CN103922757A - Direct-coagulation injection molding method for non-oxide ceramics - Google Patents
Direct-coagulation injection molding method for non-oxide ceramics Download PDFInfo
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- CN103922757A CN103922757A CN201410130619.4A CN201410130619A CN103922757A CN 103922757 A CN103922757 A CN 103922757A CN 201410130619 A CN201410130619 A CN 201410130619A CN 103922757 A CN103922757 A CN 103922757A
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Abstract
The invention belongs to the technical field of inorganic nonmetal ceramic solidification methods and particularly relates to a direct-coagulation injection molding method for non-oxide ceramics. The method is used for realizing the direct-coagulation molding of the non-oxide ceramics through reaction between acid decomposed from esters and a dispersant in ceramic slurry. The method mainly comprises the following steps of firstly, mixing ceramic powder, a dispersant and water, and carrying out sufficient ball milling to obtain ceramic slurry; then, adding an ester curing agent into the slurry, degassing the obtained slurry, then, injecting the degassed slurry to a nonporous die, keeping the slurry in the nonporous die at the temperature of 15-70 DEG C for 15-60min, demoulding to obtain a wet ceramic blank, and drying to obtain a dry blank; next, sintering at the temperature of 1700-2100 DEG C to obtain a ceramic sinter. The method provided by the invention has the advantages of high curing speed, environment friendliness, excellent performance and the like, and is simple in operation and convenient for large-scale production.
Description
Technical field
The invention belongs to inorganic non-metallic ceramic solidification method and technology field, particularly a kind of Direct Coagulation Casting method of non-oxide ceramics.
Background technology
Direct coagulation casting (Direct Coagulation Casting, DCC) be to utilize urease or autocatalysis reaction, make the inner chemical reaction that occurs of slurry increase the salt ionic concentration (Δ I method) in slurry or regulate the pH value of slurry to iso-electric point (Δ pH method), thereby realize solidifying of ceramic size.Because the iso-electric point of pottery of the same race is not different, need to find different reaction systems and corresponding enzyme, cause regulating slurry pH value to the method for iso-electric point to be difficult to applicable all systems.In addition, the price comparison of enzyme is expensive, is difficult to realize suitability for industrialized production.And the method that increases ionic strength is to increase monovalent ion (NH4+, HCO by urease catalyzes decomposing urea
3 -) concentration realize solidifying of ceramic size, this method needs higher urea concentration just can make slurry curing, and set time very long (1～3 day), ceramic wet blank easily cracks, thereby affects ceramic performance.
The invention provides a kind of Direct Coagulation Casting method of non-oxide ceramics, the acid generating by ester-type hydrolysis and the dispersion agent in ceramic size react, and make ceramic size generation unstability and direct curing molding.The method that the present invention adopts have set time short, be applicable to the advantages such as all non-oxide ceramics systems and excellent performance, effectively solved that in Δ pH method, to find in reaction system difficulty and Δ I method set time long, the problem such as easily crack.
Summary of the invention
In order to overcome long, the shortcoming such as cost is high, universality is not strong existing direct coagulation casting method set time, the object of the present invention is to provide a kind of Direct Coagulation Casting method of non-oxide ceramics.
A Direct Coagulation Casting method for non-oxide ceramics, its concrete steps are as follows:
(1) dispersion agent, water are mixed with non-oxide ceramics powder, ball milling mixes, and obtains solid volume fraction and be 50%～55% non-oxide ceramics slurry, and wherein the quality of dispersion agent is 0.1%～2.5% of non-oxide ceramics powder quality;
(2) in non-oxide ceramics slurry, add solidifying agent, under vacuum condition, stir, to remove bubble, the addition of described solidifying agent is 1%～5% of non-oxide ceramics slurry volume;
(3) the non-oxide ceramics slurry that will process through step (2) vacuum stripping injects without punch die, at 15 ℃～70 ℃, processes 15～60 minutes, and the demoulding obtains the wet base of non-oxide ceramics, after being dried, obtains non-oxide ceramics dry body;
(4) step (3) gained non-oxide ceramics dry body is placed in to electric furnace, temperature rise rate with 5 ℃～15 ℃ of per minutes is warming up to 1700 ℃～2100 ℃, be incubated 1～3 hour, complete the Direct Coagulation Casting of non-oxide ceramics, obtain non-oxide ceramics sintered compact.
Dispersion agent described in step (1) is one or more in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide and TPAOH.
Non-oxide ceramics powder described in step (1) is one or more in silicon nitride, boron nitride, Sialon, silicon carbide, wolfram varbide and norbide.
Described in step (1), the Ball-milling Time of ball milling is 24～48 hours.
Described in step (2), solidifying agent is ester compound, and described ester compound is one or more in glyceryl diacetate, vanay, gluconic acid lactone, ethyl acetate and ethyl hexanoate.
The churning time stirring described in step (2) is 10～30 minutes.
Dry drying temperature described in step (3) is 80 ℃～100 ℃, and be 24～48 hours time of drying.
Beneficial effect of the present invention is:
(1) set time short, be applicable to all non-oxide ceramics systems;
(2) simple to operate, be convenient to suitability for industrialized production;
(3) little, any surface finish of forming ceramic base substrate internal stress, dimensional precision are high;
(4) compare with traditional Direct Coagulation Casting technique, hardener dose is few;
(5) ceramic micro-structure is even, and relative density is 95～99%, has higher mechanical property.
Embodiment
A kind of Direct Coagulation Casting method that the invention provides non-oxide ceramics, below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Glyceryl diacetate solidifies the Direct Coagulation Casting method of silicon nitride ceramics slurry:
160 grams of silicon nitride ceramics powders, 3 grams of Tetramethylammonium hydroxide and 50 grams of water are mixed, and ball milling is after 48 hours, obtains solid volume fraction and be 50% ceramic size; Add 2 grams of glyceryl diacetate fat, vacuum stirring 10 minutes, to remove bubble again; Then inject metal die, at 50 ℃ of temperature, place 20 minutes after the demoulding, at 80 ℃ of temperature dry 24 hours, then sintering obtains ceramic sintered bodies for 2 hours at 1800 ℃ of temperature.
Embodiment 2
Vanay solidifies the Direct Coagulation Casting method of silicon carbide ceramics slurry:
161 grams of Silicon Carbide Powders, 4 grams of tetraethyl ammonium hydroxides and 50 grams of water are mixed, and ball milling is after 36 hours, obtains solid volume fraction and be 50% ceramic size; Add again 4 grams of vanays, vacuum stirring 10 minutes, to remove bubble, in injected plastic mould, at 40 ℃ of temperature, place 30 minutes after the demoulding, at 80 ℃ of temperature dry 24 hours, then sintering obtains ceramic sintered bodies for 2 hours at 2000 ℃ of temperature.
Embodiment 3
Ethyl acetate is solidified the Direct Coagulation Casting method of boron carbide ceramics slurry:
125 grams of boron carbide ceramics powders, 2 grams of TPAOH and 50 grams of water are mixed, and ball milling is after 36 hours, obtains solid volume fraction and be 50% ceramic size; Add again 3 grams of ethyl acetate, vacuum stirring 10 minutes, to remove bubble, in injected plastic mould, at 60 ℃ of temperature, place 15 minutes after the demoulding, at 80 ℃ of temperature dry 24 hours, then sintering obtains ceramic sintered bodies for 2 hours at 2100 ℃ of temperature.
Embodiment 4
Gluconolactone solidifies the Direct Coagulation Casting method of boron nitride ceramics slurry:
115 grams of boron carbide powders, 2 grams of tetraethyl ammonium hydroxides and 50 grams of water are mixed, and ball milling is after 36 hours, obtains solid volume fraction and be 50% ceramic size; Add again 3 grams of Gluconolactones, vacuum stirring 10 minutes, to remove bubble, in injected plastic mould, at 25 ℃ of temperature, place 50 minutes after the demoulding, at 80 ℃ of temperature dry 24 hours, then sintering obtains ceramic sintered bodies for 2 hours at 1800 ℃ of temperature.
Embodiment 5
Ethyl hexanoate solidifies the Direct Coagulation Casting method of tungsten carbide ceramics slurry:
80 grams of tungsten carbide powders, 1 gram of tetraethyl ammonium hydroxide and 50 grams of water are mixed, and ball milling is after 36 hours, obtains solid volume fraction and be 50% ceramic size; Add again 2 acetoacetic esters of restraining oneself, vacuum stirring 10 minutes, to remove bubble, in injected plastic mould, at 70 ℃ of temperature, place 10 minutes after the demoulding, at 80 ℃ of temperature dry 24 hours, then sintering obtains ceramic sintered bodies at 1900 ℃ of temperature.
Claims (7)
1. a Direct Coagulation Casting method for non-oxide ceramics, is characterized in that, concrete steps are as follows:
(1) dispersion agent, water are mixed with non-oxide ceramics powder, ball milling mixes, and obtains solid volume fraction and be 50%～55% non-oxide ceramics slurry, and wherein the quality of dispersion agent is 0.1%～2.5% of non-oxide ceramics powder quality;
(2) in non-oxide ceramics slurry, add solidifying agent, under vacuum condition, stir, to remove bubble, the addition of described solidifying agent is 1%～5% of non-oxide ceramics slurry volume;
(3) the non-oxide ceramics slurry that will process through step (2) vacuum stripping injects without punch die, at 15 ℃～70 ℃, processes 15～60 minutes, and the demoulding obtains the wet base of non-oxide ceramics, after being dried, obtains non-oxide ceramics dry body;
(4) step (3) gained non-oxide ceramics dry body is placed in to electric furnace, temperature rise rate with 5 ℃～15 ℃ of per minutes is warming up to 1700 ℃～2100 ℃, be incubated 1～3 hour, complete the Direct Coagulation Casting of non-oxide ceramics, obtain non-oxide ceramics sintered compact.
2. the Direct Coagulation Casting method of a kind of non-oxide ceramics according to claim 1, is characterized in that: dispersion agent described in step (1) is one or more in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide and TPAOH.
3. the Direct Coagulation Casting method of a kind of non-oxide ceramics according to claim 1, is characterized in that: non-oxide ceramics powder described in step (1) is one or more in silicon nitride, boron nitride, Sialon, silicon carbide, wolfram varbide and norbide.
4. the Direct Coagulation Casting method of a kind of non-oxide ceramics according to claim 1, is characterized in that: described in step (1), the Ball-milling Time of ball milling is 24～48 hours.
5. the Direct Coagulation Casting method of a kind of non-oxide ceramics according to claim 1, it is characterized in that: described in step (2), solidifying agent is ester compound, described ester compound is one or more in glyceryl diacetate, vanay, gluconic acid lactone, ethyl acetate and ethyl hexanoate.
6. the Direct Coagulation Casting method of a kind of non-oxide ceramics according to claim 1, is characterized in that: the churning time stirring described in step (2) is 10～30 minutes.
7. the Direct Coagulation Casting method of a kind of non-oxide ceramics according to claim 1, is characterized in that: dry drying temperature described in step (3) is 80 ℃～100 ℃, and be 24～48 hours time of drying.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106079032A (en) * | 2016-06-15 | 2016-11-09 | 武汉工程大学 | A kind of based on agarose, the gel-casting method of ceramic size mixed solution |
| CN106348736A (en) * | 2016-08-24 | 2017-01-25 | 华中科技大学 | Method for rapidly curing ceramic slurry |
| CN106565248A (en) * | 2016-11-03 | 2017-04-19 | 清华大学 | Method for curing ceramic suspension through hydrolysis invalidation of dispersing agent and ceramic forming method |
| CN109574652A (en) * | 2018-11-26 | 2019-04-05 | 华中科技大学 | A kind of self-curing near net shaping method of easy removal calcium phosphate ceramic type core |
| CN110204313A (en) * | 2018-02-28 | 2019-09-06 | 清华大学 | A kind of method and shaping method of ceramics of dispersing agent crosslinking solidification ceramic suspension body in situ |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898141A (en) * | 2012-10-31 | 2013-01-30 | 中南大学 | Preparation method of high-heat-conduction aluminum nitride ceramic shaped part |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898141A (en) * | 2012-10-31 | 2013-01-30 | 中南大学 | Preparation method of high-heat-conduction aluminum nitride ceramic shaped part |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106079032A (en) * | 2016-06-15 | 2016-11-09 | 武汉工程大学 | A kind of based on agarose, the gel-casting method of ceramic size mixed solution |
| CN106348736A (en) * | 2016-08-24 | 2017-01-25 | 华中科技大学 | Method for rapidly curing ceramic slurry |
| CN106565248A (en) * | 2016-11-03 | 2017-04-19 | 清华大学 | Method for curing ceramic suspension through hydrolysis invalidation of dispersing agent and ceramic forming method |
| CN110204313A (en) * | 2018-02-28 | 2019-09-06 | 清华大学 | A kind of method and shaping method of ceramics of dispersing agent crosslinking solidification ceramic suspension body in situ |
| CN110204313B (en) * | 2018-02-28 | 2021-10-15 | 清华大学 | Method for cross-linking and in-situ solidifying ceramic suspension by using dispersing agent and ceramic forming method |
| CN109574652A (en) * | 2018-11-26 | 2019-04-05 | 华中科技大学 | A kind of self-curing near net shaping method of easy removal calcium phosphate ceramic type core |
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