CN103342547B - Method for preparing high-density fused quartz ceramic - Google Patents
Method for preparing high-density fused quartz ceramic Download PDFInfo
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- CN103342547B CN103342547B CN201310288678.XA CN201310288678A CN103342547B CN 103342547 B CN103342547 B CN 103342547B CN 201310288678 A CN201310288678 A CN 201310288678A CN 103342547 B CN103342547 B CN 103342547B
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Abstract
The invention provides a method for preparing a high-density fused quartz ceramic, belonging to the field of ceramic materials. The method comprises the following steps of: catalyzing ethyl orthosilicate to be hydrolyzed to generate silica solution by controlling a hydrolysis condition, coating homogeneous sol on the surface of ultrasonically-dispersed fused quartz powder, controlling a coating technology to obtain the well-coated fused quartz ceramic powder, filtering, drying, levigating, and calcining to obtain the coated powder for pressing and sintering. The dense fused quartz ceramic is prepared by a pressing and sintering technology, the sintering can be promoted due to the high activity of the silica solution in the process of sintering, and the density can be improved. The density of the prepared fused quartz ceramic is more than 98%, the room-temperature bending strength is more than 60MPa, and the phenomenon of devitrification can be avoided. The method provided by the invention is simple in technology and low in energy consumption, raw materials are easy to obtain and low in cost, and the method can be used for preparing the high-performance fused quartz ceramic.
Description
Technical field
The present invention relates to powder metallurgical technology, belong to the category of stupalith.Provide especially a kind of homogeneity colloidal sol that utilizes to carry out powder surface modification, then through calcining, compacting sintering technique, prepared the method for high-compactness fused quartz ceramic.
Technical background
Fused quartz ceramic is owing to there being excellent thermal shock resistance, and low thermal conductivity and the low a series of premium propertiess such as thermal expansivity, obtain applying more and more widely in a plurality of fields such as metallurgy, glass, chemical industry, space flight.All dropping into larger strength both at home and abroad studies fused quartz ceramic.
A series of excellent properties such as fused quartz ceramic has Heat stability is good, thermal expansivity is little, specific inductivity is low, acid-alkali-corrosive-resisting is good, electrical insulating property is good, cost is low, therefore since coming out, under refractory materials and moderate temperature, resist rapidly in the fierce structural material applications changing of temperature and obtained popularization, its Application Areas just progressively expands, having related to the industrial circles such as spaceship, rocket, guided missile, radar, nuclear power, electronics, iron and steel, coking, non-ferrous metal, glass, is a kind of up-and-coming stupalith.
Quartz-ceramics goods have good thermal performance characteristics, and in glass production, quartz-ceramics is widely used as Quartz Ceramic Roller, ceramic orifice plate and collet, ceramic ingate cup, air guide nozzle, agitator and ceramic plunger etc.The furnace bottom roll that is used as fused silica nozzle and sheet metal strip continuous annealing furnace at metallurgy industry, in U.S.'s essence casting industry, the use of fused quartz is only second to aluminium-silicon based material, considerably beyond other refractory materialss such as zircons.
In aerospace industry, quartz-ceramics is used as ceramic radome, and it can meet the requirement that radar wave is little through loss and distortion is little, has met again the requirement of the aspects such as guided missile aerodynamic configuration, resistance to Aerodynamic Heating and structural strength.In addition, quartz-ceramics can be used as the lagging material of aerospacecraft, also can be used for the positions such as nozzle, head and cup of rocket engine simultaneously.In sun power industry, quartz-ceramics is used as crucible, is the key part of solar energy polycrystalline silicon ingot furnace, for the production and preparation of polysilicon.
Although quartz-ceramics has above-mentioned good characteristic, but compare with other structural ceramicss, its intensity is obviously on the low side, this is mainly because the temperature of the main raw material fused quartz generation cristobalite crystallization of production fused quartz ceramic is lower, conventionally the firing temperature of fused quartz ceramic need to be controlled at below 1200 ℃, and this temperature is very unfavorable to the sintering of material.In order to improve the low-temperature sintering performance of quartz-ceramics, prepare fine and close fused silica ceramic material, conventionally adding sintering aid is a kind of effective means, sintering aid (H is found in research
3bO
3, H
3pO
4, Si
3n
4, Y
2o
3) can promote within the specific limits the sintering of fused quartz ceramic, but when adding sintering agent, also promoted the crystallization of fused quartz, and with the increase of sintering agent content, crystallization is more serious, and the thermal expansivity of admixture cannot mate with fused quartz, can cause the thermostability of material to decline to some extent, in use occur destroying.So, how to solve the crystallization of fused quartz ceramic and the contradiction between densification sintering, make at a lower temperature quartz-ceramics fine and close, prevent that sintering process generation crystallization from seeming particularly important simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of energy to obtain the method with high-compactness, high purity, high-intensity fused quartz ceramic, solve the crystallization of fused quartz ceramic and the contradiction between densification sintering.
The technical solution adopted in the present invention is: adopt teos hydrolysis to produce silicon sol, at ultrasonic scattered fused quartz powder surface, carry out the coated of homogeneity colloidal sol, by controlling cladding process, obtain coated good fused quartz ceramic powder, after filtration, dry, levigate and calcining after obtain the cladded type powder for compacting sintering, adopt compacting sintering technique to prepare fine and close fused quartz ceramic, in sintering process, utilize the high reactivity of silicon sol to carry out acceleration of sintering, improve density.Avoid the introducing of impurity simultaneously, can not promote crystallization to change.
A method of preparing high-compactness fused quartz ceramic, comprises following processing step:
1, the preparation of cladded type fused quartz powder
Take Virahol as cosolvent, under machine,massing effect, hydrochloric acid catalysis tetraethoxy (TEOS) hydrolysis with 0.01mol/L～0.1mol/L, tetraethoxy add-on is 20%～40% of reaction system total volume fraction, water silicon is than (mol ratio of water and TEOS) R (n (H2O): n (TEOS))=5～35,40～80 ℃ of heating of water-bath, after reaction 2～6h, generate silicon sol, then by insert continuation stirring 2～6h in beaker through the ultrasonic fused quartz powder of having dispersed, complete coated; Experiment end is washed, filters, is dried sample and be levigate;
2, calcining
Described surface-coated powder is placed in to calcining furnace, and calcining temperature is 600～700 ℃, and calcination time is 1～2h, obtains surface for the cladding powder of compacting sintering;
3, densification
Adopt mold pressing or isostatic cool pressing, mold pressing pressing pressure is 200～400MPa, and the dwell time is 5～30s; Isostatic cool pressing pressure is 150～300MPa, and the dwell time is 30～90min; The employing electric furnace sintering that is rapidly heated, sintering temperature is 1100～1250 ℃, and soaking time is 1～4h, and low thermophase burns slowly, middle temperature insulation binder removal, hot stage burns rapid cooling soon.
Adopt above technical scheme, the invention has the advantages that:
1, abundant raw material is easy to get, with low cost, and technique is simple;
2, the coated of homogeneity colloidal sol both can be improved ceramic dense degree, can not introduce again and cause material crystallization " impurity ", kept the excellent properties of fused quartz ceramic;
3, under lower sintering temperature, can obtain relative density and reach more than 98% quartz-ceramics goods, room temperature bending strength is greater than 60MPa, and crystallization does not occur.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that the present invention prepares high-compactness fused quartz ceramic.
Fig. 2 is the coated front SEM photo of fused quartz powder.
Fig. 3 is the SEM photo after fused quartz powder is coated
Specific embodiments
Embodiment 1:
1, the preparation of cladded type fused quartz powder
Take Virahol as cosolvent, under machine,massing effect, use the teos hydrolysis of the hydrochloric acid catalysis 5ml of 0.02mol/L, 45 ℃ of heating of water-bath, after reaction 3h, generate silicon sol, then by insert continuation stirring 4h in beaker through ultrasonic scattered fused quartz powder, complete coated; Experiment end is washed, filters, is dried sample and be levigate;
2, calcining
Described surface-coated powder is placed in to calcining furnace, and calcining temperature is 600 ℃, and calcination time is 2h, obtains surface for the cladding powder of compacting sintering;
3, densification
Described homogeneity Sol-gel Coated fused quartz powder is adopted to compacting sintering technique, obtain high-compactness fused silica ceramic material.
1) compacting: adopt die forming, mold pressing pressing pressure is 200MPa, and the dwell time is 15s;
2) sintering: adopt the electric furnace sintering that is rapidly heated, sintering temperature is 1150 ℃, and soaking time is 2h, and low thermophase burns slowly, middle temperature insulation binder removal, hot stage burns rapid cooling soon.
Embodiment 2:
1, the preparation of cladded type fused quartz powder
Take Virahol as cosolvent, under machine,massing effect, with the teos hydrolysis of 0.03mol/L hydrochloric acid catalysis 10ml, 60 ℃ of heating of water-bath, after reaction 4h, generate silicon sol, then by insert continuation stirring 4h in beaker through ultrasonic scattered fused quartz powder, complete coated; Experiment end is washed, filters, is dried sample and be levigate;
2, calcining
Described surface-coated powder is placed in to calcining furnace, and calcining temperature is 650 ℃, and calcination time is 2h, obtains surface for the cladding powder of compacting sintering;
3, densification
Described homogeneity Sol-gel Coated fused quartz powder is adopted to compacting sintering technique, obtain high-compactness fused silica ceramic material.
1) compacting: adopt cold isostatic compaction, pressing pressure 200MPa, the dwell time is 60min;
2) sintering: adopt the electric furnace sintering that is rapidly heated, sintering temperature is 1200 ℃, and soaking time is 2.5h, and low thermophase burns slowly, middle temperature insulation binder removal, hot stage burns rapid cooling soon.
Embodiment 3:
1, the preparation of cladded type fused quartz powder
Take Virahol as cosolvent, under machine,massing effect, teos hydrolysis with the hydrochloric acid catalysis 15ml of 0.03mol/L, 70 ℃ of heating of water-bath, after reaction for some time 4h, generate silicon sol, then by insert continuation stirring 5h in beaker through ultrasonic scattered fused quartz powder, complete coated; Experiment end is washed, filters, is dried sample and be levigate;
2, calcining
Described surface-coated powder is placed in to calcining furnace, and calcining temperature is 700 ℃, and calcination time is 2h, obtains surface for the cladding powder of compacting sintering;
3, densification
Described homogeneity Sol-gel Coated fused quartz powder is adopted to compacting sintering technique, obtain high-compactness fused silica ceramic material.
1) compacting: adopt die forming, mold pressing pressing pressure is 300MPa, and the dwell time is 30s;
2) sintering: adopt the electric furnace sintering that is rapidly heated, sintering temperature is 1250 ℃, and soaking time is 2h, and low thermophase burns slowly, middle temperature insulation binder removal, hot stage burns rapid cooling soon.
Claims (1)
1. a method of preparing high-compactness fused quartz ceramic, is characterized in that: comprise following processing step:
1) preparation of homogeneity Sol-gel Coated fused quartz powder: take Virahol as cosolvent, under machine,massing effect, with hydrochloric acid catalysis tetraethoxy (TEOS), be hydrolyzed, heating in water bath, reaction generates silicon sol, then by inserting through ultrasonic scattered fused quartz powder in silicon sol, continue to have stirred cladding process, stirrer rotating speed is controlled at 1000rad/min～3000rad/min; After being covered to complete to sample wash, filter, dry and levigate, obtain cladding powder;
2) calcining: described surface-coated powder is placed in to calcining furnace, and calcining temperature is 600～700 ℃, and calcination time is 2～3h, obtains the cladding powder after calcining;
3) densification: the cladding powder after calcining is adopted to compacting sintering technique, obtain high-compactness fused silica ceramic material;
Step 1 wherein) described cladding process is:
The concentration of used catalyst hydrochloric acid is 0.01mol/L～0.1mol/L, and tetraethoxy add-on is 20%～40% of reaction system total volume fraction, and water silicon is than (mol ratio of water and TEOS) R (n (H
2o): n (TEOS))=5～35,40 ℃～80 ℃ of bath temperatures;
Step 3) described compacting sintering technique is:
1) compacting: adopt mold pressing or isostatic cool pressing, mold pressing pressing pressure is 200MPa～400MPa, and the dwell time is 5～30s; Isostatic cool pressing pressure is 150～300MPa, dwell time 30～90min;
2) sintering: adopt the electric furnace sintering that is rapidly heated, sintering temperature is 1100～1250 ℃, and soaking time is 1～4h, and low thermophase burns slowly, middle temperature insulation binder removal, hot stage burns rapid cooling soon.
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| CN108101573A (en) * | 2017-12-27 | 2018-06-01 | 清远先导材料有限公司 | Quartzy filter and preparation method thereof |
| CN108164137B (en) * | 2018-01-02 | 2021-04-20 | 江西嘉捷信达新材料科技有限公司 | Method for preparing high-density fused quartz material by using Grignard reagent |
| CN108892367A (en) * | 2018-07-20 | 2018-11-27 | 西南交通大学 | A kind of SiO2The isostatic cool pressing sintering knot preparation method of glass |
| CN112266237A (en) * | 2020-11-04 | 2021-01-26 | 浙江玉釉新材料科技有限公司 | Water-based inorganic nano-polymer luminous ceramic material and preparation method thereof |
| CN112321326A (en) * | 2020-11-10 | 2021-02-05 | 镇江润驰新材料科技有限公司 | Method for modifying surface of quartz ceramic |
| CN113896516B (en) * | 2021-11-08 | 2022-07-29 | 连云港太阳光石英陶瓷有限公司 | Preparation method of quartz ceramic roller |
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| CN102807312A (en) * | 2011-05-30 | 2012-12-05 | 比亚迪股份有限公司 | Crucible preparation method and crucible |
| CN103130405A (en) * | 2013-03-15 | 2013-06-05 | 连云港利思特电子材料有限公司 | Preparation method of precision casting fused quartz powder and quartz powder produced by same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102807312A (en) * | 2011-05-30 | 2012-12-05 | 比亚迪股份有限公司 | Crucible preparation method and crucible |
| CN103130405A (en) * | 2013-03-15 | 2013-06-05 | 连云港利思特电子材料有限公司 | Preparation method of precision casting fused quartz powder and quartz powder produced by same |
Non-Patent Citations (2)
| Title |
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| 3 种共溶剂对正硅酸乙酯水解的影响;霍玉秋 等;《东北大学学报(自然科学版)》;20040229;第25卷(第2期);摘要、1.2正硅酸乙酯水解溶胶-凝胶过程、图2 * |
| 霍玉秋 等.3 种共溶剂对正硅酸乙酯水解的影响.《东北大学学报(自然科学版)》.2004,第25卷(第2期),摘要、1.2正硅酸乙酯水解溶胶-凝胶过程、图2. * |
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