CN103072182A - Gellan gum gel-based ceramic gel injection molding method - Google Patents
Gellan gum gel-based ceramic gel injection molding method Download PDFInfo
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- CN103072182A CN103072182A CN201310006430XA CN201310006430A CN103072182A CN 103072182 A CN103072182 A CN 103072182A CN 201310006430X A CN201310006430X A CN 201310006430XA CN 201310006430 A CN201310006430 A CN 201310006430A CN 103072182 A CN103072182 A CN 103072182A
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Abstract
The invention discloses a gellan gum gel-based ceramic gel injection molding method, which belongs to the technical field of inorganic non-metal ceramic. The method comprises the following steps of: mixing ceramic powder, a dispersant and water to prepare ceramic slurry; defoaming under vacuum and then preserving heat in a water bath of 50-70 DEG C for 10-20 minutes; meanwhile, heating mixture of gellan gum and water to 70-80 DEG C to prepare uniform and stable aqueous solution with mass fraction of 1-5 percent; and adding the gellan gum aqueous solution and the aqueous solution containing calcium ions or magnesium ions with mass fraction of 1-10 percent into the prepared ceramic slurry and stirring for 5-10 minutes; finally preparing a ceramic blank in an imperforated mold; and sintering the ceramic blank to obtain a compact ceramic sintered body. The method provided by the invention has the advantages of economy, environmental friendliness, easiness in operation and convenience in industrial production, and the prepared compact ceramic sintered body has superior performance and wide application.
Description
Technical field
The invention belongs to inorganic non-metallic ceramic technology field, particularly a kind of ceramic gel-casting method based on the gellan gum gel.
Background technology
Ceramic by colloidal molding method has low, simple to operate, the suitable preparation complicated shape of cost ceramic part, has removed the complicated advantages such as machining steps from, therefore, and once extensive attention both domestic and external occurring being subject to.Colloidal shaping method is having unrivaled advantage aspect the ceramic component of preparation complicated shape really, and can effectively control the microstructure of material, reduces the various defectives of material internal, has improved the mechanical property of material and the reliability of use.Further improving the requirement of reliability of material, reduction manufacturing cost, minimizing operating procedure and adaptation environmental protection, and they are converted into the commercial production method that promotes the use, is the main target of from now on forming technique development.
The ceramic near-net-shape technology of gel casting forming (gelcasting) a kind of novelty that to be U.S.'s Oak Ridge National Laboratory at first invent in people such as eighties of last century M. at beginning of the nineties A. professors Janney.This technique combines traditional grouting process and polymer chemistry, the method of polymer chemistry monomer polymerization is incorporated in the moulding process of pottery neatly, the concentrate suspension of preparation low viscosity, high solid volume fraction, under the effect of catalyst and initator, make the organic monomer cross-linked polymeric in the concentrate suspension become tridimensional network, thereby make the moulding of concentrate suspension in-situ solidifying.The gel injection molding and forming technology remarkable advantage is that slurry solids content is high, and blank strength is high, is convenient to machining.Shortcoming is that drying condition is harsh, and base substrate easily ftractures, and the monomer acrylamide has harm to nerve system of human body, and the automaticity of technique is not high yet.Although people have been developed a series of non-toxic gel, its gel effect does not have acrylamide monomer effective, and industrial applications is restricted.
Summary of the invention
In order to overcome the defects of ceramic component tradition moulding process and existing gel-casting method, the present invention proposes a kind of ceramic gel-casting method based on the gellan gum gel.
Gellan gum is that a kind of molecular weight is up to 2～3 * 10
5Daltonian anion line style microbial polysaccharide.The basic structure of gellan gum molecule is a main chain, exists with two kinds of forms: high acyl gellan gum (also claiming natural gellan gum) and low-acyl gellan gum.Product on the market mainly is low-acyl gellan gum now, and high acyl gellan gum is because the limits product of its extraction process and application is fewer.Gellan gum solution after the heating forms hot reversible gel with monovalent cation (such as potassium ion or sodium ion) or when not adding ion after cooling, form heat irreversible type gel with bivalent cation (such as magnesium ion or calcium ion).Gellan gum gel-forming temperature and gel strength and ionic species and concentration are closely related.
A kind of ceramic gel-casting method based on the gellan gum gel is characterized in that the method comprises the steps:
(1) ceramic powder, dispersant are mixed with water; Described dispersant is any one in ammonium citrate, ammonium polyacrylate, TMAH and the tetraethyl ammonium hydroxide, and its quality accounts for 0.2 ~ 2% of ceramic powder quality; In the optional self-alumina of described ceramic powder, zirconia, silicon nitride, carborundum, lead zirconate titanate, boron nitride and the zirconium silicate any one;
(2) step (1) gained mixture ball milling being made solid volume fraction in 10 ~ 48 hours is 50 ~ 60% ceramic size, is preferably 55%;
(3) with the ceramic size of step (2) gained froth in vacuum 10 ~ 30 minutes at room temperature;
(4) will in 50 ~ 70 ℃ of water-baths, be incubated 10 ~ 20 minutes through the ceramic size after step (3) de-bubble;
(5) mixture with gellan gum and water is heated to 70 ~ 80 ℃, makes the aqueous solution that mass fraction is 1 ~ 5% stable homogeneous;
(6) the preparation quality mark is 1 ~ 10% the aqueous solution that contains calcium ion or magnesium ion;
Wherein, the preparation employed compound of the aqueous solution that contains calcium ion can be selected from one or more in calcium chloride, calcium nitrate and the calcium lactate; The employed compound of the aqueous solution that preparation contains magnesium ion can be selected from one or more in magnesium chloride, magnesium sulfate and the magnesium nitrate;
(7) aqueous solution with step (5) and step (6) preparation is added in the slurry of step (4) preparation, stirs 5 ~ 10 minutes;
(8) slurry that step (7) is obtained injects without punch die, and then cool to room temperature leaves standstill the demoulding after 3 ~ 10 hours, and then 80 ~ 100 ℃ of dryings namely obtained ceramic body in 24 ~ 48 hours; Wherein, described mold materials is without in mesoporous metal, plastics, rubber and the glass any one;
(9) ceramic body that step (8) is obtained can obtain fine and close ceramic sintered bodies through oversintering.Wherein, the temperature of sintering is 1000 ~ 2000 ℃.
Beneficial effect of the present invention is:
1, the ceramic component of plastic various complicated shape and size;
2, the gellan gum used of moulding is nontoxic, environmental friendliness, and consumption is few, and is simple to operate, is convenient to suitability for industrialized production;
3, this forming method only need add a small amount of organic matter, avoids the defectives such as cracking that binder removal causes, distortion.
The specific embodiment
The present invention will be further described in detail below in conjunction with specific embodiment:
Embodiment 1: the electronegative aluminium oxide ceramics slurry of gellan gum gel casting forming
220 gram aluminium oxide, 0.8 gram ammonium citrate and 45 gram water are mixed, and ball milling final vacuum de-bubble in 12 hours 30 minutes is prepared into solid volume fraction and is 55% ceramic size; Described ceramic size is positioned over 70 ℃ of water bath heat preservations 10 minutes; 0.3 gram gellan gum is added in the 10 gram water, be warming up to 70 ℃ and be prepared into the aqueous solution; To be prepared into the aqueous solution in 0.05 gram calcium chloride adding, the 1 gram water; Be added into gellan gum solution and calcium chloride solution in the ceramic size and stirred 8 minutes, in the injected plastic mould, be cooled to room temperature, the demoulding after 5 hours, 80 ℃ lower dry 48 hours, obtain ceramic sintered bodies at 1550 ℃ of lower sintering.
Embodiment 2: gellan gum gel casting forming positively charged aluminium oxide ceramics slurry
220 gram aluminium oxide, 7 gram 2mol/L hydrochloric acid solutions and 45 gram water are mixed, and ball milling final vacuum de-bubble in 24 hours 30 minutes is prepared into solid volume fraction and is 55% ceramic size; Described ceramic size is positioned over 70 ℃ of water bath heat preservations 10 minutes; 0.3 gram gellan gum is added in the 10 gram water, be warming up to 70 ℃ and be prepared into the aqueous solution; To be prepared into the aqueous solution in 0.06 gram magnesium chloride adding, the 1 gram water; Be added into gellan gum solution and calcium chloride solution in the ceramic size and stirred 5 minutes, inject stainless steel mould, be cooled to room temperature, the demoulding after 8 hours, 100 ℃ lower dry 24 hours, obtain ceramic sintered bodies at 1550 ℃ of lower sintering.
Embodiment 3: gellan gum gel casting forming zirconia ceramics slurry
220 gram zirconias, 5 gram ammonium polyacrylates and 45 gram water are mixed, and ball milling final vacuum de-bubble in 24 hours 30 minutes is prepared into solid volume fraction and is 55% ceramic size; Described ceramic size is positioned over 70 ℃ of water bath heat preservations 10 minutes; 0.4 gram gellan gum is added in the 10 gram water, be warming up to 70 ℃ and be prepared into the aqueous solution; To be prepared into the aqueous solution in 0.1 gram magnesium sulfate adding, the 1 gram water; Be added into gellan gum solution and calcium chloride solution in the ceramic size and stirred 5 minutes, inject rubber mold, be cooled to room temperature, the demoulding after 10 hours, 100 ℃ lower dry 24 hours, obtain ceramic sintered bodies at 1650 ℃ of lower sintering.
Embodiment 4: gellan gum gel casting forming silicon nitride ceramics slurry
220 gram silicon nitrides, 3 gram tetraethyl ammonium hydroxides and 45 gram water are mixed, and ball milling final vacuum de-bubble in 36 hours 30 minutes is prepared into solid volume fraction and is 55% ceramic size; Described ceramic size is positioned over 70 ℃ of water bath heat preservations 10 minutes; 0.5 gram gellan gum is added in the 10 gram water, be warming up to 70 ℃ and be prepared into the aqueous solution; To be prepared into the aqueous solution in 0.05 gram magnesium chloride adding, the 1 gram water; Be added into gellan gum solution and calcium chloride solution in the ceramic size and stirred 5 minutes, in the implantation glass mould, be cooled to room temperature, the demoulding after 10 hours, 100 ℃ lower dry 24 hours, obtain ceramic sintered bodies at 1800 ℃ of lower sintering.
Embodiment 5: gellan gum gel casting forming silicon carbide ceramics slurry
220 gram carborundum, 2.5 gram TMAHs and 45 gram water are mixed, and ball milling final vacuum de-bubble in 36 hours 30 minutes is prepared into solid volume fraction and is 55% ceramic size; Described ceramic size is positioned over 70 ℃ of water bath heat preservations 10 minutes; 0.4 gram gellan gum is added in the 10 gram water, be warming up to 70 ℃ and be prepared into the aqueous solution; To be prepared into the aqueous solution in 0.08 gram magnesium nitrate adding, the 1 gram water; Be added into gellan gum solution and calcium chloride solution in the ceramic size and stirred 5 minutes, in the injected plastic mould, be cooled to room temperature, the demoulding after 10 hours, 100 ℃ lower dry 24 hours, obtain ceramic sintered bodies at 1750 ℃ of lower sintering.
Claims (7)
1. the ceramic gel-casting method based on the gellan gum gel is characterized in that, described method comprises the steps:
(1) ceramic powder, dispersant are mixed with water; The quality of described dispersant accounts for 0.2 ~ 2% of ceramic powder quality;
(2) step (1) gained mixture ball milling being made solid volume fraction in 10 ~ 48 hours is 50 ~ 60% ceramic size;
(3) with the ceramic size of step (2) gained froth in vacuum 10 ~ 30 minutes at room temperature;
(4) will in 50 ~ 70 ℃ of water-baths, be incubated 10 ~ 20 minutes through the ceramic size after step (3) de-bubble;
(5) mixture with gellan gum and water is heated to 70 ~ 80 ℃, makes the aqueous solution that mass fraction is 1 ~ 5% stable homogeneous;
(6) the preparation quality mark is 1 ~ 10% the aqueous solution that contains calcium ion or magnesium ion;
(7) aqueous solution with step (5) and step (6) preparation is added in the slurry of step (4) preparation, stirs 5 ~ 10 minutes;
(8) slurry that step (7) is obtained injects without punch die, and then cool to room temperature leaves standstill the demoulding after 3 ~ 10 hours, and then 80 ~ 100 ℃ of dryings namely obtained ceramic body in 24 ~ 48 hours;
(9) ceramic body that step (8) is obtained namely obtains fine and close ceramic sintered bodies through oversintering.
2. the ceramic gel-casting method based on the gellan gum gel according to claim 1, it is characterized in that, the dispersant described in the step (1) is any one in ammonium citrate, ammonium polyacrylate, TMAH and the tetraethyl ammonium hydroxide.
3. the ceramic gel-casting method based on the gellan gum gel according to claim 1, it is characterized in that, the ceramic powder described in the step (1) is selected from any one in aluminium oxide, zirconia, silicon nitride, carborundum, lead zirconate titanate, boron nitride and the zirconium silicate.
4. the ceramic gel-casting method based on the gellan gum gel according to claim 1 is characterized in that, it is 55% ceramic size that step (1) gained mixture ball milling was made solid volume fraction in 10 ~ 48 hours.
5. the ceramic gel-casting method based on the gellan gum gel according to claim 1 is characterized in that, in the step (6), the employed compound of the aqueous solution that preparation contains calcium ion is selected from one or more in calcium chloride, calcium nitrate and the calcium lactate; The employed compound of the aqueous solution that preparation contains magnesium ion is selected from one or more in magnesium chloride, magnesium sulfate and the magnesium nitrate.
6. the ceramic gel-casting method based on the gellan gum gel according to claim 1 is characterized in that, in the step (8), described mold materials is without in mesoporous metal, plastics, rubber and the glass any one.
7. the ceramic gel-casting method based on the gellan gum gel according to claim 1 is characterized in that, the sintering temperature in the step (9) is 1000 ~ 2000 ℃.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242044A (en) * | 2013-05-23 | 2013-08-14 | 哈尔滨工业大学 | Gel-casting preparation method of BN/Si3N4 composite ceramics |
| CN104341158A (en) * | 2014-10-20 | 2015-02-11 | 中国科学院上海硅酸盐研究所 | Method for controlling gelcasting gelatinization and syneresis process through high-valence metal ions |
| CN105347790A (en) * | 2015-11-30 | 2016-02-24 | 东莞信柏结构陶瓷有限公司 | Zirconia ceramic bearing preparation method based on gel casting technology |
| CN105347791A (en) * | 2015-11-30 | 2016-02-24 | 东莞信柏结构陶瓷有限公司 | Zirconia ceramic artwork preparation method based on gel casting technology |
| CN105503183A (en) * | 2015-11-30 | 2016-04-20 | 东莞信柏结构陶瓷股份有限公司 | Gel-casting process-based zirconia ceramic cutter preparation method |
| 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 |
| CN106278290A (en) * | 2016-08-09 | 2017-01-04 | 武汉工程大学 | Based on low concentration agarose, the ceramic of compact gel-casting method of low-solid content slurry |
| CN108276004A (en) * | 2018-03-06 | 2018-07-13 | 济南大学 | A kind of preparation method based on guar gum gel casting forming boron nitride biscuit |
| CN109503155A (en) * | 2018-12-26 | 2019-03-22 | 宁波泰科先进陶瓷有限公司 | A kind of ceramics hair-clippers blade and preparation method |
| CN112408989A (en) * | 2019-08-20 | 2021-02-26 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride powder pretreatment and low-defect blank injection molding method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103242044A (en) * | 2013-05-23 | 2013-08-14 | 哈尔滨工业大学 | Gel-casting preparation method of BN/Si3N4 composite ceramics |
| CN104341158A (en) * | 2014-10-20 | 2015-02-11 | 中国科学院上海硅酸盐研究所 | Method for controlling gelcasting gelatinization and syneresis process through high-valence metal ions |
| CN105503183B (en) * | 2015-11-30 | 2020-11-03 | 东莞信柏结构陶瓷股份有限公司 | Preparation method of zirconia ceramic cutter based on gel casting process |
| CN105347790A (en) * | 2015-11-30 | 2016-02-24 | 东莞信柏结构陶瓷有限公司 | Zirconia ceramic bearing preparation method based on gel casting technology |
| CN105347791A (en) * | 2015-11-30 | 2016-02-24 | 东莞信柏结构陶瓷有限公司 | Zirconia ceramic artwork preparation method based on gel casting technology |
| CN105503183A (en) * | 2015-11-30 | 2016-04-20 | 东莞信柏结构陶瓷股份有限公司 | Gel-casting process-based zirconia ceramic cutter preparation method |
| 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 |
| CN106278290A (en) * | 2016-08-09 | 2017-01-04 | 武汉工程大学 | Based on low concentration agarose, the ceramic of compact gel-casting method of low-solid content slurry |
| CN106278290B (en) * | 2016-08-09 | 2019-05-03 | 武汉工程大学 | Ceramic of compact gel-casting method based on low concentration agarose, low-solid content slurry |
| CN108276004A (en) * | 2018-03-06 | 2018-07-13 | 济南大学 | A kind of preparation method based on guar gum gel casting forming boron nitride biscuit |
| CN109503155A (en) * | 2018-12-26 | 2019-03-22 | 宁波泰科先进陶瓷有限公司 | A kind of ceramics hair-clippers blade and preparation method |
| CN112408989A (en) * | 2019-08-20 | 2021-02-26 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride powder pretreatment and low-defect blank injection molding method |
| CN112408989B (en) * | 2019-08-20 | 2022-11-15 | 山东工业陶瓷研究设计院有限公司 | Silicon nitride powder pretreatment and low-defect blank injection molding method |
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