-09-14 | 河南科技学院 | Method for sintering art ceramic product |
| CN105801128A (en) * | 2016-06-02 | 2016-07-27 | 吴依妮 | Silicon nitride ceramic and method for preparing same |
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