CN112225458A - A kind of high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite material and preparation method thereof - Google Patents
A kind of high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite material and preparation method thereof Download PDFInfo
- Publication number
- CN112225458A CN112225458A CN202010812519.5A CN202010812519A CN112225458A CN 112225458 A CN112225458 A CN 112225458A CN 202010812519 A CN202010812519 A CN 202010812519A CN 112225458 A CN112225458 A CN 112225458A
- Authority
- CN
- China
- Prior art keywords
- glass
- powder
- temperature
- ceramic
- bonding
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002002 slurry Substances 0.000 title claims abstract description 40
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 89
- 239000002562 thickening agent Substances 0.000 claims abstract description 34
- 239000002270 dispersing agent Substances 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 30
- 239000000853 adhesive Substances 0.000 claims abstract description 18
- 230000001070 adhesive effect Effects 0.000 claims abstract description 18
- 229910000174 eucryptite Inorganic materials 0.000 claims abstract description 14
- 239000011812 mixed powder Substances 0.000 claims abstract description 4
- 239000002241 glass-ceramic Substances 0.000 claims abstract 16
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract 3
- 239000011230 binding agent Substances 0.000 claims abstract 2
- 239000011521 glass Substances 0.000 claims description 89
- 238000001035 drying Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000000498 ball milling Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 16
- 239000002893 slag Substances 0.000 claims description 16
- 238000010791 quenching Methods 0.000 claims description 15
- 230000000171 quenching effect Effects 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical group CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 8
- 229940116411 terpineol Drugs 0.000 claims description 8
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 4
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- 239000000020 Nitrocellulose Substances 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 239000010431 corundum Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- 229920001220 nitrocellulos Polymers 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims 1
- 239000001913 cellulose Substances 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 claims 1
- 235000010980 cellulose Nutrition 0.000 claims 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 229920000768 polyamine Polymers 0.000 claims 1
- 229940124530 sulfonamide Drugs 0.000 claims 1
- 150000003456 sulfonamides Chemical class 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 11
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 230000009477 glass transition Effects 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 24
- 239000006121 base glass Substances 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 11
- 239000002131 composite material Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 150000001412 amines Chemical class 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 description 8
- 239000001856 Ethyl cellulose Substances 0.000 description 7
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 7
- 229920002845 Poly(methacrylic acid) Polymers 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 7
- 229920001249 ethyl cellulose Polymers 0.000 description 7
- 235000019325 ethyl cellulose Nutrition 0.000 description 7
- 239000000835 fiber Substances 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 239000010453 quartz Substances 0.000 description 7
- 238000012216 screening Methods 0.000 description 7
- 238000007605 air drying Methods 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 238000005352 clarification Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000005219 brazing Methods 0.000 description 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000006060 molten glass Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical group O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
Abstract
本发明涉及一种陶瓷基复合材料用耐高温低膨胀系数粘接浆料及其制备方法。该粘接浆料包括重量百分比为55％～85％的微晶玻璃粉和15％～45％的有机粘接相；所述微晶玻璃粉为SiO2‑Al2O3‑B2O3‑MgO‑BaO‑ZnO‑ZrO2系微晶玻璃粉与β‑锂霞石微晶玻璃粉的混合粉体；所述有机粘接相包括有机溶剂、分散剂和增稠剂。本发明通过对微晶玻璃粉中各氧化物的种类及含量的调整，实现对微晶玻璃粉的热膨胀系数、介电常数、介电损耗、玻璃化温度、软化温度、析晶温度等的调节，最终可使粘接浆料的热膨胀系数与陶瓷基材的热膨胀系数相当，能够满足特定频段的透波使用要求；利用该粘接浆料连接的陶瓷材料样件具有良好的结合性能。The invention relates to a high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite materials and a preparation method thereof. The bonding paste comprises 55%-85% by weight of glass-ceramic powder and 15-45% of organic bonding phase; the glass-ceramic powder is SiO 2 -Al 2 O 3 -B 2 O 3 -MgO-BaO-ZnO-ZrO 2 -series glass-ceramic powder and β-eucryptite glass-ceramic powder mixed powder; the organic binder phase includes an organic solvent, a dispersant and a thickening agent. The invention realizes the adjustment of the thermal expansion coefficient, dielectric constant, dielectric loss, glass transition temperature, softening temperature, crystallization temperature, etc. of the glass-ceramic powder by adjusting the type and content of each oxide in the glass-ceramic powder Finally, the thermal expansion coefficient of the adhesive paste can be equal to the thermal expansion coefficient of the ceramic substrate, which can meet the requirements of wave transmission in a specific frequency band; the ceramic material samples connected by the adhesive paste have good bonding performance.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a high-temperature bonding slurry for a wave-transparent ceramic matrix composite and a preparation method thereof.
Background
In recent years, ceramic-based Frequency Selective Surface (FSS) radomes are more and more widely applied in stealth, and FSS structures need to withstand high-temperature airflow scouring in the flight process and can work for a long time in a severe pneumatic environment. To ensure the reliability of the FSS structure, it is a feasible solution to place the FSS structure inside the ceramic substrate. In this case, the combined connection of the outer wave-transmitting protective layer and the FSS-containing structural layer is an important point of research.
The ceramic radome is made of a fiber reinforced ceramic matrix composite material which has poor processability and a loose structure and is difficult to manufacture large or complex-shaped components, and the current common connecting method comprises the following steps: welding, mechanical connection and bonding. The brazing connection is a widely used connection mode between ceramic matrix composite materials, but the process temperature is high, the equipment cost is high, the damage to a base material is heavy, and the surface inertness of the ceramic matrix materials also enables brazing filler metal not to be easily wetted on the surface of the brazing filler metal. Mechanical connection refers to the joining of materials by mechanical fasteners such as pins, screws, rivets and bolts. At present, metal fasteners are numerous, but the matching performance of the metal fasteners and ceramics is poor, the engineering application of high-temperature-resistant and high-strength ceramics and composite material joints thereof is immature, and in addition, the composite materials are damaged to different degrees in the hole making process, so that the mechanical property of the connecting piece and the reliability of products are seriously influenced. The adhesives used for bonding connection are mainly divided into organic adhesives, inorganic adhesives and organic-inorganic mixed adhesives, the heat resistance of the organic adhesives is generally not more than 350 ℃, and the high-temperature environment requirements are difficult to meet. Therefore, an inorganic adhesive with high temperature resistance, good wave permeability and good matching with the base material needs to be developed. CN 110511682A invents a high-universality high-temperature-resistant aluminum phosphate salt adhesive and a preparation method thereof, but the aluminum phosphate salt adhesive has large dielectric loss at high temperature and is difficult to meet the wave-transmitting performance requirement of a ceramic-based FSS radome.
Because glass has bonding characteristics and the properties of the glass can be changed by adjusting the chemical composition, the inorganic bonding agent can be made into glass by adding organic solvent, thickening agent and dispersing agent into glass powder as a functional phaseAnd (5) bonding the slurry. However, the thermal expansion coefficient of the commonly used glass powder is higher and far higher than that of the quartz ceramic (0.47-0.58 multiplied by 10)-6/° c). The mismatch of the thermal expansion coefficients causes great thermal stress between the FSS layer and the wave-transparent protection layer, so that the FSS layer and the wave-transparent protection layer also need good matching on the basis of ensuring the matching between the FSS layer and the base material, and the reliability of the integral component can be improved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides high-temperature-resistant low-expansion-coefficient bonding slurry for a ceramic matrix composite material and a preparation method thereof, which are used for making basic research work for the combined connection of the ceramic matrix wave-transparent composite material.
The technical scheme of the invention is as follows:
in a first aspect, the invention provides high-temperature-resistant low-expansion-coefficient bonding slurry for a ceramic matrix composite, which comprises 55-85 wt% of microcrystalline glass powder and 15-45 wt% of an organic bonding phase; the microcrystalline glass powder is SiO2-Al2O3-B2O3-MgO-BaO-ZnO-ZrO2Is mixed powder of microcrystalline glass powder and beta-eucryptite microcrystalline glass powder; the organic binding phase includes an organic solvent, a dispersant, and a thickener.
Further, the microcrystalline glass powder is SiO2-Al2O3-B2O3-MgO-BaO-ZnO-ZrO2Is a mixed powder of microcrystalline glass powder and beta-eucryptite microcrystalline glass powder, which comprises SiO 55-72 wt% (based on the total weight of the microcrystalline glass powder)26 to 20% of Al2O32-13% of B2O31-8% of MgO, 0-3% of BaO, 0-3% of ZnO, 0-2% of CaO and 0-2% of ZrO20-3% of rare earth oxide and 3-15% of beta-eucryptite microcrystalline glass powder;
the organic bonding phase comprises 70-85 wt% of organic solvent, 2-15 wt% of dispersant and 2-15 wt% of thickener.
Further, the microcrystalline glass powder has a coefficient of thermal expansion of 0.5 × 10-6/℃～1.6×10-6/℃。
Further, the organic solvent is at least one of terpineol, butyl carbitol acetate and diethylene glycol ethyl ether.
Further, the dispersant is at least one of triamines citrate, polymethacrylic acid amine and 1, 4-dihydroxysulfonic acid amine.
Further, the thickener is a polymer thickener, and the polymer thickener is at least one of ethyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, nitrocellulose and tributyl citrate.
Further, the rare earth oxide is La2O3、Gd2O3、Y2O3、Er2O3、CeO2、Nd2O3One or more of them.
Furthermore, the viscosity range of the high-temperature resistant bonding slurry for the ceramic matrix composite material is 50 Pa.S-120 Pa.S, and the fineness is less than 12 mu m.
In a second aspect, the present invention further provides a preparation method of the high temperature resistant low expansion coefficient bonding slurry for ceramic matrix composite, including the following steps:
step 1, preparing base glass powder: preparing ingredients according to the weight percentage in the formula, mixing the ingredients in a mixer for 2-24h, uniformly mixing the ingredients, putting the mixture into a corundum crucible, keeping the temperature of 1500-1700 ℃ in a resistance furnace for 1-4 h to obtain clear glass liquid, then quenching the glass liquid in deionized water, taking out the glass liquid, putting the glass liquid into a blast drying box, drying the glass liquid for 2-6h at 80-120 ℃ to obtain glass slag, then putting the glass slag into a planetary ball mill for ball milling for 4-8h, sieving the glass slag with a 400-sand-screening 500-mesh sieve to obtain basic glass powder, and controlling the average particle size of the powder to be lower than 3 mu m;
step 2, preparing microcrystalline glass powder: adding beta-eucryptite into the glass powder obtained in the step 1, ball-milling for 2-5h, drying, sieving by using a 300-plus 400-mesh sieve, then melting, water quenching and drying to obtain the microcrystalline glass powder, and controlling the average particle size of the powder to be 1.0-2.5 um;
step 3, preparing an organic bonding phase: accurately weighing an organic solvent, a thickening agent and a dispersing agent, then putting the organic solvent, the thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving the organic solvent, the thickening agent and the dispersing agent for 1-3 hours at a constant temperature of 80-85 ℃ to obtain a clear and transparent fluid;
step 4, preparing bonding slurry: stirring and dispersing the microcrystalline glass powder and the organic bonding phase in a container, then repeatedly grinding the mixture in a three-roll grinder, and controlling the fineness to be below 12um and the viscosity range to be 50 Pa.S-120 Pa.S to obtain the bonding slurry.
Further, the average particle size of the powder in the step 1 is controlled to be 1.0-2.5 μm; the melting temperature in the step 2 is 1250-.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) the invention provides a high-temperature resistant adhesive for ceramic matrix composite materials and a preparation method thereof, which are used as adhesives among wave-transparent ceramic materials, and the adjustment of the thermal expansion coefficient, the dielectric constant, the dielectric loss, the glass transition temperature, the softening temperature, the crystallization temperature and the like of microcrystalline glass powder is realized by adjusting the types and the contents of oxides in the microcrystalline glass powder, so that the thermal expansion coefficient of the adhesive slurry is equivalent to that of a ceramic substrate, the dielectric constant of 9GHz is 4.5-6.0, and the dielectric loss tangent is 3 multiplied by 10-3-5×10-3The wave-transparent use requirement of a specific frequency band can be met;
(2) SiO in glass powder composition2And Al2O3The content of (A) is higher, the melting temperature and the high-temperature viscosity are both very high, and after rare earth element oxide is added into the rare earth element oxide, because the radius of rare earth ions is large and the coordination number is higher, when the introduced amount is less, the network structure can be damaged, the network connectivity is reduced, the viscosity is reduced, and the adhesive force of the slurry after sintering is improved.
(3) The ceramic material sample connected by the bonding slurry has the tensile shear strength at room temperature of not less than 7.0MPa, the compressive shear strength of not less than 10.0MPa, good bonding performance and no defects of spalling, warping, cracks and the like caused by mismatching of interface layers.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, the present invention shall be described in further detail with reference to specific examples.
Example 1
The high-temperature-resistant low-expansion-coefficient bonding slurry for the ceramic matrix composite and the preparation method thereof comprise the following steps of:
1. preparing base glass powder: weighing 65% by mass of SiO214% of Al2O37% of B2O36% of MgO, 2% of BaO, 2% of CaO, 2% of ZnO, 2% of ZrO2Uniformly mixing in a mixer for 12 hours; then keeping the temperature of 1600 ℃ in a high-temperature resistance furnace for 1.5h to obtain clear molten glass; then, water quenching the glass liquid in deionized water, taking out, putting into a forced air drying oven, and drying for 4 hours at 100 ℃ to obtain glass slag; ball-milling the glass slag in a planetary ball mill for 8 hours, and sieving with a 500-mesh sieve to obtain base glass powder with the particle size of 1.0-2.5 mu m;
2. preparing microcrystalline glass powder: adding 5% of beta-eucryptite into the basic glass powder, performing ball milling for 2h, drying, screening by using a 400-mesh sieve, preserving the heat of the screened raw material in a resistance furnace at 1300 ℃ for 1h, and performing water quenching, ball milling and drying after clarification to obtain the microcrystalline glass powder;
specifically, the test shows that the softening point of the microcrystalline glass powder is 720 ℃, and the thermal expansion coefficient is 1.2 multiplied by 10-6/℃。
3. Preparing an organic bonding phase: accurately weighing an organic solvent, a high-molecular thickening agent and a dispersing agent, then putting the organic solvent, the high-molecular thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving at a constant temperature of 80-85 ℃ for 1-3 hours to obtain a clear and transparent fluid;
specifically, the organic solvent comprises 55% by weight of terpineol and 35% by weight of butyl carbitol; the macromolecular thickener comprises 8 percent of ethyl cellulose by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine;
4. preparing bonding slurry: 67% by weight of microcrystalline glass powder and 33% by weight of organic bonding phase were stirred and dispersed in a container, and then repeatedly ground in a three-roll grinder to obtain a bonding slurry.
The silica-based composite material reinforced with quartz fiber was bonded with the above bonding slurry in a size prescribed by the standard, and the bonded sample was dried at 120 ℃ for 0.5 hour and then heat-treated at 950 ℃ for 0.5 hour. Then, the tensile shear strength and the bending shear strength are tested, and the test results are as follows: the tensile shear strength was 7.5MPa and the compressive shear strength was 11.2 MPa.
Example 2
1. Preparing base glass powder: weighing 70% by mass of SiO213% of Al2O35% of B2O33% of MgO, 2% of BaO, 0% of CaO, 2% of ZnO, 2% of ZrO2And 3% of La2O3Uniformly mixing in a mixer for 20 hours; then keeping the temperature of 1600 ℃ in a high-temperature resistance furnace for 2 hours to obtain clear glass liquid; then, water quenching the glass liquid in deionized water, taking out, putting into a forced air drying oven, and drying for 4 hours at 100 ℃ to obtain glass slag; ball-milling the glass slag in a planetary ball mill for 8 hours, and sieving with a 500-mesh sieve to obtain base glass powder with the particle size of 1.0-2.5 mu m;
2. preparing microcrystalline glass powder: adding 5% of beta-eucryptite into the basic glass powder, performing ball milling for 2h, drying, screening by using a 400-mesh sieve, preserving the heat of the screened raw material in a resistance furnace at 1300 ℃ for 1h, and performing water quenching, ball milling and drying after clarification to obtain the microcrystalline glass powder;
specifically, the test shows that the softening point of the microcrystalline glass powder is 705 ℃, and the thermal expansion coefficient is 1.55 multiplied by 10-6/℃。
3. Preparing an organic bonding phase: accurately weighing an organic solvent, a high-molecular thickening agent and a dispersing agent, then putting the organic solvent, the high-molecular thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving at a constant temperature of 80-85 ℃ for 1-3 hours to obtain a clear and transparent fluid;
specifically, the organic solvent comprises 55% by weight of terpineol and 35% by weight of butyl carbitol; the macromolecular thickener comprises 8 percent of ethyl cellulose by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine;
4. preparing bonding slurry: 67 wt% of microcrystalline glass powder and 33 wt% of organic bonding phase are stirred and dispersed in a container, and then the mixture is repeatedly ground in a three-roll grinder to obtain inorganic bonding slurry.
The silica-based composite material reinforced with quartz fiber was bonded with the above bonding slurry in a size prescribed by the standard, and the bonded sample was dried at 120 ℃ for 0.5 hour and then heat-treated at 950 ℃ for 0.5 hour. Then, the tensile shear strength and the bending shear strength are tested, and the test results are as follows: the tensile shear strength is 7.2MPa, and the compressive shear strength is 10.8 MPa.
Example 3
1. Preparing base glass powder: weighing 70% by mass of SiO213% of Al2O35% of B2O33% of MgO, 2% of BaO, 0% of CaO, 2% of ZnO, 2% of ZrO2And 3% of CeO2Uniformly mixing in a mixer for 20 hours; then keeping the temperature of 1600 ℃ in a high-temperature resistance furnace for 2 hours to obtain clear glass liquid; then, water quenching the glass liquid in deionized water, taking out, putting into a forced air drying oven, and drying for 4 hours at 100 ℃ to obtain glass slag; ball-milling the glass slag in a planetary ball mill for 8 hours, and sieving with a 500-mesh sieve to obtain base glass powder with the particle size of 1.0-2.5 mu m;
2. preparing microcrystalline glass powder: adding 10% of beta-eucryptite into the basic glass powder, performing ball milling for 2h, drying, screening by using a 400-mesh sieve, preserving the heat of the screened raw material in a resistance furnace at 1300 ℃ for 1h, and performing water quenching, ball milling and drying after clarification to obtain the microcrystalline glass powder;
specifically, the microcrystalline glass powder has a softening point of 740 ℃ and a coefficient of thermal expansion of 0.96 multiplied by 10 after being tested-6/℃。
3. Preparing an organic bonding phase: accurately weighing an organic solvent, a high-molecular thickening agent and a dispersing agent, then putting the organic solvent, the high-molecular thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving at a constant temperature of 80-85 ℃ for 1-3 hours to obtain a clear and transparent fluid;
specifically, the organic solvent comprises 55% by weight of terpineol and 35% by weight of butyl carbitol; the macromolecular thickener comprises 8 percent of ethyl cellulose by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine;
4. preparing bonding slurry: 67 wt% of microcrystalline glass powder and 33 wt% of organic bonding phase are stirred and dispersed in a container, and then the mixture is repeatedly ground in a three-roll grinder to obtain inorganic bonding slurry.
The silica-based composite material reinforced with quartz fiber was bonded with the above bonding slurry in a size prescribed by the standard, and the bonded sample was dried at 120 ℃ for 0.5 hour and then heat-treated at 950 ℃ for 0.5 hour. Then, the tensile shear strength and the bending shear strength are tested, and the test results are as follows: the tensile shear strength is 8.3MPa, and the compressive shear strength is 12.4 MPa.
Example 4
1. Preparing base glass powder: weighing 72% by mass of SiO212% of Al2O36% of B2O3Uniformly mixing 4% of MgO, 2% of BaO, 2% of CaO and 2% of ZnO in a mixer for 12 hours; then keeping the temperature of 1600 ℃ in a high-temperature resistance furnace for 1.5h to obtain clear molten glass; then, water quenching the glass liquid in deionized water, taking out, putting into a forced air drying oven, and drying for 4 hours at 100 ℃ to obtain glass slag; ball-milling the glass slag in a planetary ball mill for 8 hours, and sieving with a 500-mesh sieve to obtain base glass powder with the particle size of 1.0-2.5 mu m;
2. preparing microcrystalline glass powder: adding 15% of beta-eucryptite into the basic glass powder, carrying out ball milling for 2h, drying, screening by using a 400-mesh sieve, preserving the heat of the screened raw material in a resistance furnace at 1300 ℃ for 1h, and carrying out water quenching, ball milling and drying after clarification to obtain the microcrystalline glass powder;
specifically, the test shows that the softening point of the microcrystalline glass powder is 790 ℃, and the thermal expansion coefficient of the microcrystalline glass powder is 0.5 multiplied by 10-6/℃。
3. Preparing an organic bonding phase: accurately weighing an organic solvent, a high-molecular thickening agent and a dispersing agent, then putting the organic solvent, the high-molecular thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving at a constant temperature of 80-85 ℃ for 1-3 hours to obtain a clear and transparent fluid;
specifically, the organic solvent comprises 55% by weight of terpineol and 35% by weight of butyl carbitol; the macromolecular thickener comprises 8 percent of ethyl cellulose by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine;
4. preparing bonding slurry: the microcrystalline glass powder with the weight percentage of 72 percent and the organic bonding phase with the weight percentage of 28 percent are stirred and dispersed in a container, and then the container is repeatedly ground in a three-roll grinder to obtain the inorganic bonding slurry.
The silica-based composite material reinforced with quartz fiber was bonded with the above bonding slurry in a size prescribed by the standard, and the bonded sample was dried at 120 ℃ for 0.5 hour and then heat-treated at 950 ℃ for 0.5 hour. Then, the tensile shear strength and the bending shear strength are tested, and the test results are as follows: the tensile shear strength is 10.8MPa, and the compressive shear strength is 16 MPa.
Example 5
1. Preparing base glass powder: weighing 72% by mass of SiO212% of Al2O36% of B2O33% MgO, 2% BaO, 2% ZnO and 3% La2O3Uniformly mixing in a mixer for 24 hours; then keeping the temperature of 1600 ℃ in a high-temperature resistance furnace for 2 hours to obtain clear glass liquid; then, water quenching the glass liquid in deionized water, taking out, putting into a forced air drying oven, and drying for 4 hours at 100 ℃ to obtain glass slag; ball-milling the glass slag in a planetary ball mill for 8 hours, and sieving with a 500-mesh sieve to obtain base glass powder with the particle size of 1.0-2.5 mu m;
2. preparing microcrystalline glass powder: adding 15% of beta-eucryptite into the basic glass powder, carrying out ball milling for 2h, drying, screening by using a 400-mesh sieve, preserving the heat of the screened raw material in a resistance furnace at 1300 ℃ for 1h, and carrying out water quenching, ball milling and drying after clarification to obtain the microcrystalline glass powder;
specifically, the microcrystalline glass powder has a softening point of 775 ℃ and a thermal expansion coefficient of 0.75 multiplied by 10-6/℃。
3. Preparing an organic bonding phase: accurately weighing an organic solvent, a high-molecular thickening agent and a dispersing agent, then putting the organic solvent, the high-molecular thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving at a constant temperature of 80-85 ℃ for 1-3 hours to obtain a clear and transparent fluid;
specifically, the organic solvent comprises 55% by weight of terpineol and 35% by weight of butyl carbitol; the macromolecular thickener comprises 8 percent of ethyl cellulose by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine;
4. preparing bonding slurry: the microcrystalline glass powder with the weight percentage of 72 percent and the organic bonding phase with the weight percentage of 28 percent are stirred and dispersed in a container, and then the container is repeatedly ground in a three-roll grinder to obtain the inorganic bonding slurry.
The silica-based composite material reinforced with quartz fiber was bonded with the above bonding slurry in a size prescribed by the standard, and the bonded sample was dried at 120 ℃ for 0.5 hour and then heat-treated at 950 ℃ for 0.5 hour. Then, the tensile shear strength and the bending shear strength are tested, and the test results are as follows: the tensile shear strength was 12MPa and the compressive shear strength was 17.4 MPa.
Example 6
1. Preparing base glass powder: weighing SiO with the mass percent of 58%218% of Al2O312% of B2O34% of MgO, 2% of BaO, 2% of CaO, 2% of ZnO, 2% of ZrO2Uniformly mixing in a mixer for 12 hours; then keeping the temperature of 1600 ℃ in a high-temperature resistance furnace for 1.5h to obtain clear molten glass; then, water quenching the glass liquid in deionized water, taking out, putting into a forced air drying oven, and drying for 4 hours at 100 ℃ to obtain glass slag; ball-milling the glass slag in a planetary ball mill for 6 hours, and sieving with a 400-mesh sieve to obtain base glass powder with the particle size of 1.0-2.5 mu m;
2. preparing microcrystalline glass powder: adding 5% of beta-eucryptite into the basic glass powder, performing ball milling for 2h, drying, screening by using a 300-mesh sieve, preserving the heat of the screened raw material in a resistance furnace at 1300 ℃ for 1h, and performing water quenching, ball milling and drying after clarification to obtain the microcrystalline glass powder;
specifically, the softening point of the microcrystalline glass powder is 735 after testingDEG C, coefficient of thermal expansion of 1.5X 10-6/℃。
3. Preparing an organic bonding phase: accurately weighing an organic solvent, a high-molecular thickening agent and a dispersing agent, then putting the organic solvent, the high-molecular thickening agent and the dispersing agent into a round-bottom flask, stirring and dissolving at a constant temperature of 80-85 ℃ for 1-3 hours to obtain a clear and transparent fluid;
specifically, the organic solvent comprises 55% by weight of terpineol and 35% by weight of butyl carbitol; the macromolecular thickener comprises 8 percent of ethyl cellulose by weight percentage; the dispersant comprises 2 weight percent of polymethacrylic acid amine;
4. preparing bonding slurry: 67% by weight of microcrystalline glass powder and 33% by weight of organic bonding phase were stirred and dispersed in a container, and then repeatedly ground in a three-roll grinder to obtain a bonding slurry.
The silica-based composite material reinforced with quartz fiber was bonded with the above bonding slurry in a size prescribed by the standard, and the bonded sample was dried at 120 ℃ for 0.5 hour and then heat-treated at 950 ℃ for 0.5 hour. Then, the tensile shear strength and the bending shear strength are tested, and the test results are as follows: the tensile shear strength is 6.1MPa, and the compressive shear strength is 8.6 MPa.
The particular embodiments of the present invention disclosed above are illustrative only and are not intended to be limiting, since various alternatives, modifications, and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The invention should not be limited to the disclosure of the embodiments in the present specification, but the scope of the invention is defined by the appended claims.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010812519.5A CN112225458B (en) | 2020-08-13 | 2020-08-13 | A kind of high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite materials and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010812519.5A CN112225458B (en) | 2020-08-13 | 2020-08-13 | A kind of high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite materials and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112225458A true CN112225458A (en) | 2021-01-15 |
| CN112225458B CN112225458B (en) | 2022-09-23 |
Family
ID=74115424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010812519.5A Active CN112225458B (en) | 2020-08-13 | 2020-08-13 | A kind of high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite materials and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112225458B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113800771A (en) * | 2021-09-13 | 2021-12-17 | 中国建筑材料科学研究总院有限公司 | Encapsulated microcrystalline glass slurry, thin film platinum resistor temperature sensor and preparation method thereof |
| CN113880426A (en) * | 2021-11-11 | 2022-01-04 | 广东省科学院新材料研究所 | Microcrystalline glass brazing filler metal for ceramic connection, preparation method thereof and ceramic connection method |
| CN114038607A (en) * | 2021-09-29 | 2022-02-11 | 航天特种材料及工艺技术研究所 | Platinum slurry for ceramic substrate FSS structure and preparation method thereof |
| CN115353407A (en) * | 2022-08-25 | 2022-11-18 | 哈尔滨工业大学 | A Repairing Method of SiO2f/SiO2 Composite Material |
| CN116178038A (en) * | 2023-02-22 | 2023-05-30 | 长春工业大学 | A method for joining transparent spinel and transparent sapphire ceramics using double-layer glass solder |
| CN116495992A (en) * | 2023-04-26 | 2023-07-28 | 华东理工大学 | Glass ceramic slurry for temperature sensor and preparation method thereof |
Citations (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1291284A (en) * | 1969-12-04 | 1972-10-04 | Anchor Hocking Corp | Compositions for use as low thermal expansion, devitrifying solder glasses or coatings |
| CN1145350A (en) * | 1990-10-04 | 1997-03-19 | 纳幕尔杜邦公司 | Method for reducing shrinkage during firing of ceramic bodies |
| US5925444A (en) * | 1992-12-09 | 1999-07-20 | Hitachi, Ltd. | Organic binder for shaping ceramic, its production method and product employing the same |
| DE19939787A1 (en) * | 1999-08-21 | 2001-02-22 | Schott Glas | Transparent glass ceramic colored using vanadium oxide additive has a crystal phase made of high quartz content mixed crystals and a specified light transmission |
| CN1424729A (en) * | 2002-12-30 | 2003-06-18 | 中国人民解放军国防科学技术大学 | Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
| US20040148869A1 (en) * | 2003-02-05 | 2004-08-05 | 3M Innovative Properties Company | Ceramics and methods of making the same |
| US20050266251A1 (en) * | 2004-05-27 | 2005-12-01 | Delaware Capital Formation, Inc. | Glass-ceramic materials and electronic packages including same |
| US20080174054A1 (en) * | 2007-01-24 | 2008-07-24 | Asml Holding N.V. | Bonding Silicon Silicon Carbide to Glass Ceramics |
| CN101364454A (en) * | 2008-09-23 | 2009-02-11 | 陕西科技大学 | Thick-film circuit resistance paste based on aluminum insulating layer and preparation method thereof |
| CN102145978A (en) * | 2010-02-10 | 2011-08-10 | 中国科学院上海硅酸盐研究所 | Glass solder for connecting SiC ceramics, and preparation method and application thereof |
| CN102515535A (en) * | 2011-12-21 | 2012-06-27 | 中国计量学院 | Lead-free low expansion coefficient glass powder for TFT-LCD sealing and preparation method thereof |
| CN104370469A (en) * | 2014-10-28 | 2015-02-25 | 蒋达光 | Colorful glass ceramic with ultralow expansion coefficient and high transparency, and parathion method thereof |
| CN106879086A (en) * | 2016-12-22 | 2017-06-20 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of aluminum-nitride-based timber-used large power thick film circuit high temperature sintering resistance slurry and preparation method thereof |
| CN107358991A (en) * | 2017-07-05 | 2017-11-17 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of dielectric paste and its preparation technology for aluminium alloy base plate thick film circuit |
| CN108147671A (en) * | 2017-12-28 | 2018-06-12 | 哈尔滨工业大学 | It is a kind of for devitrified glass solder of connecting silicon nitride ceramics and preparation method thereof |
| CN109776086A (en) * | 2017-11-15 | 2019-05-21 | 中国科学院上海硅酸盐研究所 | A kind of glass and ceramic composite zero-expansion material and preparation method thereof |
| CN110550864A (en) * | 2019-09-29 | 2019-12-10 | 长沙新材料产业研究院有限公司 | low-expansion-coefficient insulating medium slurry and preparation method thereof |
| CN110776259A (en) * | 2019-11-01 | 2020-02-11 | 湖南嘉盛电陶新材料股份有限公司 | Low-expansion-coefficient medium-low temperature environment-friendly glass powder and preparation method and application thereof |
-
2020
- 2020-08-13 CN CN202010812519.5A patent/CN112225458B/en active Active
Patent Citations (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1291284A (en) * | 1969-12-04 | 1972-10-04 | Anchor Hocking Corp | Compositions for use as low thermal expansion, devitrifying solder glasses or coatings |
| CN1145350A (en) * | 1990-10-04 | 1997-03-19 | 纳幕尔杜邦公司 | Method for reducing shrinkage during firing of ceramic bodies |
| US5925444A (en) * | 1992-12-09 | 1999-07-20 | Hitachi, Ltd. | Organic binder for shaping ceramic, its production method and product employing the same |
| DE19939787A1 (en) * | 1999-08-21 | 2001-02-22 | Schott Glas | Transparent glass ceramic colored using vanadium oxide additive has a crystal phase made of high quartz content mixed crystals and a specified light transmission |
| CN1424729A (en) * | 2002-12-30 | 2003-06-18 | 中国人民解放军国防科学技术大学 | Medium sizing agent and its producing process for high-power thick-film circuit based on stainless steel substrate |
| US20040148869A1 (en) * | 2003-02-05 | 2004-08-05 | 3M Innovative Properties Company | Ceramics and methods of making the same |
| US20050266251A1 (en) * | 2004-05-27 | 2005-12-01 | Delaware Capital Formation, Inc. | Glass-ceramic materials and electronic packages including same |
| US20080174054A1 (en) * | 2007-01-24 | 2008-07-24 | Asml Holding N.V. | Bonding Silicon Silicon Carbide to Glass Ceramics |
| CN101364454A (en) * | 2008-09-23 | 2009-02-11 | 陕西科技大学 | Thick-film circuit resistance paste based on aluminum insulating layer and preparation method thereof |
| CN102145978A (en) * | 2010-02-10 | 2011-08-10 | 中国科学院上海硅酸盐研究所 | Glass solder for connecting SiC ceramics, and preparation method and application thereof |
| CN102515535A (en) * | 2011-12-21 | 2012-06-27 | 中国计量学院 | Lead-free low expansion coefficient glass powder for TFT-LCD sealing and preparation method thereof |
| CN104370469A (en) * | 2014-10-28 | 2015-02-25 | 蒋达光 | Colorful glass ceramic with ultralow expansion coefficient and high transparency, and parathion method thereof |
| CN106879086A (en) * | 2016-12-22 | 2017-06-20 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of aluminum-nitride-based timber-used large power thick film circuit high temperature sintering resistance slurry and preparation method thereof |
| CN107358991A (en) * | 2017-07-05 | 2017-11-17 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of dielectric paste and its preparation technology for aluminium alloy base plate thick film circuit |
| CN109776086A (en) * | 2017-11-15 | 2019-05-21 | 中国科学院上海硅酸盐研究所 | A kind of glass and ceramic composite zero-expansion material and preparation method thereof |
| CN108147671A (en) * | 2017-12-28 | 2018-06-12 | 哈尔滨工业大学 | It is a kind of for devitrified glass solder of connecting silicon nitride ceramics and preparation method thereof |
| CN110550864A (en) * | 2019-09-29 | 2019-12-10 | 长沙新材料产业研究院有限公司 | low-expansion-coefficient insulating medium slurry and preparation method thereof |
| CN110776259A (en) * | 2019-11-01 | 2020-02-11 | 湖南嘉盛电陶新材料股份有限公司 | Low-expansion-coefficient medium-low temperature environment-friendly glass powder and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| YANRU JI等: "Enhanced bonding strength of Al2O3/AlN ceramics joined via glass frit with", 《CERAMICS INTERNATIONAL》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113800771A (en) * | 2021-09-13 | 2021-12-17 | 中国建筑材料科学研究总院有限公司 | Encapsulated microcrystalline glass slurry, thin film platinum resistor temperature sensor and preparation method thereof |
| CN114038607A (en) * | 2021-09-29 | 2022-02-11 | 航天特种材料及工艺技术研究所 | Platinum slurry for ceramic substrate FSS structure and preparation method thereof |
| CN113880426A (en) * | 2021-11-11 | 2022-01-04 | 广东省科学院新材料研究所 | Microcrystalline glass brazing filler metal for ceramic connection, preparation method thereof and ceramic connection method |
| CN115353407A (en) * | 2022-08-25 | 2022-11-18 | 哈尔滨工业大学 | A Repairing Method of SiO2f/SiO2 Composite Material |
| CN116178038A (en) * | 2023-02-22 | 2023-05-30 | 长春工业大学 | A method for joining transparent spinel and transparent sapphire ceramics using double-layer glass solder |
| CN116178038B (en) * | 2023-02-22 | 2024-05-31 | 长春工业大学 | Method for connecting transparent spinel and transparent sapphire ceramic by adopting double-layer glass solder |
| CN116495992A (en) * | 2023-04-26 | 2023-07-28 | 华东理工大学 | Glass ceramic slurry for temperature sensor and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112225458B (en) | 2022-09-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112225458B (en) | A kind of high temperature resistant and low expansion coefficient bonding slurry for ceramic matrix composite materials and preparation method thereof | |
| CN100568598C (en) | Method of making metal to glass, metal to metal or metal to ceramic joins | |
| CN108373324B (en) | Light sagger for roasting lithium battery anode material and preparation method thereof | |
| CN105669223B (en) | Sagger | |
| CN102145978B (en) | Glass solder for connecting SiC ceramics, and preparation method and application thereof | |
| CN112299825B (en) | A kind of preparation method of low dielectric and low temperature co-fired ceramic material | |
| CN110330356B (en) | A kind of silicon carbide ceramic brazing connection method | |
| CN109836141B (en) | High-thermal-conductivity low-temperature co-fired ceramic material and preparation method thereof | |
| CN107556885B (en) | A kind of near-infrared radiation ceramic coating for ethylene cracking furnace and its preparation method and application | |
| CN108623158A (en) | A kind of acidproof enamel enamel and preparation method thereof | |
| CN112225462A (en) | Low-expansion coefficient and low-dielectric constant glass-ceramic powder for electronic paste and preparation method thereof | |
| CN113880426A (en) | Microcrystalline glass brazing filler metal for ceramic connection, preparation method thereof and ceramic connection method | |
| CN105502946B (en) | A kind of high emissivity glass glaze and the method that high emissivity coating is prepared by the glaze | |
| CN105948748A (en) | Silicon-boron-carbon-nitrogen-zirconium ceramic composite material and preparation method thereof | |
| CN105481253B (en) | A kind of preparation method of compound low temperature sealing glass solder soldering paste | |
| CN108822792A (en) | A kind of high temperature adhesive preparation method suitable for nickel-base alloy | |
| CN106882950B (en) | Method for enhancing high-temperature-resistant phosphate adhesive by using silica sol | |
| CN111148345A (en) | Blue dielectric paste for thick film circuit and preparation method and application thereof | |
| CN109081678B (en) | High-thermal-stability feldspar ceramic blank and preparation method of product thereof | |
| CN114804840A (en) | Alumina ceramic substrate and preparation method and application thereof | |
| CN114920575A (en) | High-performance ceramic connecting piece and preparation method and application thereof | |
| CN113816774A (en) | A kind of high-purity alumina corundum ceramic metallization method | |
| CN118084541A (en) | High-temperature cofiring ceramic metalized slurry and preparation method thereof | |
| CN106588123A (en) | Activated molybdenum-manganese slurry used in ceramic metallization and preparing method thereof | |
| CN108329055B (en) | Method for repairing SiC setter plate or sagger and repairing bonding material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |