CN106278211A - A kind of preparation method of labyrinth quartz ceramic - Google Patents

A kind of preparation method of labyrinth quartz ceramic Download PDF

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CN106278211A
CN106278211A CN201610726923.4A CN201610726923A CN106278211A CN 106278211 A CN106278211 A CN 106278211A CN 201610726923 A CN201610726923 A CN 201610726923A CN 106278211 A CN106278211 A CN 106278211A
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preparation
powder
quartz
vitreous silica
tissuemat
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麦浩
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Bright Cities And Towns Gaoming District Foshan City New Forms Of Energy New Material Industry Innovation Centers
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Bright Cities And Towns Gaoming District Foshan City New Forms Of Energy New Material Industry Innovation Centers
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Abstract

The invention discloses the preparation method of a kind of labyrinth quartz ceramic, including step A, high-purity vitreous silica powder is mixed；Above-mentioned high-purity vitreous silica powder is added and accounts for the lactic acid and 0.1 0.2% sodium sesquicarbonate that quartz powder materials quality is 0.35 0.42%, be uniformly mixing to obtain mixed powder；B, weigh and account for the binding agent of quartz powder materials quality 10 18% in step A, heating and melting in a water bath, then the mixed powder of preparation in step A is poured in binding agent, stir, obtain slurry；C, the slurry prepared in step B is injected in mould, utilizes the cooling system of mould that slurry carries out cooling and be allowed to cool solidification, take out molding blank；D, the molding blank in step C is heated, until Tissuemat E and vaseline in molding blank all evaporate or flows out, then furnace temperature is risen to 1,050 1250 DEG C be fired, be incubated 4 6h, furnace cooling, i.e. obtain required quartz ceramic.

Description

A kind of preparation method of labyrinth quartz ceramic
Technical field
The invention belongs to quartz-ceramics preparation field, be specifically related to the preparation side of a kind of labyrinth quartz ceramic Method.
Background technology
Quartz-ceramics refers to quartz glass or vitreous silica as raw material, through broken, molding, the series of ceramic such as burns till Goods prepared by processing technology, are also called fused quartz ceramic, ceramics quartz glass, quartz glass sintered article etc..Quartz pottery Porcelain, owing to having the advantages such as thermal coefficient of expansion good, good thermal shock stability, chemerosiveness resistent number, is widely used.But It is that, owing to quartz-ceramics viscosity is big, volatility increases also with the rising of temperature, so being difficult to generally producing glassy silicate The technique of glass goods produces large-scale complex-shaped quartz ceramic.
Current technology mostly uses the method for plaster model Slurry casting to produce quartz-ceramics based article, be somebody's turn to do Method has the disadvantage that: 1) utilize plaster model, and the face shaping of quartz ceramic is easily guaranteed that, but internal structure cannot Ensureing, once model is the most complicated or uneven, easily occurs the phenomenon such as bubble, reunion inside ceramic；2) cannot prepare The quartz ceramic that molding thickness is bigger and complex-shaped；3) raw material that granularity is bigger cannot be utilized.
Summary of the invention
In view of prior art is prepared problem present in quartz ceramic technique, the present invention changes prior art In adopt the liquid phase used water as in quartz powder materials slip, but by quartz powder materials after with the addition of auxiliary agent with the binding agent melted Mix, enhance the attachment force between its mobility and powder, good solve shape and internal structure is complex The formation problems of quartz ceramic.
The technical problem to be solved is achieved by following steps:
The preparation method of a kind of labyrinth quartz ceramic that the present invention provides, comprises the steps:
A, being mixed by high-purity vitreous silica powder, wherein particle size distribution and the shared mass fraction of vitreous silica powder is: 5-8 μm, 2-5wt%；8-21 μm, 6-8wt%；21-58 μm, 10-20wt%；58-114 μm, 35-39wt%；114-160 μm, 18-25 wt %；160-175 μm, 8-15 wt %；The addition of above-mentioned high-purity vitreous silica powder is accounted for quartz powder materials quality is 0.35-0.42% Lactic acid and 0.1-0.2% sodium sesquicarbonate, be uniformly mixing to obtain mixed powder；
B, weigh and account for the binding agent of quartz powder materials quality 10-18%, in a water bath heating and melting in step A, then by step A The mixed powder of preparation is poured in binding agent, stirs, obtains slurry；
The composition of described binding agent and mass percent be: Tissuemat E 60-75wt%, vaseline 15-25wt%, Cera Flava 5- 10wt%, Colophonium 2-5wt%；
C, by step B prepare slurry be injected in mould, utilize the cooling system of mould that slurry is carried out cooling and make it cold But solidify, take out molding blank；
D, the molding blank in step C is heated, until Tissuemat E in molding blank and vaseline all evaporates or Person is flowed out, then furnace temperature is risen to 1050-1250 DEG C is fired, and is incubated 4-6h, furnace cooling, i.e. obtains required quartz-ceramics system Product.
The strict particle size range controlling vitreous silica powder and shared mass percent in the present invention, and add appropriate breast Acid and sodium sesquicarbonate are as surfactant, and main purpose is to enable vitreous silica powder dispersed in a binder, And contribute to strengthening the mobility of slurry.Binding agent uses Tissuemat E, vaseline, Cera Flava and the mixture of Colophonium, wherein The Tissuemat E of steady quality good fluidity is as the bulk composition of binding agent, and the most preferably, Tissuemat E molecular weight is 1500-1650。
Further preferably raw material, the high-purity vitreous silica powder purity in step A is more than 99.99wt%.
Further, the high-purity vitreous silica powder in step A is additionally added to account for its mass percent be 0.5-1.0%'s Si3N4Powder body, Al2O3One in powder body, MgO powder body.The diameter of particle of described interpolation is 20-60 μm.This step is added On the one hand mineral powder can exist as sintering aid, and the above-mentioned powder body of the most appropriate interpolation can effectively suppress in sintering process In Crystallization Process, reduce quartz ceramic internal flaw.
It is further preferred that the bath temperature melting binding agent in step B is 80-95 DEG C.
It is further preferred that hot briquetting base substrate to Tissuemat E and vaseline all evaporates or flows out in step C Ambient temperature is 120-150 DEG C.Further preferred scope, in step C, hot briquetting base substrate is complete to Tissuemat E and vaseline Portion's evaporation or the ambient temperature flowed out are 135-140 DEG C.
Further, step D forms by a firing step particularly as follows: risen to 600 DEG C with 4-6 DEG C/min by room temperature, insulation After 20min, then rise to 1050-1250 DEG C with 7-10 DEG C/min, furnace cooling after insulation.
Fused quartz ceramic is affected by cristobalite crystallize, and the temperature formed by a firing is no more than 1300 DEG C.The present invention Middle first it is warming up to 600 DEG C, then by being rapidly heated to required sintering temperature, the receipts formed by a firing can be controlled to the full extent Shrinkage.Add appropriate sintering aid and contribute to improving further sintering degree and the compactness extent of note solidification forming goods.
There is advantages that
1, the preparation method of the quartz ceramic in the present invention does not use plaster model Slurry casting of the prior art Method, but use by quartz powder materials after with the addition of auxiliary agent with melt binding agent mix, then by heating Remove binding agent, the technical process being finally fired, utilize the method in the present invention enhance powdery pulp mobility and Attachment force between powder particles, the good molding solving shape and the complex quartz ceramic of internal structure is asked Topic.
2, the method by providing in the present invention can prepare the quartz ceramic designing complex structure, and makes The standby quartz ceramic outward appearance obtained is good, internal flaw is few.
Detailed description of the invention
Below by embodiment, present disclosure is conducted further description.
Embodiment 1
Step 1: powder mixes
The high-purity vitreous silica powder material purity selected is more than 99.99wt%.
Being mixed by selected vitreous silica powder, wherein particle size distribution and the shared quality of vitreous silica powder is divided Number is: 5-8 μm, 4wt%；8-21 μm, 8wt%；21-58 μm, 20wt%；58-114 μm, 39wt%；114-160 μm, 19 wt %； 160-175 μm, 10wt %；Above-mentioned high-purity vitreous silica powder is added and accounts for the lactic acid and 0.15% that quartz powder materials quality is 0.4% Sodium sesquicarbonate, is uniformly mixing to obtain mixed powder.
Step 2: prepare slurry
Carry out being mixed and made into binding agent by 75wt% Tissuemat E, 18wt% vaseline, 5wt% Cera Flava, 2wt% Colophonium, at 90 DEG C of water Heating and melting in bath, then pours in binding agent by the mixed powder in step 1, stirs, obtain slurry, wherein binding agent Quality is in step 1 the 16% of quartz powder materials quality.
The Tissuemat E molecular weight used in binding agent is 1500-1650, and Tissuemat E molecular weight is the least volatile, once Requirement can not reached more than 1650 mobility.Vaseline selected in this step the most so selects, and can try one's best Selecting the product that commercially available prod middle-molecular-weihydroxyethyl is less, mobility is more preferable.
Step 3: base, burn till
The slurry prepared in step 2 is injected in mould, utilizes the cooling system of mould that slurry is carried out cooling and be allowed to cool Solidification, takes out molding blank.
By molding blank continuous heating under the conditions of 140 DEG C, until Tissuemat E and vaseline in molding blank are whole Evaporation or flow out, then furnace temperature is risen to 1200 DEG C be fired, it is incubated 6h, furnace cooling, i.e. obtains required quartz-ceramics system Product.Form by a firing step particularly as follows: risen to 600 DEG C with 5 DEG C/min by room temperature, after insulation 20min, then rise to 10 DEG C/min 1200 DEG C, furnace cooling after insulation.
Embodiment 2
In the present embodiment, process conditions and raw material keep consistent with embodiment 1, and difference is: high-purity vitreous silica in step 1 Powder is also added with account for the Si that its mass percent is 0.6%3N4Powder body.Diameter of particle is 30 μm.
Embodiment 3
In the present embodiment, process conditions and raw material keep consistent with embodiment 1, and difference is: high-purity vitreous silica in step 1 Powder is also added with account for the Al that its mass percent is 1%2O3Powder body.Diameter of particle is 30 μm.
Embodiment 4
In the present embodiment, process conditions and raw material keep consistent with embodiment 1, and difference is: high-purity vitreous silica in step 1 Powder is also added with account for the MgO powder body that its mass percent is 1%.Diameter of particle is 30 μm.
The quartz ceramic any surface finish burnt out in embodiment 1-4 is smooth, and outward appearance, without visual defects, is cut by machinery The mode of cutting observes the situation that inside is fired, and does not also observe open defect.Quartz-ceramics compared with conventional mud cast preparation Goods, almost without defect (bubble-free is without projection) inside the ceramic in embodiment, it is adaptable to prepare the quartz of labyrinth Ceramic.
It is last it should be noted that it is only entered by above example in order to the technical scheme of the embodiment of the present invention to be described Row limits, although the embodiment of the present invention being described in detail with reference to preferred embodiment, and those of ordinary skill in the art Be to be understood that and still the technical scheme of the embodiment of the present invention can be modified or equivalent, and these amendment or etc. Also amended technical scheme can not be made the scope of embodiment of the present invention technical scheme is departed from replacement.

Claims (9)

1. the preparation method of a labyrinth quartz ceramic, it is characterised in that comprise the steps:
A, being mixed by high-purity vitreous silica powder, wherein particle size distribution and the shared mass fraction of vitreous silica powder is: 5-8 μm, 2-5wt%；8-21 μm, 6-8wt%；21-58 μm, 10-20wt%；58-114 μm, 35-39wt%；114-160 μm, 18-25 wt %；160-175 μm, 8-15 wt %；The addition of above-mentioned high-purity vitreous silica powder is accounted for quartz powder materials quality is 0.35-0.42% Lactic acid and 0.1-0.2% sodium sesquicarbonate, be uniformly mixing to obtain mixed powder；
B, weigh and account for the binding agent of quartz powder materials quality 10-18%, in a water bath heating and melting in step A, then by step A The mixed powder of preparation is poured in binding agent, stirs, obtains slurry；
The composition of described binding agent and mass percent be: Tissuemat E 60-75wt%, vaseline 15-25wt%, Cera Flava 5- 10wt%, Colophonium 2-5wt%；
C, by step B prepare slurry be injected in mould, utilize the cooling system of mould that slurry is carried out cooling and make it cold But solidify, take out molding blank；
D, the molding blank in step C is heated, until Tissuemat E in molding blank and vaseline all evaporates or Person is flowed out, then furnace temperature is risen to 1050-1250 DEG C is fired, and is incubated 4-6h, furnace cooling, i.e. obtains required quartz-ceramics system Product.
2. preparation method as claimed in claim 1, it is characterised in that: the high-purity vitreous silica powder purity in step A is more than 99.99wt%。
3. preparation method as claimed in claim 1, it is characterised in that: the high-purity vitreous silica powder in step A is additionally added Account for the Si that its mass percent is 0.5-1.0%3N4Powder body, Al2O3One in powder body, MgO powder body.
4. preparation method as claimed in claim 3, it is characterised in that: the diameter of particle of described interpolation is 20-60 μm.
5. preparation method as claimed in claim 1, it is characterised in that: in step B, Tissuemat E molecular weight is 1500-1650.
6. preparation method as claimed in claim 1, it is characterised in that: the bath temperature melting binding agent in step B is 80-95 ℃。
7. preparation method as claimed in claim 1, it is characterised in that: in step C, hot briquetting base substrate is to Tissuemat E and all The ambient temperature that intellectual circle is all evaporated or flowed out is 120-150 DEG C.
8. preparation method as claimed in claim 7, it is characterised in that: in step C, hot briquetting base substrate is to Tissuemat E and all The ambient temperature that intellectual circle is all evaporated or flowed out is 135-140 DEG C.
9. preparation method as claimed in claim 1, it is characterised in that: step D forms by a firing step particularly as follows: with 4-6 DEG C/ Min is risen to 600 DEG C by room temperature, after insulation 20min, then rises to 1050-1250 DEG C with 7-10 DEG C/min, furnace cooling after insulation.
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Cited By (5)

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CN107285753A (en) * 2017-07-06 2017-10-24 常州瞻驰光电科技股份有限公司 A kind of preparation method of low-refraction deposition material
CN110053140A (en) * 2019-05-23 2019-07-26 黄锡清 Mold insert structure is used in a kind of production of fused quartz ceramic air bearing transmission platform
CN112645721A (en) * 2020-12-23 2021-04-13 山东乐鹏新材料有限公司 Refractory material for high-temperature kiln and preparation method thereof
CN112897885A (en) * 2021-03-26 2021-06-04 江苏神汇新型陶瓷材料科技有限公司 High-purity silica glass ceramic material and preparation method thereof
CN114988856A (en) * 2022-07-01 2022-09-02 徐州协鑫太阳能材料有限公司 Composite quartz ceramic feeding cone for pulling single crystal and manufacturing method thereof

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CN103482873A (en) * 2013-09-06 2014-01-01 天津大学 Vibration slip casting method for preparing fused quartz ceramic
CN103833371A (en) * 2012-11-29 2014-06-04 洛阳中苑陶瓷科技有限公司 Method for preparing quartz ceramic crucible for casting in dentistry

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CN102515725A (en) * 2011-10-25 2012-06-27 河北联合大学 Preparation method of fused quartz ceramic material containing boron carbide and silicon nitride
CN103833371A (en) * 2012-11-29 2014-06-04 洛阳中苑陶瓷科技有限公司 Method for preparing quartz ceramic crucible for casting in dentistry
CN103482873A (en) * 2013-09-06 2014-01-01 天津大学 Vibration slip casting method for preparing fused quartz ceramic

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* Cited by examiner, † Cited by third party
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CN107285753A (en) * 2017-07-06 2017-10-24 常州瞻驰光电科技股份有限公司 A kind of preparation method of low-refraction deposition material
CN110053140A (en) * 2019-05-23 2019-07-26 黄锡清 Mold insert structure is used in a kind of production of fused quartz ceramic air bearing transmission platform
CN112645721A (en) * 2020-12-23 2021-04-13 山东乐鹏新材料有限公司 Refractory material for high-temperature kiln and preparation method thereof
CN112897885A (en) * 2021-03-26 2021-06-04 江苏神汇新型陶瓷材料科技有限公司 High-purity silica glass ceramic material and preparation method thereof
CN112897885B (en) * 2021-03-26 2022-05-10 连云港神汇硅材料科技有限公司 High-purity silica glass ceramic material and preparation method thereof
CN114988856A (en) * 2022-07-01 2022-09-02 徐州协鑫太阳能材料有限公司 Composite quartz ceramic feeding cone for pulling single crystal and manufacturing method thereof

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Application publication date: 20170104