CN114751758A - Release agent and preparation method and application thereof - Google Patents
Release agent and preparation method and application thereof Download PDFInfo
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- CN114751758A CN114751758A CN202210365736.3A CN202210365736A CN114751758A CN 114751758 A CN114751758 A CN 114751758A CN 202210365736 A CN202210365736 A CN 202210365736A CN 114751758 A CN114751758 A CN 114751758A
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- release agent
- crucible
- ceramic matrix
- matrix composite
- ball milling
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- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 85
- 239000011153 ceramic matrix composite Substances 0.000 claims abstract description 48
- 239000000463 material Substances 0.000 claims abstract description 40
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 35
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 32
- 238000000498 ball milling Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 29
- 230000008595 infiltration Effects 0.000 claims description 25
- 238000001764 infiltration Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 14
- 238000000746 purification Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 239000006082 mold release agent Substances 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 15
- 239000010453 quartz Substances 0.000 abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 12
- 239000002131 composite material Substances 0.000 abstract description 7
- 239000010431 corundum Substances 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 abstract 1
- 229910052582 BN Inorganic materials 0.000 description 30
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 30
- 238000000227 grinding Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 230000003578 releasing effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000003801 milling Methods 0.000 description 3
- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
Abstract
The invention provides a release agent, and a preparation method and application thereof, and belongs to the field of preparation of ceramic matrix composite materials. The release agent provided by the invention comprises 60-90% of BN and 5-35% of B by mass percentage2O3And 5-15% of Al2O3. The invention takes BN as the base material, which can lead the BN to have better demoulding effect; b2O3The high-temperature inertia of the release agent can be improved, so that the release agent is prevented from reacting with the quartz crucible to be adhered; al (aluminum)2O3Can play a synergistic action with BN, further improve the high temperature resistance of the release agent, thereby improving the release effect of the BN and solving the problem of the release of the corundum crucible. The results of the examples show that when the release agent provided by the invention is used for preparing the ceramic matrix composite at the temperature of 1400-1700 ℃, the release agent cannot be adhered to a crucible, and the prepared composite can be taken out conveniently and cannot be applied to the composite and the ceramic matrix compositeThe crucible is damaged.
Description
Technical Field
The invention relates to the field of preparation of ceramic matrix composite materials, in particular to a release agent and a preparation method and application thereof.
Background
With the continuous improvement of the working temperature of the turbine of the aero-engine, a more rigorous requirement is provided for the high temperature resistance and the high bearing capacity of the aero-engine material, and the latest aero-engine in the world already adopts the ceramic matrix composite material as the high temperature structural material of the latest generation of engine, so that the research on the preparation of the ceramic matrix composite material applied to the field of aero-engines is urgently needed to be developed.
The ceramic matrix composite material has the compatibility of the traditional composite material preparation method, and various preparation processes and preparation methods exist. The process scheme of the process for preparing the ceramic matrix composite material by the reactive infiltration method has a relatively short preparation period, and the process scheme of the process for preparing the ceramic matrix composite material with relatively good prospect in the future is considered to be a process scheme for preparing the ceramic matrix composite material with relatively good prospect.
In the process of preparing the composite material by using the reaction infiltration process, the infiltration raw material needs to be melted and infiltrated into the fiber woven body by adopting high temperature to prepare the required material, and in the process, the residual raw material is adhered to a reaction container (crucible) after being cooled, so that the material is difficult to demould. Although the traditional release agent BN can improve the release effect to a certain extent, the BN can be partially bonded with the crucible at high temperature, so that the release effect is poor, and the obtained material and the crucible are damaged during release.
Therefore, it is an urgent technical problem in the art to provide a release agent which is suitable for a reaction infiltration process and has a good release effect.
Disclosure of Invention
The invention aims to provide a release agent, a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a mold release agent which comprises, by mass, 60-90% of BN and 5-35% of B2O3And 5-15% of Al2O3。
Preferably, the release agent comprises 60-80% of BN and 10-25% of B in percentage by mass2O3And 5-10% of Al2O3。
Preferably, the release agent comprises 60-70% of BN and 15-25% of B in percentage by mass2O3And 10-15% of Al2O3。
Preferably, the mold release agent comprises 90% of BN and 5% of B in percentage by mass2O3And 5% of Al2O3。
The invention provides a preparation method of the release agent in the technical scheme, which comprises the following steps:
(1) BN, B2O3And Al2O3Performing ball milling and mixing to obtain ball milling powder;
(2) and (2) sequentially drying and purifying the ball-milled powder obtained in the step (1) to obtain the release agent.
Preferably, the rotation speed of ball milling in the step (1) is 200-600 r/min, and the ball milling time is 1-5 h.
Preferably, the temperature of the drying treatment in the step (2) is 60-100 ℃, and the time of the drying treatment is 5-10 h.
Preferably, the temperature of the purification treatment in the step (2) is 200-300 ℃, and the time of the purification treatment is 0.5-2 h.
The invention provides a method for preparing a ceramic matrix composite material by adopting a reaction infiltration process, which is characterized in that a release agent prepared by adopting the technical scheme or the preparation method of the technical scheme is used as the release agent.
Preferably, the method for preparing the ceramic matrix composite material by adopting the reaction infiltration process comprises the following steps of:
1) uniformly coating a release agent on the inner surface of the crucible, and then compacting to obtain a non-adhesive crucible;
2) adding the raw materials of the ceramic matrix composite material into the non-adhesive crucible obtained in the step 1), and carrying out infiltration treatment to obtain the ceramic matrix composite material.
The invention provides a mold release agent which comprises, by mass, 60-90% of BN and 5-35% of B2O3And 5-15% of Al2O3. The invention takes BN as the base material, which can make it have better demoulding effect; by adding B2O3The high-temperature inertia of the release agent can be improved, so that the release agent is prevented from reacting with the quartz crucible to be adhered; al (Al)2O3Can play a synergistic action with BN, further improve the high temperature resistance of the release agent, thereby improving the release effect of the BN and solving the problem of the release of the corundum crucible. The results of the examples show that when the release agent provided by the invention is used for preparing the ceramic matrix composite material at the temperature of 1400-1700 ℃ by adopting the reaction infiltration process, the release agent cannot be adhered to a crucible, the prepared composite material can be taken out conveniently, and the composite material and the crucible cannot be damaged.
Drawings
FIG. 1 is a macroscopic view of a ceramic matrix composite and a high purity quartz crucible obtained in application example 1 of the present invention;
FIG. 2 is a macroscopic view of the high purity quartz crucible after the ceramic matrix composite material is taken out in application example 1 of the present invention;
FIG. 3 is a macroscopic view of the ceramic matrix composite prepared in application example 1 of the present invention;
FIG. 4 is a macroscopic view of the ceramic matrix composites prepared according to application example 2 and comparative example 1 of the present invention.
Detailed Description
The invention provides a release agent which comprises, by mass, 60-90% of BN and 5-35% of B2O3And 5-15% of Al2O3。
In the present invention, the BN, B2O3And Al2O3The particle size of (B) is preferably 100 mesh or more. The invention is directed to the BN, B2O3And Al2O3The source of (A) is not particularly limited, and commercially available products known to those skilled in the art may be used. According to the invention, the particle size of each component is controlled within the range, so that the components can be mixed more uniformly, and the high temperature resistance and the demolding effect of the demolding agent are further improved.
In the invention, the release agent preferably comprises 60-80% of BN and 10-25% of B in percentage by mass2O3And 5-10% of Al2O3Or preferably 60 to 70% of BN and 15 to 25% of B 2O3And 10-15% of Al2O3. The invention adjusts B in the release agent2O3And Al2O3The content of (2) enables the release agent to be suitable for quartz crucibles of different models.
In the present invention, the release agent is preferably 90% BN or 5% B in mass percentage2O3And 5% of Al2O3. In the present invention, when the components of the release agent satisfy the above conditions, the release agent is more suitable for use in a graphite crucible.
The release agent provided by the invention comprises 60-90% of BN (boron nitride), preferably 65-85%, more preferably 70-80%, and further preferably 75-80% by mass. In the present invention, the BN as a base material can provide a good mold release effect.
According to the mass percentage, the release agent provided by the invention comprises 5-35% of B2O3Preferably 10 to 30%, more preferably 15 to 25%, and still more preferably 20 to 25%. The invention is realized by adding B2O3The high-temperature inertia of the release agent can be improved, so that the release agent is prevented from reacting with the quartz crucible to cause adhesion.
According to the mass percentage, the release agent provided by the invention comprises 5-15% of Al2O3Preference is given to5 to 10 percent. In the present invention, the Al2O3The high-temperature-resistant BN releasing agent can play a synergistic role with BN, so that the high-temperature-resistant performance of the releasing agent is further improved, the releasing effect of the BN is improved, and the releasing problem of the corundum crucible is solved; by controlling Al 2O3The dosage of the silicon carbide powder can play an excellent demoulding effect on crucibles of different materials.
The release agent provided by the invention has a good high-temperature resistant effect, and can not react with a crucible at the high temperature of infiltration, so that the release agent has a good release effect.
The invention provides a preparation method of the release agent in the technical scheme, which comprises the following steps:
(1) BN, B2O3And Al2O3Performing ball milling and mixing to obtain ball milling powder;
(2) and (2) sequentially drying and purifying the ball-milled powder obtained in the step (1) to obtain the release agent.
BN, B2O3、Al2O3Ball milling and mixing are carried out to obtain ball milling powder.
In the present invention, the milling balls used for the ball milling are preferably zirconia balls. In the present invention, the BN, B2O3And Al2O3Preferably the ratio of the total mass of (a) to the mass of the grinding balls is 1: (1-2), more preferably 1: 1. the particle size of the grinding ball is not particularly limited in the present invention, and may be selected according to the technical common knowledge of those skilled in the art.
In the invention, the ball milling medium used for ball milling is preferably a mixture of absolute ethyl alcohol and deionized water, and the volume ratio of the absolute ethyl alcohol to the deionized water is preferably 1: 1. by adopting the ball milling medium, the components can be mixed more uniformly.
In the present invention, the ratio of the mass of the milling balls to the volume of the milling medium is preferably 1: 4 g/mL. The invention can further improve the grinding effect by controlling the proportion.
In the invention, the rotation speed of the ball milling is preferably 200-600 r/min, more preferably 300-500 r/min, and further preferably 400 r/min; the time for ball milling is preferably 1-5 h, more preferably 2-4 h, and further preferably 3 h. The invention can make the particle size of each component meet the requirement by controlling the ball milling parameter, and simultaneously, the components are uniformly mixed.
After the ball milling and mixing are finished, the ball milling product is preferably filtered to obtain ball milling powder.
In the present invention, the filtration treatment is preferably performed using a buchner funnel. The specific operation of the filtration treatment in the present invention is not particularly limited, and the treatment may be performed according to the common technical knowledge of those skilled in the art. The invention can remove the grinding balls in the ball-milling product by filtering treatment.
After ball milling powder is obtained, the ball milling powder is sequentially subjected to drying treatment and purification treatment to obtain the release agent.
In the invention, the temperature of the drying treatment is preferably 60-100 ℃, more preferably 70-90 ℃, and further preferably 80 ℃; the drying time is preferably 5 to 10 hours, more preferably 6 to 9 hours, and further preferably 7 to 8 hours. The ball milling medium in the ball milling powder can be removed through drying treatment.
In the present invention, the purification treatment is preferably heated in an oxidizing atmosphere. In the invention, the purification treatment temperature is preferably 200-300 ℃, more preferably 220-280 ℃, and further preferably 250-270 ℃; the time of the purification treatment is preferably 0.5-2 h, and more preferably 1-1.5 h; the atmosphere for the purification treatment is preferably oxygen. In the present invention, the purification treatment is preferably performed in an oxidation furnace. According to the invention, through purification treatment, impurities in the ball-milling powder can be removed, so that the release agent and the crucible are further prevented from being adhered.
The preparation method is simple and can be prepared by simple equipment.
The invention provides a method for preparing a ceramic matrix composite material by adopting a reaction infiltration process, and the release agent in the technical scheme or the release agent prepared by the preparation method in the technical scheme is used as the release agent.
The method for preparing the ceramic matrix composite material by adopting the reaction infiltration process preferably comprises the following steps of:
1) uniformly coating a release agent on the inner surface of the crucible, and then compacting to obtain a non-adhesive crucible;
2) adding the raw materials of the ceramic matrix composite material into the non-sticking crucible obtained in the step 1), and carrying out infiltration treatment to obtain the ceramic matrix composite material.
According to the invention, the release agent is preferably uniformly coated on the inner surface of the crucible, and then the crucible is compacted to obtain the non-stick crucible.
In the present invention, the crucible is preferably a high purity quartz crucible. The crucible of the present invention is not particularly limited in its specific origin, and commercially available products known to those skilled in the art may be used.
Before the release agent is uniformly coated on the inner surface of the crucible, the inner surface of the crucible is preferably subjected to surface treatment in the present invention. In the present invention, the surface treatment is preferably performed by using 800-mesh sandpaper or hydrofluoric acid. The surface treatment of the invention can make the inner surface of the crucible have certain roughness, thereby being beneficial to the coating of the release agent.
In the present invention, the coating is preferably performed by brushing the release agent on the inner surface of the crucible using a brush. According to the invention, the inner surface of the crucible can be completely filled with the release agent by the coating mode.
In the invention, the coating thickness of the release agent is preferably not less than 0.5mm, and more preferably 0.5-2 mm. According to the invention, by controlling the thickness of the release agent, the contact between the molten material and the crucible can be avoided, and the release effect is further improved.
In the present invention, the compacting is preferably performed by using a glass rod or a metal cylinder. The invention can avoid the release agent from falling off by compacting.
After the non-sticking crucible is obtained, the raw materials of the ceramic matrix composite material are preferably added into the non-sticking crucible for infiltration treatment, so that the ceramic matrix composite material and the non-sticking crucible are obtained.
The specific type of the raw materials of the ceramic matrix composite material is not specially limited, and the raw materials can be determined according to the required ceramic matrix composite material.
In the invention, the temperature of the infiltration treatment is preferably 1400-1700 ℃, and more preferably 1500-1600 ℃; the atmosphere of the infiltration treatment is preferably a vacuum or an inert atmosphere. The invention can ensure the smooth preparation of the composite material by controlling the parameters of the infiltration treatment.
When the method provided by the invention is used for preparing the ceramic matrix composite, the smooth removal of the sample after the preparation process of the ceramic matrix composite is finished can be realized.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The release agent comprises 60 mass percent of BN and 25 mass percent of B2O3And 15% of Al2O3(ii) a BN, B2O3And Al2O3The granularity of (A) is 100 meshes;
the preparation method of the release agent comprises the following steps:
(1) BN, B2O3And Al2O3Performing ball milling and mixing, and then performing filtration treatment by using a Buchner funnel to obtain ball milling powder; the grinding balls used for ball milling are zirconia balls; BN, B2O3And Al2O3The mass ratio of the total mass to the grinding balls is 1: 1; the ball milling medium used for ball milling is a mixture of absolute ethyl alcohol and deionized water, and the volume ratio of the absolute ethyl alcohol to the deionized water is 1: 1; the mass of the grinding balls and the volume ratio of the grinding mediumIs 1: 4 g/mL; the rotation speed of the ball milling is 600r/min, and the ball milling time is 5 h;
(2) sequentially drying and purifying the ball-milled powder obtained in the step (1) to obtain a release agent; the drying temperature is 80 ℃, and the drying time is 6 h; the temperature of the purification treatment is 250 ℃, the time of the purification treatment is 1h, and the purification treatment is carried out in an oxidation furnace.
Example 2
A release agent, which comprises 90 percent of BN and 5 percent of B by mass percentage 2O3And 5% of Al2O3(ii) a BN, B2O3And Al2O3The particle size of (a) is 100 meshes;
the preparation method of the release agent is the same as that of the example 1.
Example 3
The release agent comprises 70% of BN and 15% of B in percentage by mass2O3And 15% of Al2O3(ii) a BN, B2O3And Al2O3The granularity of (A) is 100 meshes;
the preparation method of the release agent is the same as that of the example 1.
Application example 1
A method for preparing ceramic matrix composite material by adopting a reaction infiltration process adopts the release agent provided by the embodiment 1 as the release agent;
the method for preparing the ceramic matrix composite material by adopting the reaction infiltration process comprises the following steps:
1) carrying out surface treatment on the inner surface of the high-purity quartz crucible by using 800-mesh abrasive paper, uniformly coating a release agent on the inner surface of the crucible by using a brush, and then compacting by using a glass rod to obtain a non-sticky crucible; the coating thickness of the release agent is 0.5 mm;
2) adding the raw material of the ceramic matrix composite material into the non-sticking crucible obtained in the step 1), and carrying out infiltration treatment to obtain the ceramic matrix composite material and the non-sticking crucible; the temperature of the infiltration treatment is 1600 ℃, and the atmosphere of the infiltration treatment is a vacuum atmosphere.
Application example 2
The release agent provided in example 2 was used as the release agent, the crucible in step 1) was a graphite crucible, the surface treatment was performed by hydrofluoric acid, and other conditions were the same as in example 1.
Application example 3
The release agent provided in example 3 was used as a release agent, and the other conditions were the same as in example 1.
Comparative example 1
A method for preparing a ceramic matrix composite by adopting a reaction infiltration process does not use a release agent, and other conditions are the same as those in application example 2.
A macroscopic view of the ceramic matrix composite obtained in application example 1 and the high purity quartz crucible is shown in FIG. 1. As can be seen from FIG. 1, the obtained ceramic matrix composite and the high-purity quartz crucible have no obvious defects.
The macroscopic view of the high-purity quartz crucible after the ceramic matrix composite material is taken out in application example 1 is shown in fig. 2. As can be seen from FIG. 2, even after the high-temperature infiltration treatment, the release agent does not react with the quartz crucible, and the ceramic matrix composite can be well released from the mold without damaging the crucible.
A macroscopic view of the ceramic matrix composite material of application example 1 is shown in FIG. 3. As can be seen from FIG. 3, the ceramic matrix composite is relatively complete after being taken out, and has small damage to the original sample, which shows that the mold release agent has good mold release effect and can not cause adhesion.
A macroscopic view of the ceramic matrix composite and the crucible prepared in application example 2 and comparative example 1 is shown in FIG. 4. In FIG. 4, the ceramic matrix composite and the crucible obtained in application example 2 are shown on the left side, and the ceramic matrix composite and the crucible obtained in comparative example 1 are shown on the right side. As can be seen from FIG. 4, after the release agent is coated on the inner surface of the crucible, the adhesion between the molten ceramic matrix composite and the crucible can be effectively prevented, and the splashing of the molten ceramic matrix composite can be prevented, so that the quality of the ceramic matrix composite is improved, and the loss of the crucible is reduced.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. The release agent comprises, by mass, 60-90% of BN and 5-35% of B2O3And 5-15% of Al2O3。
2. The release agent as claimed in claim 1, wherein the release agent comprises 60 to 80% of BN and 10 to 25% of B by mass2O3And 5-10% of Al2O3。
3. The release agent as claimed in claim 1, wherein the release agent comprises 60 to 70% of BN and 15 to 25% of B by mass2O3And 10-15% of Al2O3。
4. Mold release agent according to claim 1, characterized in that it comprises, in mass percent, 90% of BN, 5% of B2O3And 5% of Al2O3。
5. A process for preparing a mold release agent as claimed in any of claims 1 to 4, comprising the steps of:
(1) BN, B2O3And Al2O3Performing ball milling and mixing to obtain ball milling powder;
(2) and (2) sequentially drying and purifying the ball-milled powder obtained in the step (1) to obtain the release agent.
6. The preparation method according to claim 5, characterized in that the rotation speed of the ball milling in the step (1) is 200-600 r/min, and the ball milling time is 1-5 h.
7. The method according to claim 5, wherein the drying treatment in the step (2) is carried out at a temperature of 60 to 100 ℃ for 5 to 10 hours.
8. The method according to claim 5, wherein the temperature of the purification treatment in the step (2) is 200 to 300 ℃ and the time of the purification treatment is 0.5 to 2 hours.
9. A method for preparing a ceramic matrix composite material by adopting a reaction infiltration process is characterized in that the release agent disclosed by any one of claims 1 to 4 or the release agent prepared by the preparation method disclosed by any one of claims 5 to 8 is adopted as the release agent.
10. The method of claim 9, comprising the steps of:
1) uniformly coating a release agent on the inner surface of the crucible, and then compacting to obtain a non-adhesive crucible;
2) adding the raw materials of the ceramic matrix composite material into the non-sticking crucible obtained in the step 1), and carrying out infiltration treatment to obtain the ceramic matrix composite material.
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Citations (7)
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JP2004067706A (en) * | 2002-08-01 | 2004-03-04 | Denki Kagaku Kogyo Kk | Lubricating release agent |
CN1805808A (en) * | 2003-06-13 | 2006-07-19 | Esk制陶两合公司 | Durable bn mould separating agents for the die casting of metals |
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CN1805808A (en) * | 2003-06-13 | 2006-07-19 | Esk制陶两合公司 | Durable bn mould separating agents for the die casting of metals |
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