High-temperature glue of silicon carbide ceramic and composite material thereof, and preparation and bonding methods thereof
阅读说明：本技术 碳化硅陶瓷及其复合材料的高温胶及其制备与粘接方法 (High-temperature glue of silicon carbide ceramic and composite material thereof, and preparation and bonding methods thereof ) 是由 张毅 崔雪峰 李晓萍 成来飞 付志强 陈旭 卫冲 于 2021-07-29 设计创作，主要内容包括：本发明公开了一种碳化硅陶瓷及其复合材料的高温胶及其制备与粘接方法,用于解决陶瓷基复合材料现有焊接方法实施过程中的高压力和高温度等条件对焊接方法限制的问题,拓宽焊接方法在大型薄壁复杂陶瓷基复合材料构件的应用。高温胶由液态先驱体溶剂、含硼粉体的活性料和惰性粉体三者配合而成,液态先驱体溶剂发挥中低温粘接作用,含硼粉体的活性料在空气环境下氧化生成硅硼玻璃起到高温粘接作用,惰性粉体填充液态先驱体裂解孔隙和微裂纹起到的传递载荷作用,三者混合均匀经固化后形成粘接强度。本发明高温胶配料简单,使用方便,空气环境高温热处理后粘接强度可达10MPa以上,适合于陶瓷基复合材料大面积粘接应用。(The invention discloses a high-temperature adhesive for silicon carbide ceramics and a composite material thereof, and a preparation method and a bonding method thereof, which are used for solving the problem that the conditions such as high pressure, high temperature and the like in the implementation process of the existing welding method for ceramic matrix composite materials limit the welding method and widening the application of the welding method in large thin-wall complex ceramic matrix composite material members. The high-temperature glue is formed by matching a liquid precursor solvent, an active material containing boron powder and inert powder, wherein the liquid precursor solvent plays a role in medium-low temperature bonding, the active material containing the boron powder is oxidized in an air environment to generate silicon-boron glass to play a role in high-temperature bonding, the inert powder fills a cracking pore and a microcrack of the liquid precursor to play a role in load transfer, and the three are uniformly mixed and cured to form bonding strength. The high-temperature adhesive has simple ingredients and convenient use, has the bonding strength of more than 10MPa after high-temperature heat treatment in air environment, and is suitable for large-area bonding application of ceramic matrix composite materials.)
1. The high-temperature adhesive for the silicon carbide ceramic and the composite material thereof is characterized by comprising the following components in percentage by mass:
40-50% of a liquid precursor solvent;
30-40% of active material containing boron powder;
the rest of inert powder;
the liquid precursor solvent is tetraethoxysilane, or a mixed solution of liquid polycarbosilane and xylene, or a mixed solution of phenolic resin and tetraethoxysilane;
the active material of the boron-containing powder is boric acid powder; or boric acid powder and BN powder and/or B4C, mixing powder; or BN powder and B4C, mixing powder;
the inert powder is Si powder and SiO2A mixture of powders, or SiO2Powder of Al2O3Powder, Y2O3A mixture of powders and CaO powders.
2. The high-temperature adhesive for silicon carbide ceramics and the composite material thereof according to claim 1, which is characterized by comprising the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
the liquid precursor solvent is a mixed solution of liquid polycarbosilane and xylene; the active materials of the boron-containing powder are boric acid and B4C, mixing powder; the inert powder is Si powder and SiO2A mixture of powders.
3. The high-temperature adhesive of silicon carbide ceramic and the composite material thereof according to claim 2, wherein: the volume ratio of the liquid polycarbosilane to the xylene is 1: 1; boric acid andB4the mass ratio of the C powder is 1: 1; si powder and SiO2The mass ratio of the powder is 1: 1.
4. the high-temperature adhesive for silicon carbide ceramics and the composite material thereof according to claim 1, which is characterized by comprising the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
the liquid precursor solvent is tetraethoxysilane, the active material of the boron-containing powder is boric acid powder, and the inert powder is SiO with the mass ratio of 1:1:1:12Powder of Al2O3Powder, Y2O3A mixture of powders and CaO powders.
5. The high-temperature adhesive of silicon carbide ceramic and the composite material thereof according to claim 1, wherein:
when the liquid precursor solvent is a mixed liquid of liquid polycarbosilane and xylene, the volume ratio of liquid polycarbosilane PCS to xylene is 1: 1; when the liquid precursor solvent is a mixed solution of phenolic resin and ethyl orthosilicate, the volume ratio of the phenolic resin to the ethyl orthosilicate is 1: 1.
6. the high-temperature adhesive of silicon carbide ceramic and the composite material thereof according to claim 5, wherein:
when the boron-containing powder is boric acid powder, BN powder and B4And in the case of the mixture of the C powder, the mass fractions of the three are as follows: 0 < boric acid powder < 30%, 30% or more and 50% or less BN powder, and the balance B4And C, powder.
7. The high-temperature adhesive of silicon carbide ceramic and the composite material thereof according to claim 6, wherein:
when the boron-containing powder is boric acid powder, BN powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1:1: 1;
when the boron-containing powder is a mixture of boric acid powder and BN powder, the mass ratio of the boric acid powder to the BN powder is 1: 1;
when the boron-containing powder is boric acid powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1: 1;
when the boron-containing powder is BN powder and B4And in the case of the mixture of the C powder, the mass ratio of the two is 1: 1.
8. A preparation method of high-temperature glue for silicon carbide ceramics and composite materials thereof is characterized by comprising the following steps:
step 1: preparing materials;
weighing liquid precursor solvent, active material containing boron powder and inert powder according to the mass fraction;
the liquid precursor solvent is tetraethoxysilane, or a mixed solution of liquid polycarbosilane and xylene, or a mixed solution of phenolic resin and tetraethoxysilane; the active material of the boron-containing powder is boric acid powder; or boric acid powder and BN powder and/or B4C powder mixture, or BN powder and B4C, mixing powder; the inert powder is Si powder and SiO2A mixture of powders, or SiO2Powder of Al2O3Powder, Y2O3A mixture of powder and CaO powder;
step 2: mixing materials;
wet grinding the mixture of liquid precursor solvent, active material containing boron powder and inert powder; after grinding for a set time, the high-temperature glue of the silicon carbide ceramic and the composite material thereof with higher viscosity is obtained.
9. The method for preparing the high-temperature adhesive of the silicon carbide ceramics and the composite materials thereof according to the claim 8, characterized in that in the step 1: when the liquid precursor solvent is a mixed liquid of liquid polycarbosilane and xylene, the volume ratio of liquid polycarbosilane PCS to xylene is 1: 1;
when the liquid precursor solvent is a mixed solution of phenolic resin and ethyl orthosilicate, the volume ratio of the phenolic resin to the ethyl orthosilicate is 1: 1.
10. the method for preparing the high-temperature adhesive of the silicon carbide ceramics and the composite materials thereof according to the claim 9, characterized in that in the step 1: when the boron-containing powder is boric acid powder, BN powder and B4And in the case of the mixture of the C powder, the mass fractions of the three are as follows: 0 < boric acid powder < 30%, 30% or more and 50% or less BN powder, and the balance B4And C, powder.
11. The method for preparing the high-temperature adhesive of the silicon carbide ceramics and the composite materials thereof according to the claim 10, characterized in that in the step 1:
when the boron-containing powder is boric acid powder, BN powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1:1: 1;
when the boron-containing powder is a mixture of boric acid powder and BN powder, the mass ratio of the boric acid powder to the BN powder is 1: 1;
when the boron-containing powder is boric acid powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1: 1;
when the boron-containing powder is BN powder and B4And in the case of the mixture of the C powder, the mass ratio of the two is 1: 1.
12. The method for preparing high-temperature adhesive of silicon carbide ceramic and composite material thereof according to claim 11, wherein in step 2: alcohol or acetone is added during the milling process.
13. The method for preparing high-temperature adhesive of silicon carbide ceramic and composite material thereof according to claim 11, wherein the time set in step 2 is 6-24 hours.
14. A high-temperature adhesive bonding method based on silicon carbide ceramic and composite materials thereof is characterized by comprising the following steps:
step 1: surface treatment;
carrying out surface pretreatment on the silicon carbide ceramic to be bonded and the composite material thereof, and removing oil stains, dust and the like on the surface to obtain the pretreated silicon carbide ceramic and the composite material thereof;
step 2: coating and bonding;
uniformly coating high-temperature glue of the silicon carbide ceramic and the composite material thereof on the surface to be bonded of the pretreated silicon carbide ceramic and the composite material thereof; the thickness of the bonding layer is 1-2 mm;
and step 3: curing;
curing for 1 day at normal temperature or curing for 12-24 hours after heating in an oven at the temperature of 40 ℃ to obtain the bonded silicon carbide ceramic and the composite material thereof.
Technical Field
The invention belongs to the field of silicon carbide ceramics and composite materials thereof, and particularly relates to a preparation method of a high-strength ceramic adhesive with 1000-1500 ℃ resistance, which is suitable for large-scale thin-wall complex ceramic matrix composite components.
Background
The silicon carbide ceramic and the composite material (CMC-SiC, mainly comprising C/SiC and SiC/SiC) thereof can meet the use requirements of long service life below 1650 ℃, limited service life below 2000 ℃ and instantaneous service life below 2800 ℃. The C/SiC has important progress in the application of weaponry and civil fields such as high thrust-weight ratio aeroengines, satellite attitude control engines, hypersonic ramjets, aerospace round-trip heat protection systems, cruise missile engines, liquid rocket engines, solid rocket engines, turbine gas power stations, nuclear reactors and the like. With the continuous expansion of the application field of CMC-SiC, the components are bigger and more complex, and higher requirements are put forward on the connection of the CMC-SiC composite material.
Welding is one of the main connection methods of CMC-SiC composite materials, and mainly comprises soldering, solid-phase reaction connection, polymer conversion ceramic connection and the like. The document "B.Ricccardi, C.A.Nannetti, T.Petrasor, J.Woltersdorf, E.Pippel, S.Libera, L.Pillon.Issues of low activation cleaving of SiCf/SiC compositions by using alloys with free silicon [ J ]. Journal of Nuclear Materials,2004,329: 562: 566", the SiCf/SiC composite is bonded by holding Si-44Cr at.% (melting point 1390 ℃) for 10min at 30-50 ℃ above the melting point of the brazing filler, the strength can reach 60 MPa. The document "C.H.Henager, R.J.Kurtz.Low-activation joining of SiCf/SiC compositions for fusion applications [ J ]. Journal of Nuclear Materials,2011,417(1): 375-. The document "M.Ferraris, M.Salvo, F.Smeacetto.ceramic coating for SiCf/SiC composites [ J ]. Journal of the European Ceramic Society,2002,22(13): 2343-. Keeping the temperature at 1700 ℃ for 1.5h, rapidly cooling by water to prepare Mg-Al-Si glass, keeping the temperature at 1180 ℃ for 1h, and keeping the coating interface continuous. The literature "P.Colombo, B.Ricccardi, A.Donato, G.Scarinci. joining of SiCf/SiC ceramic matrix composites for fusion reactor applications [ J ]. Journal of Nuclear Materials,2000,278(2): 127-.
The above-mentioned CMC-SiC soldering method requires that under the conditions of a certain pressure and high temperature or multiple dipping, etc., the bonding layer is formed by the reaction of the solder and the CMC-SiC. The application of the welding method to large-scale thin-wall complex CMC-SiC components is limited, and the development of ceramic high-temperature glue with simple glue application process and high bonding strength becomes an important direction for promoting the engineering application of CMC-SiC welding to large-scale thin-wall complex components.
Disclosure of Invention
Aiming at the problem that the welding method is limited by conditions such as high pressure, high temperature and the like in the implementation process of the traditional CMC-SiC welding method, the invention provides a CMC-SiC room temperature adhesive which forms a ceramic bonding layer through the chemical reaction of the adhesive in a high-temperature service environment and plays a role in connecting a CMC-SiC composite material. The aim is realized by adopting a matching mode of a liquid precursor solvent, an active material containing boron powder and inert powder.
The technical scheme adopted by the invention for solving the technical problems is to provide the high-temperature adhesive of the silicon carbide ceramic and the composite material thereof, which is characterized by comprising the following components in percentage by mass:
40-50% of a liquid precursor solvent;
30-40% of active material containing boron powder;
the rest of inert powder;
the liquid precursor solvent is tetraethoxysilane, or a mixed solution of liquid polycarbosilane and xylene, or a mixed solution of phenolic resin and tetraethoxysilane;
the active material of the boron-containing powder is boric acid powder; or boric acid powder and BN powder and/or B4C, mixing powder; or BN powder and B4C, mixing powder;
the inert powder is Si powder and SiO2A mixture of powders, or SiO2Powder of Al2O3Powder, Y2O3A mixture of powders and CaO powders.
Further, the high-temperature adhesive of the silicon carbide ceramic and the composite material thereof comprises the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
the liquid precursor solvent is a mixed solution of liquid polycarbosilane and xylene; the active materials of the boron-containing powder are boric acid and B4C, mixing powder; the inert powder is Si powder and SiO2A mixture of powders.
Further, the volume ratio of the liquid polycarbosilane to the xylene is 1: 1; boric acid and B4The mass ratio of the C powder is 1: 1; si powder and SiO2The mass ratio of the powder is 1: 1.
in order to further improve the bonding strength, the high-temperature adhesive of the silicon carbide ceramic and the composite material thereof consists of the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
the liquid precursor solvent is tetraethoxysilane, the active material of the boron-containing powder is boric acid powder, and the inert powder is SiO with the mass ratio of 1:1:1:12Powder of Al2O3Powder, Y2O3A mixture of powders and CaO powders.
Further, when the liquid precursor solvent is a mixed solution of liquid polycarbosilane and xylene, the volume ratio of liquid polycarbosilane PCS to xylene is 1: 1; when the liquid precursor solvent is a mixed solution of phenolic resin and ethyl orthosilicate, the volume ratio of the phenolic resin to the ethyl orthosilicate is 1: 1.
further, when the boron-containing powder isBoric acid powder, BN powder and B4And in the case of the mixture of the C powder, the mass fractions of the three are as follows: 0 < boric acid powder < 30%, 30% or more and 50% or less BN powder, and the balance B4And C, powder.
Further, when the boron-containing powder is boric acid powder, BN powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1:1: 1;
when the boron-containing powder is a mixture of boric acid powder and BN powder, the mass ratio of the boric acid powder to the BN powder is 1: 1;
when the boron-containing powder is boric acid powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1: 1;
when the boron-containing powder is BN powder and B4And in the case of the mixture of the C powder, the mass ratio of the two is 1: 1.
The invention also provides a preparation method of the high-temperature adhesive for the silicon carbide ceramic and the composite material thereof, which is characterized by comprising the following steps:
step 1: preparing materials;
weighing liquid precursor solvent, active material containing boron powder and inert powder according to the mass fraction;
the liquid precursor solvent is tetraethoxysilane, or a mixed solution of liquid polycarbosilane and xylene, or a mixed solution of phenolic resin and tetraethoxysilane; the active material of the boron-containing powder is boric acid powder; or boric acid powder and BN powder and/or B4C powder mixture, or BN powder and B4C, mixing powder; the inert powder is Si powder and SiO2A mixture of powders, or SiO2Powder of Al2O3Powder, Y2O3A mixture of powder and CaO powder;
step 2: mixing materials;
wet grinding the mixture of liquid precursor solvent, active material containing boron powder and inert powder; after grinding for a set time, the high-temperature glue of the silicon carbide ceramic and the composite material thereof with higher viscosity is obtained.
Further, in step 1: when the liquid precursor solvent is a mixed liquid of liquid polycarbosilane and xylene, the volume ratio of liquid polycarbosilane PCS to xylene is 1: 1;
when the liquid precursor solvent is a mixed solution of phenolic resin and ethyl orthosilicate, the volume ratio of the phenolic resin to the ethyl orthosilicate is 1: 1.
further, in step 1: when the boron-containing powder is boric acid powder, BN powder and B4And in the case of the mixture of the C powder, the mass fractions of the three are as follows: 0 < boric acid powder < 30%, 30% or more and 50% or less BN powder, and the balance B4And C, powder.
Further, in step 1:
when the boron-containing powder is boric acid powder, BN powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1:1: 1;
when the boron-containing powder is a mixture of boric acid powder and BN powder, the mass ratio of the boric acid powder to the BN powder is 1: 1;
when the boron-containing powder is boric acid powder and B4When the powder C is a mixture, the mass ratio of the powder C to the powder C is 1: 1;
when the boron-containing powder is BN powder and B4And in the case of the mixture of the C powder, the mass ratio of the two is 1: 1.
Further, in step 2: alcohol or acetone is added during the milling process.
Furthermore, the time set in the step 2 is 6-24 hours.
The invention also provides a bonding method of the high-temperature adhesive based on the silicon carbide ceramic and the composite material thereof, which is characterized by comprising the following steps:
step 1: surface treatment;
carrying out surface pretreatment on the silicon carbide ceramic to be bonded and the composite material thereof, and removing oil stains, dust and the like on the surface to obtain the pretreated silicon carbide ceramic and the composite material thereof;
step 2: coating and bonding;
uniformly coating high-temperature glue of the silicon carbide ceramic and the composite material thereof on the surface to be bonded of the pretreated silicon carbide ceramic and the composite material thereof; the thickness of the bonding layer is 1-2 mm;
and step 3: curing;
curing for 1 day at normal temperature or curing for 12-24 hours after heating in an oven at the temperature of 40 ℃ to obtain the bonded silicon carbide ceramic and the composite material thereof.
The invention has the beneficial effects that:
1. the high-temperature adhesive is prepared by adopting a liquid precursor solvent, an active material containing boron powder and inert powder, three groups of components supplement each other, the liquid precursor solvent immediately plays a role in medium-low temperature bonding after being cured, the active material containing boron powder is oxidized by air to generate silicon-boron glass in the use process to play a role in high-temperature bonding, the inert powder fills the cracking pores and microcracks of the liquid precursor to play a role in transferring load, and the inert powder, the liquid precursor solvent, the active material containing boron powder and the inert powder are uniformly mixed and cooperate with each other to form bonding strength after being cured.
2. The active material of the invention is boron-containing powder, and the active material is BN powder and B4The mixture of the C powder and the boric acid powder reacts with oxygen in the air at a high temperature of 1000-1500 ℃ to generate B2O3The glass, the active material, the auxiliary material and the solvent interact with each other, so that the high-temperature adhesive has high bonding strength in an air environment at 1000-1500 ℃.
3. The high-temperature resistant high-strength ceramic high-temperature glue disclosed by the invention is simple in ingredient and convenient to use, the bonding strength can reach more than 10MPa after high-temperature heat treatment in an air environment, and the high-temperature resistant high-strength ceramic high-temperature glue is suitable for application of large thin-wall complex ceramic matrix composite members.
Drawings
FIG. 1 is a flow chart of the preparation method of the high-temperature adhesive for silicon carbide ceramics and the composite material thereof.
Detailed Description
The invention is further described in detail below with reference to the drawings and the specific embodiments.
Example 1
The high-temperature adhesive for the silicon carbide ceramic and the composite material thereof comprises the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
wherein the liquid precursor solvent is a mixed solution of liquid Polycarbosilane (PCS) and xylene, the volume ratio of the liquid Polycarbosilane (PCS) to the xylene is 1:1, and different volume ratios can be selected in other embodiments; the active material of the boron-containing powder is boric acid powder; the inert powder is Si powder and SiO2The mass fractions of the powder mixture and the powder mixture are both 50%, and different mass fractions can be selected in other embodiments.
Referring to fig. 1, this example prepares a high temperature glue by the following steps:
step 1: preparing materials;
weighing 40% of liquid precursor solvent, 40% of active material of boron-containing powder and the balance of inert powder of 20% according to mass fraction. Wherein, the liquid precursor solvent is a mixed solution of liquid PCS and dimethylbenzene. The active material of the boron-containing powder is boric acid powder. The inert powder is Si powder and SiO2The mass fraction of the mixture of the powder is 50 percent.
Step 2: mixing materials;
and grinding the mixture of the liquid precursor solvent, the active material containing boron powder and the inert powder by a wet grinding method for 24 hours to obtain the high-temperature adhesive of the silicon carbide ceramic and the composite material thereof with higher viscosity.
The bonding is achieved by the following steps:
step 1: surface treatment;
and (3) carrying out surface pretreatment on the 2D C/SiC composite material to be bonded, and removing oil stains, dust and the like on the surface to obtain the pretreated 2D C/SiC composite material.
Step 2: coating and bonding;
uniformly coating the silicon carbide ceramic and the high-temperature glue of the composite material thereof on the surface to be bonded of the pretreated 2D C/SiC composite material, wherein the coating thickness of the bonding layer is 1-2 mm.
And step 3: curing;
curing for 1 day at normal temperature to obtain the bonded silicon carbide ceramic and the composite material thereof.
The following performance tests are carried out on the high-temperature adhesive of the prepared silicon carbide ceramic and the composite material thereof:
and placing the bonded 2D C/SiC composite material in a muffle furnace, heating to 1000 ℃, and keeping the temperature for 1 hour, and then testing the normal-temperature bonding strength of the material to be 6.92 and 6.15 MPa. After warming to 1200 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 6.61, 8.22 and 7.47 MPa. After heating to 1300 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 5.86, 6.47 and 4.84 MPa. After heating to 1400 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 10.59, 9.95 and 7.29 MPa. After heating to 1500 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 10.95, 14.93 and 9.41 MPa. The conventional adhesive is heated to 1000 ℃ and kept warm for 1 hour, and then the normal-temperature adhesive strength is about 10MPa, but when the conventional adhesive is heated to 1500 ℃ and kept warm for 1 hour, the normal-temperature adhesive strength is reduced to about 5 MPa. It can be seen that this embodiment high temperature glue has the advantage that service temperature is wider, and bonding strength is higher, and the performance is more stable with current bonding glue.
Example 2
The high-temperature adhesive for the silicon carbide ceramic and the composite material thereof comprises the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
wherein the liquid precursor solvent is a mixed solution of liquid Polycarbosilane (PCS) and dimethylbenzene; the active materials of the boron-containing powder are boric acid and B4And C, powder mixture, wherein the mass fraction of the powder mixture is 50%. The inert powder is Si powder and SiO2The mass fraction of the mixture of the powder is 50 percent.
Referring to fig. 1, this example prepares a high temperature glue by the following steps:
step 1: preparing materials;
weighing 40% of liquid precursor solvent, 40% of active material of boron-containing powder and the balance of inert powder of 20% according to mass fraction. Wherein, the liquid precursor solvent is a mixed solution of liquid PCS and dimethylbenzene. The active material of the boron-containing powder is a mixture of boric acid and B4C powder, and the mass fractions of the boric acid and the B4C powder are both 50%. The inert powder is a mixture of Si powder and SiO2 powder, and the mass fraction of the inert powder is 50%.
Step 2: mixing materials;
and grinding for 24 hours by adopting a wet grinding method to obtain the silicon carbide ceramic with higher viscosity and the high-temperature adhesive of the composite material thereof.
The bonding is achieved by the following steps:
step 1: surface treatment;
and (3) carrying out surface pretreatment on the 2D C/SiC composite material to be bonded, and removing oil stains, dust and the like on the surface to obtain the pretreated 2D C/SiC composite material.
Step 2: coating and bonding;
and uniformly coating the high-temperature glue of the silicon carbide ceramic and the composite material thereof on the surface to be bonded of the silicon carbide ceramic and the composite material thereof. The thickness of the bonding layer is 1-2 mm.
And step 3: curing;
and (3) heating the mixture in a 40-DEG oven and then curing the mixture for 12 hours to obtain the bonded silicon carbide ceramic and the composite material thereof.
The following performance tests were carried out on the high temperature adhesive prepared above: and placing the bonded 2D C/SiC composite material in a muffle furnace, heating to 1000 ℃, and keeping the temperature for 1 hour to test the normal-temperature bonding strength of the material to be 11.18 MPa and 8.39 MPa. After heating to 1200 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 10.26, 12.15 and 12.15 MPa. After heating to 1300 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 6.98, 4.84 and 5.05 MPa. After heating to 1400 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 6.91, 8.49 and 7.78 MPa. After heating to 1500 ℃ and holding for 1 hour, the normal temperature bonding strength was tested to be 7.43, 7.36 and 9.94 MPa. The conventional adhesive is heated to 1000 ℃ and kept warm for 1 hour, and then the normal-temperature adhesive strength is about 10MPa, but when the conventional adhesive is heated to 1500 ℃ and kept warm for 1 hour, the normal-temperature adhesive strength is reduced to about 5 MPa. It can be seen that this embodiment high temperature glue has the advantage that service temperature is wider, and bonding strength is higher, and the performance is more stable with current bonding glue.
Example 3
The high-temperature adhesive for the silicon carbide ceramic and the composite material thereof comprises the following components in percentage by mass:
50% of liquid precursor solvent;
40% of active material of boron-containing powder;
10% of inert powder;
wherein the liquid precursor solvent is a mixed solution of phenolic resin and tetraethoxysilane. The active material of the boron-containing powder is BN powder, boric acid and B4The mass ratio of the powder C mixture to the powder C mixture is 1:1:1, and the mass fractions of the powder C mixture and the powder C mixture in other embodiments meet the following requirements: 0 < boric acid powder < 30%, 30% or more and 50% or less BN powder, and the balance B4C powder, can achieve better effect. The inert powder is SiO2Powder of Al2O3Powder, Y2O3A mixture of powders and CaO powders.
Referring to fig. 1, this example prepares a high temperature glue by the following steps:
step 1: preparing materials;
weighing 50% of liquid precursor solvent and 40% of active material of boron-containing powder according to mass fraction. Wherein the liquid precursor solvent is a mixed solution of phenolic resin and tetraethoxysilane. The active material of the boron-containing powder is a mixture of BN powder, boric acid and B4C powder, and the mass ratio of the BN powder to the boric acid to the B4C powder is 1:1: 1. The inert powder is SiO2Powder of Al2O3Powder, Y2O3The weight ratio of the powder to the CaO powder can be 1:1:1:1, or any other ratio.
Step 2: mixing materials;
grinding by wet grinding method. Grinding for 24 hours to obtain the high-temperature glue of the silicon carbide ceramic and the composite material thereof with higher viscosity.
The bonding is achieved by the following steps:
step 1: and (6) surface treatment. And (3) carrying out surface pretreatment on the 2D C/SiC composite material to be bonded, and removing oil stains, dust and the like on the surface to obtain the pretreated 2D C/SiC composite material.
Step 2: and (6) coating and bonding. And uniformly coating the high-temperature glue of the silicon carbide ceramic and the composite material thereof on the surface to be bonded of the silicon carbide ceramic and the composite material thereof. The thickness of the bonding layer is 1-2 mm.
And step 3: and (5) curing. And (3) heating the mixture in a 40-DEG oven and then curing the mixture for 12 hours to obtain the bonded silicon carbide ceramic and the composite material thereof.
The following performance tests were carried out on the high temperature adhesive prepared above: and placing the bonded 2D C/SiC composite material in a muffle furnace, heating to 1000 ℃, and keeping the temperature for 1 hour, and then testing the normal-temperature bonding strength of the material to be 10.45 and 10.16 MPa. After heating to 1500 ℃ and holding for 1 hour, the normal temperature adhesive strength was tested to be 7.41, 7.29 and 9.80 MPa. The conventional adhesive is heated to 1000 ℃ and kept warm for 1 hour, and then the normal-temperature adhesive strength is about 10MPa, but when the conventional adhesive is heated to 1500 ℃ and kept warm for 1 hour, the normal-temperature adhesive strength is reduced to about 5 MPa. It can be seen that this embodiment high temperature glue has the advantage that service temperature is wider, and bonding strength is higher, and the performance is more stable with current bonding glue.
Example 4
The high-temperature adhesive for the silicon carbide ceramic and the composite material thereof comprises the following components in percentage by mass:
40% of liquid precursor solvent;
40% of active material of boron-containing powder;
20% of inert powder;
wherein the liquid precursor solvent is tetraethoxysilane. The active material of the boron-containing powder is boric acid powder, and the inert powder is SiO2Powder of Al2O3Powder, Y2O3The weight ratio of the powder to the CaO powder is 1:1:1: 1.
Referring to fig. 1, this example prepares a high temperature glue by the following steps:
step 1: preparing materials;
weighing 40% of liquid precursor solvent, 40% of active material of boron-containing powder and the balance of inert powder of 20% according to mass fraction. Wherein the liquid precursor solvent is tetraethoxysilane. The active material of the boron-containing powder is boric acid powder. The inert powder is SiO2Powder of Al2O3Powder, Y2O3Mixture of powder and CaO powderThe amount fraction was 25%.
Step 2: mixing materials;
grinding by wet grinding method. Grinding for 6 hours to obtain the silicon carbide ceramic with higher viscosity and the high-temperature adhesive of the composite material thereof.
The bonding is achieved by the following steps:
step 1: surface treatment;
and (3) carrying out surface pretreatment on the 2D C/SiC composite material to be bonded, and removing oil stains, dust and the like on the surface to obtain the pretreated 2D C/SiC composite material.
Step 2: coating and bonding;
and uniformly coating the high-temperature glue of the silicon carbide ceramic and the composite material thereof on the surface to be bonded of the silicon carbide ceramic and the composite material thereof. The thickness of the bonding layer is 1-2 mm.
And step 3: curing;
and (3) heating the mixture in a 40-DEG oven and then curing the mixture for 12 hours to obtain the bonded silicon carbide ceramic and the composite material thereof.
The following performance tests were carried out on the high temperature adhesive prepared above: and placing the bonded 2D C/SiC composite material in a vacuum furnace, heating to 1200 ℃, and keeping the temperature for 1 hour, and then testing the normal-temperature bonding strength of the material to be 19.53 MPa and 16.06 MPa. After the conventional adhesive is heated to 1200 ℃ and kept warm for 1 hour, the normal-temperature adhesive strength is about 10MPa in a test, and the high-temperature adhesive has the advantage of higher adhesive strength compared with the conventional adhesive.
Example 5
The high-temperature adhesive for the silicon carbide ceramic and the composite material thereof comprises the following components in percentage by mass:
50% of liquid precursor solvent;
30% of active material of boron-containing powder;
20% of inert powder;
wherein the liquid precursor solvent is tetraethoxysilane. The active material of the boron-containing powder is boric acid powder, and in other embodiments, a mixture of boric acid powder and BN powder with the volume ratio of 1:1 or boric acid powder and B with the volume ratio of 1:1 can also be adopted4C powderOr BN powder and B in a volume ratio of 1:14C, mixing powder; the inert powder is SiO2Powder of Al2O3Powder, Y2O3The weight ratio of the powder to the CaO powder is 1:1:1: 1.
Referring to fig. 1, this example prepares a high temperature glue by the following steps:
step 1: preparing materials;
weighing 40% of liquid precursor solvent, 40% of active material of boron-containing powder and the balance of inert powder of 20% according to mass fraction. Wherein the liquid precursor solvent is tetraethoxysilane. The active material of the boron-containing powder is boric acid powder. The inert powder is SiO2Powder of Al2O3Powder, Y2O3The mass fraction of the mixture of the powder and the CaO powder is 25 percent.
Step 2: mixing materials;
grinding by wet grinding method. Grinding for 6 hours to obtain the silicon carbide ceramic with higher viscosity and the high-temperature adhesive of the composite material thereof.
The bonding is achieved by the following steps:
step 1: surface treatment;
and (3) carrying out surface pretreatment on the 2D C/SiC composite material to be bonded, and removing oil stains, dust and the like on the surface to obtain the pretreated 2D C/SiC composite material.
Step 2: coating and bonding;
and uniformly coating the high-temperature glue of the silicon carbide ceramic and the composite material thereof on the surface to be bonded of the silicon carbide ceramic and the composite material thereof. The thickness of the bonding layer is 1-2 mm.
And step 3: curing;
and (3) heating the mixture in a 40-DEG oven and then curing the mixture for 12 hours to obtain the bonded silicon carbide ceramic and the composite material thereof.
The following performance tests were carried out on the high temperature adhesive prepared above: and placing the bonded 2D C/SiC composite material in a vacuum furnace, heating to 1200 ℃, and keeping the temperature for 1 hour, and then testing the normal-temperature bonding strength of the material to be 16.36 MPa and 14.59 MPa. After the conventional adhesive is heated to 1200 ℃ and is kept warm for 1 hour, the normal-temperature adhesive strength is about 10MPa, so that the adhesive has the advantage of higher adhesive strength compared with the conventional adhesive.
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