CN103304227B - Alumina-based ceramic core for directional solidification and preparation method thereof - Google Patents

Alumina-based ceramic core for directional solidification and preparation method thereof Download PDF

Info

Publication number
CN103304227B
CN103304227B CN201310269759.5A CN201310269759A CN103304227B CN 103304227 B CN103304227 B CN 103304227B CN 201310269759 A CN201310269759 A CN 201310269759A CN 103304227 B CN103304227 B CN 103304227B
Authority
CN
China
Prior art keywords
powder
ceramic core
temperature
alumina
warming
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310269759.5A
Other languages
Chinese (zh)
Other versions
CN103304227A (en
Inventor
娄延春
于波
苏贵桥
刘孝福
李长春
郭新力
税国彦
李彪
关阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenyang Foundry Research Institute Co Ltd Of China National Machinery Research Institute Group
Shenyang Research Institute of Foundry Co Ltd
Original Assignee
Shenyang Research Institute of Foundry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenyang Research Institute of Foundry Co Ltd filed Critical Shenyang Research Institute of Foundry Co Ltd
Priority to CN201310269759.5A priority Critical patent/CN103304227B/en
Publication of CN103304227A publication Critical patent/CN103304227A/en
Application granted granted Critical
Publication of CN103304227B publication Critical patent/CN103304227B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention relates to an alumina-based ceramic core for directional solidification and a preparation method thereof. The refractory materials used in the alumina-based ceramic core include 65-95% of EC95 fused mullite, 5-30% of zirconium silicate, 2-8% of silica powder, 1-5% of titania powder and 1-10% of aluminium powder by weight percent, wherein EC95 fused mullite, F200 powder accounts for 10-30%, F320 powder accounts for 40-70% and F600 powder accounts for 10-30%. The preparation method is characterized by comprising the following steps: ball-milling the above powders and mixing the powder uniformly, putting the mixture into a molten plasticizer to be mixed, forming on a ceramic core forming machine through hot pressing, finishing a ceramic core formed through hot pressing and correcting the shape of the ceramic core, roasting in a box-type resistance furnace, and adopting a high-temperature reinforcer and a room-temperature reinforcer to respectively carry out high-temperature reinforcement and room-temperature reinforcement on the ceramic core discharged from the furnace. The alumina-based ceramic core prepared by the preparation method has the characteristics of high high-temperature strength, good creep resistance, small firing shrinkage, low firing temperature and good metallurgical and chemical properties.

Description

A kind of directional freeze alumina based ceramic core and preparation method
Technical field
The present invention relates to a kind of gas turbine component, specifically alumina based ceramic core and preparation method for a kind of directional freeze.This alumina based ceramic core hot strength is high, creep-resistant property good, burn till shrink little, firing temperature is low, not with superalloy melt generation chemical reaction.Not only can be for casting undersized aircraft engine equiax crystal, orientation and single crystal blade, and can be used for casting large-sized heavy duty gas turbine equiax crystal, orientation and single crystal blade.
Background technology
High-pressure turbine blade is the vitals of internal combustion turbine, for improving constantly fuel gas inlet temperature before turbine, hollow blade manufacture is developed into from solid vane manufacture in countries in the world, and from polycrystalline blade orientation and single crystal blade till now, its object is just constantly to improve the over-all properties of internal combustion turbine.Before advanced aero-turbine, inlet temperature has reached 1757 DEG C at present, and before heavy duty gas turbine turbine, inlet temperature also reaches 1600 DEG C, and the front inlet temperature of turbine reaches the heavy duty gas turbine of 1700 DEG C also just in Design and manufacture.This just need to improve blade inner chamber cooling structure, improves cooling efficiency.Blade inner chamber cooling structure is more complicated, also higher to being used to form the ceramic core performance requriements of its inner chamber.Under silica-based ceramic core hot conditions, easily there is softening sex change, core shift, leakage core, during higher than 1550 DEG C, silicon oxide be easy to superalloy in active element Al, Hf, C etc. occur chemical reaction, cause blade interior air cooling passage generation chemical scab, worsen the inner chamber quality of blade, reduce the air cooling effect of blade.And the features such as the high refractoriness that aluminum oxide has due to self, high chemical stability, high thermal stability are good with alumina ceramic core stable chemical performance, the creep-resistant property of its manufacture.
The known body material of preparing alumina based ceramic core employing is fused corundom powder, and other mineralizer and additive have activated alumina, porous alumina, alumina hollow ball, silicon carbide, magnesium oxide, yttrium oxide, lanthanum trioxide, Graphite Powder 99 etc.Chinese patent (patent No.: CN1994964A) has disclosed a kind of compound alumina ceramic core material and forming preparation process that adopts alumina hollow ball, in raw material, each weight percentages of components is fused corundom powder 32.5~60.5%, alumina hollow ball 20~50%, silicon carbide 3~5%, all the other are softening agent, injection-compression molding.United States Patent (USP) (the patent No.: 5143777) disclosed the alumina hollow ball of a kind of employing 200 object fused corundom powder and 0-0.25mm, ratio is 30:70, adds binding agent, the method for gravity slurry molding alumina ceramic core.Although these two kinds of methods have improved the porosity of alumina based ceramic core, because the density of alumina hollow ball is less, and the density of fused corundom is larger, and raw material mixes inhomogeneous, ceramic core unstable properties.It is 45~66% fused corundom powder that Chinese patent (patent No.: CN101229975A) has disclosed a kind of employing weight percent, 15~30% activated alumina, 1~5% Graphite Powder 99, the method of hot-injection molding alumina based ceramic core, changes γ-Al gradually into during due to porous active aluminium oxide calcining 2o 3and α-Al 2o 3process in be accompanied by larger volumetric shrinkage, cause this ceramic core shrinking percentage larger.United States Patent (USP) (the patent No.: 4837187,5409871,5580837) disclosed respectively and in aluminum oxide, added the yttrium oxide of 1~20% left and right, 1~5% MgO, the Graphite Powder 99 of 1~7% left and right, or in aluminum oxide, add 10~40% yttrium aluminum garnet, the method of injection-compression molding alumina based ceramic core improves the high-temperature behavior of ceramic core performance, but the sintering temperature of core is up to 1600~1700 DEG C.
Summary of the invention
Object of the present invention, is to have unstable properties, burn till and shrink the problem large, firing temperature is high for above-mentioned alumina based ceramic core, and a kind of directional freeze alumina based ceramic core is provided.By adding suitable additive, make the bending strength >=5MPa of 1550 DEG C of alumina based ceramic cores, deformation induced by gravity amount≤1mm, burns till contraction≤1%, and firing temperature is lower than 1450 DEG C.Can ensure the dimensional precision of superalloy turbine blade and good surface of internal cavity quality.
Another object of the present invention, is to provide the preparation method of a kind of directional freeze oxygen Al-base ceramic core.
The technical scheme adopting is:
A kind of directional freeze alumina based ceramic core, is characterized in that taking EC95 electrofused mullite as base-material, and EC95 electrofused mullite is to add weight percent taking high-quality alundum to form as mineralizer >=2000 DEG C of pyrotic smeltings of warp in electric arc furnace of 2~6%.
EC95 electrofused mullite after smelting is with a-Al 2o 3, 3Al 2o 32SiO 2for main xln, wherein α-Al 2o 3content 80~95%, 3Al 2o 32SiO 2content 5~20%, be a kind of have compact structure, folding strength large, expand evenly, the good high-temperature creep resistance such as thermal stability is good, refractoriness under load is high, high temperature creep value is little and the high grade refractory of high-temperature stability.Through pulverizing shaping, magnetic separation de-iron, is sieved into granularity and is the powder of No. F200, No. F320, No. F600, and pickling is dry.
Mineralizer adopts zirconium silicate, silicon dioxide powder, titanium dioxide powder and aluminium powder.Zirconium silicate granularity is No. F320, silicon dioxide powder, and granularity is No. F320, SiO in powder 2content>=96%, titanium dioxide powder size≤30 μ m, TiO 2content>=97%, aluminum powder size≤50 μ m, active A l content>=98%.
A preparation method for alumina based ceramic core for directional freeze, is characterized in that comprising following processing step:
1, take powder: the EC95 electrofused mullite powder, zirconium silicate powder, silicon dioxide powder, titanium dioxide powder, the aluminium powder that weigh respectively certainweight are put into ball grinder.EC95 electrofused mullite 65~95% by weight percentage in powder, zirconium silicate 5~30%, silicon dioxide powder 2~8%, titanium dioxide powder 1~5%, aluminium powder 1~10%.Wherein in EC95 electrofused mullite, F200 powder accounts for 10~30%, F320 powder content 40~70%, and F600 powder accounts for 10~30%.
2, ball is mixed: add the oleic acid that accounts for powder weight 0.5~2%, add zirconia ceramics ball to mix by ratio of grinding media to material 1.5:1, the ball 4~8h that does time.
3, join softening agent: take the softening agent that accounts for the weight of mixed powder described in step 1 14~18%, in softening agent, paraffin and poly ratio are 46~49:1.Softening agent is put into core material stirrer heat fused, and temperature of fusion is 90~110 DEG C.
4, mixing: the mixed powder mixing described in step 1 slowly to be joined in core material stirrer, continue to stir 6~8h, make softening agent and powder mixing evenly.
5, hot-injection molding.Utilize ceramic core press injector, according to the size of ceramic core and complexity, controlling injection temperature is the molding parameters such as 90 DEG C, 45 DEG C of die temperatures, injection pressure 2MPa, dwell time 120s, and mixing uniform core material pressure injection, in ceramic core mould, is made to ceramic core biscuit.
6, finishing, school type: ceramic core biscuit, after finishing, school type, is put into the industrial alumina packing of saggar and buried reality.
7, roasting.The saggar that ceramic core biscuit and commercial alumina filler are housed is put into chamber type electric resistance furnace and carry out roasting, roasting system is: be warming up to 200~300 DEG C with the temperature rise rate of 2~5 DEG C/min, insulation 3~6h, be warming up to 400~500 DEG C with the temperature rise rate of 3~6 DEG C/min, insulation 2~4h, be warming up to 600~700 DEG C with the temperature rise rate of 4~7 DEG C/min, insulation 1~2h, be warming up to 900~1000 DEG C with 6~9 DEG C/min temperature rise rate, insulation 1~2h, be warming up to 1100~1200 DEG C with the temperature rise rate of 6~9 DEG C/min, insulation 2~3h, be warming up to 1300~1450 DEG C with the temperature rise rate of 1~2 DEG C/min, insulation 4~8h, then cool to room temperature with the furnace.
In roasting process there is complicated physicochemical change in alumina based ceramic core.Lower than 500 DEG C, the softening agent in ceramic core biscuit melts, in filler, moves, until decompose volatilization.Generate γ-Al at 500~1100 DEG C of aluminium powder oxidations 2o 3and follow 28% volumetric expansion, be oxidized the γ-Al generating 2o 3there is very high activity.Temperature is elevated to 1200 DEG C, and under the katalysis of titanium dioxide, zirconium silicate decomposes generation SiO 2and ZrO 2, decompose the SiO generating 2there is high reactivity.Highly active SiO 2high reactivity γ-Al with aluminium powder oxidation generation 2o 3reaction generates mullite.Temperature is higher than 1200 DEG C, at highly active SiO 2high reactivity Al with aluminium powder oxidation generation 2o 3in the mullite seed crystal matrix that reaction generates, the α-Al in additive silicon-dioxide and EC95 2o 3reaction generates mullite.The generation of mullite is accompanied by 6~10% volumetric expansion.Meanwhile, titanium dioxide is solidly soluted in zirconium dioxide, plays stabilized zirconia, has avoided zirconium dioxide to change low temperature monoclinic form into from high temperature tetragonal structure.Have neither part nor lot in the γ-Al of reaction 2o 3be greater than 1200 DEG C of generation crystal conversions generation α-Al 2o 3.The chemical reaction of whole process is as follows:
4Al+3O 2 →2γ-Al 2 O 3
ZrSiO 4 →ZrO 2 +SiO 2
3γ-Al 2 O 3 +2SiO 2 →3Al 2 O 3 ·2SiO 2
3α-Al 2 O 3 +2SiO 2 →3Al 2 O 3 ·2SiO 2
ZrO 2 +TiO 2 →ZrO 2 ·TiO 2
γ-Al 2 O 3 →α-Al 2 O 3
8, High-Temperature Strengthening.Ceramic core after coming out of the stove adopts silicate hydrolyzate liquid to carry out High-Temperature Strengthening.Reinforcer contains tetraethyl silicate 81~83% by weight percentage, alcohol 11~12%, and distilled water 4~6%, hydrochloric acid 1~1.5% content carries out proportioning, the temperature of strict controlled hydrolysis liquid in hydrolytic process, temperature will be used water quench at once higher than 54 DEG C.
9, room temperature strengthening.High-Temperature Strengthening dried ceramic core are carried out to room temperature strengthening, in reinforcer, contain by weight percentage phenolic aldehyde spirit varnish 50~55%, ethanol 40~45%, hexamethylenetetramine 2~5%.
The invention has the advantages that:
(1) reduce and burn till contraction.In roasting process, aluminium powder oxidation generates aluminum oxide and silicon-dioxide reacts the volumetric expansion that generates mullite generation with aluminum oxide, has compensated the volumetric shrinkage that core roasting occurs.Burning till of alumina-based ceramic core shunk to be reduced to below 1%.
(2) reduce firing temperature.The decomposition temperature of zirconium silicate is 1540 DEG C, and titanium dioxide promotes zirconium silicate to decompose, and makes the decomposition temperature of zirconium silicate be reduced to 1200 DEG C.The generation temperature of mullite is also 1540 DEG C of left and right.And the temperature of the high reactivity silicon dioxde reaction generation mullite that the oxide of high activity aluminium that aluminium powder oxidation generates and zirconium silicate decomposition generate is 1200 DEG C, greatly reduces the generation temperature of mullite.The firing temperature of alumina-based ceramic core is reduced to 1300~1450 DEG C.
(3) improve high-temperature behavior.The high-temperature agglomerant mullite that chemical reaction generates is a kind of refractory materials of excellent performance.Fusing point is 1890 ± 90 DEG C, and hot strength and refractoriness under load are high, has good thermal shock resistance and high temperature creep property.And zirconium silicate decomposes the zirconium dioxide fusing point generating up to 2680 DEG C, strengthen the high-temperature behavior of alumina-based ceramic core.By the strengthening effect of mullite and zirconium dioxide, bending strength >=5MPa that alumina-ceramic core is 1550 DEG C, deformation induced by gravity amount≤1mm.
Brief description of the drawings
Fig. 1 is alumina-based ceramic core preparation process schema.
Fig. 2 is alumina-based ceramic core roasting system schematic diagram.
Embodiment
specific embodiment 1
A kind of directional freeze alumina based ceramic core, is characterized in that taking EC95 electrofused mullite as base-material, and EC95 electrofused mullite is to add weight percent taking high-quality alundum in electric arc furnace, to form through 2100 DEG C of pyrotic smeltings as 2% mineralizer.EC95 electrofused mullite after smelting is with a-Al 2o 3, 3Al 2o 32SiO 2for main xln, wherein α-Al 2o 3content 93%, 3Al 2o 32SiO 2content 7%.
A preparation method for alumina based ceramic core for directional freeze, comprises the steps:
1, take powder: the EC95 electrofused mullite after smelting is pulverized to shaping, and magnetic separation de-iron, is sieved into granularity and is the powder of No. F200, No. F320, No. F600, and pickling is dry.Take by weight percentage 15% F200 EC95,50% F320 EC95,15% F600 EC95,10% zirconium silicate powder, 5% silicon dioxide powder, 2% titanium dioxide, 3% aluminium powder.
2, ball is mixed: add the oleic acid that accounts for the weight of mixed powder described in step 1 1%, add zirconia ceramics ball to mix by ratio of grinding media to material 1.5:1, the ball 4h that does time.
3, join softening agent: take the softening agent that accounts for the weight of mixed powder described in step 1 14%, in softening agent, paraffin and poly ratio are 49:1.Softening agent is put into core material stirrer heat fused, and temperature of fusion is 110 DEG C.
4, mixing: the mixed powder mixing described in step 1 slowly to be joined in core material stirrer, continue to stir 8h, make softening agent and powder mixing evenly.
5, hot-injection molding: utilize ceramic core press injector, controlling injection temperature is 90 DEG C, 45 DEG C of die temperatures, injection pressure 2MPa, dwell time 120s, and mixing uniform core material pressure injection, in ceramic core mould, is made to ceramic core biscuit.
6, finishing, school type: ceramic core biscuit, after finishing, school type, is put into the industrial alumina packing of saggar and buried reality.
7, roasting: the saggar that ceramic core biscuit and commercial alumina filler are housed is put into chamber type electric resistance furnace and carry out roasting, roasting system is: be warming up to 240 DEG C with the temperature rise rate of 2 DEG C/min, insulation 4h, be warming up to 500 DEG C with the temperature rise rate of 3 DEG C/min, insulation 4h, be warming up to 700 DEG C with the temperature rise rate of 4 DEG C/min, insulation 1.5h, be warming up to 1000 DEG C with 6 DEG C/min temperature rise rate, insulation 1h, is warming up to 1200 DEG C with the temperature rise rate of 7 DEG C/min, insulation 2.5h, be warming up to 1350 DEG C with the temperature rise rate of 2 DEG C/min, insulation 6h, then cools to room temperature with the furnace.
8, High-Temperature Strengthening: the ceramic core after coming out of the stove adopts silicate hydrolyzate liquid to carry out High-Temperature Strengthening.Reinforcer contains tetraethyl silicate 81% by weight percentage, alcohol 12%, and distilled water 6%, hydrochloric acid 1% content carries out proportioning, the temperature of strict controlled hydrolysis liquid in hydrolytic process, temperature will be used water quench at once higher than 54 DEG C.
9, room temperature strengthening: High-Temperature Strengthening dried ceramic core are carried out to room temperature strengthening, contain by weight percentage phenolic aldehyde spirit varnish 53%, ethanol 44%, hexamethylenetetramine 3% in reinforcer.
specific embodiment 2
A kind of directional freeze alumina based ceramic core, is characterized in that taking EC95 electrofused mullite as base-material, and EC95 electrofused mullite is to add weight percent taking high-quality alundum in electric arc furnace, to form through 2150 DEG C of pyrotic smeltings as 3.5% mineralizer.EC95 electrofused mullite after smelting is with a-Al 2o 3, 3Al 2o 32SiO 2for main xln, wherein α-Al 2o 3content 88%, 3Al 2o 32SiO 2content 12%.
A preparation method for alumina based ceramic core for directional freeze, comprises the steps:
1, take powder: the EC95 electrofused mullite after smelting is pulverized to shaping, and magnetic separation de-iron, is sieved into granularity and is the powder of No. F200, No. F320, No. F600, and pickling is dry.Take by weight percentage 10% F200 EC95,45% F320 EC95,12% F600 EC95,20% zirconium silicate powder, 2% silicon dioxide powder, 1% titanium dioxide, 10% aluminium powder.
2, ball is mixed: add the oleic acid that accounts for the weight of mixed powder described in step 1 1.5%, add zirconia ceramics ball to mix by ratio of grinding media to material 1.5:1, the ball 6h that does time.
3, join softening agent: take the softening agent that accounts for the weight of mixed powder described in step 1 16%, in softening agent, paraffin and poly ratio are 48:1.Softening agent is put into core material stirrer heat fused, and temperature of fusion is 100 DEG C.
4, mixing: the mixed powder mixing described in step 1 slowly to be joined in core material stirrer, continue to stir 7h, make softening agent and powder mixing evenly.
5, hot-injection molding: utilize ceramic core press injector, controlling injection temperature is 95 DEG C, 40 DEG C of die temperatures, injection pressure 3MPa, dwell time 150s, and mixing uniform core material pressure injection, in ceramic core mould, is made to ceramic core biscuit.
6, finishing, school type: ceramic core biscuit, after finishing, school type, is put into the industrial alumina packing of saggar and buried reality.
7, roasting: the saggar that ceramic core biscuit and commercial alumina filler are housed is put into chamber type electric resistance furnace and carry out roasting, roasting system is: be warming up to 260 DEG C with the temperature rise rate of 2.5 DEG C/min, insulation 5h, be warming up to 480 DEG C with the temperature rise rate of 4 DEG C/min, insulation 3h, be warming up to 650 DEG C with the temperature rise rate of 5 DEG C/min, insulation 2h, be warming up to 950 DEG C with 7 DEG C/min temperature rise rate, insulation 1.5h, is warming up to 1150 DEG C with the temperature rise rate of 9 DEG C/min, insulation 3h, be warming up to 1400 DEG C with the temperature rise rate of 1.5 DEG C/min, insulation 4h, then cools to room temperature with the furnace.
8, High-Temperature Strengthening: the ceramic core after coming out of the stove adopts silicate hydrolyzate liquid to carry out High-Temperature Strengthening.Reinforcer contains tetraethyl silicate 82% by weight percentage, alcohol 11%, and distilled water 5.5%, hydrochloric acid 1.5% content carries out proportioning, the temperature of strict controlled hydrolysis liquid in hydrolytic process, temperature will be used water quench at once higher than 54 DEG C.
9, room temperature strengthening: High-Temperature Strengthening dried ceramic core are carried out to room temperature strengthening, contain by weight percentage phenolic aldehyde spirit varnish 50%, ethanol 45%, hexamethylenetetramine 5% in reinforcer.
specific embodiment 3
A kind of directional freeze alumina based ceramic core, is characterized in that taking EC95 electrofused mullite as base-material, and EC95 electrofused mullite is to add weight percent taking high-quality alundum in electric arc furnace, to form through 2200 DEG C of pyrotic smeltings as 5.5% mineralizer.EC95 electrofused mullite after smelting is with a-Al 2o 3, 3Al 2o 32SiO 2for main xln, wherein α-Al 2o 3content 80.5%, 3Al 2o 32SiO 2content 19.5%.
A preparation method for alumina based ceramic core for directional freeze, comprises the steps:
1, take powder: the EC95 electrofused mullite after smelting is pulverized to shaping, and magnetic separation de-iron, is sieved into granularity and is the powder of No. F200, No. F320, No. F600, and pickling is dry.Take by weight percentage 12% F200 EC95,40% F320 EC95,13% F600 EC95,25% zirconium silicate powder, 1% silicon dioxide powder, 4% titanium dioxide, 5% aluminium powder.
2, ball is mixed: add the oleic acid that accounts for the weight of mixed powder described in step 1 0.5%, add zirconia ceramics ball to mix by ratio of grinding media to material 1.5:1, the ball 8h that does time.
3, join softening agent: take the softening agent that accounts for the weight of mixed powder described in step 1 16%, in softening agent, paraffin and poly ratio are 47:1.Softening agent is put into core material stirrer heat fused, and temperature of fusion is 105 DEG C.
4, mixing: the mixed powder mixing described in step 1 slowly to be joined in core material stirrer, continue to stir 8h, make softening agent and powder mixing evenly.
5, hot-injection molding: utilize ceramic core press injector, controlling injection temperature is 100 DEG C, 50 DEG C of die temperatures, injection pressure 5MPa, dwell time 180s, and mixing uniform core material pressure injection, in ceramic core mould, is made to ceramic core biscuit.
6, finishing, school type: ceramic core biscuit, after finishing, school type, is put into the industrial alumina packing of saggar and buried reality.
7, roasting: the saggar that ceramic core biscuit and commercial alumina filler are housed is put into chamber type electric resistance furnace and carry out roasting, roasting system is: be warming up to 300 DEG C with the temperature rise rate of 4 DEG C/min, insulation 6h, be warming up to 500 DEG C with the temperature rise rate of 6 DEG C/min, insulation 2h, be warming up to 600 DEG C with the temperature rise rate of 6 DEG C/min, insulation 1h, be warming up to 900 DEG C with 8 DEG C/min temperature rise rate, insulation 2h, is warming up to 1100 DEG C with the temperature rise rate of 8 DEG C/min, insulation 2h, be warming up to 1450 DEG C with the temperature rise rate of 2 DEG C/min, insulation 8h, then cools to room temperature with the furnace.
8, High-Temperature Strengthening: the ceramic core after coming out of the stove adopts silicate hydrolyzate liquid to carry out High-Temperature Strengthening.Reinforcer contains tetraethyl silicate 82% by weight percentage, alcohol 12%, and distilled water 5%, hydrochloric acid 1% content carries out proportioning, the temperature of strict controlled hydrolysis liquid in hydrolytic process, temperature will be used water quench at once higher than 54 DEG C.
9, room temperature strengthening: High-Temperature Strengthening dried ceramic core are carried out to room temperature strengthening, contain by weight percentage phenolic aldehyde spirit varnish 55%, ethanol 43%, hexamethylenetetramine 2% in reinforcer.

Claims (2)

1. a directional freeze alumina based ceramic core, is characterized in that taking EC95 electrofused mullite as base-material, and EC95 electrofused mullite is to add weight percent taking alundum in electric arc furnace, to form through >=2000 DEG C of pyrotic smeltings as the mineralizer of 2-6%;
EC95 electrofused mullite is with α-Al 2o 3, 3Al 2o 32SiO 2for main xln, wherein α-Al 2o 3content 80~95%, 3Al 2o 32SiO 2content 5~20%, through pulverizing shaping, magnetic separation de-iron, is sieved into granularity and is the powder of No. F200, No. F320, No. F600, and pickling is dry;
Mineralizer adopts zirconium silicate, silicon dioxide powder, titanium dioxide powder and aluminium powder; Zirconium silicate granularity is No. F320, silicon dioxide powder, and granularity is No. F320, SiO in powder 2content>=96%, titanium dioxide powder size≤30 μ m, TiO 2content>=97%, aluminum powder size≤50 μ m, active A l content>=98%.
2. a preparation method for alumina based ceramic core for directional freeze, is characterized in that comprising following processing step:
1) take powder: the EC95 electrofused mullite powder, zirconium silicate powder, silicon dioxide powder, titanium dioxide powder, the aluminium powder that weigh respectively certainweight are put into ball grinder; EC95 electrofused mullite 65~95% by weight percentage in powder, zirconium silicate 5~30%, silicon dioxide powder 2~8%, titanium dioxide powder 1~5%, aluminium powder 1~10%; Above-mentioned each component concentration sum is 100%; Wherein in EC95 electrofused mullite, F200 powder accounts for 10~30%, F320 powder content 40~70%, and F600 powder accounts for 10~30%; EC95 electrofused mullite is to add weight percent taking alundum in electric arc furnace, to form through >=2000 DEG C of pyrotic smeltings as the mineralizer of 2-6%;
2) ball is mixed: add the oleic acid that accounts for powder weight 0.5~2%, add zirconia ceramics ball to mix by ratio of grinding media to material 1.5:1, the ball 4~8h that does time;
3) join softening agent: take the softening agent that accounts for the weight of mixed powder described in step 1 14~18%, in softening agent, paraffin and poly ratio are 46~49:1; Softening agent is put into core material stirrer heat fused, and temperature of fusion is 90~110 DEG C;
4) mixing: the mixed powder mixing described in step 1 slowly to be joined in core material stirrer, continue to stir 6~8h, make softening agent and powder mixing evenly;
5) hot-injection molding; Utilize ceramic core press injector, according to the size of ceramic core and complexity, controlling injection temperature is 90 DEG C, 450 DEG C of die temperatures, injection pressure 2MPa, dwell time 120s molding parameter, and mixing uniform core material pressure injection, in ceramic core mould, is made to ceramic core biscuit;
6) finishing, school type: ceramic core biscuit, after finishing, school type, is put into the industrial alumina packing of saggar and buried reality;
7) roasting: the saggar that ceramic core biscuit and commercial alumina filler are housed is put into chamber type electric resistance furnace and carry out roasting, roasting system is: be warming up to 200~300 DEG C with the temperature rise rate of 2~5 DEG C/min, insulation 3~6h, be warming up to 400~500 DEG C with the temperature rise rate of 3~6 DEG C/min, insulation 2~4h, be warming up to 600~700 DEG C with the temperature rise rate of 4~7 DEG C/min, insulation 1~2h, be warming up to 900~1000 DEG C with 6~9 DEG C/min temperature rise rate, insulation 1~2h, be warming up to 1100~1200 DEG C with the temperature rise rate of 6~9 DEG C/min, insulation 2~3h, be warming up to 1300~1450 DEG C with the temperature rise rate of 1~2 DEG C/min, insulation 4~8h, then cool to room temperature with the furnace.
CN201310269759.5A 2013-07-01 2013-07-01 Alumina-based ceramic core for directional solidification and preparation method thereof Active CN103304227B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310269759.5A CN103304227B (en) 2013-07-01 2013-07-01 Alumina-based ceramic core for directional solidification and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310269759.5A CN103304227B (en) 2013-07-01 2013-07-01 Alumina-based ceramic core for directional solidification and preparation method thereof

Publications (2)

Publication Number Publication Date
CN103304227A CN103304227A (en) 2013-09-18
CN103304227B true CN103304227B (en) 2014-08-13

Family

ID=49129989

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310269759.5A Active CN103304227B (en) 2013-07-01 2013-07-01 Alumina-based ceramic core for directional solidification and preparation method thereof

Country Status (1)

Country Link
CN (1) CN103304227B (en)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103553635B (en) * 2013-10-30 2015-02-18 东方电气集团东方汽轮机有限公司 Method for producing ceramic die core
CN103693196A (en) * 2013-12-29 2014-04-02 陈俞任 Front-upper air suction and rear-lower air jet type vertical takeoff and landing aircraft
CN104311144B (en) * 2014-09-19 2015-12-30 大连理工大学 A kind of containing perpendicular to bed interface stratiform aluminum oxide-epoxy resin composite material aligning whisker and preparation method thereof
CN104402415B (en) * 2014-11-10 2016-05-18 无锡康伟工程陶瓷有限公司 The production method of the dark footpath of a kind of controllable silicon product
DE102015220395A1 (en) 2015-10-20 2017-04-20 Bayerische Motoren Werke Aktiengesellschaft soot sensor
CN105669198B (en) * 2016-01-16 2018-08-03 上海大学 A kind of preparation method of lanthanum oxide-based ceramic core
CN110128159A (en) * 2019-06-01 2019-08-16 安徽齐鑫新材料科技有限公司 A kind of preparation method of rare earth oxide Al-base ceramic core
CN110342914A (en) * 2019-07-03 2019-10-18 金永和精工制造股份有限公司 A kind of ceramic core and preparation method
CN110256077A (en) * 2019-07-09 2019-09-20 中国航发北京航空材料研究院 A kind of hot investment casting yttria-base ceramic core and preparation method thereof
CN112047726A (en) * 2020-09-02 2020-12-08 上海交通大学 Preparation method of mullite whisker reinforced aluminum-based ceramic core for directional solidification
CN113370344B (en) * 2021-04-28 2023-02-21 潍坊科技学院 Preparation process of directional solidification ceramic part
CN113354398B (en) * 2021-07-08 2022-08-05 西安石油大学 Aluminum oxide-based high-entropy eutectic ceramic and preparation method thereof
CN113860896A (en) * 2021-11-03 2021-12-31 贵州安吉华元科技发展有限公司 High-temperature precision casting low-creep corundum mullite and manufacturing method thereof
CN114349491A (en) * 2022-01-19 2022-04-15 北航(四川)西部国际创新港科技有限公司 Composition for preparing silicon-based ceramic core, silicon-based ceramic core blade of aircraft engine and preparation method of silicon-based ceramic core blade
CN116924815A (en) * 2023-07-27 2023-10-24 中国科学院金属研究所 Hot-pressed ceramic mold core and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101386546A (en) * 2008-10-14 2009-03-18 华南理工大学 Self-reacting alumina-base composite ceramic mold core for fine casting and preparation method thereof
CN101734910A (en) * 2009-12-04 2010-06-16 沈阳黎明航空发动机(集团)有限责任公司 Method for preparing porous alumina ceramic core
CN102531648A (en) * 2011-12-26 2012-07-04 北京航空航天大学 Calcium oxide-based ceramic core for casting titanium alloy and manufacturing method thereof
CN102989994A (en) * 2012-11-28 2013-03-27 沈阳铸造研究所 Preparation method of composite mold core for casting of titanium alloy

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101386546A (en) * 2008-10-14 2009-03-18 华南理工大学 Self-reacting alumina-base composite ceramic mold core for fine casting and preparation method thereof
CN101734910A (en) * 2009-12-04 2010-06-16 沈阳黎明航空发动机(集团)有限责任公司 Method for preparing porous alumina ceramic core
CN102531648A (en) * 2011-12-26 2012-07-04 北京航空航天大学 Calcium oxide-based ceramic core for casting titanium alloy and manufacturing method thereof
CN102989994A (en) * 2012-11-28 2013-03-27 沈阳铸造研究所 Preparation method of composite mold core for casting of titanium alloy

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
定向凝固铸造用氧化铝型壳热强度性能研究;张世东 等;《铸造》;20110430;第60卷(第04期);第338页左栏第1段,第338-339页2试验结果与分析部分,表2,第340页结论部分 *
张世东 等.定向凝固铸造用氧化铝型壳热强度性能研究.《铸造》.2011,第60卷(第04期),第338页左栏第1段,第338-339页2试验结果与分析部分,表2,第340页结论部分.

Also Published As

Publication number Publication date
CN103304227A (en) 2013-09-18

Similar Documents

Publication Publication Date Title
CN103304227B (en) Alumina-based ceramic core for directional solidification and preparation method thereof
CN110845245B (en) Compact high-purity zirconia refractory product
CN101928142B (en) High-purity heavy zirconia refractory product and preparation method
CN103242036B (en) Method for preparing composite ceramic core
CN102531648B (en) Calcium oxide-based ceramic core for casting titanium alloy and manufacturing method thereof
CN101386546B (en) Self-reacting alumina-base composite ceramic mold core for fine casting and preparation method thereof
CN102432332B (en) Method for preparing aluminum oxide porous ceramics by gel-foaming method
CN103979980A (en) Preparation method of zirconia metering nozzle
CN106747369B (en) Silicon-based ceramic core and preparation method thereof
CN104387073B (en) The method of ultra-fine high tenacity thyrite is manufactured based on reaction sintering
CN105732007B (en) A kind of calcium oxide-based ceramic-mould fast preparation method for complex parts manufacture
CN105127373A (en) Manufacturing method of hollow ceramic core for double-wall hollow blade
CN108424124A (en) Magnesium oxide-based crucible of a kind of magnesia crystal whisker fabricated in situ spinelle enhancing and preparation method thereof
CN108546093B (en) Alumina short fiber reinforced magnesium oxide base crucible and preparation method thereof
CN105967668A (en) Preparation method of cordierite-mullite porous ceramic based on rice hulls
CN107540391A (en) A kind of preparation method of high-strength compact zirconium oxide forsterite composite
CN103771878B (en) A kind of method for making of andalusite brick
CN105859297A (en) Silicon carbide composite refractory material and preparation method thereof
CN112028642B (en) Zirconia refractory material and preparation method thereof
CN101186499A (en) Zirconium oxide quaternary system composite ceramic material containing mullite component
CN111807834A (en) Aluminum titanate ceramic for casting and preparation method thereof
CN106565250A (en) High-strength alkali-resistant sialon-corundum composite refractory material and preparation method thereof
CN101486572A (en) Process for preparing ZrO2-Al2TiO5 composite material
CN102584301A (en) Method for preparing zirconium oxide metering nozzle
CN105503208B (en) A kind of method that metering nozzle is prepared using plural gel stabilizing zirconia as matrix

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CP01 Change in the name or title of a patent holder
CP01 Change in the name or title of a patent holder

Address after: No.17, Yunfeng South Street, Tiexi District, Shenyang City, Liaoning Province

Patentee after: SHENYANG RESEARCH INSTITUTE OF FOUNDRY Co.,Ltd.

Address before: No.17, Yunfeng South Street, Tiexi District, Shenyang City, Liaoning Province

Patentee before: Shenyang Research Institute OF Foundry

Address after: No.17, Yunfeng South Street, Tiexi District, Shenyang City, Liaoning Province

Patentee after: Shenyang Foundry Research Institute Co., Ltd. of China National Machinery Research Institute Group

Address before: No.17, Yunfeng South Street, Tiexi District, Shenyang City, Liaoning Province

Patentee before: SHENYANG RESEARCH INSTITUTE OF FOUNDRY Co.,Ltd.