CN100515997C - Zirconia injection molding process - Google Patents
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- CN100515997C CN100515997C CNB2007100350857A CN200710035085A CN100515997C CN 100515997 C CN100515997 C CN 100515997C CN B2007100350857 A CNB2007100350857 A CN B2007100350857A CN 200710035085 A CN200710035085 A CN 200710035085A CN 100515997 C CN100515997 C CN 100515997C
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Abstract
The present invention is zirconia injection molding process and organic carrier for zirconia powder. Zirconia powder as the main material is added with certain amount of optimized organic carrier, injection molded into biscuit, defatted and sintered to produce high performance zirconia ceramic product. The organic carrier for the zirconia powder consists of polyethylene 10-30 wt%, polypropylene 10-30 wt%, vegetable oil 5-40 wt%, oleic acid1-5 wt%, and paraffin 5-50 wt%; and the weight ratio between the zirconia powder and the organic carrier is 100 to 10-80.
Description
Technical field
The present invention relates to a kind of making method and rational degreasing process of structural ceramics, refer in particular to a kind of injection molding making method and rational degreasing process of ceramic articles based on zirconium oxide, belong to structural ceramics processing and fabricating field, be mainly used in processing and fabricating zirconium white structural ceramics goods.
Background technology
Zirconia ceramics has the beyond challenge advantages of traditional ceramics such as high rigidity, high tenacity, high-density, mechanical property excellence, is that 21st century is the most promising, one of structural ceramic material of tool economic benefit.The zirconium white structural ceramics is widely used for all conglomeraties such as space flight, communication, machinery, chemical industry.Zirconium white is a kind of changeable crystalline material, if do not take feedstock production technology stable or that partially stabilized crystal changes mutually, ceramic volumetric expansion or contraction because of crystal transition in sintering process cracked, thereby can't produce the zirconia ceramic product of high strength, high rigidity, high tenacity.
At present, domestic existing how tame institution of higher learning, institute successfully develop submicron order PSZ (PSZ) powder.Form the existing number man of enterprise of sub-micron zirconium oxide powder industrialization.Thereby on material, guaranteed the high-quality performance of zirconium white structural ceramics.
By material supply section scholar's research trial repeatedly,, adopt a kind of ceramic injection forming technology in order to improve the performance of zirconia ceramics.Ceramic injection forming technology can produce complex-shaped high degree of accuracy pottery component, and is easy to mass-producing and automatic production.The eighties in 20th century, started the upsurge of high-performance ceramics industrialization in the world.Originally forming process of ceramics injection technique is that a large amount of macromolecule resins and ceramic powder are made of mixing injection material, injection molding then.Owing to contain a large amount of high polymer binders, make the degreasing of base substrate become an impassable difficult problem, and blank be yielding, forms defectives such as pore easily, has seriously restricted its application and development.Therefore, the forming process of ceramics technology turns to the research that contains a small amount of organism forming technique gradually in recent years.And certain progress arranged in some aspects.
Chinese patent literature (number of patent application 200410029886.9, name is called " high-intensity high-tenacity zirconia-based ceramics and preparation method thereof ") discloses a kind of high-intensity high-tenacity pottery and preparation method thereof.This invention is coated on nano zircite (containing 4.37～6.04% yttrium oxide) powder surface with aluminium hydroxide, and thermal treatment is combined into Zirconia-alumina composite micro-powder (tetragonal phase zirconium oxide content accounts for the 70-90% of zirconium white total amount in the micro mist).With this composite micro-powder, acrylamide, linking agent and dispersion agent is the injection material, prepares green compact by injection molding, the pottery of this invention of preparation under normal pressure-sintered condition, and intensity is 700～1000MPa, toughness reaches 15～17MPam1/2.Another one Chinese patent literature (99123098.1, name is called " chemical extraction method for dewaxing injection-shaped ceramics ") a kind of de-waxing method of injection moulding pottery disclosed, after porcelain powder and tackiness agent cooperated by a certain percentage, obtain work in-process through heating, stirring, cooling, injection moulding, then, this invention is carried out the chemical extraction de-waxing to work in-process, be about to work in-process and put into solvent, soak for some time at a certain temperature, treat that paraffin dissolving back taking-up is dry, promptly finish the de-waxing process.
However, also there are a lot of difficult problems in existing zirconia ceramics injection molding technology.Because the powder specific surface is big, particle agglomeration is serious; Organic or the organic composite material amount of admixture is many, and base substrate void content height makes the sintering difficulty, shrinks greatly, causes product percent of pass low, the production cost height.Seriously restricted the application of zirconia ceramics.
Summary of the invention
One of purpose of the present invention is exactly the deficiency at existing zirconia ceramics injection molding technology, and a kind of new zirconia ceramics injection moulding method and degreasing process are provided, and this technology guarantees that zirconia ceramics has high rigidity, high tenacity, precision height, easily processing.Particularly by rationally selecting powder and powder organic carrier for use, implementing rational process system and make that the base substrate void content is low, sintering is easy, shrink little, thereby fundamentally improve the quality of zirconia ceramic product.
The objective of the invention is to be achieved through the following technical solutions: by the analysis revealed to zirconia ceramics, zirconia ceramics changes to oblique system by tetragonal system and reaches transformation toughening and tiny crack toughness reinforcing two big toughness reinforcing substantially principles strengthen ceramics toughness.Want to reach above-mentioned two toughness reinforcing results preferably, emphasis is the granularity that reduces Zirconium powder, the suitable distribution of strict controlled oxidation zirconium powder body particle, particle diameter scope, the stablizer quantity of foreign matter content and admixture and the classification of stablizer.Make zirconia ceramics have very high intensity and toughness, just must make the thing in the microstructure of zirconia material have the submicron order yardstick mutually, that is to say that its grain-size, second distributes mutually, defect size all is on the level of submicron order.According to the above-mentioned technical scheme that analysis proposed be: the first selects a kind of quality oxide zirconium powder body to guarantee this premium properties requirement of zirconia ceramics from material.It two is injection moulding method and powder organic carrier and the rational degreasing process that adopt a kind of zirconia ceramics: based on Zirconium oxide powder, the organic carrier that adds certain deal through optimum combination, adopt injection molding technique to make base substrate, make high performance zirconia ceramic product by rational degreasing, sintering process.Described powder organic carrier comprises: polyethylene, polypropylene, vegetables oil, oleic acid, paraffin.The proportioning of described zirconium white powder and powder organic carrier is 100: the 10-30 parts by weight.The proportioning of selecting for use of described powder organic carrier is the polyethylene 10-30% of powder organic carrier gross weight, polypropylene 10-30%, and vegetables oil 5-40%, oleic acid 1-5%, paraffin 5-50%, the powder organic carrier can assembly arbitrarily in selected scope.
Described zirconia ceramic product manufacture craft comprises:
1, close experienced step: earlier the internal mixer temperature is transferred to the 80-260 degree, the organic carrier of 10-30 weight part is added the indoor close white silk of close white silk with 2-4 stage gradation, zirconia powder with 100 weight parts adds the indoor close white silk of close white silk with 2-4 stage gradation simultaneously, the two hockets, and closes close experienced chamber after 20-30 minute.Temperature rises to the 80-260 degree, gets material after close experienced 40-80 minute.Cooling.Particle makes the injection material that granularity is not more than 5 millimeters.
2, injection molding step: will inject material and be added on hopper, and obtain molding blank by injector.Processing condition are: mould temperature 40-50 degree, penetrate temperature 110-250 degree, and penetrate pressure 50-100Mpa.
3, media defatting step: will fix base substrate and place in the porose box, and immerse in the container of the organic liquid media that fills a kind of 30-60% of containing alkane, unsaturated hydrocarbons, aromatic hydrocarbon, cyclic hydrocarbon etc., and entire container be inserted carried out degreasing in the tank again; The media degreasing comprises cold degreasing and hot degreasing, and the fs is cold degreasing, under the room temperature, and time 0-12 hour; Subordinate phase is hot degreasing, to different products, with 0.02-0.5 degree/minute different temperature rise rates, rises to the 45-60 degree from room temperature stage by stage, is incubated 1-16 hour.Used media can reclaim again and use.
4, heating defatting step: the base substrate behind the media degreaser drying is moved in the debinding furnace with 0.5-2 degree/minute rise to 160-180 degree, be incubated 1-6 hour, again with 0.5-1 degree/minute rise to 260 degree, be incubated 1-4 hour, with 0.01-3 degree/minute rise to 500 degree, be incubated 2-3 hour again, again with 1-5 degree/minute rise to 800-1000 degree, be incubated 1-3 hour, be cooled to room temperature.
5, sintering step: degreasing blank with 0.5-5 degree/minute different temperature rise rates, is warming up to sintering temperature stage by stage, is incubated 1-6 hour.Sintering range 1380-1680 degree adopts normal pressure-sintered.The stove internal cooling gets product.
The present invention adopts polyethylene, polypropylene, vegetables oil, oleic acid, paraffin as organic carrier, adopts injection molding technique to make base substrate, makes high performance zirconia ceramic product by rational degreasing, sintering process.Utilize the zirconia ceramics blank density of this Technology moulding even, intensity is high, again through sintering, can produce the high-quality ceramic component of complex structure, uniform microstructure, zero defect and near-net-shape.Low, the good uniformity of base substrate organic content of institute's moulding, sintered compact excellent performance, qualification rate height.The manufacturing cost of pottery is reduced more than 50%, and reliability is enhanced about more than once.
Embodiment
The invention will be further elaborated below in conjunction with specific embodiment.
Embodiment one
A kind of injection moulding method of zirconia ceramics and powder organic carrier, based on Zirconium oxide powder, add organic carrier according to Zirconium oxide powder and 100: 30 parts by weight of organic carrier, adopt injection molding technique to make base substrate, make high performance zirconia ceramic product by media degreasing, heating degreasing and sintering again.
Described powder organic carrier comprises: polyethylene, polypropylene, vegetables oil, oleic acid, paraffin.The proportioning of selecting for use of described powder organic carrier is the polyethylene 10% of powder organic carrier gross weight, polypropylene 30%, vegetables oil 5%, oleic acid 5%, paraffin 50%.
Described zirconia ceramic product manufacture craft comprises:
1, close experienced step: earlier the internal mixer temperature is transferred to 160 degree, with the organic carrier of 80 weight parts and the zirconia powder of 100 weight parts, with an organic carrier, once oxidation zirconium powder, the two alternative mode is divided and is added the indoor close white silk of close white silk for 4 times, closes close experienced chamber after 30 minutes.Temperature rises to 180 degree, and close white silk was got material after 80 minutes.Cooling.Particle makes the injection material that granularity is not more than 5 millimeters.
2, injection molding step: will inject material and be added on hopper, and obtain molding blank by injector.Processing condition are: mould temperature 50 degree, penetrate temperature 200 degree, and penetrate pressure 100Mpa.
3, media defatting step: will fix base substrate and place in the porose box, and immerse in the container fill a kind of organic liquid media that contains 30% alkane, unsaturated hydrocarbons, aromatic hydrocarbon, cyclic hydrocarbon etc., and entire container be inserted carried out degreasing in the tank again; Fs is cold degreasing, and under the room temperature, 12 hours time, subordinate phase is hot degreasing, from room temperature with temperature rise rate 0.5 degree/minute, rise to 60 degree, be incubated 16 hours; Used media can reclaim again and use.
4, heating defatting step: the base substrate behind the media degreaser drying is moved in the debinding furnace with 2 degree/minute rise to, 180 degree, be incubated 2 hours, again with 1 degree/minute rise to, 260 degree, be incubated 3 hours, with 3 degree/minute rise to 500 degree, be incubated 3 hours again, again with 5 degree/minute rise to 1000 to spend, be incubated 3 hours, be cooled to room temperature.
5, sintering step: degreasing blank with temperature rise rate 5 degree/minute different temperature rise rates, is warming up to sintering temperature stage by stage, is incubated 6 hours.Sintering range 1680 degree adopt normal pressure-sintered.The stove internal cooling gets product.
Embodiment two
A kind of injection moulding method of zirconia ceramics and powder organic carrier, based on Zirconium oxide powder, add organic carrier according to Zirconium oxide powder and 100: 10 parts by weight of organic carrier, adopt injection molding technique to make base substrate, make high performance zirconia ceramic product by media degreasing, heating degreasing and sintering again.
Described powder organic carrier comprises: polyethylene, polypropylene, vegetables oil, oleic acid, paraffin.The proportioning of selecting for use of described powder organic carrier is the polyethylene 30% of powder organic carrier gross weight, polypropylene 10%, vegetables oil 40%, oleic acid 1%, paraffin 19%.
Described zirconia ceramic product manufacture craft comprises:
1, close experienced step: earlier the internal mixer temperature is transferred to 80 degree, with the organic carrier of 10 weight parts and the zirconia powder of 100 weight parts, with an organic carrier, once oxidation zirconium powder, the two alternative mode is divided and is added the indoor close white silk of close white silk for 2 times, closes close experienced chamber after 30 minutes.Temperature rises to 180 degree, and close white silk was got material after 80 minutes.Cooling.Particle makes the injection material that granularity is not more than 5 millimeters.
2, injection molding step: will inject material and be added on hopper, and obtain molding blank by injector.Processing condition are: mould temperature 40 degree, penetrate temperature 140 degree, and penetrate pressure 50Mpa.
3, media defatting step: will fix base substrate and place in the porose box, immersion fills in a kind of container of the organic liquid media that contains 60% alkane, unsaturated hydrocarbons, aromatic hydrocarbon, cyclic hydrocarbon etc., again entire container is inserted and directly carried out hot degreasing in the tank, from room temperature with temperature rise rate 0.02 degree/minute, rise to 40 degree, be incubated 1 hour; Used media can reclaim again and use.
4, heating defatting step: the base substrate behind the media degreaser drying is moved in the debinding furnace with 0.5 degree/minute rise to, 160 degree, be incubated 1 hour, again with 0.5 degree/minute rise to, 260 degree, be incubated 1 hour, with 0.01 degree/minute rise to 500 degree, be incubated 2 hours again, again with 1 degree/minute rise to 800 to spend, be incubated 1 hour, be cooled to room temperature.
5, sintering step: degreasing blank with temperature rise rate 0.5 degree/minute different temperature rise rates, is warming up to sintering temperature stage by stage, is incubated 1 hour.Sintering range 1380 degree adopt normal pressure-sintered.The stove internal cooling gets product.
Embodiment three
A kind of injection moulding method of zirconia ceramics and powder organic carrier, based on Zirconium oxide powder, add organic carrier according to Zirconium oxide powder and 100: 50 parts by weight of organic carrier, adopt injection molding technique to make base substrate, make high performance zirconia ceramic product by media degreasing, heating degreasing and sintering again.
Described powder organic carrier comprises: polyethylene, polypropylene, vegetables oil, oleic acid, paraffin.The proportioning of selecting for use of described powder organic carrier is the polyethylene 20% of powder organic carrier gross weight, polypropylene 20%, vegetables oil 30%, oleic acid 5%, paraffin 25%.
Described zirconia ceramic product manufacture craft comprises:
1, close experienced step: earlier the internal mixer temperature is transferred to 120 degree, with the organic carrier of 50 weight parts and the zirconia powder of 100 weight parts, with an organic carrier, once oxidation zirconium powder, the two alternative mode is divided and is added the indoor close white silk of close white silk for 3 times, closes close experienced chamber after 25 minutes.Temperature rises to 180 degree, and close white silk was got material after 60 minutes.Cooling.Particle makes the injection material that granularity is not more than 5 millimeters.
2, injection molding step: will inject material and be added on hopper, and obtain molding blank by injector.Processing condition are: mould temperature 45 degree, penetrate temperature 160 degree, and penetrate pressure 80Mpa.
3, media defatting step: will fix base substrate and place in the porose box, and immerse in the container fill a kind of organic liquid media that contains 40% alkane, unsaturated hydrocarbons, aromatic hydrocarbon, cyclic hydrocarbon etc., and entire container be inserted carried out degreasing in the tank again; The media degreasing comprises cold degreasing and/or hot degreasing, and the fs is cold degreasing, under the room temperature, and 2 hours time; Subordinate phase is hot degreasing, to different products, with 0.05 degree/minute different temperature rise rates, rises to 50 degree from room temperature stage by stage, is incubated 6 hours.Used media can reclaim again and use.
4, heating defatting step: the base substrate behind the media degreaser drying is moved in the debinding furnace with 1 degree/minute rise to, 170 degree, be incubated 2 hours, again with 0.8 degree/minute rise to, 260 degree, be incubated 2 hours, with 0.3 degree/minute rise to 500 degree, be incubated 2 hours again, again with 2 degree/minute rise to 900 to spend, be incubated 2 hours, be cooled to room temperature.
5, sintering step: degreasing blank with temperature rise rate 2 degree/minute different temperature rise rates, is warming up to sintering temperature stage by stage, is incubated 3 hours.Sintering range 1480 degree adopt normal pressure-sintered.The stove internal cooling gets product.
Embodiment four
Embodiment four is the same substantially with embodiment three, and the just proportioning of selecting for use of powder organic carrier is the polyethylene 30% of powder organic carrier gross weight, polypropylene 30%, vegetables oil 30%, oleic acid 5%, paraffin 5%.Other is the same with embodiment three.
Claims (1)
1, a kind of zirconium white injection molding forming method, based on Zirconium oxide powder, the organic carrier that adds certain deal, adopt injection molding technique to make base substrate, make high performance zirconia ceramic product by rational degreasing, sintering process, it is characterized in that: described zirconia ceramic product manufacture craft comprises:
A, close experienced step: earlier the internal mixer temperature is transferred to the 80-160 degree, the organic carrier of 10-80 weight part is added the indoor close white silk of close white silk with 2-4 stage gradation, zirconia powder with 100 weight parts adds the indoor close white silk of close white silk with 2-4 stage gradation simultaneously, the two hockets, and closes close experienced chamber after 20-30 minute; Temperature rises to 180 degree, gets material after close experienced 40-80 minute; Cooling; Particle makes the injection material that granularity is not more than 5 millimeters;
B, injection molding step: will inject material and be added on hopper, and obtain molding blank by injector; Processing condition are: mould temperature 40-50 degree, penetrate temperature 140-200 degree, and penetrate pressure 50-100Mpa;
C, media defatting step: will fix base substrate and place in the porose box, and immerse in a kind of container that fills the organic liquid media that contains 30-60% alkane, unsaturated hydrocarbons, aromatic hydrocarbon and cyclic hydrocarbon, and entire container be inserted carried out degreasing in the tank again; The media degreasing comprises cold degreasing and/or hot degreasing, at room temperature carries out≤12 hours during cold degreasing, to different products, with 0.02-0.5 degree/minute different temperature rise rates, rises to the 45-60 degree from room temperature stage by stage during hot degreasing, is incubated 1-16 hour; Used media can reclaim again and use;
D, heating defatting step: the base substrate behind the media degreaser drying is moved in the debinding furnace with 0.5-2 degree/minute rise to 160-180 degree, be incubated 1-2 hour, again with 0.5-1 degree/minute rise to 260 degree, be incubated 1-3 hour, with 0.01-3 degree/minute rise to 500 degree, be incubated 2-3 hour again, again with 1-5 degree/minute rise to 800-1000 degree, be incubated 1-3 hour, be cooled to room temperature;
E, sintering step: degreasing blank with temperature rise rate 0.5-5 degree/minute different temperature rise rates, is warming up to sintering temperature stage by stage, is incubated 1-6 hour; Sintering range 1380-1680 degree adopts normal pressure-sintered; The stove internal cooling gets product.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102010199B (en) * | 2010-11-19 | 2013-06-05 | 湖南正阳精密陶瓷有限公司 | Production method of zirconia ceramic bushing |
| CN104261820B (en) * | 2014-09-01 | 2016-04-06 | 河北智康通信技术有限公司 | Ceramic lock pin based on zirconium oxide and production technique thereof |
| CN104628382B (en) * | 2014-10-16 | 2017-03-08 | 深圳市商德先进陶瓷有限公司 | Reclaim the processing method that feeding injected by zirconia ceramics |
| CN105481364B (en) * | 2015-12-15 | 2019-01-11 | 东莞信柏结构陶瓷股份有限公司 | The preparation method of ceramic watchcase |
| CN109776090B (en) * | 2017-11-15 | 2021-09-10 | 辽宁爱尔创科技有限公司 | Preparation method of 3D zirconia ceramic mobile phone backboard and prepared product |
| CN110540424B (en) * | 2018-05-29 | 2021-12-21 | 山东工业陶瓷研究设计院有限公司 | Feed for zirconia ceramic injection molding and preparation method thereof |
| CN110467458A (en) * | 2019-08-15 | 2019-11-19 | 上海普拉博冶金检测探头有限公司 | Zirconia ceramics powder and preparation method thereof and zirconia ceramics prepared therefrom |
| CN110947029B (en) * | 2019-12-16 | 2022-03-01 | 浙江全景医疗科技有限公司 | Manufacturing and weaving process of full-zirconia cellucotton and application thereof |
| CN113666739B (en) * | 2021-09-30 | 2022-12-16 | 湖南华联瓷业股份有限公司 | Preparation method of zirconia ceramic |
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Effective date of registration: 20200602 Address after: Dingshuzhen pottery road Yixing City, Jiangsu province 214000 Wuxi City No. 138 Patentee after: Jiangsu Hengxin Technology Co.,Ltd. Address before: 412200 ceramic industry park, Hunan, Liling Patentee before: HUNAN ZHENGYANG PRECISION CERAMICS Co.,Ltd. |
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