CN113735600B - Method for preparing ceramic sheet and sealing assembly - Google Patents
Method for preparing ceramic sheet and sealing assembly Download PDFInfo
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- CN113735600B CN113735600B CN202110984145.XA CN202110984145A CN113735600B CN 113735600 B CN113735600 B CN 113735600B CN 202110984145 A CN202110984145 A CN 202110984145A CN 113735600 B CN113735600 B CN 113735600B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 156
- 238000007789 sealing Methods 0.000 title claims abstract description 103
- 238000000034 method Methods 0.000 title description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 81
- 239000011148 porous material Substances 0.000 claims abstract description 38
- 239000002002 slurry Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 51
- 239000007788 liquid Substances 0.000 claims description 48
- 239000002245 particle Substances 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 19
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 18
- 239000011230 binding agent Substances 0.000 claims description 15
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 13
- 239000004014 plasticizer Substances 0.000 claims description 13
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 239000001087 glyceryl triacetate Substances 0.000 claims description 9
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 229960002622 triacetin Drugs 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 7
- 239000011833 salt mixture Substances 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000007731 hot pressing Methods 0.000 claims description 4
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 claims 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- 238000005868 electrolysis reaction Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 description 21
- 238000002844 melting Methods 0.000 description 11
- 230000008018 melting Effects 0.000 description 11
- 239000007787 solid Substances 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 230000007704 transition Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000003993 interaction Effects 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
- 239000012782 phase change material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5007—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing
- C04B41/501—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with salts or salty compositions, e.g. for salt glazing containing carbon in the anion, e.g. carbonates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The application discloses a preparation method of a ceramic wafer and a sealing assembly, wherein the preparation method of the ceramic wafer comprises the following steps: step 1: obtaining slurry; step 2: pouring the slurry into a model to form a ceramic plate, wherein the ceramic plate is internally provided with pores, and the porosity of the ceramic plate is more than or equal to 30%; step 3: immersing the ceramic wafer in molten salt so that the molten salt fills the pores of the ceramic wafer; step 4: and (5) drying. The ceramic wafer prepared by the preparation method of the ceramic wafer can be used as a sealing gasket under a high-temperature working condition (such as the field of high-temperature water electrolysis equipment). The sealing assembly comprises a ceramic plate, a first flange and a second flange, wherein the ceramic plate is clamped between the first flange and the second flange and used as a sealing gasket.
Description
Technical Field
The application relates to the technical field of sealing, in particular to a preparation method of a ceramic plate and a sealing assembly with the ceramic plate.
Background
The polymer sealing gasket commonly adopted in the water electrolysis equipment in the related art is used as a sealing component, but the polymer sealing gasket has certain requirements on the temperature of the water to be electrolyzed, can only be applied to the water electrolysis equipment at normal temperature, and has certain limitation in application to the water electrolysis equipment at high temperature.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent.
Therefore, the embodiment of the invention provides a preparation method of the ceramic sheet, and the ceramic sheet prepared by the preparation method has high-temperature sealing performance.
The embodiment of the invention also provides a sealing component which can be applied to high-temperature water electrolysis equipment to achieve the sealing effect.
The preparation method of the ceramic sheet according to the embodiment of the invention comprises the following steps:
step 1: obtaining slurry, wherein the slurry is a mixture containing a solvent, powder and an additive, the powder is inorganic powder, and the slurry is stirred to be uniform;
step 2: pouring the slurry into a model, drying the model in an environment of 20-70 ℃ for more than 20 hours to evaporate a solvent, cooling the model to room temperature, and forming the slurry into a ceramic plate, wherein the ceramic plate is internally provided with pores, the porosity of the ceramic plate is more than or equal to 30%, and the pore diameter of the pores is 0.1-1 micron;
step 3: obtaining molten salt, soaking the ceramic wafer prepared in the step 2 in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic wafer, and soaking for more than 10 hours;
step 4: and taking out the ceramic plate, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic plate into salt particles.
According to the preparation method of the ceramic plate, provided by the embodiment of the invention, salt particles are filled in the pores of the ceramic plate, the salt particles have a melting temperature, and when the service temperature of the ceramic plate is higher than the melting temperature of the salt particles, the salt particles can be melted to form molten salt. Under capillary effect, the molten salt remains filled in the pores, forming a wet seal. Therefore, the ceramic plate prepared by the preparation method of the ceramic plate provided by the embodiment of the invention can be used as a sealing gasket under a high-temperature working condition (such as the field of high-temperature water electrolysis equipment), and the structural performance of the ceramic plate cannot be changed at high temperature due to the inherent high-temperature resistance of the ceramic plate.
In some embodiments, step 2 further comprises: and (5) carrying out hot pressing on the formed ceramic sheet.
In some embodiments, the molten salt includes 60% -70% molar content of lithium carbonate and 30% -40% molar content of potassium carbonate.
In some embodiments, the additive comprises a binder, a dispersant, and a plasticizer, the binder is polyvinyl alcohol, the dispersant is lactic acid, and the plasticizer is a mixture of glycerol, glyceryl triacetate, and ethylene glycol.
In some embodiments, the powder is 20.0 parts to 40.0 parts by weight and the solvent is 1.0 to 5.0 times the powder by weight.
In some embodiments, the molten salt has a melting temperature of 180 ℃ to 920 ℃.
According to another aspect of the present invention, a seal assembly is provided, including a ceramic sheet, where the ceramic sheet is a ceramic sheet prepared by the method for preparing a ceramic sheet according to any one of the above embodiments; the ceramic plate is arranged between the first flange and the second flange in a clamping mode, and the gas through hole, the first hole and the second hole form a communicated channel relatively in the first direction.
In some embodiments, the seal assembly further comprises a solid-liquid seal medium defining an annular first seal chamber between the ceramic wafer and the first flange, and an annular second seal chamber between the ceramic wafer and the second flange, both the first seal chamber and the second seal chamber surrounding the channel, the solid-liquid seal medium filling the first seal chamber and the second seal chamber.
In some embodiments, a portion of the solid-liquid sealing medium in a liquid state is capable of entering and filling in the gap between the first flange and the ceramic wafer and the gap between the second flange and the ceramic wafer.
In some embodiments, the solid-liquid sealing medium is a salt mixture that melts to form a molten salt.
Drawings
FIG. 1 is a cross-sectional view of the overall structure of a seal assembly according to an embodiment of the present application.
Fig. 2 is a schematic structural view of a ceramic wafer according to an embodiment of the present application.
Fig. 3 is a schematic structural view of a first flange according to an embodiment of the present application.
Reference numerals:
the mounting screw 1, the screw cap 2, the first flange 3, the ceramic plate 4, the first sealing chamber 5, the second mounting hole 6, the gas through hole 7, the first opening 8, the second opening 9, the second flange 10, the second sealing chamber 11, the first connecting pipe 12, the second connecting pipe 13, the annular groove 14 and the first mounting hole 15.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
The application discloses a preparation method of a ceramic wafer, which comprises the following steps:
step 1: obtaining a slurry, wherein the slurry is a mixture containing a solvent, powder, salt particles and an additive, the powder comprises lithium aluminum oxide powder, and the slurry is stirred to be uniform;
step 2: pouring the slurry into a model, drying the model in an environment of 20-70 ℃ for more than 20 hours to evaporate a solvent, cooling the model to room temperature, and forming the slurry into a ceramic plate, wherein the ceramic plate is internally provided with pores, the porosity of the ceramic plate is more than or equal to 30%, and the pore diameter of the pores is 0.1-1 micron;
step 3: obtaining molten salt, soaking the ceramic wafer prepared in the step 2 in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic wafer, and soaking for more than 10 hours;
step 4: and taking out the ceramic plate, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic plate into salt particles.
Optionally, the powder in step 1 comprises one or more of lithium alumina powder, magnesium oxide powder, lithium cobaltate powder, lithium manganate powder, aluminum oxide powder. The molten salt in the step 3 is obtained from a molten salt mixture, the ceramic sheet with the pores is soaked in the liquid molten salt, and the molten salt gradually enters and fills the pores of the ceramic sheet according to capillary effect. And 4, cooling and drying, and solidifying the liquid molten salt in the pores of the ceramic sheet into solid, namely salt particles.
In some embodiments, the method for preparing a ceramic sheet further comprises a hot pressing step, i.e., step 3: step 2 further comprises: and (5) carrying out hot pressing on the formed ceramic sheet.
According to the preparation method of the ceramic plate, provided by the embodiment of the invention, salt particles are filled in the pores of the ceramic plate, the salt particles have a melting temperature, and when the service temperature of the ceramic plate is higher than the melting temperature of the salt particles, the salt particles can be melted to form molten salt. Under capillary effect, the molten salt remains filled in the pores, forming a wet seal. Therefore, the ceramic plate prepared by the preparation method of the ceramic plate provided by the embodiment of the invention can be used as a sealing gasket under a high-temperature working condition (such as the field of high-temperature water electrolysis equipment), and the structural performance of the ceramic plate cannot be changed at high temperature due to the inherent high-temperature resistance of the ceramic plate.
Alternatively, the salt particles have a melting temperature of 180 ℃ to 920 ℃. That is, when the operating temperature of the ceramic sheet exceeds the melting temperature of the salt particles, the salt particles may melt into molten salt, filling the pores of the ceramic sheet to form a wet seal. It should be noted that, the melting temperature of the salt particles is related to the composition of the salt particles, and when a person skilled in the art selects the salt particles, a person skilled in the art may select salt particles with a suitable melting temperature as the filling material of the ceramic sheet according to the usage conditions of the ceramic sheet.
Alternatively, the molten salt comprises 60% -70% molar content of lithium carbonate and 30% -40% molar content of potassium carbonate.
Optionally, the additive comprises a binder, a dispersant and a plasticizer, wherein the binder is polyvinyl alcohol, the dispersant is lactic acid, and the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol. The solvent is water, n-butanol, ethanol or chloroform.
Optionally, the weight fraction of the powder is 20.0-40.0 parts, and the weight fraction of the solvent is 1.0-5.0 times that of the powder. The weight fraction of the binder is 7.0-12.0 parts, the weight fraction of the dispersing agent is 1.5-3.0 parts, and the weight fraction of the plasticizer is 4.0-8.0 parts.
Specific examples of the method for producing the ceramic sheet of the present invention are provided below.
Embodiment one:
step 1: preparing materials, wherein the powder material adopts lithium aluminum oxide powder, the powder material with the particle size of more than 1 mu m accounts for 70% -80% of the total weight of the powder material, and the powder material with the particle size of less than 1 mu m accounts for 10% -30% of the total weight of the powder material; the dispersing agent is lactic acid; the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol, wherein the glycerol: glyceryl triacetate: ethylene glycol is 1:1:1; the solvent is water;
the weight fraction of the powder is 20.0 parts; the weight fraction of the binder is 7.0 parts; the weight fraction of the dispersant is 1.5 parts; 4.0 parts by weight of plasticizer; the weight fraction of the solvent is 1.0 times of that of the powder;
uniformly stirring and mixing the ingredients according to a proportion to obtain slurry;
step 2: pouring the slurry obtained in the step 1 into a model, drying for more than 20 hours in an environment of 20-70 ℃ to evaporate the solvent, cooling to room temperature, and forming the slurry into a ceramic plate, wherein the porosity of the ceramic plate is 34.65%;
step 3: obtaining molten salt, wherein the molten salt comprises 60 mol% of lithium carbonate and 40 mol% of potassium carbonate; the binder is polyvinyl alcohol, and the ceramic sheet prepared in the step 2 is soaked in the molten salt so that the molten salt is soaked in and filled in the pores of the ceramic sheet, and the soaking time is more than 10 hours;
step 4: and taking out the ceramic plate, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic plate into salt particles.
Embodiment two:
step 1: preparing materials, wherein the powder material adopts lithium aluminum oxide powder, the powder material with the particle size of more than 1 mu m accounts for 70% -80% of the total weight of the powder material, and the powder material with the particle size of less than 1 mu m accounts for 10% -30% of the total weight of the powder material; the binder is polyvinyl alcohol; the dispersing agent is lactic acid; the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol, wherein the glycerol: glyceryl triacetate: ethylene glycol is 1:1:1; the solvent is n-butanol;
the weight fraction of the powder is 40.0 parts; the weight fraction of the binder is 12.0 parts; 3.0 parts of dispersing agent by weight; the weight fraction of the plasticizer is 8.0 parts; the weight fraction of the solvent is 5.0 times of that of the powder;
uniformly stirring and mixing the ingredients according to a proportion to obtain slurry;
step 2: pouring the slurry obtained in the step 1 into a model, drying for more than 20 hours in an environment of 20-70 ℃ to evaporate the solvent, cooling to room temperature, and forming the slurry into a ceramic plate, wherein the porosity of the ceramic plate is 56.89%;
step 3: obtaining molten salt, wherein the molten salt comprises 70 mol% of lithium carbonate and 30 mol% of potassium carbonate; the binder is polyvinyl alcohol, and the ceramic sheet prepared in the step 2 is soaked in the molten salt so that the molten salt is soaked in and filled in the pores of the ceramic sheet, and the soaking time is more than 10 hours;
step 4: and taking out the ceramic plate, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic plate into salt particles.
Embodiment III:
step 1: preparing materials, wherein the powder material adopts lithium aluminum oxide powder, the powder material with the particle size of more than 1 mu m accounts for 70% -80% of the total weight of the powder material, and the powder material with the particle size of less than 1 mu m accounts for 10% -30% of the total weight of the powder material; the binder is polyvinyl alcohol; the dispersing agent is lactic acid; the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol, wherein the glycerol: glyceryl triacetate: ethylene glycol is 1:1:1; the solvent is n-butanol;
the weight fraction of the powder is 30.0 parts; the weight fraction of the binder is 10.0 parts; the weight fraction of the dispersant is 2.0 parts; the weight fraction of the plasticizer is 6.0 parts; the weight fraction of the solvent is 3.0 times of that of the powder;
uniformly stirring and mixing the ingredients according to a proportion to obtain slurry;
step 2: pouring the slurry obtained in the step 1 into a model, drying for more than 20 hours in an environment of 20-70 ℃ to evaporate the solvent, cooling to room temperature, and forming the slurry into a ceramic plate, wherein the porosity of the ceramic plate is 49.76%;
step 3: obtaining molten salt, wherein the molten salt comprises 65 mol% of lithium carbonate and 35 mol% of potassium carbonate; the binder is polyvinyl alcohol, and the ceramic sheet prepared in the step 2 is soaked in the molten salt so that the molten salt is soaked in and filled in the pores of the ceramic sheet, and the soaking time is more than 10 hours;
step 4: and taking out the ceramic plate, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic plate into salt particles.
The embodiment of the application also discloses a sealing assembly which comprises a ceramic plate 4, a first flange 3 and a second flange 10. The ceramic sheet 4 is a ceramic sheet prepared according to the preparation method of the ceramic sheet of any one of the above embodiments. The ceramic plate 4 is sandwiched between the first flange 3 and the second flange 10.
The ceramic wafer 4 is provided with a gas through hole 7, the first flange 3 and the second flange 10 are provided with a first opening 8 and a second opening 9, and the gas through hole 7 and the first opening 8 and the second opening 9 form a communicating channel in the first direction. The channel is used for the circulation of a sealing medium (gas).
When the sealing component provided by the embodiment of the invention is applied to a high-temperature working condition, the phase change of salt particles in the pores is converted from solid state to liquid state, namely, the salt particles are melted to form molten salt. The liquid molten salt forms a wet seal in the pores of the ceramic plate 4, which acts to prevent leakage of gas in the channels through the pores. Therefore, the sealing component provided by the embodiment of the invention has excellent sealing performance under high-temperature working conditions (such as the field of high-temperature water electrolysis equipment). If the temperature is lowered below the melting temperature, the molten salt filled in the pores of the ceramic sheet 4 is converted into solid salt particles, filled as a filler in the pores of the ceramic sheet 4, and melted again into liquid molten salt at the next high temperature application, achieving wet sealing.
In some embodiments, the seal assembly further comprises a solid-liquid seal medium, the solid-liquid seal medium being a phase change material. The solid-liquid sealing medium has a phase transition temperature below which the solid-liquid sealing medium is in a solid state and above which the solid-liquid sealing medium is in a liquid state. The first flange 3 and the ceramic plate 4 define an annular first sealing chamber 5 therebetween, and the second flange 10 and the ceramic plate 4 define an annular second sealing chamber 11 therebetween. The first sealed chamber 5 and the second sealed chamber 11 are each disposed around the channel.
In some embodiments, the solid-liquid sealing medium fills the first sealed chamber 5 and the second sealed chamber 11 and may undergo a phase change reaction in the first sealed chamber 5 and the second sealed chamber 11, converting from solid to liquid. As an example, below the phase transition temperature, a solid-liquid sealing medium in solid form is accommodated in the first sealing chamber 5 and the second sealing chamber 11 when the sealing assembly is assembled. The assembled sealing assembly is applied to a high-temperature working condition, and as the working condition temperature of the sealing assembly gradually rises, solid-liquid sealing mediums in the first sealing chamber 5 and the second sealing chamber 11 are subjected to phase change, and the solid-liquid sealing mediums are converted from solid state to liquid state.
The liquid solid-liquid sealing medium in the first and second sealing chambers 5, 11 forms a wet seal in the sealing chambers, preventing gas in the channels from leaking through the assembly gap. In this way, the molten salt in liquid state in the pores of the ceramic sheet 4 and the solid-liquid sealing medium in liquid state in the first sealing chamber 5 and the second sealing chamber 11 form "double sealing protection", so that the sealing assembly provided by the embodiment of the invention has excellent sealing performance and is especially suitable for high-temperature working conditions, such as the field of high-temperature water electrolysis equipment.
Further, a part of the liquid solid-liquid sealing medium in the first sealing chamber 5 and the second sealing chamber 11 may enter and fill in the gap between the first flange 3 and the ceramic sheet 4 and the gap between the second flange 10 and the ceramic sheet 4 by capillary effect.
The gap between the first flange 3 and the ceramic plate 4 and the gap between the second flange 10 and the ceramic plate 4 are gaps generated during the assembly process. Alternatively, the gap size is 0.1 microns to 1 micron. The liquid solid-liquid sealing medium filled in the gap between the first flange 3 and the ceramic wafer 4 and the gap between the second flange 10 and the ceramic wafer 4 can further avoid leakage of gas through the assembly gap.
As the working time increases, the first and second sealing chambers 5 and 11 still retain part of the liquid solid-liquid sealing medium, so that a wet seal line in the first and second sealing chambers 5 and 11 can be ensured. Thus, when the seal assembly is assembled, sufficient solid-liquid sealing medium should be contained in the first seal chamber 5 and the second seal chamber 11.
Therefore, the liquid solid-liquid sealing medium remaining in the first sealing chamber 5 and the second sealing chamber 11, the liquid solid-liquid sealing medium in the gap between the first flange 3 and the ceramic wafer 4 and the gap between the second flange 10 and the ceramic wafer 4, and the liquid molten salt in the pores of the ceramic wafer 4 form a multiple sealing line, further improving the sealing performance of the sealing assembly.
In some embodiments, the solid-liquid sealing medium is a salt mixture, the salt mixture melts to form molten salt, the molten salt is a molten mass formed after the salt melts, and the molten salt is in a liquid mode.
Optionally, the salt mixture includes at least two salt species, each having a common melting point, i.e., having the same (or a relatively similar) phase transition temperature.
Alternatively, the salt mixture in this example is 60% -70% molar lithium carbonate and 30% -40% molar potassium carbonate.
Optionally, the solid-liquid sealing medium has a phase transition temperature of 180 ℃ to 920 ℃.
Fig. 1 is a cross-sectional view of an overall structure according to an embodiment of the present application, and as shown in fig. 1, an embodiment of the present application discloses a sealing assembly, including a ceramic sheet 4, a first flange 3, a second flange 10, and a solid-liquid sealing medium, wherein the ceramic sheet 4 is disposed between the first flange 3 and the second flange 10. That is, the first flange 3 and the second flange 10 are provided on both sides of the ceramic sheet 4, respectively.
Fig. 2 is a schematic structural view of a ceramic wafer according to an embodiment of the present application, and fig. 3 is a schematic structural view of a first flange according to an embodiment of the present application. As shown in fig. 1 and 2, the ceramic wafer 4 is provided with a gas through hole 7, the first flange is provided with a first opening 8, the second flange 10 is provided with a second opening 9, the axes of the gas through hole 7, the first opening 8 and the second opening 9 coincide, and the gas through hole 7, the first opening 8 and the second opening 9 form a communicating channel in the first direction. The channel is used for the circulation of a sealing medium (gas).
In this embodiment, an annular first sealing chamber 5 is formed between the ceramic plate 4 and the first flange 3, and an annular second sealing chamber 11 is formed between the ceramic plate 4 and the second flange 10, and the first sealing chamber 5 and the second sealing chamber 11 are respectively disposed around the channels. That is, a first sealing chamber 5 and a second sealing chamber 11 are formed between both sides of the ceramic sheet 4 and the first flange 3 and the second flange 10, respectively.
In this embodiment, as shown in fig. 1, the side of the first flange 3 adjacent to the ceramic plate 4 is provided with an annular groove 14 surrounding the channel, and a first sealing chamber 5 is defined between the annular groove 14 and the side of the ceramic plate 4 adjacent to the first flange 3. That is, an annular groove 14 centered on the channel is formed on the first flange 3 and on the side close to the ceramic plate 4, and an annular first sealing chamber 5 is formed between the annular groove 14 and the ceramic plate 4.
Similar to the first flange 3, the side of the second flange 10 adjacent to the ceramic plate 4 is provided with an annular groove surrounding the channel, the annular groove and the side of the ceramic plate 4 adjacent to the second flange 10 defining the second sealing chamber 11 therebetween. That is, an annular groove centered on the channel is formed on the second flange 10 and near the other side of the ceramic plate 4, and an annular second sealing chamber 11 is formed between the annular groove and the ceramic plate 4.
In other embodiments, the side of the ceramic plate 4 adjacent to the first flange 3 may be provided with an annular groove surrounding the channel and defining a first sealed chamber 5 with the side of the first flange 3 adjacent to the ceramic plate 4. The side of the ceramic plate 4 adjacent to the second flange 10 may be provided with an annular groove surrounding the channel, the annular groove and the side of the second flange adjacent to the ceramic plate 4 defining a second sealed chamber 11 therebetween.
Alternatively, in other embodiments, the side of the first flange 3 adjacent to the ceramic plate 4 is provided with a first annular groove surrounding the channel, and the side of the ceramic plate 4 adjacent to the first flange 3 is provided with a second annular groove surrounding the channel, the first annular groove being opposite to the second annular groove and defining the first sealed chamber 5. That is, a first annular groove is provided on one side of the first flange 3, a second annular groove is provided on the side of the ceramic sheet 4 corresponding to the first flange 3, the first annular groove and the second annular groove are both arranged centering on the channel, and an annular first seal chamber 5 is formed between the first annular groove and the second annular groove.
Similarly to the first flange 3, the side of the second flange 10 adjacent to the ceramic plate 4 is provided with a third annular groove surrounding the channel, and the side of the ceramic plate 4 adjacent to the second flange 10 is provided with a fourth annular groove surrounding the channel, opposite to the fourth annular groove and defining a second sealed chamber 11. That is, a third annular groove is formed on one side of the second flange 10, a fourth annular groove is formed on the side of the ceramic plate 4 corresponding to the second flange 10, the third annular groove and the fourth annular groove are both arranged centering on the channel, and an annular second sealing chamber 11 is formed between the third annular groove and the fourth annular groove.
In some embodiments, the first sealing chamber 5 may include a plurality of first sealing chambers 5, and a plurality of first sealing chambers 5 are sleeved in sequence. That is, a plurality of concentric annular first sealing chambers 5, i.e., a plurality of first sealing chambers 5 may be provided between the first flange 3 and the ceramic plate 4 centering on the passage, and radially disposed along the ceramic plate 4 with different radii. It should be noted that a plurality of second seal chambers 11 may be disposed as well, and a plurality of second seal chambers 11 may be disposed radially of the ceramic sheet according to different radii, and a plurality of second seal chambers 11 may be disposed sequentially at a certain pitch or may be disposed at different pitches.
The arrangement of the plurality of first sealing chambers 5 and the plurality of second sealing chambers 11 can increase the accommodating space of the solid-liquid sealing medium, and can further increase the sealing line, so that the sealing assembly forms stronger wet sealing at high temperature and has more excellent sealing effect.
As shown in fig. 1, the first flange 3 is connected to the first connection pipe 12, and the first connection pipe 12 communicates with the first opening 8, the second flange 10 is connected to the second connection pipe 13, and the second connection pipe 13 communicates with the second opening 9. The first connecting pipe 12 communicates with the second connecting pipe 13 through the first opening 8, the gas through hole 7 and the second opening 9, and integrally constitutes a passage extending in the first direction. It should be noted that the first connecting tube 12 and the second connecting tube 13 may be respectively inserted into the first opening 8 and the second opening 9. Of course, the first connecting pipe 12 and the second connecting pipe 13 may be fixed to the first flange 3 and the second flange 10, respectively, the end of the first connecting pipe 12 communicates with the end of the first opening 8, and the end of the second connecting pipe 13 communicates with the end of the second opening 9.
As shown in fig. 1-3, the ceramic plate 4 is provided with a first mounting hole 15, the first flange 3 is provided with a second mounting hole 6, and the second flange 10 is provided with a third mounting hole. The mounting screw 1 passes through the first, second and third mounting holes 15, 6 and 10 to connect the ceramic plate 4, the first and second flanges 3 and 10. That is, the second mounting hole 6, the third mounting hole and the first mounting hole 15 are formed in the first flange 3, the second flange 10 and the ceramic plate 4, respectively, the centers of the first mounting hole 15, the second mounting hole 6 and the third mounting hole are on the same straight line, the second mounting hole 6, the first mounting hole 15 and the third mounting hole are penetrated by the mounting screw 1, and the screw cap 2 is used for screwing, so that the first flange 3, the second flange and the ceramic plate 4 are relatively fixed.
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; may be mechanically connected, may be electrically connected or may be in communication with each other; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (6)
1. A seal assembly, comprising:
the ceramic plate is provided with a gas through hole;
the ceramic plate is clamped between the first flange and the second flange, and the gas through hole, the first opening and the second opening form a communicated channel relatively in a first direction;
the ceramic plate and the first flange define an annular first sealing chamber therebetween, the ceramic plate and the second flange define an annular second sealing chamber therebetween, the first sealing chamber and the second sealing chamber both encircle the channel, and the solid-liquid sealing medium is filled in the first sealing chamber and the second sealing chamber;
the preparation method of the ceramic sheet comprises the following steps:
step 1: obtaining slurry, wherein the slurry is a mixture containing a solvent, powder and an additive, the powder is inorganic powder, and the slurry is stirred to be uniform; the powder comprises one or more of lithium aluminum oxide powder, magnesium oxide powder, lithium cobalt oxide powder, lithium manganate powder and aluminum oxide powder; the weight fraction of the powder is 20.0-40.0 parts, and the weight fraction of the solvent is 1.0-5.0 times of that of the powder;
step 2: pouring the slurry into a model, drying the model in an environment of 20-70 ℃ for more than 20 hours to evaporate a solvent, cooling the model to room temperature, and forming the slurry into a ceramic plate, wherein the ceramic plate is internally provided with pores, the porosity of the ceramic plate is more than or equal to 30%, and the pore diameter of the pores is 0.1-1 micron;
step 3: obtaining molten salt, soaking the ceramic wafer prepared in the step 2 in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic wafer, and soaking for more than 10 hours; the temperature of the molten salt is 180-920 ℃;
step 4: and taking out the ceramic plate, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic plate into salt particles.
2. The seal assembly of claim 1, wherein step 2 further comprises: and (5) carrying out hot pressing on the formed ceramic sheet.
3. The seal assembly of claim 1 wherein the molten salt comprises 60% -70% molar content of lithium carbonate and 30% -40% molar content of potassium carbonate.
4. The seal assembly of claim 1, wherein the additive comprises a binder, a dispersant, and a plasticizer, the binder being polyvinyl alcohol, the dispersant being lactic acid, the plasticizer being a mixture of glycerol, glyceryl triacetate, and ethylene glycol.
5. The seal assembly of claim 1, wherein a portion of the solid-liquid sealing medium in a liquid state is capable of entering and filling in a gap between the first flange and the ceramic wafer and a gap between the second flange and the ceramic wafer.
6. The seal assembly of claim 1 or 5, wherein the solid-liquid sealing medium is a salt mixture.
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| CN202110984145.XA CN113735600B (en) | 2021-08-25 | 2021-08-25 | Method for preparing ceramic sheet and sealing assembly |
| PCT/CN2022/077523 WO2023024462A1 (en) | 2021-08-25 | 2022-02-23 | Preparation method for ceramic sheet and sealing component |
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| CN202110984145.XA CN113735600B (en) | 2021-08-25 | 2021-08-25 | Method for preparing ceramic sheet and sealing assembly |
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| CN113735600B true CN113735600B (en) | 2023-05-23 |
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| US5942345A (en) * | 1997-08-11 | 1999-08-24 | University Of Chicago | High performance electrolytes for MCFC |
| CN101799102A (en) * | 2010-03-31 | 2010-08-11 | 益科博能源科技（上海）有限公司 | Vacuum heat insulation pipeline and manufacturing method thereof |
| CN102299350B (en) * | 2010-06-23 | 2014-09-03 | 中国科学院大连化学物理研究所 | Diaphragm of molten carbonate fuel cell and preparation of diaphragm with composite pore structure |
| CN102314957B (en) * | 2011-07-06 | 2013-07-03 | 中国电子科技集团公司第五十五研究所 | Multilayer high-temperature co-fired-ceramic thick-film tungsten conductor paste and preparation method thereof |
| CN104282930B (en) * | 2013-07-10 | 2017-04-12 | 中国科学院大连化学物理研究所 | Molten carbonate fuel cell structure |
| CN104344120B (en) * | 2014-09-09 | 2016-08-24 | 中国科学院上海应用物理研究所 | Sealing and connecting device and method thereof for high-temperature molten salt |
| CN108630863A (en) * | 2017-03-21 | 2018-10-09 | 旭成（福建）科技股份有限公司 | A kind of preparation method of high porosity ceramic diaphragm |
| CN108218422A (en) * | 2018-01-18 | 2018-06-29 | 东莞信柏结构陶瓷股份有限公司 | Wear-resistant ceramic tape casting slurry and its application process |
| CN109135683B (en) * | 2018-08-22 | 2021-01-12 | 北京科技大学 | Method for preparing molten salt-ceramic phase change heat storage material |
| CN112707721B (en) * | 2020-12-30 | 2022-11-11 | 无锡市高宇晟新材料科技有限公司 | Silicon carbide toughened microwave dielectric ceramic material and preparation method thereof |
| CN113735600B (en) * | 2021-08-25 | 2023-05-23 | 中国华能集团清洁能源技术研究院有限公司 | Method for preparing ceramic sheet and sealing assembly |
| CN113800920B (en) * | 2021-08-25 | 2023-02-28 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of ceramic chip and sealing assembly |
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| WO2023024462A1 (en) | 2023-03-02 |
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