CN114773039A - Spinel ball cover isostatic pressing forming method - Google Patents
Spinel ball cover isostatic pressing forming method Download PDFInfo
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- CN114773039A CN114773039A CN202210696230.0A CN202210696230A CN114773039A CN 114773039 A CN114773039 A CN 114773039A CN 202210696230 A CN202210696230 A CN 202210696230A CN 114773039 A CN114773039 A CN 114773039A
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
- C04B35/6455—Hot isostatic pressing
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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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
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/9646—Optical properties
Abstract
The invention discloses a spinel ball cover isostatic compaction method, which comprises the specific steps of ball-milling and mixing spinel powder and sintering aid, drying, sieving by using a screen and calcining sequentially to obtain prefabricated powder, polishing and wiping a mould base, spraying a layer of lubricant on the surface of the prefabricated powder, sleeving a rubber sleeve on the surface of the prefabricated powder, pouring the powder into a mould from a feed inlet, wrapping the whole mould by dust-free paper, sealing the whole mould in vacuum, carrying out cold isostatic compaction by adopting a two-step pressurization method to obtain a required spinel ball cover biscuit, carrying out pressureless sintering and hot isostatic compaction treatment on the spinel ball cover biscuit, and finally obtaining a spinel ball cover. The method can effectively solve the problem of biscuit cracking caused by oil leakage and oil leakage in the cold isostatic pressing process of the spinel ball cover, thereby ensuring the integrity of the biscuit of the ball cover and being beneficial to industrial batch production.
Description
Technical Field
The invention relates to the technical field of forming of transparent ceramic materials, in particular to an isostatic pressing forming method of a spinel ball cover.
Background
Current window materials such as zinc sulfide, magnesium fluoride and calcium aluminate have excellent properties, but their strength and hardness are not sufficient for future window applications. Among the hard, transparent crystalline materials, only single crystal sapphire, polycrystalline aluminum oxynitride, and polycrystalline magnesium aluminate spinel are viable candidates; in recent years, magnesium aluminate spinel has been widely studied due to its high strength and excellent transmittance characteristics. The spinel has a transmission range of electromagnetic waves from ultraviolet light range to middle infrared wavelength range (0.2-5.5 μm), and the magnesia-alumina spinel has a wider transmission wavelength range compared with the aluminum oxynitride transparent ceramic and sapphire, and the wavelength of 4.5-5.5 μm is a critical band for infrared detection guidance and imaging system. The magnesia-alumina spinel has good light transmission in the wave band range of 0.19-7 mu m, the highest theoretical transmittance can reach 87%, and the magnesia-alumina spinel can be used for manufacturing high-performance optical elements, such as lenses, infrared windows and infrared fairings;
however, the magnesia-alumina spinel ball cover powder is fluffy, has large deformation degree during compression, has high requirements on the material quality of a die, and can easily cause biscuit cracking during conventional one-step cold press molding, thereby reducing the yield. Therefore, the isostatic pressing forming method of the spinel ball cover is provided.
Disclosure of Invention
The invention aims to solve the problems and provides a spinel ball cover isostatic pressing method.
In order to achieve the purpose, the invention provides the following technical scheme: a spinel ball cover isostatic pressing method is characterized in that: the molding method comprises the following steps:
ball-milling and mixing spinel powder and a sintering aid, and sequentially drying the ball-milled powder for 12 hours, sieving the powder by using a screen and calcining the powder for 5 to 10 hours to obtain prefabricated powder;
secondly, polishing the base of the die by using abrasive paper, cleaning the base by using alcohol cotton, and spraying a layer of lubricant on the surface of the base;
after the lubricant is dried, firmly sleeving the rubber sleeve with the base, sealing edges by using an adhesive tape, and pouring the prefabricated powder into a die from the feeding hole;
fourthly, vibrating to compact the powder, wrapping the whole mould by using dust-free paper, filling the mould into a bag, vacuumizing and sealing;
applying a small pressure to perform cold isostatic pressing, keeping the pressure for 1-5 min, taking out the biscuit, polishing the edges and corners of the biscuit, filling the biscuit into a bag, vacuumizing and sealing the biscuit, applying a large pressure to perform cold isostatic pressing, and keeping the pressure for 2-10min to obtain a spinel ball cover biscuit;
sixthly, sintering the spinel ball cover biscuit in the air for 3-6h, then performing hot isostatic pressing treatment, and maintaining the pressure for 1-6h to obtain the final spinel ball cover.
Preferably, the drying temperature of the powder after ball milling in the step (i) is 50-80 ℃; the screen mesh is 200 meshes; the calcination temperature is 500-700 ℃.
Preferably, the material of the die is stainless steel; the sand paper is 800-plus 2000-mesh metallographic sand paper; the spraying thickness of the lubricant is 0.5-1 mm.
Preferably, the rubber sleeve is formed by rubber injection molding for 12-24h, and the feed inlet is arranged at the top of the rubber sleeve.
Preferably, the mold is wrapped with a plurality of layers of dust-free paper.
Preferably, the smaller pressure is 20-100MPa, and the larger pressure is 100-250 MPa.
Preferably, the step of sixthly, the biscuit pressureless sintering temperature is 1700 ℃; the hot isostatic pressing temperature is 1600-1800 ℃, the pressure is 150-250 Mpa, and the pressurizing medium is argon.
The invention has the beneficial effects that: through the setting of secondary cold isostatic pressing, the spinel ball cover biscuit is obtained by utilizing secondary pressurizing cold isostatic pressing, so that the spinel ball cover biscuit is prevented from cracking in the cold isostatic pressing, and the integrity of the spinel ball cover biscuit is ensured;
through the setting of emollient, utilize emollient to separate powder and mould, prevent that powder and mould from adhering mutually to be convenient for the drawing of patterns.
Drawings
FIG. 1 is a schematic view of the structure of the mold of the present invention.
Fig. 2 is a schematic structural view of the rubber boot of the present invention.
FIG. 3 is a schematic view of the structure of a spinel ball cover biscuit according to the invention.
Illustration of the drawings: 1, a mould; 2, a rubber sleeve; 201 a feed inlet; 3, spinel ball cover biscuit.
Detailed Description
The isostatic compaction method for spinel ball cover according to the present invention is further described below with reference to the accompanying drawings.
Referring to fig. 1-3, the isostatic compaction method for spinel ball cover in the present embodiment is characterized in that: the molding method comprises the following steps:
firstly, mixing spinel powder with a sintering aid, carrying out ball milling for 12 hours, drying the ball-milled powder at 50 ℃ for 12 hours, sieving the powder by using a 200-mesh sieve, and calcining the powder at 500 ℃ for 5 hours to obtain prefabricated powder;
then, polishing the base of the die by using 800-mesh metallographic abrasive paper, cleaning the base by using alcohol cotton, and spraying a layer of lubricant with the thickness of 0.5mm on the base of the die;
waiting for 2min, drying the lubricant, cutting a hole at the top of the rubber sleeve to serve as a feeding port, sleeving the rubber sleeve on a base of a mold, fixing the rubber sleeve through an adhesive tape, and pouring 320g of prefabricated powder into the mold through the feeding port in the rubber sleeve;
pouring the prefabricated powder into a mould, compacting while chamfering, wrapping two layers of dust-free paper outside the whole mould after pouring, putting the mould into a bag, vacuumizing and sealing, performing primary cold isostatic pressing at a pressure of 100MPa for 2min, taking out the mould from the bag, demolding, polishing edges and corners of a biscuit by using 800-mesh metallographic abrasive paper, putting the polished biscuit into the bag again, vacuumizing and sealing for secondary cold isostatic pressing at a pressure of 250MPa for 2min, and taking out the biscuit to obtain a complete spinel ball cover biscuit;
and then placing the complete spinel ball cover biscuit at 1400 ℃ for pressureless sintering for 3 hours, and carrying out hot isostatic pressing treatment on the sintered spinel ball cover biscuit at 1600 ℃, wherein the pressurizing medium is argon, the pressure is 250Mpa, and the time is 1 hour, so as to obtain the final spinel ball cover.
The above embodiments are illustrative of the present invention, and are not intended to limit the present invention, and any simple modifications of the present invention are within the scope of the present invention.
Claims (7)
1. A spinel ball cover isostatic compaction method is characterized in that: the molding method comprises the following steps:
ball-milling and mixing spinel powder and sintering aid, drying the ball-milled powder for 12 hours, sieving the powder by using a screen and calcining the powder for 5 to 10 hours to obtain prefabricated powder;
polishing a base of the die by using abrasive paper, cleaning the base by using alcohol cotton, and spraying a layer of lubricant on the surface of the base;
after the lubricant is dried, firmly sleeving the rubber sleeve with the base, sealing edges by using an adhesive tape, and pouring the prefabricated powder into a mold from the feeding hole;
vibrating to compact the powder, wrapping the whole mould with dust-free paper, filling into a bag, and vacuumizing and sealing;
applying a small pressure to carry out cold isostatic pressing, keeping the pressure for 1-5 min, taking out the biscuit, polishing the edges and corners of the biscuit, packaging the biscuit into a bag, vacuumizing and sealing the bag, applying a large pressure to carry out cold isostatic pressing, and keeping the pressure for 2-10min to obtain a spinel ball cover biscuit;
and (3) placing the spinel ball cover biscuit in the air, sintering for 3-6h, performing hot isostatic pressing treatment, and maintaining the pressure for 1-6h to obtain the final spinel ball cover.
2. The method for isostatic pressing of a spinel ball cover according to claim 1, wherein: drying the powder subjected to ball milling at 50-80 ℃; the screen mesh is 200 meshes; the calcination temperature is 500-700 ℃.
3. The method for isostatic pressing of a spinel ball cover according to claim 1, wherein: secondly, the die is made of stainless steel; the sand paper is 800-mesh 2000-mesh metallographic sand paper; the spraying thickness of the lubricant is 0.5-1 mm.
4. The method for isostatic pressing of a spinel ball cover according to claim 1, wherein: and step three, the rubber sleeve is formed by rubber injection molding for 12-24 hours, and the feeding hole is arranged at the top of the rubber sleeve.
5. The method for isostatic pressing of a spinel ball cover according to claim 1, wherein: fourthly, wrapping a plurality of layers of dust-free paper outside the mould.
6. The method for isostatic pressing of a spinel ball cover according to claim 1, wherein: the smaller pressure is 20-100Mpa, and the larger pressure is 100-250 Mpa.
7. The method for isostatic pressing of a spinel ball cover according to claim 1, wherein: step (1700 deg.c) of pressureless sintering of biscuit at 1400 deg.c; the hot isostatic pressing temperature is 1600-1800 ℃, the pressure is 150-250 Mpa, and the pressurizing medium is argon.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210696230.0A CN114773039A (en) | 2022-06-20 | 2022-06-20 | Spinel ball cover isostatic pressing forming method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210696230.0A CN114773039A (en) | 2022-06-20 | 2022-06-20 | Spinel ball cover isostatic pressing forming method |
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Citations (8)
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|---|---|---|---|---|
| JPH093636A (en) * | 1995-06-26 | 1997-01-07 | Kobe Steel Ltd | Manufacture of large sputtering target |
| JP2006282485A (en) * | 2005-04-05 | 2006-10-19 | Denki Kagaku Kogyo Kk | Method for producing boron nitride fired compact |
| CN101823286A (en) * | 2010-05-11 | 2010-09-08 | 刘先兵 | Method for molding large ceramic element through two steps by using cold isostatic pressing |
| CN104609867A (en) * | 2015-02-15 | 2015-05-13 | 上海材料研究所 | Densifying method for selective laser sintered ceramic parts |
| KR20200000020A (en) * | 2018-06-22 | 2020-01-02 | 주식회사 더파인콜 | cooking vessel having ceramics within cooking plate and composition for plate |
| CN110814338A (en) * | 2019-12-02 | 2020-02-21 | 株洲硬质合金集团有限公司 | Preparation method of large hard alloy wear-resistant block with complex shape |
| CN111499371A (en) * | 2020-04-08 | 2020-08-07 | 哈尔滨工业大学 | Preparation method of magnesia-alumina spinel transparent ceramic |
| CN114085084A (en) * | 2020-08-25 | 2022-02-25 | 西安增材制造国家研究院有限公司 | High-strength silicon nitride ceramic and preparation method thereof |
-
2022
- 2022-06-20 CN CN202210696230.0A patent/CN114773039A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH093636A (en) * | 1995-06-26 | 1997-01-07 | Kobe Steel Ltd | Manufacture of large sputtering target |
| JP2006282485A (en) * | 2005-04-05 | 2006-10-19 | Denki Kagaku Kogyo Kk | Method for producing boron nitride fired compact |
| CN101823286A (en) * | 2010-05-11 | 2010-09-08 | 刘先兵 | Method for molding large ceramic element through two steps by using cold isostatic pressing |
| CN104609867A (en) * | 2015-02-15 | 2015-05-13 | 上海材料研究所 | Densifying method for selective laser sintered ceramic parts |
| KR20200000020A (en) * | 2018-06-22 | 2020-01-02 | 주식회사 더파인콜 | cooking vessel having ceramics within cooking plate and composition for plate |
| CN110814338A (en) * | 2019-12-02 | 2020-02-21 | 株洲硬质合金集团有限公司 | Preparation method of large hard alloy wear-resistant block with complex shape |
| CN111499371A (en) * | 2020-04-08 | 2020-08-07 | 哈尔滨工业大学 | Preparation method of magnesia-alumina spinel transparent ceramic |
| CN114085084A (en) * | 2020-08-25 | 2022-02-25 | 西安增材制造国家研究院有限公司 | High-strength silicon nitride ceramic and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 中国冶金百科全书总编辑委员会《耐火材料》卷编辑委员会: "《中国模具设计大典：第4卷，锻模与粉末冶金模设计》", 哈尔滨工业大学出版社, pages: 1226 * |
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