CN106747352B - 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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CN106747352B
CN106747352B CN201611128298.XA CN201611128298A CN106747352B CN 106747352 B CN106747352 B CN 106747352B CN 201611128298 A CN201611128298 A CN 201611128298A CN 106747352 B CN106747352 B CN 106747352B
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ceramics
biscuit
ultrathin transparent
sintering
ultrathin
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CN106747352A (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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    • 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
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    • 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
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    • 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
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    • 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
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Abstract

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

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 methods of ultrathin transparent ceramics curtain coating biscuit, and it is raw to belong to thin slice ceramic product Produce technical field.
Background technique
The preparation of crystalline ceramics includes two big processing steps of biscuit of ceramics molding and sintering.Biscuit of ceramics moulding process is to pottery The transparent larger impact of porcelain finished product, briquetting pressure is big, and biscuit density height is 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 tape casting etc., dry-pressing formed to have Simple process, easy to operate, the period is short, but benefit is low, die wear is big, processing is complicated, at high cost, pressurization when pressure be distributed not Uniformly lead to Density inhomogeneity, so that phenomena such as generating cracking, layering.Injection forming can prepare complex-shaped green body, but after Dumping period phase is long complicated;Isostatic pressing pressure function and effect are good;Blank density is high, but cannot produce complex-shaped base Body.
Since the face thickness rate of superthin section crystalline ceramics is very big, above several moulding process are not suitable for preparing ultra-thin ceramic base Body, and tape casting is the drying on mould band by stream of slurry, thickness can be controlled by scraper, can prepare ultra-thin ceramic base Body, this external equipment is simple, process stabilizing, and molding is controllable, and high production efficiency is, it can be achieved that the advantages that automating.
However, will appear the problems such as serious contraction distortion after preparing ceramic green, in sintering process.Although biscuit Density is than more uniform, but ultra-thin biscuit is prevented when being sintered on plate, and meeting can not with plate contact surface in contraction process The generation frictional force avoided, along with contraction process, the ceramic surface after firing has corrugated " arching upward ".Although can lead to The modes such as regulation heating rate and temperature increasing schedule are crossed to control, but problem on deformation can not be fully solved.Common experience uses upper The mode of ballast can also hinder the free shrink process of ceramics, influence to densify.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 such that ceramic sheet is heated evenly Reach and shrink uniform purpose, is reconfigured a smooth briquette in addition to fire smooth ceramics.Patent CN 101219898A is used The method of flame-proof sphere is laid with to solve the problems, such as ceramic deformation.But the above anti-deformation mode is not suitable for thin slice crystalline ceramics, because Ceramics are very thin, easily broken, cause yield rate low, increased costs.
Summary of the invention
Aiming at the problem that thin slice biscuit of ceramics in existing sintering process deforms, the present invention designs a kind of ultrathin transparent ceramics stream Prolong the sintering anti-deformation method of biscuit, which is characterized in that pass through using the ultrathin transparent biscuit of ceramics that doctor-blade casting process is prepared After dumping, during vacuum-sintering is obtained and densified, ultrathin transparent biscuit of ceramics is fixed in the form of " sandwich " anti- Between the smooth flat tungsten plate of the two of deformation device;
The anti-deformation device includes two blocks of smooth flat tungsten plates with size, the through-hole of smooth flat four corners of tungsten plate Through there is series connection screw rod above and below interior, the series connection screw rod both ends are cased with fixture nut, the fixture nut and smooth flat tungsten plate table Tungsten spring is equipped between face;It is intracavitary and horizontal by 30 °~90 ° angles that the anti-deformation device is placed in vacuum drying oven.
Further, described two smooth flat tungsten plate spacings and ultrathin transparent biscuit of ceramics thickness are mutually all 1~3mm, the light Sliding flat tungsten board size is 1.2~2.0 times of ultrathin transparent biscuit of ceramics size.
Further, area of the ultrathin transparent biscuit of ceramics after pre-burning dumping is (50~300) mm × (50~300) Mm, with a thickness of 50 μm~2mm.
Further, the series connection screw rod and ultrathin transparent biscuit of ceramics edge keep 1~5cm.
With this come control in sintering process because green body shrink inconsistent generation face type distortion, guarantee flatness.
The invention has the benefit that
1. the present invention provides a kind of method for preparing ultrathin transparent ceramics, low for equipment requirements, at low cost, high-efficient, Thickness is controllable.Scale can be suitble to produce in enormous quantities, improve product quality degree of unification.This preparation method is very suitable to prepare 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 It during sintering shrinkage, shrinks in real time under the action of the spring, smooth flat tungsten plate and ceramic body is persistently made to keep being in close contact. At the same time, anti-deformation device has certain gradient, and ceramics can freely discharge under gravity during sintering answers Power can be kept for the problem of deforming with effective solution.
Detailed description of the invention
Fig. 1 is anti-deformation device side view;
Fig. 2 is anti-deformation device top view.
Wherein: 1, smooth flat tungsten plate;2, series connection screw rod;3, tungsten spring;4, fixture nut;5, vacuum furnace chamber;6, ultra-thin Bright biscuit of ceramics.
Specific embodiment
Below with reference to specific example, the present invention is described further, but protection model of the invention should not be limited with this It encloses.
As shown in Figures 1 and 2, a kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit, which is characterized in that adopt The ultrathin transparent biscuit of ceramics 6 being prepared with doctor-blade casting process obtains the process of densification in vacuum-sintering after dumping In, ultrathin transparent biscuit of ceramics 6 is fixed in the form of " sandwich " between two smooth flat tungsten plates 1 of anti-deformation device;It is described anti- Deformation device includes two blocks of smooth flat tungsten plates 1 with size, and running through up and down in the through-hole of smooth flat 1 four corners of tungsten plate has Series connection screw rod 2,2 both ends of series connection screw rod are cased with fixture nut 4, set between the fixture nut 4 and smooth flat 1 surface of tungsten plate There is tungsten spring 3.By synchronizing the nut 4 that is locked, make two pieces of smooth flat 1 spacing of tungsten plate and 6 thickness of ultrathin transparent biscuit of ceramics Unanimously;For the anti-deformation device horizontal by 30 °~90 ° angles, ceramics can under gravity freely during sintering Stress is discharged, can be kept for the problem of deforming with effective solution.
Embodiment one: YAG ultrathin transparent ceramics
By YAG slurry (n (Y2O3)/n(Al2O3)=3:5) it is cast, the green body area after dumping is 50mm × 300mm, thick Degree is 1mm.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 2 edge of bar keeps 3cm, 1.5 times having a size of 6 size of ultrathin transparent biscuit of ceramics of smooth flat tungsten plate 1, with a thickness of 2mm.Anti-deformation Device is horizontal by 60 °.For 24 hours, anneal 8h at 1200 DEG C for vacuum-sintering at 1850 DEG C, obtains smooth ultra-thin Bright ceramic sheet.
Embodiment two: Y2O3Ultrathin transparent ceramics
By Y2O3Slurry is cast, and the green body area after dumping is 100mm × 200mm, with a thickness of 50 μm.It will be super after dumping Thin crystalline ceramics biscuit 6 is placed on anti-deformation device, and keeps 1cm with 2 edge of screw rod of connecting on anti-deformation device, smooth flat 1.2 times having a size of 6 size of ultrathin transparent biscuit of ceramics of tungsten plate 1, with a thickness of 1mm.Anti-deformation device is horizontal by 30 °.Through 1500 DEG C of air are pre-sintered 8h again in 1700 DEG C of HIP sintering 12h, and anneal 8h at 1200 DEG C, obtain smooth surpass Thin crystalline ceramics thin slice.
Embodiment 3 three: AlN ultrathin transparent ceramics
AlN slurry is cast, the green body area after dumping is 300mm × 200mm, with a thickness of 2mm.It will be ultra-thin after dumping Crystalline ceramics biscuit 6 is placed on anti-deformation device, and keeps 5cm, smooth flat tungsten with 2 edge of screw rod of connecting on anti-deformation device 2 times having a size of 6 size of ultrathin transparent biscuit of ceramics of plate 1, with a thickness of 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 sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit, which is characterized in that prepared using doctor-blade casting process Obtained ultrathin transparent biscuit of ceramics (6) is after dumping, during vacuum-sintering is obtained and densified, by ultrathin transparent ceramics Biscuit (6) is fixed between two smooth flat tungsten plates (1) of anti-deformation device in the form of " sandwich ";
The anti-deformation device includes two pieces of smooth flat tungsten plates (1) with size, and described smooth (1) four corner of flat tungsten plate leads to Up and down through having series connection screw rod (2) in hole, series connection screw rod (2) both ends are cased with fixture nut (4), the fixture nut (4) Be equipped 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 sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit according to claim 1, which is characterized in that Two smooth flat tungsten plate (1) spacing is identical as ultrathin transparent biscuit of ceramics (6) thickness and is 1~3mm, the smooth flat tungsten plate (1) 1.2~2.0 times having a size of ultrathin transparent biscuit of ceramics (6) size.
3. a kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit according to claim 1, which is characterized in that Area of the ultrathin transparent biscuit of ceramics (6) after pre-burning dumping is (50~300) mm × (50~300) mm, with a thickness of 50 μ M~2mm.
4. a kind of sintering anti-deformation method of ultrathin transparent ceramics curtain coating biscuit according to claim 1, which is characterized in that The series connection screw rod (2) and ultrathin transparent biscuit of ceramics (6) edge keep 1~5cm.
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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
CN110411153B (en) * 2019-07-16 2023-06-16 山东工业陶瓷研究设计院有限公司 Rapid drying method for thin-wall hollow ceramic flat membrane blank
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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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

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