CN102603275B - Preparation method of silicon-based ceramic core - Google Patents

Preparation method of silicon-based ceramic core Download PDF

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Publication number
CN102603275B
CN102603275B CN201210028770.8A CN201210028770A CN102603275B CN 102603275 B CN102603275 B CN 102603275B CN 201210028770 A CN201210028770 A CN 201210028770A CN 102603275 B CN102603275 B CN 102603275B
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powder
silicon
ceramic core
base ceramic
softening agent
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CN102603275A (en
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田刚
王平
谷苍
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BEIJING CHANGHANG PRECISON CASTING Co Ltd
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BEIJING CHANGHANG PRECISON CASTING Co Ltd
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Abstract

The invention relates to a preparation method of a silicon-based ceramic core. The method comprises the steps of: firstly, mixing powder; secondly, preparing a sizing agent, thirdly, compression moulding; and fourthly, sintering. In the step of preparing the sizing agent, the components of a plasticizer comprise: 91-95 percent of paraffin, 4-6 percent of beewax and 1-2 percent of EVA (ethylene-vinyl acetate). The plasticizer accounts for 12-15 percent of the mixed powder. The technical problem to be solved is to ensure that the silicon-based ceramic core has less cracks, less breakage and little deformation during sintering, therefore, the percent of pass of the product is improved.

Description

The preparation method of silicon-base ceramic core
Technical field
The present invention relates to a kind of ceramic core, be specifically related to a kind of preparation method who is applied to the silicon-base ceramic core in precision casting field.
Background technology
Ceramic core is widely used in the precision casting field, casting is one of fundamental technology of modern mechanical manufacturing industry, so to say that, the development of foundry engieering and the lifting of innovating the production strength that indicates a country, although being one, China manufactures big country, but China is not a technology power, due on high-end technology and product, China is implemented to blockade on new techniques abroad always, cause the production technology of China's ceramic core and to compare gap abroad larger, higher level and the market-oriented enterprise of professional production ceramic core preferably also do not appear having in China now.
Ceramic core is a kind of core of manufacturing according to the needed hole of part or chamber, silicon-base ceramic core is little because having the coefficient of expansion, anti-rapid heat cycle ability is strong, physical strength is high, chemical stability is good, the characteristics such as depoling is convenient, and be widely used in the precision casting field, for example, the casting of the turbine blade of aircraft engine, must could form needed hollow shape by means of ceramic core, therefore, the quality of ceramic core can produce great impact to the quality of turbine blade and the performance of engine, during the essence casting, determine the cavity shape of foundry goods and the wall thickness of foundry goods by ceramic core and shell.
Body material as ceramic core must possess five conditions: one, high refractoriness (fusing point or softening temperature are on 1600 ℃); Two, with alloy, higher uncompatibility is arranged; Three, can carry out depoling by chemical process; Four, the linear expansivity be complementary with shell; Five, there is no too much high low temperature crystal conversion after burning till.At present, the body material of ceramic core employed both at home and abroad has silica glass, fused corundom, zircon, magnesium oxide, mullite, spinel or rare earth oxide to guarantee and improves the warm ability of holding of Tao Xin.Except body material, also need to add some subsidiary material in ceramic core, these subsidiary material comprise mineralizer that can acceleration of sintering and promote the softening agent etc. of moulding.The mineralizer role is to form sosoloid or eutectic with matrix in the process of core roasting, and does not form the low melting glass phase.Mineralizer commonly used is zirconium white, magnesium oxide, mullite, commercial alumina and calcium oxide both at home and abroad at present.
The common method of the preparation of ceramic core is hot drape process both at home and abroad at present, the technical process of hot drape process as shown in Figure 1, due to ceramic core in the directional freeze process for a long time in the condition of high temperature, so must there is enough refractoriness and intensity, this is to estimate the major criterion whether ceramic core has good use properties, but also to consider whether easily problem of follow-up depoling, want depoling convenient, must there is certain porosity, simultaneously, must consider the formability of the shape of various complexity, therefore, for ceramic core, be not that performance in a certain respect is better, the use properties of last Tao Xin is just better, a but over-all properties requirement.
Ceramic core more commonly used is silicon oxide series Tao Xin at present, silicon oxide series Tao Xin is usingd fused silica powder as body material, add zirconium English powder, mullite or rare earth oxide etc. as mineralizer, the quantity of dependence controlling party quartz guarantees the over-all properties of Tao Xin.
Disclose the preparation method of a kind of blade of aviation engine with silicon-base ceramic core in Chinese invention patent application prospectus CN102079653A, comprised the following steps: the mixing of the first step, powder; Second step, prepare slurry; The 3rd step, compression moulding; The 4th step, sintering.Wherein, second step, the process for preparing slurry are: softening agent is put in the agitator that oil bath temperature is 70-90 ℃ and dissolved, obtain the first intermediate; The mixture that softening agent is paraffin and beeswax, the mass ratio of paraffin and beeswax is 9/1; Then dry mixed powder step 1 made is added in the first intermediate for 5~10min/ time by the time interval under whipped state, obtains the second intermediate; Tensio-active agent is added in the second intermediate under whipped state, obtains the 3rd intermediate; The 3rd intermediate is carried out to the vacuumizing and exhausting bubble and process, the vacuum meter reading is 0.002~0.02MPa, after vacuumizing 10min~60min, obtains uniform sizing material; The stirring velocity of agitator is 20~60r/min; Required softening agent 10g~12g in the dry mixed powder of consumption: 100g, tensio-active agent 1~2ml.The technical problem easily occurred in technique scheme is will cause the core moulding rate low because the consumption of softening agent is very few.
Softening agent is generally organic thermoplastic material, in their roasting process afterwards, be melted in filler, and volatilization, softening agent is not the moiety of silicon-base ceramic core, just when pressure injection, play the effect of moulding, the add-on of softening agent is generally 15%~20% of powder, the softening agent add-on has significant impact to the core performance, although the add-on of softening agent too much can make core moulding easy, but also can make the percent of firing shrinkage of core and void content increase, and cause the reduction of bending strength and volume density, therefore, should control the usage quantity of softening agent.
The main component of softening agent is paraffin and beeswax, melting point of paraffin wax is at 47 ℃~64 ℃, the fusing point of beeswax is at 62 ℃~64 ℃, because the fusing point of paraffin and beeswax is lower, those skilled in the art person it is generally acknowledged and is being prepared slurry more than 120 ℃, can cause the aging and inharmonious of softening agent, fully mix with softening agent in order to make powder, the agitator speed general control is at 20~60r/min.
Softening agent can cause crackle in sintering process, fracture, in order to solve the problem cracked, general those skilled in the art tends to doing a lot of research aspect the configuration of powder, seldom there is the technician to do in depth research preparing aspect slurry, in fact, each step before sintering can exert an influence to last sintering process, when cracking, not only in the configuration of powder, find reason, simultaneously also should find reason preparing aspect slurry, it is extremely important for the production of silicon-base ceramic core that second step prepares slurry, if that stirs is inhomogeneous, will produce silicon-base ceramic core sintering after strain or crackle.Therefore guarantee how that silicon-base ceramic core few distortion in the process of sintering, few crackle, few fracture are technical barriers urgently to be resolved hurrily.
Summary of the invention
The technical problem to be solved in the present invention be how to make silicon-base ceramic core in the process of sintering, be out of shape little, crackle is few, few fracture, to improve the qualification rate of product, therefore the invention provides a kind of preparation method of silicon-base ceramic core.
For achieving the above object, by the following technical solutions:
A kind of preparation method of silicon-base ceramic core, specific as follows:
The configuration of step 1, powder and mixing
The proportioning of powder is: 75%~82% fused quartz and glass grating powder, 17%~24% zirconium English powder, 1.5%~2% nanometer titanium dioxide silicon quartzite powder;
Fused silica glass grating powder, zirconium English powder, nanometer titanium dioxide silicon quartzite powder are mixed, the powder of mixing is placed in the ball grinder that appropriate distilled water is housed and grinds, obtain powder mix liquid, Ball-milling Time is 110min~130min; Put into the drying baker baking after powder mix liquid is sieved, obtain dry powder mix, drying temperature is 140 ℃~200 ℃, and be 220min~250min time of drying;
Step 2, prepare slurry
The proportioning of softening agent is: 91%~95% paraffin, 4%~6% beeswax, 1%~2% EVA;
Softening agent accounts for 12%~15% of powder mix;
Softening agent is melted up to 160 ℃~180 ℃, by the softening agent melted pour into fast turning round and be preheating in the stirrer of 120 ℃, then powder is added in stirrer fast in batches, add 20~70ml oleic acid simultaneously, after reinforced the beginning, the rotating speed of stirring is increased to 1500r/min; After having fed in raw material, with 1500r/min, stir 1 hour, reduction of speed was to 700r/min continuously stirring 4 hours, and stirrer is cooled to 80~85 ℃ simultaneously;
Step 3, compression moulding
To in step 2, by Tao Xin press injector injection-compression molding, make it form the idiosome of silicon-base ceramic core by resulting slurry; The pressure of Tao Xin press injector is 2MPa~4MPa, and temperature is 80 ℃~90 ℃;
Step 4, sintering
Comprise dewaxing stage and the high-temperature roasting stage of silicon-base ceramic core in step 4, the idiosome of the silicon-base ceramic core that will make in step 3 is placed in the saggar of sintering special use, and cover with low sodium high temperature oxidation aluminium powder, the saggar that then idiosome of silicon-base ceramic core will be housed is put into High Temperature Furnaces Heating Apparatus, carries out low temperature dewaxing and high-temperature roasting.
Especially, in described step 3, when the temperature of Tao Xin press injector rises to 75 ℃~80 ℃, keep homo(io)thermism 60min~70min.
Especially, described paraffin is 58 ° of SEMI-REFINED PARAFFIN WAX or 58 ° of paraffin wax fully refineds.
The beneficial effects of the utility model are: because softening agent accounts for 12%~15% of powder mix, softening agent is melted up to 160 ℃~180 ℃, by the softening agent melted pour into fast turning round and be preheating in the stirrer of 120 ℃, then powder is added in stirrer fast in batches, add 20~70ml oleic acid simultaneously, after reinforced the beginning, the rotating speed of stirring is increased to 1500r/min, after having fed in raw material, with 1500r/min, stir 1 hour, reduction of speed was to 700r/min continuously stirring 4 hours, stirrer is cooled to 80~85 ℃ simultaneously, form slurry, so the paraffin in softening agent is not by before high temperature ageing, under the rapid condition that is 1300r/min~1600r/min at the rotating speed of stirrer, form slurry, can guarantee that like this softening agent mixes with the sufficient of powder, reduced again the consumption of softening agent, and shortened the churning time while preparing slurry, therefore can reduce the disadvantageous effect that softening agent produces sintering simultaneously, greatly reduced the silicon-base ceramic core distortion, crackle, the generation of phenomenon of rupture, thereby guaranteed the conforming product rate of silicon-base ceramic core.
The accompanying drawing explanation
Below according to embodiment and accompanying drawing, the present invention is described in further detail.
Fig. 1 is silicon-base ceramic core preparation technology schema of the prior art.
Embodiment
For avoiding silicon-base ceramic core to produce the generation of distortion, crackle, phenomenon of rupture in the process of sintering, the first embodiment of the present invention is:
The configuration of step 1, powder and mixing
The proportioning of powder is: 77% fused quartz and glass grating powder, 21% zirconium English powder, 2% nanometer titanium dioxide silicon quartzite powder;
Fused silica glass grating powder, zirconium English powder, nanometer titanium dioxide silicon quartzite powder are mixed, the powder of mixing is poured in the ball grinder that appropriate distilled water is housed and ground, obtain powder mix liquid, Ball-milling Time is 110min; Powder mix liquid is put into to the drying baker baking, obtain dry powder mix, drying temperature is 125 ℃, and be 230min time of drying;
Step 2, prepare slurry
The proportioning of softening agent is: 92% paraffin, 6% beeswax, 2% EVA;
Softening agent accounts for 12% of powder mix;
Softening agent is melted up to 160 ℃~180 ℃, by the softening agent liquid melted put into temperature be 120 ℃ stirrer and start running, the powder that will be heated to fast 160 ℃~180 ℃ adds fast in batches, the limit edged gradually raising speed to the stirrer of 1500r/min, until all add, add the oleic acid of 20-100ml simultaneously and be cooled to 80 ℃~85 ℃; Keep 1500r/min to stir 1 hour, then reduction of speed is standby to 700r/min continuously stirring 4 hours;
Step 3, compression moulding
To in step 2, by Tao Xin press injector injection-compression molding, make it form the idiosome of silicon-base ceramic core by resulting slurry; The pressure of Tao Xin press injector is 4MPa, and temperature is 90 ℃; When the temperature of Tao Xin press injector rises to 75 ℃, keep homo(io)thermism, the mold clearing temperature of Tao Xin is not more than 24 ℃ and is advisable;
Step 4, sintering
Comprise dewaxing stage and the high-temperature roasting stage of silicon-base ceramic core in step 4, the idiosome of the silicon-base ceramic core that will make in step 3 is placed in the saggar of sintering special use, and cover with low sodium high temperature oxidation aluminium powder, the saggar that then idiosome of silicon-base ceramic core will be housed is put into High Temperature Furnaces Heating Apparatus, carries out low temperature dewaxing and high-temperature roasting.
The second embodiment of the present invention is:
The configuration of step 1, powder and mixing
The proportioning of powder is: 82% fused quartz and glass grating powder, 16.5% zirconium English powder, 1.5% nanometer titanium dioxide silicon quartzite powder;
Fused silica glass grating powder, zirconium English powder, nanometer titanium dioxide silicon quartzite powder are mixed, the powder of mixing is poured in the ball grinder that appropriate distilled water is housed and ground, obtain powder mix liquid, Ball-milling Time is 130min; Powder mix liquid is sieved and puts into drying baker baking, obtain dry powder mix, drying temperature is to 140 ℃~200 ℃, time of drying 250min;
Step 2, prepare slurry
The proportioning of softening agent is: 95% paraffin, 4% beeswax, 1% EVA;
Softening agent accounts for 15% of powder mix;
Softening agent is melted, the softening agent liquid melted is placed in the stirrer run up, it is stirred in 180 ℃ of temperature, under the condition that the rotating speed of stirrer is 1300r/min, carry out, to adding powder after oven dry and the oleic acid of 90ml in stirrer, churning time is 4min, forms slurry again;
Step 3, compression moulding
To in step 2, by Tao Xin press injector injection-compression molding, make it form the idiosome of silicon-base ceramic core by resulting slurry; The pressure of Tao Xin press injector is 3MPa, and temperature is 80 ℃; The Tao Xin mold clearing temperature is not more than 24 ℃;
Step 4, sintering
Comprise dewaxing stage and the high-temperature roasting stage of silicon-base ceramic core in step 4, the idiosome of the silicon-base ceramic core that will make in step 3 is placed in the saggar of sintering special use, and cover with low sodium high temperature oxidation aluminium powder, the saggar that then idiosome of silicon-base ceramic core will be housed is put into High Temperature Furnaces Heating Apparatus, carries out low temperature dewaxing and high-temperature roasting.
Above embodiment has just set forth ultimate principle of the present invention and characteristic; the present invention is not limited by above-described embodiment; without departing from the spirit and scope of the present invention, the present invention also has various variations and change, and these variations and change all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (3)

1. the preparation method of a silicon-base ceramic core is characterized in that:
The configuration of step 1, powder and mixing
The proportioning of powder is: 75%~82% fused quartz and glass grating powder, 17%~24% zirconium English powder, 1.5%~2% nanometer titanium dioxide silicon quartzite powder, and above each proportioning sum is 100%;
Fused silica glass grating powder, zirconium English powder, nanometer titanium dioxide silicon quartzite powder are mixed, the powder of mixing is placed in the ball grinder that appropriate distilled water is housed and grinds, obtain powder mix liquid, Ball-milling Time is 110min~130min; Put into the drying baker baking after powder mix liquid is sieved, obtain dry powder mix, drying temperature is 140 ℃~200 ℃, and be 220min~250min time of drying;
Step 2, prepare slurry
The proportioning of softening agent is: 91%~95% paraffin, 4%~6% beeswax, 1%~2% EVA, and above each proportioning sum is 100%;
Softening agent accounts for 12%~15% of powder mix;
Softening agent is melted up to 160 ℃~180 ℃, by the softening agent melted pour into fast turning round and be preheating in the stirrer of 120 ℃, then powder is added in stirrer fast in batches, add 20~70ml oleic acid simultaneously, after reinforced the beginning, the rotating speed of stirring is increased to 1500r/min; After having fed in raw material, with 1500r/min, stir 1 hour, reduction of speed was to 700r/min continuously stirring 4 hours, and stirrer is cooled to 80~85 ℃ simultaneously;
Step 3, compression moulding
To in step 2, by Tao Xin press injector injection-compression molding, make it form the idiosome of silicon-base ceramic core by resulting slurry; The pressure of Tao Xin press injector is 2MPa~4MPa, and temperature is 80 ℃~90 ℃;
Step 4, sintering
Comprise dewaxing stage and the high-temperature roasting stage of silicon-base ceramic core in step 4, the idiosome of the silicon-base ceramic core that will make in step 3 is placed in the saggar of sintering special use, and cover with low sodium high temperature oxidation aluminium powder, the saggar that then idiosome of silicon-base ceramic core will be housed is put into High Temperature Furnaces Heating Apparatus, carries out low temperature dewaxing and high-temperature roasting.
2. the preparation method of a kind of silicon-base ceramic core according to claim 1, is characterized in that: in described step 3, when the temperature of Tao Xin press injector rises to 75 ℃~80 ℃, keep homo(io)thermism 60min~70min.
3. the preparation method of a kind of silicon-base ceramic core according to claim 1, it is characterized in that: described paraffin is 58 ° of SEMI-REFINED PARAFFIN WAX or 58 ° of paraffin wax fully refineds.
CN201210028770.8A 2012-02-09 2012-02-09 Preparation method of silicon-based ceramic core Expired - Fee Related CN102603275B (en)

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