CN103242036A - Method for preparing composite ceramic core - Google Patents

Method for preparing composite ceramic core Download PDF

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Publication number
CN103242036A
CN103242036A CN2012100329698A CN201210032969A CN103242036A CN 103242036 A CN103242036 A CN 103242036A CN 2012100329698 A CN2012100329698 A CN 2012100329698A CN 201210032969 A CN201210032969 A CN 201210032969A CN 103242036 A CN103242036 A CN 103242036A
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ceramic core
preparation
powder
composite ceramic
slip
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CN103242036B (en
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姜卫国
张健
韩汾汾
王莉
郝红全
刘涛
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Institute of Metal Research of CAS
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Abstract

The invention provides a method for preparing a composite ceramic core. An inner layer of the composite ceramic core is made from a silica-based material, and an outer layer of the composite ceramic core is made from an alumina-based or yttria-based ceramic material. The method provided by the invention mainly comprises the steps of preparing slurry, molding, baking, soaking, drying, sintering and the like. By adopting the method for preparing the composite ceramic core, provided by the invention, the composite ceramic core which has high strength and is easy to remove is prepared, and the need that airplane engine turbine blades are prepared in an efficient cooling manner is met.

Description

A kind of composite ceramic core preparation technology
Technical field
The invention belongs to field of ceramic material preparation, particularly precision casting aircraft engine turbine blade ceramic core technology of preparing.
Background technology
Along with the development of modern technical aeronautics, also more and more higher to the requirement of holding warm ability of aircraft engine turbine blade, in general, the every raising of inlet temperature is 100 ℃ before the turbine, and motor power can increase about 10%; For inlet temperature before the turbine that turbine part is adapted to improve constantly, must improve the working temperature of turbine blade from following two aspects, the one, improve the warm ability of holding of blade material itself, the 2nd, by improving the cooling performance that blade cooling structure improves blade.Up to the present, the high temperature capabilities of bearing of blade material has had large increase, but compares with the blade actual demand, also far can not reach requirement, therefore, needs to bring in constant renewal in blade cooling structure, improves the blade cooling performance, satisfies the requirement of advanced engine.
The efficient air cooling but typical feature of blade is that blade has cavity structure, and this cavity structure is very complicated, blade adopts the method preparation of precision casting in the traditional technology, the cavity of blade need adopt ceramic core to form, ceramic core will have higher intensity under hot environment, higher creep resisting ability, after the blade casting, also must be able to adopt chemical process to remove easily simultaneously, therefore, ceramic core will have suitable density, if density is too low, then hot strength and creep resisting ability obviously descend, if density is too high, then are unfavorable for removing of ceramic core; Therefore, the preparation ceramic core that has higher high-temperature behavior and adopt chemical process to remove easily also will keep certain porosity when then needing to keep the intensity of ceramic core, and this contradiction has brought sizable difficulty for the preparation of ceramic core.
Summary of the invention
Purpose of the present invention: in order addressing the above problem, to the invention provides that a kind of preparation has high strength and the method for the ceramic core that easily removes, to have satisfied the needs that efficient cooling prepares the aircraft engine turbine blade.
Concrete technology of the present invention:
1, preparation softening agent: with paraffin or its mixture melt, under this state, add polyethylene gradually, constantly stir, be warming up to 120 ℃-160 ℃, after polyethylene is dissolved into fully in the paraffin, stirs, filter, standby;
2, preparation silica slurry: with the softening agent fusing, add the hot powder of silicon-dioxide gradually, the limit adds the powder limit stirs, and stirs the tensio-active agent that also will add 0.5%-1.0% simultaneously, churning time 2-8 hour;
3, internal layer ceramic core moulding: at 100-140 ℃, adopt injection molding to carry out the moulding of internal layer ceramic core the control of silica slurry temperature;
4, roasting: the internal layer ceramic core packed into carry out roasting in the aluminum oxide powder filler, burning temperature eventually is 1150-1190 ℃, time 3-5 hour;
5, preparation aluminum oxide or yttrium oxide or zirconium white slip: slip be combined as aluminum oxide powder and aluminium colloidal sol or yttrium oxide powder and yttrium oxide colloidal sol or zirconium white and zirconium colloidal sol composition;
6, immersion, drying: under condition of negative pressure, ceramic core is immersed in aluminum oxide or yttrium oxide or the zirconium white slip 2-6 hour, in air, carries out drying then;
7, sintering: dried ceramic core is carried out sintering again, and burning temperature eventually is 1350-1550 ℃, time 20-60 minute, makes composite ceramic core at last.
In the technology of the present invention, in the softening agent, the paraffin mass percent is 80-95%, and polyethylene is 2-5%, and all the other are beeswax or stearic acid;
In the technology of the present invention, internal layer core ceramic powder is the silicon dioxide base ceramic powder;
In the technology of the present invention, the tensio-active agent that adds in the silicon dioxide base ceramic powder is oleic acid or other aliphatic alcohols materials;
In the technology of the present invention, injection molding mode moulding is adopted in the moulding of silicon dioxide base ceramic size, and forming pressure is 0.4-0.8MPa, and be 20-120 second inject time, and the dwell time is 20-120 second;
In the technology of the present invention, the softening agent in the silicon-dioxide base ceramic core adopts stuffing means to remove, and filler adopts the aluminium sesquioxide powder, and granularity is the industrial oxidation aluminium powder of 100-300 order;
In the technology of the present invention, the silicon-dioxide base ceramic core dewaxing stage is adopted the low temperature sintering that slowly heats up, and temperature is lower than 500 ℃; The whole sintering stage is adopted high temperature sintering, and silica-based sintering is at 1150 ℃-1190 ℃, and soaking time 3-5 hour, stove was chilled to room temperature then;
In the technology of the present invention, aluminum oxide or yttrium oxide or the zirconium white slip of preparation, be combined as aluminum oxide powder and aluminium colloidal sol or yttrium oxide and the yttrium oxide colloidal sol or zirconium white and zirconium colloidal sol of slip are formed, powder liquid mass ratio is (1-2): 1, the particle diameter of powder is 100nm-1000nm, and size of particles is 5-20nm in the colloidal sol;
In the technology of the present invention, the internal layer ceramic core carries out aluminum oxide or yttrium oxide or zirconium white slip and soaks under condition of negative pressure, and pressure is 0.01-0.05MPa;
In the technology of the present invention, after the internal layer ceramic core soaks aluminum oxide or yttrium oxide or zirconium white slip, need under 22-24 ℃ of relative humidity 50%-70% condition dry 4-12 hour, then ceramic core is soaked and dry more again, repeat this process 2-5 time, outer layer thickness is controlled at 0.05-2mm; At last with this ceramic core 1300 ℃-1550 ℃ sintering 20-120 minute, furnace cooling;
In the technology of the present invention, behind the ceramic core sintering, immerse ceramic core in the heat-reactive phenolic resin or in the urea, take out at air drying.
Beneficial effect of the present invention is: the composite ceramic core that adopts preparation method's preparation of the present invention, the higher-strength that under 1500-1580 ℃ hot environment, has 12-25MPa, higher non-deformability (amount of deflection is 0.5-1.8mm), ceramic core has the suitable density of 34-37% simultaneously, is beneficial to removing of ceramic core.
Description of drawings
Fig. 1 is the outside drawing of the composite ceramic core of the preferred embodiment of the present invention one preparation.
Fig. 2 is the outside drawing of the composite ceramic core of the preferred embodiment of the present invention two preparations.
Embodiment
Embodiment one
With melted paraffin wax and add 1% polyethylene, constantly stir, be warming up to 130 ℃, be dissolved into fully in the paraffin until polyethylene, add hot powder gradually, the mass ratio of powder and softening agent is 85: 15, powder is thick silica powder and thin silica powder, and the quality proportioning of the two is 30: 70, and the limit adds the ceramic powder limit and stirs, stir the tensio-active agent oleic acid that also will add total mass 1.0% simultaneously, churning time 6 hours; After treating that softening agent, powder, tensio-active agent mix, temperature remains between 120 ℃.Adopt injection press ceramic core, forming pressure is 0.4MPa, and be 20 seconds inject time, and the dwell time is 60 seconds; Ceramic core is packed in the filler, and filler adopts the aluminium sesquioxide powder, and granularity is the industrial oxidation aluminium powders of 200 orders; The ceramic core dewaxing stage is adopted the low temperature sintering that slowly heats up, and heat-up rate is 5 ℃/minute, and insulation is 1 hour when rising to 500 ℃; Burn 1150 ℃ of temperature, 4 hours time eventually.The preparation alumina slurry, slip consist of aluminum oxide powder and aluminium sol solution composition, powder liquid mass ratio is 1: 1, the particle diameter of aluminum oxide powder is 200nm, size of particles is 10nm in the colloidal sol; The internal layer ceramic core was soaked 20 minutes in the alumina slurry under the 0.01MPa condition, take out ceramic core then under 24 ℃ of relative humidity 70% conditions dry 4 hours, repeat this technological process 4 times, then with this ceramic core at 1450 ℃ of sintering 20 minutes, furnace cooling; At last, immerse ceramic core in the heat-reactive phenolic resin or in the urea, take out at air drying.
The ceramic core of preparation is seen Fig. 1, and the composite ceramic core of the embodiment of the invention one preparation has typical ectonexine structure as can be seen from Figure 1; Have excellent comprehensive performances simultaneously, 1500 ℃ of high-temperature bending strengths can reach 15MPa after testing, and deflection value can reach 0.8mm; And adopting its 1500 ℃ of high-temperature bending strengths of ceramic core of silica-based preparation only to reach 7MPa in the traditional preparation process technology, deflection value has reached 1.8mm.
Embodiment two
With melted paraffin wax and add 1% polyethylene, constantly stir, be warming up to 130 ℃, be dissolved into fully in the paraffin until polyethylene, add hot powder gradually, the mass ratio of powder and softening agent is 85: 15, powder is thick silica powder and thin silica powder, and the quality proportioning of the two is 30: 70, and the limit adds the ceramic powder limit and stirs, stir the tensio-active agent oleic acid that also will add total mass 1.0% simultaneously, churning time 6 hours; After treating that softening agent, powder, tensio-active agent mix, temperature remains between 120 ℃.Adopt injection press ceramic core, forming pressure is 0.4MPa, and be 20 seconds inject time, and the dwell time is 60 seconds; Ceramic core is packed in the filler, and filler adopts the aluminium sesquioxide powder, and granularity is the industrial oxidation aluminium powders of 200 orders; The ceramic core dewaxing stage is adopted the low temperature sintering that slowly heats up, and heat-up rate is 5 ℃/minute, and insulation is 1 hour when rising to 500 ℃; Burn 1150 ℃ of temperature, 4 hours time eventually.Preparation zirconium white slip, slip consist of zirconia powder and zirconium sol solution composition, powder liquid mass ratio is 1: 1, the particle diameter of zirconia powder is 200nm, size of particles is 10nm in the colloidal sol; The internal layer ceramic core was soaked 20 minutes in the zirconium white slip under the 0.01MPa condition, take out ceramic core then under 24 ℃ of relative humidity 70% conditions dry 4 hours, repeat this technological process 4 times, then with this ceramic core at 1390 ℃ of sintering 40 minutes, furnace cooling; At last, immerse ceramic core in the heat-reactive phenolic resin or in the urea, take out at air drying.
Fig. 2 is the outside drawing of the composite ceramic core of the preferred embodiment of the present invention two preparations, as can be seen from the figure composite ceramic core has typical ectonexine structure, have excellent comprehensive performances, 1550 ℃ of high-temperature bending strengths can reach 12MPa, and deflection value can reach 1.2mm; And adopting its 1550 ℃ of high-temperature bending strengths of ceramic core of silica-based preparation only to reach 3MPa in the traditional preparation process technology, deflection value has reached 3.2mm.
Embodiment three
With melted paraffin wax and add 1% polyethylene, constantly stir, be warming up to 130 ℃, be dissolved into fully in the paraffin until polyethylene, add hot powder gradually, the mass ratio of powder and softening agent is 85: 15, powder is thick silica powder and thin silica powder, and the quality proportioning of the two is 30: 70, and the limit adds the ceramic powder limit and stirs, stir the tensio-active agent oleic acid that also will add total mass 1.0% simultaneously, churning time 6 hours; After treating that softening agent, powder, tensio-active agent mix, temperature remains between 120 ℃.Adopt injection press ceramic core, forming pressure is 0.4MPa, and be 20 seconds inject time, and the dwell time is 60 seconds; Ceramic core is packed in the filler, and filler adopts the aluminium sesquioxide powder, and granularity is the industrial oxidation aluminium powders of 200 orders; The ceramic core dewaxing stage is adopted the low temperature sintering that slowly heats up, and heat-up rate is 5 ℃/minute, and insulation is 1 hour when rising to 500 ℃; Burn 1150 ℃ of temperature, 4 hours time eventually.Preparation yttrium oxide slip, slip consist of yttrium oxide powder and yttrium sol solution composition, powder liquid mass ratio is 1: 1, the particle diameter of yttrium oxide powder is 200nm, size of particles is 10nm in the colloidal sol; The internal layer ceramic core was soaked 20 minutes in the yttrium oxide slip under the 0.01MPa condition, take out ceramic core then under 24 ℃ of relative humidity 70% conditions dry 4 hours, repeat this technological process 5 times, then with this ceramic core at 1400 ℃ of sintering 30 minutes, furnace cooling; At last, immerse ceramic core in the heat-reactive phenolic resin or in the urea, take out at air drying.
The composite ceramic core of embodiment three preparations has typical ectonexine structure, has excellent comprehensive performances, and 1500 ℃ of high-temperature bending strengths can reach 18MPa, and deflection value can reach 0.9mm.And its 1500 ℃ of high-temperature bending strengths of ceramic core that adopt silica-based preparation only reach 7MPa, and deflection value has reached 1.8mm.
In sum, adopt the composite ceramic core of preparation method's preparation of the present invention, the higher-strength that under 1500-1580 ℃ hot environment, has 12-25MPa, higher non-deformability (amount of deflection is 0.5-1.8mm), ceramic core has the suitable density of 34-37% simultaneously, be beneficial to removing of ceramic core, satisfied the needs that efficient cooling prepares the aircraft engine turbine blade.
The above is preferred embodiment of the present invention only, is not in order to limit application range of the present invention; All other do not break away from the equivalence of finishing under the disclosed essence and change or modification, all should be included in following claims scope.

Claims (7)

1. composite ceramic core preparation method, the internal layer of described composite ceramic core is silica-based materials, skin is alumina base or yttria-base or zirconia-based material; It is characterized in that: described composite ceramic core preparation method comprises the steps:
(1) preparation softening agent: will add polyethylene behind the melted paraffin wax, constantly stir, be warming up to 120 ℃-160 ℃, after polyethylene is dissolved into fully in the paraffin, stirs, filter;
(2) preparation silica slurry: with described softening agent fusing, add the hot powder of silicon-dioxide gradually, stir while adding, stir the tensio-active agent that adds 0.5%-1.0% simultaneously, churning time 2-8 hour;
(3) internal layer ceramic core moulding: at 100-140 ℃, adopt injection molding to carry out moulding described silica slurry temperature control;
(4) roasting (removing softening agent);
(5) the outer slip of preparation ceramic core;
(6) soak, drying: under the 0.01-0.05MPa condition of negative pressure, the internal layer ceramic core is immersed in the outer slip 2-6 hour, then at air drying;
(7) sintering: dried ceramic core is carried out sintering again, and burning temperature eventually is 1350-1550 ℃, time 20-60 minute, makes composite ceramic core at last.
2. composite ceramic core preparation method according to claim 1, it is characterized in that: the paraffin mass percent in the described step 1 softening agent is 80-95%, and the polyethylene mass percent is 2-5%, and all the other are beeswax or stearic acid.
3. composite ceramic core preparation method according to claim 1 and 2, it is characterized in that: the tensio-active agent in the described step 2 is oleic acid or other aliphatic alcohols materials.
4. according to each described composite ceramic core preparation method of claim 1~3, it is characterized in that: described injection molding forming pressure is 0.4-0.8MPa, and be 20-120 second inject time, and the dwell time is 20-120 second.
5. composite ceramic core preparation method according to claim 1, it is characterized in that: in described roasting (the removing softening agent) step, with the described internal layer ceramic core aluminium sesquioxide powder of packing into, granularity is to carry out roasting in the industrial oxidation aluminium powder of 100-300 order, burning temperature eventually is 1150-1190 ℃, time 3-5 hour.
6. composite ceramic core preparation method according to claim 1, it is characterized in that: the outer slip of described preparation ceramic core, be preparation aluminum oxide or yttrium oxide or zirconium white slip, be combined as aluminum oxide powder and aluminium colloidal sol or yttrium oxide powder and the yttrium oxide colloidal sol or zirconia powder and zirconia sol of slip are formed, powder liquid mass ratio is (1-2): 1, the particle diameter of powder is 100nm-1000nm, and size of particles is 5-20nm in the colloidal sol.
7. composite ceramic core preparation method according to claim 1, it is characterized in that: after the internal layer ceramic core soaks aluminum oxide or yttrium oxide or zirconium white slip, need under 22-24 ℃ of relative humidity 50%-70% condition dry 4-12 hour, then ceramic core is soaked again and dry again, repeat this process 2-5 time, outer slurry thickness control is at 0.05-1mm; At last with this ceramic core 1300 ℃-1550 ℃ sintering 20-120 minute, furnace cooling.
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Cited By (14)

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Publication number Priority date Publication date Assignee Title
CN103693976A (en) * 2013-12-09 2014-04-02 中国航空工业集团公司北京航空材料研究院 Method for preparing silicon oxide-based ceramic core for titanium and titanium alloy casting
CN104446576A (en) * 2013-09-18 2015-03-25 辽宁省轻工科学研究院 Ceramic core enhanced by quart fiber
CN104649685A (en) * 2013-11-19 2015-05-27 中国科学院金属研究所 Plasticizer used in injection moulding of ceramic core and preparation method thereof
CN105272181A (en) * 2015-10-16 2016-01-27 沈阳工业大学 Preparation technology of composite ceramic core
CN107640963A (en) * 2017-10-20 2018-01-30 东方电气集团东方汽轮机有限公司 A kind of preparation method of graded ceramicses core material
CN108178637A (en) * 2016-12-08 2018-06-19 辽宁法库陶瓷工程技术研究中心 A kind of yttrium oxide single crystal casting ceramic core and preparation method
CN108484140A (en) * 2018-03-01 2018-09-04 辽宁航安特铸材料有限公司 The ceramic layered core of two-component
CN109304424A (en) * 2018-10-22 2019-02-05 沈阳明禾石英制品有限责任公司 Modified oxidized silicon powder and preparation method thereof, ceramic core and preparation method thereof
CN109928780A (en) * 2017-12-18 2019-06-25 沈阳航发精密铸造有限公司 A kind of manufacturing method of ceramic core surface inertness coat
CN111593287A (en) * 2020-05-29 2020-08-28 深圳市万泽中南研究院有限公司 Method for forming ceramic core aluminum oxide coating by supersonic plasma spraying
CN114180945A (en) * 2021-12-29 2022-03-15 华中科技大学 Additive manufacturing method for ceramic core-type shell integrated piece
CN114273612A (en) * 2021-12-27 2022-04-05 江苏永瀚特种合金技术股份有限公司 Preparation method of ceramic core for refining surface grains of inner cavity of high-temperature alloy casting
CN114804842A (en) * 2022-05-11 2022-07-29 西安交通大学 Preparation method of ceramic core with controllable pore distribution and atmosphere
CN114988852A (en) * 2022-05-13 2022-09-02 潍坊科技学院 Preparation method of ceramic core with multilayer sandwich structure

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Cited By (19)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104446576A (en) * 2013-09-18 2015-03-25 辽宁省轻工科学研究院 Ceramic core enhanced by quart fiber
CN104649685A (en) * 2013-11-19 2015-05-27 中国科学院金属研究所 Plasticizer used in injection moulding of ceramic core and preparation method thereof
CN104649685B (en) * 2013-11-19 2017-11-17 中国科学院金属研究所 A kind of ceramic core injection moulding plasticizer and preparation method thereof
CN103693976A (en) * 2013-12-09 2014-04-02 中国航空工业集团公司北京航空材料研究院 Method for preparing silicon oxide-based ceramic core for titanium and titanium alloy casting
CN105272181A (en) * 2015-10-16 2016-01-27 沈阳工业大学 Preparation technology of composite ceramic core
CN108178637A (en) * 2016-12-08 2018-06-19 辽宁法库陶瓷工程技术研究中心 A kind of yttrium oxide single crystal casting ceramic core and preparation method
CN107640963B (en) * 2017-10-20 2020-09-29 东方电气集团东方汽轮机有限公司 Preparation method of gradient ceramic core material
CN107640963A (en) * 2017-10-20 2018-01-30 东方电气集团东方汽轮机有限公司 A kind of preparation method of graded ceramicses core material
CN109928780A (en) * 2017-12-18 2019-06-25 沈阳航发精密铸造有限公司 A kind of manufacturing method of ceramic core surface inertness coat
CN108484140A (en) * 2018-03-01 2018-09-04 辽宁航安特铸材料有限公司 The ceramic layered core of two-component
CN109304424A (en) * 2018-10-22 2019-02-05 沈阳明禾石英制品有限责任公司 Modified oxidized silicon powder and preparation method thereof, ceramic core and preparation method thereof
CN111593287A (en) * 2020-05-29 2020-08-28 深圳市万泽中南研究院有限公司 Method for forming ceramic core aluminum oxide coating by supersonic plasma spraying
CN111593287B (en) * 2020-05-29 2022-09-30 深圳市万泽中南研究院有限公司 Method for forming ceramic core aluminum oxide coating by supersonic plasma spraying
CN114273612A (en) * 2021-12-27 2022-04-05 江苏永瀚特种合金技术股份有限公司 Preparation method of ceramic core for refining surface grains of inner cavity of high-temperature alloy casting
CN114273612B (en) * 2021-12-27 2023-09-05 江苏永瀚特种合金技术股份有限公司 Preparation method of ceramic core for refining grains on inner cavity surface of superalloy casting
CN114180945A (en) * 2021-12-29 2022-03-15 华中科技大学 Additive manufacturing method for ceramic core-type shell integrated piece
CN114804842A (en) * 2022-05-11 2022-07-29 西安交通大学 Preparation method of ceramic core with controllable pore distribution and atmosphere
CN114804842B (en) * 2022-05-11 2022-12-09 西安交通大学 Preparation method of ceramic core with controllable pore distribution and atmosphere
CN114988852A (en) * 2022-05-13 2022-09-02 潍坊科技学院 Preparation method of ceramic core with multilayer sandwich structure

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