CN106278276B - A kind of preparation method densifying carborundum based material - Google Patents

A kind of preparation method densifying carborundum based material Download PDF

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CN106278276B
CN106278276B CN201610672922.6A CN201610672922A CN106278276B CN 106278276 B CN106278276 B CN 106278276B CN 201610672922 A CN201610672922 A CN 201610672922A CN 106278276 B CN106278276 B CN 106278276B
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silicon carbide
biscuit
preparation
particle
carbon composite
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CN106278276A (en
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梅庆波
王龙
陆娜
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Ningbo Ocean Fine Ceramic Technology Co., Ltd.
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NINGBO OCEAN FINE CERAMIC TECHNOLOGY Co Ltd
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Abstract

The invention discloses a kind of preparation methods for densifying carborundum based material, belong to technical field of material.The present invention takes carbon nano-particle and silicon powder as raw material, silicon carbide/carbon composite granule is made by Mechanochemical Effect, and and ethanol solution, tetramethylammonium hydroxide, carboxymethyl cellulose carries out ball mill mixing slurrying, spheric granules and aluminium oxide are made after spray-dried, zirconium dioxide mixing is placed in mold, it is pressed into biscuit, and it uniformly sprays and uses calcium carbonate, the crushing such as cordierite and water mix the glaze slurries of preparation in biscuit surface, up to densification carborundum based material after drying and calcining, solves the defect that low-temperature cracks easily occurs in Conventional silicon carbide composite material, glaze slurry infiltration enters hole, reduce voidage, densify composite material more, with excellent use value.

Description

A kind of preparation method densifying carborundum based material
Technical field
The invention discloses a kind of preparation methods for densifying carborundum based material, belong to material preparation technology neck Domain.
Background technique
With the development of new engine and the development of new concept space launch vehicle, high-temperature structural material is proposed higher Requirement.Fiber reinforced ceramic matrix composites because having high intensity, high tenacity, high temperature resistant, corrosion resistance good at high temperature and The excellent performances such as low-density are with a wide range of applications in the fields such as strategic arms and space technology, in recent years increasingly by To the attention of material worker.In defence and military and aerospace field, carborundum based material is in novel aerospace craft Etc. show wide application prospect.In the civil fields such as communications and transportation and new energy, nuclear fusion plasma generating device And brake block of bullet train, express elevator etc. also proposes strong demand to carborundum based material.
Carborundum based material has that high temperature resistant, density is low, intensity is high, anticorrosive and low thermal expansion coefficient etc. is excellent Structural behaviour, it has also become most potential one of the high temperature structural material of the hot-end components such as aero-engine.Due to preparation The limitation of technique, material inevitably remains 10~15% hole during the preparation process, simultaneously as composite material is each The thermal expansion coefficient of structural unit is different, and residual thermal stress makes material itself generate a large amount of micro-crack.Hole and crackle are deposited It is especially even more serious to the influence of strength and stiffness in the mechanical property for influencing composite material.Silicon carbide ceramics has good Elevated temperature strength, high-temperature stability and high-temperature oxidation resistance, but due to the bonding feature of its molecular structure, lack plastic deformation ability Power shows as brittleness, has seriously affected its application as structural material.Carbon fiber possesses good mechanical behavior under high temperature and heat Performance, being still able to maintain its mechanical property not more than 2000 DEG C in inert environments reduces.With carbon fibre reinforced silicon carbide ceramics, material Material absorbs energy by mechanism such as crack deflection, fibrous fracture and spike protein genes in fracture process, has both enhanced the strong of material Degree and toughness, and maintain the good high-temperature behavior of silicon carbide ceramics.But still have 10% or so by modified composite material Hole, can not further densify, to influence its intensity and rigidity property, also have complex process, long preparation period, at The disadvantages of this is high, fibre reinforced carbon fiber and silicon carbide substrate thermal expansion matching are not ideal enough, and there are more low-temperature cracks to lack Fall into, when being more than 1400 DEG C using temperature, the fusing of silicon and so that material is lost mechanical strength, affect silicon carbide fiber reinforced base The high-temperature behavior of composite material constrains the development of composite material.
Summary of the invention
Present invention mainly solves the technical issues of：For current Conventional silicon carbide based composites, there are carbon fibers and carbonization Silicon substrate matching degree is not high, leads to defect often cracked under low-temperature condition, and the present invention takes carbon nano-particle and silicon powder to make For raw material, silicon carbide/carbon composite granule is made by Mechanochemical Effect, and and ethanol solution, tetramethylammonium hydroxide, carboxylic Methylcellulose carries out ball mill mixing slurrying, and spheric granules is made after spray-dried and is placed in aluminium oxide, zirconium dioxide mixing In mold, it is pressed into biscuit, and uniformly the crushing such as sprinkling calcium carbonate, cordierite and water mix the glaze slurries of preparation in biscuit Surface solves Conventional silicon carbide composite material and low temperature easily occurs up to densification carborundum based material after drying and calcining The defect of crackle, glaze slurry infiltration enter hole, reduce voidage, densify composite material more, have excellent Use value.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
（1）200 ~ 240g carbon nano-particle is weighed, 280 ~ 300g silicon powder is added in vacuum ball grinder, is evacuated to after sealing Vacuum degree is 1 ~ 10Pa in tank, and being passed through argon gas to pressure inside the tank is 0.1 ~ 0.2MPa, is placed on planetary ball mill, with 150 ~ 200r/min ball milling 20 ~ for 24 hours, obtain silicon carbide/carbon composite granule；
（2）The above-mentioned silicon carbide/carbon composite granule of 200 ~ 300g is weighed, is fitted into ball grinder, 300 ~ 350mL mass point is added Counting is 65% ethanol solution, 2 ~ 3g tetramethylammonium hydroxide, and 6 ~ 9g carboxymethyl cellulose stirs evenly to obtain mixed liquor, and loads 400 ~ 600g diameter is 10 ~ 15mm polyurethane steel ball, ball grinder is placed in three-dimensional material mixer, wet ball grinding to in-tank mixing liquid Viscosity is 2000 ~ 2500mPas, obtains mixed slurry；
（3）By above-mentioned mixed slurry, it is to continue to heat in 110 ~ 120 DEG C of spray dryers that addition, which is preheated to inlet temperature, It is 150 ~ 160 DEG C to inlet temperature, slurry is sprayed into atomization through drive nozzle under 0.05 ~ 0.10MPa pressure, at 80 ~ 90 DEG C 3 ~ 4h of lower drying, the particle after collecting drying cross 200 meshes and obtain silicon carbide/carbon composite spheroidal particle, spare；
（4）23 ~ 25g calcium carbonate, 33 ~ 35g aluminium oxide, 40 ~ 45g cordierite, 4 ~ 5g potassium feldspar, addition crushing are weighed respectively It is crushed in machine, crosses 200 meshes, the powder after sieving is added after mixing in 300 ~ 320mL deionized water, with 500 ~ 600r/min stirs 1 ~ 2h, obtains glaze slurries；
（5）Weigh 200 ~ 250g above-mentioned steps（3）The silicon carbide/carbon composite spheroidal particle of preparation, 5 ~ 7g aluminium oxide, 2 ~ 4g Zirconium dioxide is uniformly mixed, and is fitted into mold, and 1 ~ 2min is suppressed at 250 ~ 300MPa, obtains biscuit, and above-mentioned glaze slurries are equal It is even to be sprayed at biscuit surface, it is transferred in vacuum oven, dry 6 ~ 8h, is placed in height for the biscuit after drying at 150 ~ 160 DEG C In warm sintering furnace, under argon atmosphere, 2000 ~ 2100 DEG C is warming up to 20 DEG C/min, 1 ~ 2h of temperature calcination is kept, is cooled to room Temperature obtains densification carborundum based material.
Composite material of silicon carbide tensile strength produced by the present invention is 450 ~ 650MPa, and elasticity modulus is 99 ~ 130GPa, is led Hot coefficient is 0.4 ~ 0.7cal/cms DEG C, and density is 2.7 ~ 2.9g/cm3, thermal expansion coefficient is 16.0 × 10-6~18.0× 10-6m/℃。
The beneficial effects of the invention are as follows：
（1）Carbon fiber and carbon-silicon carbide substrate thermal expansion matching are good, and composite material low-temperature cracks defect substantially reduces, low Warm antioxygenic property improves, and Modulus of Composites reduces, and fracture of composite materials toughness improves；
（2）The preparation method period of the present invention is short, at low cost, can facilitate carry out matrices of composite material structure design and it is excellent Change, the matrices of composite material of preparation is uniform, and consistency is high, good mechanical performance, good in oxidation resistance and large-scale production is suitble to answer With.
Specific embodiment
200 ~ 240g carbon nano-particle is weighed first, and 280 ~ 300g silicon powder is added in vacuum ball grinder, is evacuated to after sealing Vacuum degree is 1 ~ 10Pa in tank, and being passed through argon gas to pressure inside the tank is 0.1 ~ 0.2MPa, is placed on planetary ball mill, with 150 ~ 200r/min ball milling 20 ~ for 24 hours, obtain silicon carbide/carbon composite granule；The above-mentioned silicon carbide/carbon composite granule of 200 ~ 300g is weighed, is packed into In ball grinder, addition 300 ~ 350mL mass fraction is 65% ethanol solution, 2 ~ 3g tetramethylammonium hydroxide, 6 ~ 9g carboxymethyl cellulose Element stirs evenly to obtain mixed liquor, and loading 400 ~ 600g diameter is 10 ~ 15mm polyurethane steel ball, ball grinder is placed in three-dimensional mixed In material machine, wet ball grinding to in-tank mixing fluid viscosity is 2000 ~ 2500mPas, obtains mixed slurry；By above-mentioned mixed slurry, add Entering to be preheated to inlet temperature is to continue to be heated to inlet temperature to be 150 ~ 160 DEG C, by slurry in 110 ~ 120 DEG C of spray dryers Atomization is sprayed under 0.05 ~ 0.10MPa pressure through drive nozzle, dry 3 ~ 4h at 80 ~ 90 DEG C, the particle after collecting drying, It crosses 200 meshes and obtains silicon carbide/carbon composite spheroidal particle, it is spare；Weigh 23 ~ 25g calcium carbonate respectively, 33 ~ 35g aluminium oxide, 40 ~ 45g cordierite, 4 ~ 5g potassium feldspar are added in pulverizer and crush, and cross 200 meshes, the powder after sieving is added after mixing In 300 ~ 320mL deionized water, 1 ~ 2h is stirred with 500 ~ 600r/min, obtains glaze slurries；Weigh the above-mentioned preparation of 200 ~ 250g Silicon carbide/carbon composite spheroidal particle, 5 ~ 7g aluminium oxide, 2 ~ 4g zirconium dioxide are uniformly mixed, are fitted into mold, in 250 ~ 300MPa 1 ~ 2min of lower compacting, obtains biscuit, and above-mentioned glaze slurries are uniformly sprayed at biscuit surface, are transferred in vacuum oven, 150 ~ Dry 6 ~ 8h, the biscuit after drying is placed in high temperature sintering furnace, under argon atmosphere, is warming up to 20 DEG C/min at 160 DEG C 2000 ~ 2100 DEG C, 1 ~ 2h of temperature calcination is kept, is cooled to room temperature, obtains densification carborundum based material.
Example 1
200g carbon nano-particle is weighed first, and 280g silicon powder is added in vacuum ball grinder, vacuum in tank is evacuated to after sealing Degree is 1Pa, and being passed through argon gas to pressure inside the tank is 0.1MPa, is placed on planetary ball mill, with 150r/min ball milling 20h, obtains carbon SiClx/carbon composite powder；The above-mentioned silicon carbide/carbon composite granule of 200g is weighed, is fitted into ball grinder, 300mL mass fraction is added For 65% ethanol solution, 2g tetramethylammonium hydroxide, 6g carboxymethyl cellulose stirs evenly to obtain mixed liquor, and loads 400g diameter For 10mm polyurethane steel ball, ball grinder is placed in three-dimensional material mixer, wet ball grinding to in-tank mixing fluid viscosity is 2000mPa S obtains mixed slurry；By above-mentioned mixed slurry, it is to continue to be heated in 110 DEG C of spray dryers that addition, which is preheated to inlet temperature, Inlet temperature is 150 DEG C, and slurry is sprayed atomization through drive nozzle under 0.05MPa pressure, and the dry 3h at 80 DEG C is collected dry Particle after dry crosses 200 meshes and obtains silicon carbide/carbon composite spheroidal particle, spare；Weigh 23g calcium carbonate respectively, 33g aluminium oxide, 40g cordierite, 4g potassium feldspar are added in pulverizer and crush, and cross 200 meshes, the powder after sieving is added after mixing In 300mL deionized water, 1h is stirred with 500r/min, obtains glaze slurries；Weigh the silicon carbide/carbon composite balls of the above-mentioned preparation of 200g Shape particle, 5g aluminium oxide, 2g zirconium dioxide are uniformly mixed, are fitted into mold, suppress 1min at 250MPa, obtain biscuit, will be upper It states glaze slurries and is uniformly sprayed at biscuit surface, be transferred in vacuum oven, the dry 6h at 150 DEG C, by the biscuit after drying It is placed in high temperature sintering furnace, under argon atmosphere, is heated up 2000 DEG C with 20 DEG C/min, keep temperature calcination 1h, be cooled to room temperature, Carborundum based material must be densified.
Composite material of silicon carbide tensile strength 450MPa produced by the present invention, elasticity modulus 99GPa, thermal coefficient 0.4cal/cms DEG C, density 2.7g/cm3, thermal expansion coefficient is 16.0 × 10-6℃。
Example 2
220g carbon nano-particle is weighed first, and 290g silicon powder is added in vacuum ball grinder, vacuum in tank is evacuated to after sealing Degree is 5Pa, and being passed through argon gas to pressure inside the tank is 0.15MPa, is placed on planetary ball mill, with 170r/min ball milling 22h, obtains carbon SiClx/carbon composite powder；The above-mentioned silicon carbide/carbon composite granule of 250g is weighed, is fitted into ball grinder, 330mL mass fraction is added For 65% ethanol solution, 2.5g tetramethylammonium hydroxide, 8g carboxymethyl cellulose stirs evenly to obtain mixed liquor, and it is straight to load 500g Diameter is 13mm polyurethane steel ball, ball grinder is placed in three-dimensional material mixer, wet ball grinding to in-tank mixing fluid viscosity is 2300mPas obtains mixed slurry；By above-mentioned mixed slurry, addition is preheated to inlet temperature and is in 115 DEG C of spray dryers, after The continuous inlet temperature that is heated to is 155 DEG C, and slurry is sprayed atomization through drive nozzle under 0.07MPa pressure, dry at 85 DEG C 3.5h, the particle after collecting drying cross 200 meshes and obtain silicon carbide/carbon composite spheroidal particle, spare；24g carbonic acid is weighed respectively Calcium, 34g aluminium oxide, 43g cordierite, 4.5g potassium feldspar are added in pulverizer and crush, and cross 200 meshes, the powder after sieving is mixed It is added in 310mL deionized water after closing uniformly, 1.5h is stirred with 550r/min, obtains glaze slurries；Weigh the above-mentioned preparation of 230g Silicon carbide/carbon composite spheroidal particle, 6g aluminium oxide, 3g zirconium dioxide are uniformly mixed, are fitted into mold, suppress at 270MPa 1.5min obtains biscuit, and above-mentioned glaze slurries are uniformly sprayed at biscuit surface, are transferred in vacuum oven, dry at 155 DEG C Biscuit after drying is placed in high temperature sintering furnace by 7h, under argon atmosphere, is warming up to 2050 DEG C with 20 DEG C/min, is kept temperature Degree calcining 1.5h, is cooled to room temperature, obtains densification carborundum based material.
Composite material of silicon carbide tensile strength 500MPa produced by the present invention, elasticity modulus 110GPa, thermal coefficient are 0.5cal/cms DEG C, density 2.8g/cm3, thermal expansion coefficient is 17.0 × 10-6℃。
Example 3
240g carbon nano-particle is weighed first, and 300g silicon powder is added in vacuum ball grinder, vacuum in tank is evacuated to after sealing Degree is 10Pa, and being passed through argon gas to pressure inside the tank is 0.2MPa, is placed on planetary ball mill, for 24 hours with 200r/min ball milling, obtains carbon SiClx/carbon composite powder；The above-mentioned silicon carbide/carbon composite granule of 300g is weighed, is fitted into ball grinder, 350mL mass fraction is added For 65% ethanol solution, 3g tetramethylammonium hydroxide, 9g carboxymethyl cellulose stirs evenly to obtain mixed liquor, and loads 600g diameter For 15mm polyurethane steel ball, ball grinder is placed in three-dimensional material mixer, wet ball grinding to in-tank mixing fluid viscosity is 2500mPa S obtains mixed slurry；By above-mentioned mixed slurry, it is to continue to be heated in 120 DEG C of spray dryers that addition, which is preheated to inlet temperature, Inlet temperature is 160 DEG C, and slurry is sprayed atomization through drive nozzle under 0.10MPa pressure, and the dry 4h at 90 DEG C is collected dry Particle after dry crosses 200 meshes and obtains silicon carbide/carbon composite spheroidal particle, spare；Weigh 25g calcium carbonate respectively, 35g aluminium oxide, 45g cordierite, 5g potassium feldspar are added in pulverizer and crush, and cross 200 meshes, the powder after sieving is added after mixing In 320mL deionized water, 2h is stirred with 600r/min, obtains glaze slurries；Weigh the silicon carbide/carbon composite balls of the above-mentioned preparation of 250g Shape particle, 7g aluminium oxide, 4g zirconium dioxide are uniformly mixed, are fitted into mold, suppress 2min at 300MPa, obtain biscuit, will be upper It states glaze slurries and is uniformly sprayed at biscuit surface, be transferred in vacuum oven, the dry 8h at 160 DEG C, by the biscuit after drying It is placed in high temperature sintering furnace, under argon atmosphere, is warming up to 2100 DEG C with 20 DEG C/min, keeps temperature calcination 2h, be cooled to room Temperature obtains densification carborundum based material.
Composite material of silicon carbide tensile strength 650MPa produced by the present invention, elasticity modulus 130GPa, thermal coefficient are 0.7cal/cms DEG C, density 2.9g/cm3, thermal expansion coefficient is 18.0 × 10-6℃。

Claims (1)

1. a kind of preparation method for densifying carborundum based material, it is characterised in that specifically preparation step is：
（1）200 ~ 240g carbon nano-particle is weighed, 280 ~ 300g silicon powder is added in vacuum ball grinder, is evacuated in tank after sealing Vacuum degree is 1 ~ 10Pa, and being passed through argon gas to pressure inside the tank is 0.1 ~ 0.2MPa, is placed on planetary ball mill, with 150 ~ 200r/ Min ball milling 20 ~ for 24 hours, obtain silicon carbide/carbon composite granule；
（2）The above-mentioned silicon carbide/carbon composite granule of 200 ~ 300g is weighed, is fitted into ball grinder, 300 ~ 350mL mass fraction, which is added, is 65% ethanol solution, 2 ~ 3g tetramethylammonium hydroxide, 6 ~ 9g carboxymethyl cellulose stir evenly to obtain mixed liquor, and load 400 ~ 600g diameter is 10 ~ 15mm polyurethane steel ball, ball grinder is placed in three-dimensional material mixer, wet ball grinding to in-tank mixing fluid viscosity For 2000 ~ 2500mPas, mixed slurry is obtained；
（3）By above-mentioned mixed slurry, addition be preheated to inlet temperature and be in 110 ~ 120 DEG C of spray dryers continue to be heated into Mouth temperature is 150 ~ 160 DEG C, and slurry is sprayed atomization through drive nozzle under 0.05 ~ 0.10MPa pressure, is done at 80 ~ 90 DEG C Dry 3 ~ 4h, the particle after collecting drying cross 200 meshes and obtain silicon carbide/carbon composite spheroidal particle, spare；
（4）Weigh 23 ~ 25g calcium carbonate respectively, 33 ~ 35g aluminium oxide, 40 ~ 45g cordierite, 4 ~ 5g potassium feldspar is added in pulverizer It crushes, crosses 200 meshes, the powder after sieving is added after mixing in 300 ~ 320mL deionized water, with 500 ~ 600r/min 1 ~ 2h is stirred, glaze slurries are obtained；
（5）Weigh 200 ~ 250g above-mentioned steps（3）The silicon carbide/carbon composite spheroidal particle of preparation, 5 ~ 7g aluminium oxide, 2 ~ 4g dioxy Change zirconium to be uniformly mixed, be fitted into mold, 1 ~ 2min is suppressed at 250 ~ 300MPa, biscuit is obtained, by step（4）Gained glaze slurries It uniformly is sprayed at biscuit surface, is transferred in vacuum oven, dry 6 ~ 8h, the biscuit after drying is placed at 150 ~ 160 DEG C In high temperature sintering furnace, under argon atmosphere, 2000 ~ 2100 DEG C is warming up to 20 DEG C/min, 1 ~ 2h of temperature calcination is kept, is cooled to Room temperature obtains densification carborundum based material.
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