CN115305019B - High-temperature adhesive and preparation method and application method thereof - Google Patents
High-temperature adhesive and preparation method and application method thereof Download PDFInfo
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- CN115305019B CN115305019B CN202210908482.5A CN202210908482A CN115305019B CN 115305019 B CN115305019 B CN 115305019B CN 202210908482 A CN202210908482 A CN 202210908482A CN 115305019 B CN115305019 B CN 115305019B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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Abstract
The invention relates to a high-temperature adhesive, a preparation method and a use method thereof. The invention solves the problems that the existing high-temperature glue temperature resistant range is not suitable for the requirement of CVI-SiC production process and has hidden trouble of introducing other impurities, the selected raw materials PVA polyvinyl alcohol, aluminum dihydrogen phosphate, acrylamide and NN-methylene bisacrylamide in the high-temperature glue are all conventional adhesive components and are used as base materials of the adhesive, and according to the principle of not introducing other impurities, siC powder is selected as a high-temperature modified filler according to the excellent high-temperature resistance of the SiC powder, graphite powder is selected as a high Wen Jiaogao temperature failure filler, the melting point of the SiC powder is higher than 2700 ℃, the introduction of the SiC powder can obviously improve the temperature resistant limit of the conventional adhesive, the oxidation phenomenon of the graphite powder starts to appear at 600 ℃ under the air atmosphere, the oxidation reaches the peak value at about 800 ℃, and the adhesive strength of the adhesive is reduced after the continuous oxidation phenomenon appears, thereby realizing the debonding, and therefore, the accurate control of the temperature resistant limit of the adhesive can be realized by controlling the addition amount of each component.
Description
Technical Field
The invention relates to a high-temperature adhesive, in particular to a high-temperature adhesive for die bonding in the preparation process of a ceramic matrix composite material, and a preparation method and a use method thereof.
Background
The development of the aerospace technology brings urgent demands for low-density and high-temperature-resistant ceramics, and the ceramic matrix composite material well meets the demands in the aerospace technology. The ceramic matrix composite material consists of a ceramic matrix, a reinforcement, an interface layer, a coating and other structural units, and in the long-term technical development process, the continuous fiber toughened ceramic matrix Composite Material (CMC) has the advantages of low density, high toughness, high strength, high temperature resistance, thermal shock resistance and no disaster damage, and becomes a main development direction of the ceramic matrix composite material, wherein the CMC-SiC ceramic composite material taking SiC ceramic as the matrix is a popular material in the aerospace technical field at present and in the future because the performances of high temperature resistance limit, mechanical strength, oxidation resistance, ablation resistance and the like of the CMC-SiC ceramic composite material are superior to those of other ceramic matrix composite materials. At present, the preparation process of the CMC-SiC ceramic composite material mainly comprises chemical vapor infiltration (Chemical Vapor Infiltration, CVI), precursor polymer thermal decomposition (Polymer Impregnation Pyrolysis, PIP) and reactive melt infiltration (Reactive Melt Infiltration, RMI), wherein the CVI method has the following advantages compared with the other two methods: 1. designability and manufacturability of multi-scale structures; 2. excellent workability; 3. metal-like connectivity. Thus, the CVI process has become the most basic process for the preparation of CMC-SiC components.
In the process of preparing the CMC-SiC composite material by the CVI method, the main process links are that the fiber preform is deposited in a high-temperature deposition furnace, and in the deposition process, in order to keep the geometric shape and the size of the fiber preform, a die is usually required to be used for fixing the fiber preform, namely, the deposition process of the SiC matrix of the CMC-SiC composite material is usually in a die deposition. The temperature in the CVI-SiC deposition process is typically about 1000 ℃, the vacuum state in the furnace is maintained in the whole deposition process, then precursor gas and other diluent and carrier gases are introduced into the furnace to react and deposit, and in this process, the pressure, temperature, purity of the gas, air inlet rate, heat preservation and pressure maintaining time and the like in the furnace bring irreversible influence on the product, so that when the mold material deposited along with the furnace is selected, firstly, whether other impurities are introduced or not needs to be considered, and secondly, the temperature resistance of the mold material needs to be considered. The graphite mold has a melting point of about 3500 ℃, does not react with carbon fibers or silicon carbide fiber preforms, and does not introduce other impurities in the CVI-SiC process, so that the graphite mold is mainly used in the CVI-SiC deposition process at present.
In the actual production process, products in the aerospace field relate to barrel-shaped, columnar and semi-closed parts, a graphite die of the products is usually required to be designed into a split type, so that demolding operation is conveniently carried out after a later CVI-SiC process link is finished, the split type graphite die is usually required to be bonded before being used due to a narrow operation space or no operation space, after the CVI-SiC process link is finished, a short high-temperature treatment is carried out again, so that an adhesive can be invalidated, at the moment, a preform is subjected to multiple CVI-SiC cycles, and the dimensional accuracy of the product is not affected by the invalidation of the adhesive between the graphite dies.
The high-temperature adhesives on the market at present can be divided into two types of organic adhesives and inorganic adhesives according to the temperature resistant range, wherein the temperature resistant range of the organic adhesives is between 150 ℃ and 550 ℃, most of the organic adhesives are concentrated between 150 ℃ and 350 ℃, and polyimide can reach 550 ℃ due to the good heat resistance, such as Chinese patent: CN 108342174 A,CN 107699166A, but still fails to meet the requirements for the temperature limit of high temperature glue during CMC-SiC production. The inorganic adhesive has a temperature resistant range of 1500-2000 ℃, wherein a phosphate type high-temperature adhesive is used as the optimal, but the inorganic high-temperature adhesive is complex in curing process, large in colloid brittleness, poor in impact resistance and poor in water resistance, and has poor low-temperature bonding strength, and most importantly, the higher the temperature limit of the high-temperature adhesive to be used in the CMC-SiC production process is, the better the higher the temperature limit is, the more the adhesive is required to fail in the temperature range of 1200-1300 ℃ in order to protect CMC-SiC products, and meanwhile, the requirement of not introducing other impurities is required to be met.
In summary, the main problems of the conventional high temperature glue are as follows:
1. the temperature resistant range is not suitable for the requirements of the CVI-SiC production process;
2. there is a risk of introducing other impurities.
Disclosure of Invention
The invention provides a high-temperature adhesive which can be used for die bonding in the preparation process of ceramic matrix composite materials and also provides a preparation method and a use method of the high-temperature adhesive, aiming at solving the problems that the existing high-temperature adhesive is not suitable for the requirements of CVI-SiC production process and has hidden danger of introducing other impurities.
The technical scheme of the invention is to provide a high-temperature adhesive, which is characterized by comprising the following components in parts by weight: 2-8 parts of PVA polyvinyl alcohol, 1-3 parts of borax, 2-6 parts of aluminum dihydrogen phosphate, 1-2 parts of acrylamide, 1-2 parts of NN-methylene bisacrylamide, 5-10 parts of graphite powder, 70-78 parts of SiC powder and 10-20 parts of water.
Further, the high-temperature adhesive comprises the following components in parts by weight: 3-5 parts of PVA polyvinyl alcohol, 2-3 parts of borax, 3-4 parts of aluminum dihydrogen phosphate, 1-2 parts of acrylamide, 1-2 parts of NN-methylene bisacrylamide, 5-6 parts of graphite powder, 70-72 parts of SiC powder and 10-14 parts of water.
In order to further ensure the fluidity of the prepared high-temperature adhesive, the high-temperature adhesive comprises the following components in parts by weight: 3 parts of PVA polyvinyl alcohol, 2 parts of borax, 4 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 5 parts of graphite powder, 70 parts of SiC powder and 14 parts of water.
In order to further optimize the temperature resistance limit of the prepared high-temperature adhesive, the high-temperature adhesive comprises the following components in parts by weight: 3 parts of PVA polyvinyl alcohol, 2 parts of borax, 4 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 5 parts of graphite powder, 72 parts of SiC powder and 12 parts of water.
In order to further optimize the distribution uniformity of the raw materials of the prepared high-temperature adhesive, the granularity of the graphite powder is 400-600 meshes, and the granularity of the SiC powder is 500-800 meshes.
The invention also provides a preparation method of the high-temperature adhesive, which is characterized by comprising the following steps:
step 1, weighing all raw materials according to the parts by weight;
and 2, heating the container to 50-80 ℃, stirring, setting the stirring speed to 200-800 r/min, sequentially adding raw materials into the container according to the sequence of water, PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, borax, graphite powder and SiC powder, uniformly stirring to ensure that the mixed adhesive is uniform in color and uniform in material dispersion, and standing the mixed solution for 12-50h in a room temperature environment after stirring.
Further, before the step 1, XRD detection is required for the graphite powder and SiC powder to distinguish whether other crystal impurities are contained, and the particle size of the powder is measured by combining a laser particle size detector and a scanning electron microscope.
The invention also provides a use method of the high-temperature adhesive, which is characterized by comprising the following steps:
step 1, the bonding surface is treated cleanly and kept dry;
step 2, uniformly coating the adhesive after standing on the surface of a graphite mold to be bonded, wherein the thickness of the adhesive layer is controlled to be 0.5-1mm;
step 3, fixing the split type die by using a tightening tool, applying a certain load to the glue coating surface, then wiping redundant adhesive at a gap of the glue coating surface by using a rag with alcohol, placing the treated graphite die in an environment range of 25-30 ℃ for standing for 12-24 hours, assembling the graphite die and the preform, and performing CVI-SiC deposition;
and 4, after the circulation of the whole CVI-SiC process link is finished, placing the composite material product with the graphite mold in a furnace, setting the temperature to 1200-1300 ℃, the heating rate to 5-50 ℃/min, the heat preservation time to 1-5 h, the cooling rate to 20-100 ℃/min, and finally cooling to 50-80 ℃ along with the furnace, opening the furnace door, and taking out the tool mold for demolding.
The beneficial effects of the invention are as follows:
1. PVA polyvinyl alcohol, aluminum dihydrogen phosphate, acrylamide and NN-methylene bisacrylamide in the selected raw materials in the high-temperature adhesive are all conventional adhesive components, the temperature resistance limit is about 500 ℃, the raw materials are used as base materials of the adhesive to play a role in adhesion, siC powder is selected as a high-temperature modified filler according to the excellent high-temperature resistance of the SiC powder, graphite powder is selected as a high-Wen Jiaogao temperature failure filler according to the excellent high-temperature resistance of the SiC powder, the melting point of the SiC powder is higher than 2700 ℃, the temperature resistance limit of the conventional adhesive can be obviously improved by introducing the SiC powder, the oxidation phenomenon of the graphite powder starts to appear at 600 ℃ under the air atmosphere, the oxidation reaches a peak value at about 800 ℃, and the adhesive strength of the adhesive is reduced after the continuous oxidation phenomenon appears, so that the debonding is realized.
2. The high-temperature adhesive is used as a die binder in the CVI-SiC process, fully protects the performance of CMC-SiC materials in the whole heating and heat preservation process, and prevents the problems of deformation or cracking of products and the like caused by the rapid heating and rapid cooling processes.
Detailed Description
So that the manner in which the above recited objects, features and advantages of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments, some of which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Example 1
The raw materials are weighed according to parts by weight, and the raw materials comprise: 3 parts of PVA polyvinyl alcohol, 2 parts of borax, 4 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 5 parts of graphite powder, 70 parts of SiC powder and 14 parts of water. The granularity of the material is 400 meshes of graphite powder and 500 meshes of SiC powder, XRD detection is carried out on the graphite powder and the SiC powder before mixing, and the granularity of the powder is measured by adopting a mode of combining a laser granularity detector and a scanning electron microscope, so that the powder does not contain other impurities, and the average value of the granularity of the powder and the granularity of the target powder is within +/-5 microns.
Taking 1 measuring cup with the volume of 5L, placing the measuring cup on a base of a heatable stirrer, starting the stirrer, setting the temperature to 50 ℃, setting the rotating speed to 300 revolutions per minute, sequentially adding raw materials into the measuring cup according to the sequence of water, PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, borax, graphite powder and SiC powder, uniformly stirring, ensuring uniform color and uniform material dispersion of the mixed adhesive, and standing the mixed solution in a room temperature environment for 12 hours after the stirring is finished.
The sizing method of the high-temperature adhesive comprises the steps of firstly removing floating ash and residual SiC deposition layer on the surface of a graphite mold, blowing the bonding surface clean by compressed air, then wiping the bonding surface clean by alcohol, and standing for 2 minutes for surface drying. And uniformly smearing the adhesive after standing on the surface of a graphite mold to be bonded, controlling the thickness of the adhesive layer to be 0.5mm, fixing the split type graphite mold by using a tightening tool, applying a certain load to the adhesive-coated surface, then wiping the redundant adhesive at the gap of the adhesive-coated surface by using a rag with alcohol, standing the treated graphite mold in an environment range of 25 ℃ for 12 hours, and assembling the graphite mold and a preform for tape mold deposition.
After the circulation of the whole CVI-SiC deposition process link is finished, placing a composite product with a graphite die into a furnace, setting the temperature to 1200 ℃, the heating rate to 10 ℃/min, the heat preservation time to 2 hours, the cooling rate to 30 ℃/min, and finally, after cooling to 80 ℃ along with the furnace, opening the furnace door, and taking out the tooling die for die stripping.
Example 2
The raw materials are weighed according to parts by weight, and the raw materials comprise: 3 parts of PVA polyvinyl alcohol, 2 parts of borax, 4 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 5 parts of graphite powder, 72 parts of SiC powder and 12 parts of water. The granularity of the material is 500 meshes of graphite powder and 600 meshes of SiC powder, XRD detection is carried out on the graphite powder and the SiC powder before mixing, and the granularity of the powder is measured by adopting a mode of combining a laser granularity detector and a scanning electron microscope, so that the powder does not contain other impurities, and the average value of the granularity of the powder and the granularity of the target powder is within +/-5 microns.
Taking 1 measuring cup with the volume of 5L, placing the measuring cup on a base of a heatable stirrer, starting the stirrer, setting the temperature to 80 ℃, setting the rotating speed to 600 revolutions per minute, sequentially adding raw materials into the measuring cup according to the sequence of PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, water, borax, graphite powder and SiC powder, uniformly stirring, ensuring uniform color and uniform material dispersion of the mixed adhesive, and standing the mixed solution in a room temperature environment for 20 hours after the stirring is finished.
The sizing method of the high-temperature adhesive comprises the steps of firstly removing floating ash and residual SiC deposition layer on the surface of a graphite mold, blowing the bonding surface clean by compressed air, then wiping the bonding surface clean by alcohol, and standing for 5 minutes for surface drying. And uniformly smearing the adhesive after standing on the surface of a graphite mold to be bonded, controlling the thickness of the adhesive layer to be 1mm, fixing the split mold by using a tightening tool, applying a certain load to the adhesive-coated surface, then wiping the redundant adhesive at the gap of the adhesive-coated surface by using a rag with alcohol, standing the treated graphite mold in an environment range of 30 ℃ for 20 hours, and assembling the graphite mold and a prefabricated body for tape mold deposition.
After the circulation of the whole CVI-SiC process link is finished, placing a composite product with a die in a furnace, setting the temperature to 1300 ℃, the heating rate to 50 ℃/min, the heat preservation time to 5 hours, the cooling rate to 100 ℃/min, and finally, after cooling to 50 ℃ along with the furnace, opening the furnace door, and taking out the tooling die for die removal.
Example 3
The raw materials are weighed according to parts by weight, and the raw materials comprise: 5 parts of PVA polyvinyl alcohol, 3 parts of borax, 3 parts of aluminum dihydrogen phosphate, 2 parts of acrylamide, 2 parts of NN-methylene bisacrylamide, 6 parts of graphite powder, 75 parts of SiC powder and 18 parts of water. The granularity of the material is 600 meshes of graphite powder and 800 meshes of SiC powder, XRD detection is carried out on the graphite powder and the SiC powder before mixing, and the granularity of the powder is measured by adopting a mode of combining a laser granularity detector and a scanning electron microscope, so that the powder does not contain other impurities, and the average value of the granularity of the powder and the granularity of the target powder is within +/-5 microns.
Taking 1 measuring cup with the volume of 5L, placing the measuring cup on a base of a heatable stirrer, starting the stirrer, setting the temperature to 80 ℃, setting the rotating speed to 800 revolutions per minute, sequentially adding raw materials into the measuring cup according to the sequence of PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, water, borax, graphite powder and SiC powder, uniformly stirring, ensuring uniform color and uniform material dispersion of the mixed adhesive, and standing the mixed solution in a room temperature environment for 40 hours after the stirring is finished.
The sizing method of the high-temperature adhesive comprises the steps of firstly removing floating ash and residual SiC deposition layer on the surface of a graphite mold, blowing the bonding surface clean by compressed air, then wiping the bonding surface clean by alcohol, and standing for 5 minutes for surface drying. And uniformly smearing the adhesive after standing on the surface of a graphite mold to be bonded, controlling the thickness of the adhesive layer to be 1mm, fixing the split mold by using a tightening tool, applying a certain load to the adhesive-coated surface, then wiping the redundant adhesive at the gap of the adhesive-coated surface by using a rag with alcohol, standing the treated graphite mold in an environment range of 30 ℃ for 20 hours, and assembling the graphite mold and a prefabricated body for tape mold deposition.
After the circulation of the whole CVI-SiC process link is finished, placing a composite product with a die in a furnace, setting the temperature to 1300 ℃, the heating rate to 5 ℃/min, the heat preservation time to 5 hours, the cooling rate to 20 ℃/min, and finally, after cooling to 80 ℃ along with the furnace, opening the furnace door, and taking out the tooling die for die disassembly.
Example 4
The raw materials are weighed according to parts by weight, and the raw materials comprise: 8 parts of PVA polyvinyl alcohol, 1 part of borax, 6 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 10 parts of graphite powder, 78 parts of SiC powder and 10 parts of water. The granularity of the material is 500 meshes of graphite powder and 600 meshes of SiC powder, XRD detection is carried out on the graphite powder and the SiC powder before mixing, and the granularity of the powder is measured by adopting a mode of combining a laser granularity detector and a scanning electron microscope, so that the powder does not contain other impurities, and the average value of the granularity of the powder and the granularity of the target powder is within +/-5 microns.
Taking 1 measuring cup with the volume of 5L, placing the measuring cup on a base of a heatable stirrer, starting the stirrer, setting the temperature to 60 ℃, setting the rotating speed to 600 revolutions per minute, sequentially adding raw materials into the measuring cup according to the sequence of PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, water, borax, graphite powder and SiC powder, uniformly stirring, ensuring uniform color and uniform material dispersion of the mixed adhesive, and standing the mixed solution in a room temperature environment for 20 hours after the stirring is finished.
The sizing method of the high-temperature adhesive comprises the steps of firstly removing floating ash and residual SiC deposition layer on the surface of a graphite mold, blowing the bonding surface clean by compressed air, then wiping the bonding surface clean by alcohol, and standing for 5 minutes for surface drying. And uniformly smearing the adhesive after standing on the surface of a graphite mold to be bonded, controlling the thickness of the adhesive layer to be 1mm, fixing the split mold by using a tightening tool, applying a certain load to the adhesive-coated surface, then wiping the redundant adhesive at the gap of the adhesive-coated surface by using a rag with alcohol, standing the treated graphite mold in an environment range of 30 ℃ for 24 hours, and assembling the graphite mold and a prefabricated body for tape mold deposition.
After the circulation of the whole CVI-SiC process link is finished, placing a composite product with a die in a furnace, setting the temperature to 1200 ℃, the heating rate to 50 ℃/min, the heat preservation time to 1h, the cooling rate to 100 ℃/min, and finally, after cooling to 50 ℃ along with the furnace, opening the furnace door, and taking out the tooling die for die removal.
Example 5
The raw materials are weighed according to parts by weight, and the raw materials comprise: 2 parts of PVA polyvinyl alcohol, 1 part of borax, 2 parts of aluminum dihydrogen phosphate, 2 parts of acrylamide, 2 parts of NN-methylene bisacrylamide, 8 parts of graphite powder, 78 parts of SiC powder and 20 parts of water. The granularity of the material is 500 meshes of graphite powder and 600 meshes of SiC powder, XRD detection is carried out on the graphite powder and the SiC powder before mixing, and the granularity of the powder is measured by adopting a mode of combining a laser granularity detector and a scanning electron microscope, so that the powder does not contain other impurities, and the average value of the granularity of the powder and the granularity of the target powder is within +/-5 microns.
Taking 1 measuring cup with the volume of 5L, placing the measuring cup on a base of a heatable stirrer, starting the stirrer, setting the temperature to 70 ℃, setting the rotating speed to 200 revolutions per minute, sequentially adding raw materials into the measuring cup according to the sequence of PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, water, borax, graphite powder and SiC powder, uniformly stirring, ensuring uniform color and uniform material dispersion of the mixed adhesive, and standing the mixed solution in a room temperature environment for 50 hours after the stirring is finished.
The sizing method of the high-temperature adhesive comprises the steps of firstly removing floating ash and residual SiC deposition layer on the surface of a graphite mold, blowing the bonding surface clean by compressed air, then wiping the bonding surface clean by alcohol, and standing for 5 minutes for surface drying. And uniformly smearing the adhesive after standing on the surface of a graphite mold to be bonded, controlling the thickness of the adhesive layer to be 1mm, fixing the split mold by using a tightening tool, applying a certain load to the adhesive-coated surface, then wiping the redundant adhesive at the gap of the adhesive-coated surface by using a rag with alcohol, standing the treated graphite mold in an environment range of 30 ℃ for 20 hours, and assembling the graphite mold and a prefabricated body for tape mold deposition.
After the circulation of the whole CVI-SiC process link is finished, placing a composite product with a die in a furnace, setting the temperature to 1300 ℃, the heating rate to 50 ℃/min, the heat preservation time to 5 hours, the cooling rate to 100 ℃/min, and finally, after cooling to 50 ℃ along with the furnace, opening the furnace door, and taking out the tooling die for die removal.
The invention adopts a compression shear experimental method to test the bonding strength of the high-temperature adhesive after heat treatment at different temperatures in the embodiment, and the bonding strength is used for representing whether the high-temperature adhesive is effective in different temperature ranges. The heat treatment equipment adopted in the experiment is a nano-Bo heat RHTH120-600 tubular sintering furnace, and the compression shear test equipment is a SANS CMT-4304 electronic universal experiment machine.
Testing experiments at the temperature ranging from 1000 ℃ to 1200 ℃ and marking HT1200; the shear strength test conditions were: an air atmosphere, a loading rate of 0.5mm/min;
the test experiment at 1200-1300 ℃ is recorded as HT1300; the shear strength test conditions were: air atmosphere, loading rate 0.5mm/min.
The test results show that the HT1200 type shear strength is 10.32MPa, the HT1300 type shear strength is 0.56MPa, and the high-temperature adhesive in the embodiment has obvious bonding strength after heat treatment at 1000-1200 ℃, and the bonding strength is obviously reduced after heat treatment at 1200-1300 ℃.
The high temperature adhesive of example 2 has been tested to have a better temperature resistance limit than the other examples in the examples described above. The high temperature adhesives of examples 1, 3, 4, 5 have better flowability.
Claims (8)
1. The high-temperature adhesive is characterized by comprising the following components in parts by weight: 2-8 parts of PVA polyvinyl alcohol, 1-3 parts of borax, 2-6 parts of aluminum dihydrogen phosphate, 1-2 parts of acrylamide, 1-2 parts of NN-methylene bisacrylamide, 5-10 parts of graphite powder, 70-78 parts of SiC powder and 10-20 parts of water.
2. The high temperature adhesive of claim 1, comprising, in parts by weight: 3-5 parts of PVA polyvinyl alcohol, 2-3 parts of borax, 3-4 parts of aluminum dihydrogen phosphate, 1-2 parts of acrylamide, 1-2 parts of NN-methylene bisacrylamide, 5-6 parts of graphite powder, 70-72 parts of SiC powder and 10-14 parts of water.
3. The high temperature adhesive according to claim 2, comprising, in parts by weight: 3 parts of PVA polyvinyl alcohol, 2 parts of borax, 4 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 5 parts of graphite powder, 70 parts of SiC powder and 14 parts of water.
4. The high temperature adhesive according to claim 2, comprising, in parts by weight: 3 parts of PVA polyvinyl alcohol, 2 parts of borax, 4 parts of aluminum dihydrogen phosphate, 1 part of acrylamide, 1 part of NN-methylene bisacrylamide, 5 parts of graphite powder, 72 parts of SiC powder and 12 parts of water.
5. The high temperature adhesive according to any one of claims 1 to 4, wherein: the granularity of the graphite powder is 400-600 meshes, and the granularity of the SiC powder is 500-800 meshes.
6. A method of preparing the high temperature adhesive of any one of claims 1-5, comprising the steps of:
step 1, weighing all raw materials according to the required weight parts;
and 2, heating the container to 50-80 ℃, stirring, setting the stirring speed to 200-800 r/min, sequentially adding the raw materials into the container according to the sequence of water, PVA polyvinyl alcohol, acrylamide, NN-methylene bisacrylamide, aluminum dihydrogen phosphate, borax, graphite powder and SiC powder, uniformly stirring, and standing the mixed solution in a room temperature environment for 12-50h after the stirring is finished.
7. The method for preparing the high-temperature adhesive according to claim 6, wherein: before step 1, graphite powder and SiC powder are detected to ensure that other crystal impurities are not contained.
8. A method of using the high temperature adhesive of any one of claims 1-5, comprising the steps of:
step 1, the bonding surface is treated cleanly and kept dry;
step 2, uniformly coating the adhesive after standing on the surface of a graphite mold to be bonded, wherein the thickness of the adhesive layer is controlled to be 0.5-1mm;
step 3, fixing the split graphite mold by using a tightening tool, loading the gluing surface, then wiping off redundant adhesive at a gap of the gluing surface, placing the treated graphite mold in an environment range of 25-30 ℃, standing for 12-24 hours, assembling the graphite mold and a preform, and performing CVI-SiC deposition;
and 4, after the circulation of the whole CVI-SiC process link is finished, placing the composite material product with the graphite mold in a furnace, setting the temperature to 1200-1300 ℃, the heating rate to 5-50 ℃/min, the heat preservation time to 1-5 h, the cooling rate to 20-100 ℃/min, and finally cooling to 50-80 ℃ along with the furnace, opening the furnace door, and taking out the tool mold for demolding.
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Citations (4)
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| JP2011026531A (en) * | 2009-06-30 | 2011-02-10 | Nippon Zeon Co Ltd | Method for producing heat-conductive pressure-sensitive adhesive composition, heat-conductive pressure-sensitive adhesion sheet and electronic part |
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| CN107163894A (en) * | 2017-05-26 | 2017-09-15 | 江苏省江南新型复合研磨材料及制品工程技术研究中心有限公司 | A kind of high-strength, quick-drying moisture-proof adhesive and preparation method thereof |
| CN107267096A (en) * | 2017-08-07 | 2017-10-20 | 伊婕 | A kind of environmental protection type resin binding agent and its preparation technology |
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| JP2012117040A (en) * | 2010-11-12 | 2012-06-21 | Nitto Denko Corp | Pressure-sensitive adhesive tape or sheet |
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| JP2011026531A (en) * | 2009-06-30 | 2011-02-10 | Nippon Zeon Co Ltd | Method for producing heat-conductive pressure-sensitive adhesive composition, heat-conductive pressure-sensitive adhesion sheet and electronic part |
| CN103965795A (en) * | 2013-01-29 | 2014-08-06 | 日东电工株式会社 | Heat Conducting Adhesion Sheet |
| CN107163894A (en) * | 2017-05-26 | 2017-09-15 | 江苏省江南新型复合研磨材料及制品工程技术研究中心有限公司 | A kind of high-strength, quick-drying moisture-proof adhesive and preparation method thereof |
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