CN106747352A - A kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit - Google Patents

A kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit Download PDF

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Publication number
CN106747352A
CN106747352A CN201611128298.XA CN201611128298A CN106747352A CN 106747352 A CN106747352 A CN 106747352A CN 201611128298 A CN201611128298 A CN 201611128298A CN 106747352 A CN106747352 A CN 106747352A
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biscuit
ceramics
ultrathin transparent
sintering
smooth flat
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CN106747352B (en
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张乐
李正
吴佳东
陈浩
高光珍
王聘
黄国灿
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Jiangsu Normal University
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Jiangsu Normal University
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/50Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds
    • C04B35/505Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on rare-earth compounds based on yttrium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped 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
    • C04B35/58Shaped 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
    • C04B35/581Shaped 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 aluminium nitride
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658Atmosphere during thermal treatment
    • C04B2235/6581Total pressure below 1 atmosphere, e.g. vacuum
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/661Multi-step sintering
    • C04B2235/662Annealing after sintering

Abstract

The invention discloses a kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit, it is characterized in that, the ultrathin transparent biscuit of ceramics (6) prepared using doctor-blade casting process is after dumping, during vacuum-sintering is densified, between ultrathin transparent biscuit of ceramics (6) to be fixed on two smooth flat tungsten plates (1) of anti-deformation device.Anti-deformation device is during biscuit of ceramics sintering shrinkage, shunk in real time in the presence of tungsten spring (3), smooth flat tungsten plate (1) and ultrathin transparent ceramic body (6) is persistently set to keep being in close contact and controlled with this in sintering process because the face type that base substrate shrinks inconsistent generation distorts, it is ensured that flatness.Scale production in enormous quantities, improve product quality degree of unification can be adapted to.

Description

A kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit
Technical field
The present invention relates to a kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit, belong to the life of thin slice ceramic product Produce technical field.
Background technology
The preparation of crystalline ceramics includes that biscuit of ceramics is molded and two big processing steps of sintering.Biscuit of ceramics moulding process is to pottery The transparent considerable influence of porcelain finished product, briquetting pressure is big, and biscuit density is high to be conducive to densified sintering product, and certain equipment requirement is high.Mesh Before, the moulding process of commonplace application has:Dry-pressing, injection forming, isostatic pressing and flow casting molding etc., it is dry-pressing formed to have Process is simple, easy to operate, cycle is short, but benefit is low, die wear big, processed complex, high cost, pressurization when pressure distribution not Uniformly cause Density inhomogeneity, so that producing the phenomenons such as cracking, layering.Injection forming can prepare complex-shaped base substrate, but after Dumping cycle phase complexity long;Isostatic pressing pressure action effect is good;Blank density is high, but can not produce complex-shaped base Body.
Because the face thickness rate of superthin section crystalline ceramics is very big, several moulding process of the above are not suitable for preparing ultra-thin ceramic base Body, and flow casting molding is that stream of slurry is dried in modular belt, thickness can prepare ultra-thin ceramic base by scraper control Body, this external equipment is simple, process stabilizing, and shaping is controllable, and production efficiency is high, is capable of achieving the advantages of automating.
However, the problems such as serious contraction distortion occurs after ceramic green is prepared, in sintering process.Although biscuit Density is than more uniform, but ultra-thin biscuit is when preventing from being sintered on flat board, can not with flat board contact surface in its contraction process The generation frictional force for avoiding, along with contraction process, the ceramic surface after burning till has corrugated " arching upward ".Although can lead to Cross the modes such as regulation and control heating rate and temperature increasing schedule to control, but problem on deformation cannot be fully solved.It is upper that common experience is used The mode of ballast can also hinder the free shrink process of ceramics, influence densification.In order to solve this problem, patent CN 202885562U devises a kind of load bearing board of large scale thin slice ceramics, and it is next that this load bearing board can be heated evenly ceramic sheet The uniform purpose of contraction is reached, a smooth briquetting is reconfigured in addition to fire smooth ceramics.Patent CN 101219898A are used The method of flame-proof sphere is laid to solve the problems, such as ceramic deformation.But above anti-deformation mode is not suitable for thin slice crystalline ceramics, because Ceramics are very thin, broken, cause yield rate low, and cost increases.
The content of the invention
For the problem of thin slice biscuit of ceramics deformation in existing sintering process, a kind of ultrathin transparent ceramics stream of present invention design Prolong the sintering anti-deformation method of biscuit, it is characterised in that the ultrathin transparent biscuit of ceramics prepared using doctor-blade casting process is passed through After dumping, during vacuum-sintering is densified, ultrathin transparent biscuit of ceramics is fixed in " sandwich " form anti- Between two smooth flat tungsten plates of deformation device;
The anti-deformation device includes two blocks of smooth flat tungsten plates with size, described smooth four through holes of corner of flat tungsten plate Inside up and down through there is series connection screw rod, the series connection screw rod two ends are cased with fixing nut, the fixing nut and smooth flat tungsten plate table Tungsten spring is provided between face;The anti-deformation device is placed in vacuum furnace chamber and horizontal by 30 °~90 ° angles.
Further, described two smooth flat tungsten plate spacing are mutually all 1~3mm, the light with ultrathin transparent biscuit of ceramics thickness The flat tungsten board size of cunning is 1.2~2.0 times of ultrathin transparent biscuit of ceramics size.
Further, the ultrathin transparent biscuit of ceramics is (50~300) mm × (50~300) through the area after pre-burning dumping Mm, thickness is 50 μm~2mm.
Further, the series connection screw rod keeps 1~5cm with ultrathin transparent biscuit of ceramics edge.
Controlled with this in sintering process because the face type that base substrate shrinks inconsistent generation distorts, it is ensured that flatness.
Beneficial effects of the present invention are:
1. the invention provides it is a kind of prepare ultrathin transparent ceramics method, low for equipment requirements, low cost, efficiency high, Thickness is controllable.Scale production in enormous quantities, improve product quality degree of unification can be adapted to.This preparation method is especially suitable for preparing thin Piece crystalline ceramics.
2. anti-deformation device can effectively solve the problems, such as to deform during ceramic post sintering.Anti-deformation device is in biscuit of ceramics During sintering shrinkage, shrink in real time under the action of the spring, persistently make smooth flat tungsten plate keep being in close contact with ceramic body. At the same time, anti-deformation device has certain gradient, and ceramics can freely discharge under gravity during sintering should Power, can effectively solve the problems, such as to keep deformation.
Brief description of the drawings
Fig. 1 is anti-deformation device side view;
Fig. 2 is anti-deformation device top view.
Wherein:1st, smooth flat tungsten plate;2nd, series connection screw rod;3rd, tungsten spring;4th, fixing nut;5th, vacuum furnace chamber;6th, it is ultra-thin Bright biscuit of ceramics.
Specific embodiment
With reference to instantiation, the present invention is described further, but should not limit protection model of the invention with this Enclose.
As shown in Figures 1 and 2, a kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit, it is characterised in that adopt The ultrathin transparent biscuit of ceramics 6 prepared with doctor-blade casting process, through dumping after, vacuum-sintering obtain densification process In, between ultrathin transparent biscuit of ceramics 6 is fixed on into two smooth flat tungsten plates 1 of anti-deformation device in " sandwich " form;It is described anti- Deformation device includes running through up and down in two blocks of smooth flat tungsten plates 1 with size, described smooth 1 four through holes of corner of flat tungsten plate to be had Series connection screw rod 2, series connection screw rod 2 two ends are cased with fixing nut 4, are set between the fixing nut 4 and the smooth flat surface of tungsten plate 1 There is tungsten spring 3.By the synchronous nut 4 that is locked, make two pieces of smooth flat spacing of tungsten plate 1 and the thickness of ultrathin transparent biscuit of ceramics 6 Unanimously;, horizontal by 30 °~90 ° angles, ceramics can under gravity freely during sintering for the anti-deformation device Release stress, can effectively solve the problems, such as to keep deformation.
Embodiment one:YAG ultrathin transparents ceramics
By YAG slurries (n (Y2O3)/n(Al2O3)=3:5) it is cast, the base substrate area after dumping is 50mm × 300mm, thick It is 1mm to spend.Ultrathin transparent biscuit of ceramics 6 after dumping is placed on anti-deformation device, and with the spiral shell of connecting on anti-deformation device The edge of bar 2 keeps 3cm, and the smooth flat size of tungsten plate 1 is 1.5 times of the size of ultrathin transparent biscuit of ceramics 6, and thickness is 2mm.Anti-deformation Device is horizontal by 60 °.The vacuum-sintering 24h at 1850 DEG C, anneal 8h at 1200 DEG C, obtains smooth ultra-thin Bright ceramic sheet.
Embodiment two:Y2O3Ultrathin transparent ceramics
By Y2O3Slurry is cast, and the base substrate area after dumping is 100mm × 200mm, and thickness is 50 μm.It is super after by dumping Thin crystalline ceramics biscuit 6 is placed on anti-deformation device, and keeps 1cm with the edge of screw rod 2 of connecting on anti-deformation device, smooth flat The size of tungsten plate 1 is 1.2 times of the size of ultrathin transparent biscuit of ceramics 6, and thickness is 1mm.Anti-deformation device is horizontal by 30 °.Through Again in 1700 DEG C of HIP sintering 12h, anneal 1500 DEG C of air pre-sintering 8h 8h at 1200 DEG C, obtains smooth surpassing Thin crystalline ceramics thin slice.
Embodiment 3 three:AlN ultrathin transparents ceramics
By AlN slurries curtain coating, the base substrate area after dumping is 300mm × 200mm, and thickness is 2mm.It is ultra-thin after by dumping Crystalline ceramics biscuit 6 is placed on anti-deformation device, and keeps 5cm, smooth flat tungsten with the edge of screw rod 2 of connecting on anti-deformation device The size of plate 1 is 2 times of the size of ultrathin transparent biscuit of ceramics 6, and thickness is 3mm.Anti-deformation device is horizontal by 90 °.1700 Vacuum-sintering 12h at DEG C, anneal 12h at 1400 DEG C, then polished obtains smooth crystalline ceramics thin slice.

Claims (4)

1. a kind of ultrathin transparent ceramics are cast the sintering anti-deformation method of biscuit, it is characterised in that prepared using doctor-blade casting process After the ultrathin transparent biscuit of ceramics (6) for obtaining is through dumping, during vacuum-sintering is densified, by ultrathin transparent ceramics Between biscuit (6) is fixed on two smooth flat tungsten plates (1) of anti-deformation device in " sandwich " form;
The anti-deformation device includes two pieces of smooth flat tungsten plates (1) with size, described (1) four corner of smooth flat tungsten plate it is logical Up and down through there is series connection screw rod (2) in hole, described series connection screw rod (2) two ends are cased with fixing nut (4), the fixing nut (4) Be provided with tungsten spring (3) between smooth flat tungsten plate (1) surface, the anti-deformation device be placed in vacuum furnace chamber (5) and with level Face is in 30 °~90 ° angles.
2. a kind of ultrathin transparent ceramics according to claim 1 are cast the sintering anti-deformation method of biscuit, it is characterised in that Two smooth flat tungsten plate (1) spacing is identical with ultrathin transparent biscuit of ceramics (6) thickness and be 1~3mm, the smooth flat tungsten plate (1) size is 1.2~2.0 times of ultrathin transparent biscuit of ceramics (6) size.
3. a kind of ultrathin transparent ceramics according to claim 1 are cast the sintering anti-deformation method of biscuit, it is characterised in that The ultrathin transparent biscuit of ceramics (6) is (50~300) mm × (50~300) mm through the area after pre-burning dumping, and thickness is 50 μ M~2mm.
4. a kind of ultrathin transparent ceramics according to claim 1 are cast the sintering anti-deformation method of biscuit, it is characterised in that Series connection screw rod (2) keeps 1~5cm with ultrathin transparent biscuit of ceramics (6) edge.
CN201611128298.XA 2016-12-09 2016-12-09 A kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit Active CN106747352B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473751A (en) * 2017-07-27 2017-12-15 佛山市非特新材料有限公司 A kind of preparation method of two-part sintering ceramic mold core
CN110411153A (en) * 2019-07-16 2019-11-05 山东工业陶瓷研究设计院有限公司 A kind of quickly drying method of thin wall hollow earthenware slab film green body
CN114603140A (en) * 2022-05-12 2022-06-10 西部宝德科技股份有限公司 Porous metal film sintering device and method

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CN2775845Y (en) * 2005-01-31 2006-04-26 同济大学 High temperature polarizing device for piezoelectric ceramics
CN1962106A (en) * 2006-12-15 2007-05-16 西部金属材料股份有限公司 Method for leveling tungsten plate with high straightness
CN202063841U (en) * 2011-06-02 2011-12-07 山东建筑大学 Fixture for polarizing piezoelectric ceramic wafers
CN203420013U (en) * 2013-08-12 2014-02-05 元鸿(山东)光电材料有限公司 Tungsten plate heater for sapphire crystal growth

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2775845Y (en) * 2005-01-31 2006-04-26 同济大学 High temperature polarizing device for piezoelectric ceramics
CN1962106A (en) * 2006-12-15 2007-05-16 西部金属材料股份有限公司 Method for leveling tungsten plate with high straightness
CN202063841U (en) * 2011-06-02 2011-12-07 山东建筑大学 Fixture for polarizing piezoelectric ceramic wafers
CN203420013U (en) * 2013-08-12 2014-02-05 元鸿(山东)光电材料有限公司 Tungsten plate heater for sapphire crystal growth

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473751A (en) * 2017-07-27 2017-12-15 佛山市非特新材料有限公司 A kind of preparation method of two-part sintering ceramic mold core
CN107473751B (en) * 2017-07-27 2019-10-25 佛山市非特新材料有限公司 A kind of production method of two-part sintering ceramic mold core
CN110411153A (en) * 2019-07-16 2019-11-05 山东工业陶瓷研究设计院有限公司 A kind of quickly drying method of thin wall hollow earthenware slab film green body
CN114603140A (en) * 2022-05-12 2022-06-10 西部宝德科技股份有限公司 Porous metal film sintering device and method
CN114603140B (en) * 2022-05-12 2022-08-05 西部宝德科技股份有限公司 Porous metal film sintering device and method

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