CN102335950A - Forming method of ceramic biscuit with impact resisting structure - Google Patents
Forming method of ceramic biscuit with impact resisting structure Download PDFInfo
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- CN102335950A CN102335950A CN2010102273170A CN201010227317A CN102335950A CN 102335950 A CN102335950 A CN 102335950A CN 2010102273170 A CN2010102273170 A CN 2010102273170A CN 201010227317 A CN201010227317 A CN 201010227317A CN 102335950 A CN102335950 A CN 102335950A
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Abstract
The invention provides a forming method of a ceramic biscuit with an impact resisting structure, mainly solving the technical problems of complex process and high cost of the traditional forming method and poorer impact resisting property or incapability of realizing massive batch production of the prepared ceramic. The forming method of the ceramic biscuit with the impact resisting structure comprises the following steps of: 2, preparing a mixed slurry: 1.1, selecting main materials; 1.2, selecting auxiliary materials, and 1.3, mixing the materials; and 2, pressurizing and discharging liquid, and demoulding to obtain the ceramic biscuit with the impact resisting structure after the liquid is discharged.
Description
Technical field
The present invention relates to a kind of forming method of biscuit, be specifically related to a kind of forming method of shock resistance structural ceramics biscuit.The present invention is mainly used in carborundum, boron carbide micro powder mixes with carbon fiber, metallic fiber, silicon carbide whisker etc., processes the biscuit that sintered ceramic is used.
Background technology
Forming of green body is a key link among the ceramic preparation technology, directly affects the quality of pottery preparation.At present, the ripe moulding process of biscuit of ceramics mainly contains dry pressing, slip casting method and extrusion molding etc.
Dry pressing is carbon source to be mixed the back adopt mechanical compaction with ceramic powder, becomes the base substrate with definite shape and intensity.The major defect of this method is: the powder of compacting generally must obtain through granulation process; Owing to reasons such as powder reunion are difficult to mix, cause the biscuit density unevenness even, intensity is lower; Can't realize that more powder mixes with the even of fiber, thereby the ceramic intensity of firing is not high.
Slip casting method is that carbon source and ceramic powder are processed slurry, is injected in the porous mold; Then, lean on the capillary force of multiple-hole die will get rid of moisture, be base substrate after the drying with definite shape and intensity.The major defect of this method is: the production cycle is long, and is particularly evident when preparing complex-shaped sample; In the process of getting rid of moisture, be easy to generate aligning of particle, cause the biscuit structure inhomogeneous, intensity is low.
Extrusion molding is to utilize pressure that compliant pug is extruded through mould, obtains the base substrate consistent with the dies cavity shape of cross section.This forming method can not prepare complex-shaped sample; The green strength of undried is low, and base substrate shrinks big, occurs defectives such as shrinkage cavity, crackle easily.
Based on above problem, occurred gel casting forming in recent years, directly solidified methods such as casting.This type technology can make slurry without dehydration, and the realization original position is solidified in no punch die, and the biscuit microstructure that it obtains is comparatively even, and is suitable for moulding complex-shaped and the large-size ceramic parts.But it still has following limitation:
Gel casting forming, though can produce the higher biscuit of intensity, it must use polymerization single polymerization monomer a large amount of, that have toxicity, contaminated environment is detrimental to health.This technology can only reduce toxicity as far as possible, but can not fundamentally solve toxicity problem.
Directly solidify casting, though pollution is lower, its demould time is long, and the production cycle is long, and the biscuit intensity that obtains is lower.
The patent No. is 200710017364.0 patent of invention, discloses a kind of preparation method of carbon/carbon/carbon-silicon carbide ceramics base composite material.This method is to adopt the fibre structure form to process directly to prepare the finished product pottery, has specifically adopted the chemical vapour infiltration method.It at first deposits one deck RESEARCH OF PYROCARBON boundary layer earlier in the prefabricated carbon fiber surface, alternating deposit RESEARCH OF PYROCARBON and SiC form (PyC/SiC) n substrates multilayer then, obtain the C/C-SiC composite.Because the whole process of production of this method all is in hot environment, to carry out, therefore, energy consumption is big, cost is high, and length consuming time, complex process, especially can't produce in batches.
Summary of the invention
The forming method of shock resistance structural ceramics biscuit provided by the invention has mainly solved existing forming method complex process, cost height, and the relatively poor technical problem that maybe can't realize large-scale mass production of the ceramic shock resistance of preparing.
Concrete technical solution of the present invention is following:
The forming method of this shock resistance structural ceramics biscuit may further comprise the steps:
(1) system mixed slurry:
(1.1) choose major ingredient:
(1.1.1) choose the major ingredient I: get enhanced carbon fiber, silicon carbide whisker, metallic fiber or alloy fiber any or any two to multiple mixing with arbitrary proportion; Wherein, The version of enhanced carbon fiber, metallic fiber or alloy fiber is long fibre, chopped strand or whisker, and the fusing point of metallic fiber and alloy fiber all is higher than 2800 ℃, all is higher than 3000 ℃ for good with fusing point; Specifically, be good with tungsten metallic fiber and tungsten alloy fiber;
(1.1.2) choose the major ingredient II: get sintered ceramic and use superfine powder; Wherein, Sintered ceramic uses superfine powder any or its two mixing with arbitrary proportion as silicon carbide super micro powder or boron carbide super fine; Sintered ceramic smaller or equal to 5 μ m, is good with particle diameter less than 1 μ m with the particle diameter of superfine powder;
(1.2) choose auxiliary material: get sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent, wherein, the proportioning of sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent is a known proportioning in the slip-casting shaping process.
(1.3) mixed slurry: with major ingredient I, major ingredient II and auxiliary material with mix with liquid mixing evenly, obtain mixed slurry; Wherein:
Mix uses liquid as water, arbitrarily concentration methyl alcohol, arbitrarily ethanol or any concentration of concentration acetone any or any two to multiple mixing with arbitrary proportion, be good with the mixed liquor of water, ethanol or water and ethanol.
Major ingredient in the mixed slurry except that mixing material and auxiliary material proportion: the shared mass percent of major ingredient I is 30～60%, and the shared mass percent of major ingredient II is 35%～68%, and the shared mass percent of auxiliary material is 1～5%;
Major ingredient and auxiliary material are 1: 0.5～3 with mixing the mass ratio that uses liquid, are good with major ingredient and auxiliary material with the mass ratio 1: 1～1.5 that mixes with liquid wherein;
(2) pressurization discharge opeing: mixed slurry is injected mould, pressurization, cavity body of mould is dwindled gradually, the liquid to mixed slurry is discharged mould, obtains thick biscuit;
Mixed slurry being injected mould, pressurization in the above step (2), specifically is earlier mixed slurry to be injected mould, pressurization more afterwards; Or marginal not is gone into mixed slurry, the limit pressurization.
In the above-described pressurization discharge opeing, specifically be to adopt odd test discharge opeing or crowded formula discharge opeing; Wherein, the pressure of odd test discharge opeing is negative pressure, pressure limit is-0.09～-0.02Mpa; The pressure that squeezes the formula discharge opeing is malleation, and pressure limit is 0.2～2Mpa.
In the above-described pressurization discharge opeing, the liquid in the mixed slurry specifically is to discharge mould through open-work on the mold wall or the sump pit on the mould inner wall; Open-work on the mold wall is ultra-fine micropore or macropore; The aperture of ultra-fine micropore is between the hydrone diameter and choose between the thing smallest particles diameter.
There was filter course the mold wall inboard when open-work on the above mold wall was macropore; Filter course adopts and to have the filtering material of ultra-fine micropore or the filtering material that molecular sieve is processed into, and the micropore size on the filter course is between the hydrone diameter and choose between the thing smallest particles diameter.。
The invention has the advantages that:
1, the forming method technology of shock resistance structural ceramics biscuit provided by the invention is simple, with short production cycle, can realize large-scale mass production; Energy-conservation; Avirulence, environmental protection.Above-mentioned all characteristics also make production cost of the present invention reduce significantly.
2, the biscuit of ceramics that adopts the present invention to prepare, have following good characteristic: biscuit density is even, and base substrate shrinks little, and intensity is high, can carry out machining; The ceramics strength of firing with this biscuit is big; Good in oxidation resistance; Anti-thermal shock; Heat endurance is good; Wear-resistant; Resistance to chemical attack.
The specific embodiment
The forming method of this shock resistance structural ceramics biscuit may further comprise the steps:
(1) system mixed slurry:
(1.1) choose major ingredient:
(1.1.1) choose the major ingredient I: get enhanced carbon fiber, silicon carbide whisker, metallic fiber or alloy fiber any or any two to multiple mixing with arbitrary proportion; Wherein, The version of enhanced carbon fiber, metallic fiber or alloy fiber is long fibre, chopped strand or whisker, and the fusing point of metallic fiber and alloy fiber all is higher than 2800 ℃, all is higher than 3000 ℃ for good with fusing point; Specifically, be good with tungsten metallic fiber and tungsten alloy fiber;
(1.1.2) choose the major ingredient II: get sintered ceramic and use superfine powder; Wherein, Sintered ceramic uses superfine powder any or its two mixing with arbitrary proportion as silicon carbide super micro powder or boron carbide super fine; Sintered ceramic smaller or equal to 5 μ m, is good with particle diameter less than 1 μ m with the particle diameter of superfine powder;
(1.2) choose auxiliary material: get sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent,
(1.3) mixed slurry: with major ingredient I, major ingredient II and auxiliary material with mix with liquid mixing evenly, obtain mixed slurry; Wherein:
Mix uses liquid as water, arbitrarily concentration methyl alcohol, arbitrarily ethanol or any concentration of concentration acetone any or any two to multiple mixing with arbitrary proportion, be good with the mixed liquor of water, ethanol or water and ethanol.
Major ingredient in the mixed slurry except that mixing material and auxiliary material proportion: the shared mass percent of major ingredient I is 30～60%, and the shared mass percent of major ingredient II is 35%～68%, and the shared mass percent of auxiliary material is 1～5%;
Major ingredient and auxiliary material are 1: 0.5～3 with mixing the mass ratio that uses liquid, are good with major ingredient and auxiliary material with the mass ratio 1: 1～1.5 that mixes with liquid wherein;
(2) pressurization discharge opeing: mixed slurry is injected mould, pressurization, can earlier mixed slurry be injected mould, afterwards pressurization again; Or marginal not goes into mixed slurry, the limit pressurization, and the liquid in the mixed slurry specifically is to discharge mould through open-work on the mold wall or the sump pit on the mould inner wall.Open-work on the mold wall is ultra-fine micropore or macropore; The aperture of ultra-fine micropore is between the hydrone diameter and choose between the thing smallest particles diameter; There was filter course the mold wall inboard when open-work on the mold wall was macropore, and filter course adopts and to have the filtering material of ultra-fine micropore or the filtering material that molecular sieve is processed into, and the micropore size on the filter course is between the hydrone diameter and choose between the thing smallest particles diameter.
The purpose of pressurization is that cavity body of mould is dwindled gradually, and the liquid to mixed slurry is discharged mould, obtains thick biscuit; Pressurization can be adopted odd test discharge opeing or crowded formula discharge opeing; Wherein, the pressure of odd test discharge opeing is negative pressure, pressure limit is-0.09～-0.02Mpa; The pressure that squeezes the formula discharge opeing is malleation, and pressure limit is 0.2～2Mpa;
Embodiment 1
(1) system mixed slurry:
(1.1) choose major ingredient:
(1.1.1) choose the major ingredient I: get chopped carbon fiber, fibre length is 1～10mm, chopped carbon fiber is carried out heat sink carbon distribution handle;
(1.1.2) choose the major ingredient II: choose sintered ceramic and use superfine powder: it is that particle diameter is the silicon carbide super micro powder less than 1 μ m that sintered ceramic uses superfine powder;
(1.2) choose auxiliary material: auxiliary material comprises sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent;
Place water to carry out ultrasonic dispersion, mix the above-mentioned thing of choosing, obtain mixed slurry; Choose the outer shared mass percent of each several part that dewaters in the thing and be respectively, weak point is cut carbon silica fibre 58%, silicon carbide super micro powder 40%, auxiliary material 2%; The mass ratio of choosing between thing and the water is 1: 1, can cause the difficulty that suspends when the water ratio is excessive, can cause mixing inhomogeneous when the water ratio is too small;
(2) pressurization discharge opeing: after the complete can of mixed slurry is to mould, the discharge opeing of pressurizeing; Mold bottom is provided with ultra-fine micropore and is convenient to liquid and discharges rapidly, and the aperture of ultra-fine micropore is greater than the hydrone diameter, less than choosing the thing diameter; Take negative pressure be-pressure of 0.09Mpa extracts liquid out; After water drained, the compression molding biscuit with the biscuit demoulding, obtained shock resistance structural ceramics biscuit after the moulding.
After the biscuit preparation is accomplished, adopt known technology that biscuit is fired, obtain the shock resistance structural ceramics, detect through test, this shock resistance structural ceramics work to break is 11.32KJm
-2, hot strength is 350.8MPa.
Embodiment 2
(1) system mixed slurry:
(1.1) choose major ingredient:
(1.1.1) choose the major ingredient I: choose carbon fiber, this carbon fiber comprises 5% long carbon fiber and 1～3mm chopped carbon fiber of 95%;
(1.1.2) choose the major ingredient II: choose sintered ceramic and use superfine powder: it is that particle diameter is the boron carbide super fine less than 0.5 μ m that sintered ceramic uses superfine powder;
(1.2) choose auxiliary material: auxiliary material comprises sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent;
Choose the outer shared mass percent of each several part that dewaters in the thing and be respectively carbon fiber 46%, boron carbide super fine 49%, auxiliary material 5%;
Place water to carry out ultrasonic dispersion, mix with superfine powder, auxiliary material chopped carbon fiber, sintered ceramic, obtain mixed slurry; The mass ratio of choosing between thing and the water is 1: 1.5, can cause the difficulty that suspends when the water ratio is excessive, can cause mixing inhomogeneous when the water ratio is too small;
(2) pressurization discharge opeing: earlier long carbon fiber is evenly distributed in the mould; Again mixed slurry is injected mould; Mold wall and mold bottom are provided with ultra-fine micropore, and through the continuous injection of mixed slurry, the mould inner pressure increase makes water discharge from ultra-fine micropore; After the injection of mixed slurry was intact, taking malleation was that the pressure of 2MPa is discharged remaining liq; After water drained, the compression molding biscuit with the biscuit demoulding, obtained shock resistance structural ceramics biscuit after the moulding.
After the biscuit preparation is accomplished, adopt known technology that biscuit is fired, obtain the shock resistance structural ceramics, detect through test, this shock resistance structural ceramics work to break is 13.32KJm
-2, hot strength is 323.2MPa.
Utilize the biscuit of the shock resistance structural ceramics that this method makes to be suitable for the ring-type biscuit.
Embodiment 3
(1) system mixed slurry:
(1.1) choose major ingredient:
(1.1.1) choose the major ingredient I: choose 1～10mm chopped carbon fiber, and in chopped carbon fiber, mix short metallic fiber or the silicon carbide whisker cut of 1～3mm;
(1.1.2) choose the major ingredient II: choose sintered ceramic and use superfine powder: it is that particle diameter is the silicon carbide super micro powder less than 5 μ m that sintered ceramic uses superfine powder;
(1.2) choose auxiliary material: choose auxiliary material: auxiliary material comprises sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent;
Place water to carry out ultrasonic dispersion, evenly mix the above-mentioned thing of choosing, obtain mixed slurry; Choose the outer shared mass percent of each several part that dewaters in the thing and be respectively fibre blend 50%, silicon carbide super micro powder 47%, auxiliary material 3%; The mass ratio of choosing between thing and the water is 1: 3;
(2) pressurization discharge opeing: after the complete can of mixed slurry is to mould, the discharge opeing of pressurizeing; Mold wall is provided with big open-work, in mould, is provided with filter course, and water is discharged through open-work after seeing through filter course, and taking malleation is that the pressure of 0.5MPa is discharged solvent; The aperture that is provided with on the filter course is greater than the hydrone diameter, less than choosing the thing diameter; After water drained, the compression molding biscuit with the biscuit demoulding, obtained shock resistance structural ceramics biscuit after the moulding.
After the biscuit preparation is accomplished, adopt known technology that biscuit is fired, obtain the shock resistance structural ceramics, detect through test, this shock resistance structural ceramics work to break is 12.77KJm
-2, hot strength is 300.2MPa.
Utilize biscuit one side of the shock resistance structural ceramics that this method makes to form metallic fibrous layer, shock resistance strengthens.
Claims (6)
1. the forming method of a shock resistance structural ceramics biscuit may further comprise the steps:
(1) system mixed slurry:
(1.1) choose major ingredient:
(1.1.1) choose the major ingredient I: get enhanced carbon fiber, silicon carbide whisker, metallic fiber or alloy fiber any or any two to multiple mixing with arbitrary proportion; Wherein, The version of enhanced carbon fiber, metallic fiber or alloy fiber is long fibre, chopped strand or whisker, and the fusing point of metallic fiber and alloy fiber all is higher than 2800 ℃;
(1.1.2) choose the major ingredient II: get sintered ceramic and use superfine powder; Wherein, Sintered ceramic uses superfine powder any or its two mixture with arbitrary proportion as silicon carbide super micro powder or boron carbide super fine, sintered ceramic with the particle diameter of superfine powder smaller or equal to 5 μ m;
(1.2) choose auxiliary material: get sintering aid, forming of green body adhesive, micro mist dispersant and suspending agent;
(1.3) mixed slurry: choose major ingredient I in the thing, major ingredient II and auxiliary material and mix with liquid mixing evenly above-mentioned, obtain mixed slurry; Wherein:
Choose in the thing, the shared mass percent of major ingredient I is 30～60%, and the shared mass percent of major ingredient II is 35%～68%, and the shared mass percent of auxiliary material is 1～5%;
Mix uses liquid as water, arbitrarily concentration methyl alcohol, arbitrarily ethanol or any concentration of concentration acetone any or any two to multiple mixing with arbitrary proportion;
Choosing thing is 1: 0.5～3 with mixing the mass ratio that uses liquid;
(2) pressurization discharge opeing: mixed slurry is injected mould, pressurization, cavity body of mould is dwindled gradually, the liquid to mixed slurry is discharged mould, obtains biscuit;
2. the forming method of shock resistance structural ceramics biscuit according to claim 1 is characterized in that: the mixed slurry in the said step (2) is injected mould, pressurization, specifically is earlier mixed slurry to be injected mould, afterwards pressurization again; Or marginal not is gone into mixed slurry, the limit pressurization.
3. the forming method of shock resistance structural ceramics biscuit according to claim 1 and 2 is characterized in that: in the described pressurization discharge opeing, specifically be to adopt odd test discharge opeing or crowded formula discharge opeing; Wherein, the pressure of odd test discharge opeing is negative pressure, pressure limit is-0.09～-0.02Mpa; The pressure that squeezes the formula discharge opeing is malleation, and pressure limit is 0.2～2Mpa.
4. the forming method of shock resistance structural ceramics biscuit according to claim 3 is characterized in that: in the described pressurization discharge opeing, the liquid in the mixed slurry specifically is to discharge mould through open-work on the mold wall or the sump pit on the mould inner wall.
5. the forming method of shock resistance structural ceramics biscuit according to claim 4 is characterized in that: the open-work on the said mold wall is ultra-fine micropore or macropore; The aperture of ultra-fine micropore is between the hydrone diameter and choose between the thing smallest particles diameter; There was filter course the mold wall inboard when open-work on the mold wall was macropore, and filter course adopts and has the filtering material of ultra-fine micropore or the filtering material that molecular sieve is processed into.Micropore size on the filter course is between the hydrone diameter and choose between the thing smallest particles diameter.
6. according to the forming method of claim 4 or 5 described shock resistance structural ceramics biscuits, it is characterized in that: said major ingredient and auxiliary material are good with the mass ratio 1: 1～1.5 that mixes with liquid; Said sintered ceramic with the particle diameter of superfine powder less than 1 μ m; Described mixing is the mixed liquor of water, ethanol or water and ethanol with liquid.
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Cited By (4)
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| CN103058698A (en) * | 2013-01-31 | 2013-04-24 | 常熟华融太阳能新型材料科技有限公司 | Shell-core-structure boron carbide/carbon fiber composite ceramic and preparation method thereof |
| CN103770195A (en) * | 2012-10-17 | 2014-05-07 | 上海久牵实业有限公司 | Fiber ceramic powder compression forming process |
| CN106458749A (en) * | 2014-05-13 | 2017-02-22 | 科里亚泰拉创新有限公司 | A mixture, a process and a mold for manufacturing recyclable and degradable articles |
| CN108610086A (en) * | 2018-06-01 | 2018-10-02 | 哈尔滨工业大学 | A kind of preparation method of three-dimensional network shape porous fibre matter heat-barrier material |
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| CN108610086B (en) * | 2018-06-01 | 2021-05-28 | 哈尔滨工业大学 | Preparation method of three-dimensional network-shaped porous fibrous heat insulation material |
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Application publication date: 20120201 |