CN106747377B - A kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite - Google Patents

A kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite Download PDF

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CN106747377B
CN106747377B CN201710089846.0A CN201710089846A CN106747377B CN 106747377 B CN106747377 B CN 106747377B CN 201710089846 A CN201710089846 A CN 201710089846A CN 106747377 B CN106747377 B CN 106747377B
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fabric
silicon dioxide
electrophoretic deposition
dioxide gel
composite
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CN106747377A (en
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曹原
张中华
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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
    • C04B35/14Shaped 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 silica
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    • 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
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/82Asbestos; Glass; Fused silica
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    • 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
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    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

A kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite, comprises the following steps:(1)By silica fibrage, the integral fabric of designated shape is formed, and the size on the fabric fibre surface is removed and dried;(2)In insulating vessel, quartz textile is placed between positive pole and negative pole, and is connected with dc source;(3)Silicon dioxide gel is injected in insulating vessel, colloidal sol is flooded electrode and fabric completely;(4)Dc source is opened, adjusts voltage, silica electrophoretic deposition is carried out to fabric, and clear liquid is extracted according to component size and supplements colloidal sol;(5)Fabric after electrophoretic deposition is taken out into drying, sintering, forms quartz fibre enhancing quartz-ceramics composite.The present invention has advantage simple to operate, reliable, the cycle is short, cost is low;The compactness and uniformity of material can be improved using the present invention.

Description

A kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite
Technical field
The present invention relates to a kind of method for preparing quartzy composite, and in particular to a kind of electrophoretic deposition silicon dioxide gel The method for preparing quartzy composite.
Background technology
Quartz fibre strengthens quartzy composite, and there is high temperature resistant, high intensity, high tenacity, low dielectric, low-loss, low-heat to lead The features such as, available for the wave transparent window material such as spaceship, or the high temperature wave transparent window material used in industrial equipment, it can support Drive more than 1000 DEG C of high temperature and there is the characteristic through electromagnetic wave.
The material preparation method is generally impregnating sol gel-sintering process, i.e., silicon dioxide gel is used into Vaccum Permeating Stain impregnates gelation and sintering after gel drying, finally gives dense composite repeatedly into quartz textile. Some existing patents of this traditional preparation method are reported with paper, such as a kind of " high wave transparent cell quartz/quartz at Chen Zhao peaks Ceramic matric composite and preparation method thereof "(CN103724037A), Cheng Zhiqiang " fibre-quartz ceramic-base composite material Enhancement Method "(CN101591192), Zhai Ping " quartz fibre strengthens the densifying method of quartz-ceramics composite " (CN104909791A), Jia Guangyao etc. " development of three-direction quartz fiber reinforced quartz composite "(《Silicate is circulated a notice of》2002,21 (1):3-6) Deng.
Because the solids content of silicon dioxide gel is generally 25% or so, and pickling efficiency is than relatively low, therefore using tradition The method for impregnating gel sintering repeatedly generally require the dipping of more than ten or even tens times, due to dipping, gelation, drying and burning Knot often, makes the long preparation period of material and cost is high, greatly limit its extensive use.
Electrophoretic deposition, for example " pulsed hydrothermal electrophoresis sedimentation prepares carbon/carbon composite material mullite external coating to yellow sword cutting edge of a knife or a sword Method "(CN101885623A), Wang Hong " preparation method based on electrophoretic deposition nano-polymer composite material " (CN102181912A), Gao Junguo " method that a kind of electrophoresis-electrolysis composite electrodeposition prepares ceramic composite coating " (CN102776549A), Huang Jianfeng " a kind of method of preparing yttrium silicate coat by cathode rotation hydrothermal electrophoretic deposition " (CN101514473), Mei Hui " a kind of preparation method of electrophoretic deposition CNTs enhancings ceramic matric composite " (CN104150939A), Guo Lingjun " preparation method of electrophoretic deposition nano wire Strengthening and Toughening SiC antioxidant coatings " (CN104591798A), Li Hejun " a kind of method that dielectrophoresis technology prepares CNT/carbon/carbon compound material " (CN103451708A), " microwave hydrothermal electrophoresis arc discharge deposition prepares carbon/carbon compound material C-AlPO4 external coatings to Cao Liyun Method "(CN102674885A), Dai Changsong is " a kind of to put forward high calcium and phosphorus-chitosan electrophoretic deposition uniformity in foam metal Method "(CN102560604A), the Yao Xuming " sides of acidifying auxiliary electrophoretic deposition initiated oxidation graphene deposition modified carbon fiber Method "(CN105696312A)Deng, but at present do not have also on electrophoretic deposition prepare quartz fibre enhancing quartz-ceramics answer The report of condensation material.
The content of the invention
The technical problem to be solved by the invention is to provide one kind can shorten manufacturing cycle, reduce the electrophoresis of manufacturing cost The method that deposition silicon dioxide gel prepares quartzy composite.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite, comprises the following steps:
(1)By silica fibrage, the integral fabric of designated shape is formed, and the size on the fabric fibre surface is gone Remove and dry;
(2)In insulating vessel, quartz textile is placed between positive pole and negative pole, and is connected with dc source;
(3)Silicon dioxide gel is injected in insulating vessel, colloidal sol is flooded electrode and fabric completely;
(4)Dc source is opened, adjusts voltage, silica electrophoretic deposition is carried out to fabric, and take out according to component size Take clear liquid and supplement colloidal sol;
(5)Fabric after electrophoretic deposition is taken out into drying, sintering, forms quartz fibre enhancing quartz-ceramics composite.
Further, step(1)In, the quartz fibre is that diameter is less than 10 microns, purity >=99.95wt% high-purity stone English fiber.Filament strength is generally higher than 1.5GPa, and fiber surface is typically with the presence of size.
Further, step(1)In, the thickness of the fabric is between 5.0-20mm.
Further, step(2)In, described positive pole, the material of negative pole are graphite material, and thickness is between 3-30mm.Just Pole, the size of negative pole and fabric are in the same size, the same fabric of shape.
Further, step(2)In, the relative position between described fabric, positive pole, negative pole three is in positive pole for fabric Between negative pole, and three is in upper-lower position.Graphite electrode is with fabric distance between 0-800mm, preferred distance 100mm.
Further, step(3)In, inject silicon dioxide gel by the way of vacuum injection silicon dioxide gel.
Further, step(4)In, described direct current power source voltage is between 0.01-20 volts, preferably 4-5 volts.
Further, step(5)In, described drying temperature is between 30-300 DEG C, preferably 100 DEG C, is dried to and not weightless is Only.
Further, step(5)In, described sintering temperature is between 500-1200 DEG C, preferably 1000 DEG C, sinters 2-9 hours.
There is composite obtained by the present invention high temperature resistant, high intensity, high tenacity, low dielectric, low-loss, low-heat to lead Characteristic, composite density are generally higher than 1.6g/cm3, bending strength is not less than 30MPa, has machinability.
The present invention makes sol particle orientated deposition gradually form densification into fabric in the presence of positive and negative electrode Gelation complex, then through high temperature sintering obtain quartz fibre enhancing quartz-ceramics composite.This method is in dipping, gel Change, sinter these three key links and only need once.
Compared with conventional method, the present invention has advantage simple to operate, reliable, the cycle is short, cost is low.In addition, utilize The present invention can improve the compactness and uniformity of material.
Embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
A kind of electrophoretic deposition silicon dioxide gel prepares the method for quartz fibre enhancing quartz-ceramics composite material flat plate, bag Include following steps:
(1)Quartz glass fibre using purity as 99.95wt%, use three-dimensional orthogonal weaving manner be prepared into size for 200*200*10mm fabric;Fiber surface size is removed using the method for calcination;
(2)In the square insulating container that size is 300*300*80mm, it is sequentially placed into and the same chi of fabric in vertical direction Very little graphite positive pole, quartz textile, graphite cathode, and be connected with dc source;
(3)Vacuum injection mass concentration is 25% silicon dioxide gel in a reservoir;
(4)Dc source is opened, adjustment voltage is 5 volts, and silica electrophoretic deposition is carried out to fabric, when discovery container After upper strata colloidal sol becomes clarification, clarification part is extracted out, then supplement the silicon dioxide gel of equivalent;
(5)After 10 hours, the fabric after electrophoretic deposition is taken out, dried 5 hours at 150 DEG C, then at 1000 DEG C Sintering 6 hours, form quartz fibre enhancing quartz-ceramics composite.
The density of the material is 1.68g/cm3, bending strength 89MPa.
Embodiment 2
A kind of electrophoretic deposition silicon dioxide gel prepares hemispheric quartz fibre enhancing quartz-ceramics composite element Method, comprise the following steps:
(1)Quartz glass fibre using purity as 99.95wt%, diameter is prepared into using the weaving manner of three-dimensional four-way 200mm thickness is 15mm hemispherical fabric;Fiber surface size is removed using the method for calcination;
(2)In a diameter of 300mm, depth is in 400mm drum insulating vessel, is sequentially placed into and fabric in vertical direction Profiling and graphite positive pole, quartz textile, the plate shaped graphite cathode of no-float, and be connected with dc source;
(3)Vacuum injection mass concentration is 27% silicon dioxide gel in a reservoir;
(4)Dc source is opened, adjustment voltage is 4 volts, and silica electrophoretic deposition is carried out to fabric, when discovery container After upper strata colloidal sol becomes clarification, clarification part is extracted out, then supplement the silicon dioxide gel of equivalent;
(5)After 20 hours, the fabric after electrophoretic deposition is taken out, dried 5 hours at 150 DEG C, after deviating from graphite electrode, Sintered 5 hours at 1000 DEG C, form hemispheric quartz fibre enhancing quartz-ceramics composite element.
The density of the material is 1.67g/cm3, bending strength 76MPa.

Claims (9)

1. a kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite, it is characterised in that comprise the following steps:
(1)By silica fibrage, the integral fabric of designated shape is formed, and the size on the fabric fibre surface is removed simultaneously Drying;
(2)In insulating vessel, quartz textile is placed between positive pole and negative pole, and is connected with dc source;
(3)Silicon dioxide gel is injected in insulating vessel, colloidal sol is flooded electrode and fabric completely;
(4)Dc source is opened, adjusts voltage, silica electrophoretic deposition is carried out to fabric, and extract clearly according to component size Liquid simultaneously supplements colloidal sol;
(5)Fabric after electrophoretic deposition is taken out into drying, sintering, forms quartz fibre enhancing quartz-ceramics composite.
2. the method that electrophoretic deposition silicon dioxide gel according to claim 1 prepares quartzy composite, its feature exist In step(1)In, the quartz fibre is that diameter is less than 10 microns, purity >=99.95wt% high purity quartz fiber.
3. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(1)In, the thickness of the fabric is between 5.0-20mm.
4. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(2)In, described positive pole, the material of negative pole are graphite material, and thickness is between 3-30mm;Positive pole, negative pole it is big It is small in the same size with fabric, the same fabric of shape.
5. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(2)In, relative position between described fabric, positive pole, negative pole three for fabric be in positive pole and negative pole it Between, and three is in upper-lower position.
6. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(3)In, inject silicon dioxide gel by the way of vacuum injection silicon dioxide gel.
7. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(4)In, described direct current power source voltage is between 0.01-20 volts.
8. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(5)In, described drying temperature between 30-300 DEG C, be dried to it is not weightless untill.
9. the method that electrophoretic deposition silicon dioxide gel according to claim 1 or 2 prepares quartzy composite, its feature It is, step(5)In, described sintering temperature sinters 2-9 hours between 500-1200 DEG C.
CN201710089846.0A 2017-02-20 2017-02-20 A kind of method that electrophoretic deposition silicon dioxide gel prepares quartzy composite Expired - Fee Related CN106747377B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1501897A (en) * 2000-09-07 2004-06-02 �Ϻ���ͨ��ѧ Electrophoretically redensified sio2 moulded body, method for the production and use thereof
CN104446580A (en) * 2014-12-16 2015-03-25 中国人民解放军国防科学技术大学 Method for preparing continuous fiber cloth reinforced silica ceramic-based composite material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1501897A (en) * 2000-09-07 2004-06-02 �Ϻ���ͨ��ѧ Electrophoretically redensified sio2 moulded body, method for the production and use thereof
CN104446580A (en) * 2014-12-16 2015-03-25 中国人民解放军国防科学技术大学 Method for preparing continuous fiber cloth reinforced silica ceramic-based composite material

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