CN113735600A - Preparation method of ceramic chip and sealing assembly - Google Patents

Preparation method of ceramic chip and sealing assembly Download PDF

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Publication number
CN113735600A
CN113735600A CN202110984145.XA CN202110984145A CN113735600A CN 113735600 A CN113735600 A CN 113735600A CN 202110984145 A CN202110984145 A CN 202110984145A CN 113735600 A CN113735600 A CN 113735600A
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China
Prior art keywords
ceramic
flange
molten salt
pores
ceramic plate
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CN202110984145.XA
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Chinese (zh)
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CN113735600B (en
Inventor
王鹏杰
王韬
王凡
刘丽萍
郭海礁
王金意
张畅
余智勇
任志博
徐显明
张欢
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Huaneng Clean Energy Research Institute
Huaneng Group Technology Innovation Center Co Ltd
Sichuan Huaneng Baoxinghe Hydropower Co Ltd
Sichuan Huaneng Kangding Hydropower Co Ltd
Huaneng Mingtai Power Co Ltd
Sichuan Huaneng Dongxiguan Hydropower Co Ltd
Sichuan Huaneng Fujiang Hydropower Co Ltd
Sichuan Huaneng Hydrogen Technology Co Ltd
Sichuan Huaneng Jialingjiang Hydropower Co Ltd
Sichuan Huaneng Taipingyi Hydropower Co Ltd
Original Assignee
Huaneng Clean Energy Research Institute
Huaneng Group Technology Innovation Center Co Ltd
Sichuan Huaneng Baoxinghe Hydropower Co Ltd
Sichuan Huaneng Kangding Hydropower Co Ltd
Huaneng Mingtai Power Co Ltd
Sichuan Huaneng Dongxiguan Hydropower Co Ltd
Sichuan Huaneng Fujiang Hydropower Co Ltd
Sichuan Huaneng Hydrogen Technology Co Ltd
Sichuan Huaneng Jialingjiang Hydropower Co Ltd
Sichuan Huaneng Taipingyi Hydropower Co Ltd
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Application filed by Huaneng Clean Energy Research Institute, Huaneng Group Technology Innovation Center Co Ltd, Sichuan Huaneng Baoxinghe Hydropower Co Ltd, Sichuan Huaneng Kangding Hydropower Co Ltd, Huaneng Mingtai Power Co Ltd, Sichuan Huaneng Dongxiguan Hydropower Co Ltd, Sichuan Huaneng Fujiang Hydropower Co Ltd, Sichuan Huaneng Hydrogen Technology Co Ltd, Sichuan Huaneng Jialingjiang Hydropower Co Ltd, Sichuan Huaneng Taipingyi Hydropower Co Ltd filed Critical Huaneng Clean Energy Research Institute
Priority to CN202110984145.XA priority Critical patent/CN113735600B/en
Publication of CN113735600A publication Critical patent/CN113735600A/en
Priority to PCT/CN2022/077523 priority patent/WO2023024462A1/en
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Publication of CN113735600B publication Critical patent/CN113735600B/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating 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
    • C04B41/5007Coating 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
    • C04B41/501Coating 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/02Hydrogen or oxygen
    • C25B1/04Hydrogen or oxygen by electrolysis of water
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen 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 wafer, wherein the ceramic wafer is internally provided with pores, and the porosity of the ceramic wafer is more than or equal to 30%; and step 3: soaking the ceramic plate in molten salt so that the molten salt is filled in the pores of the ceramic plate; and 4, step 4: and (5) drying. The ceramic sheet prepared by the preparation method of the ceramic sheet provided by the application 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, and the ceramic plate is clamped between the first flange and the second flange and used as a sealing gasket.

Description

Preparation method of ceramic chip and sealing assembly
Technical Field
The application relates to the technical field of sealing, in particular to a preparation method of a ceramic chip and a sealing assembly with the ceramic chip.
Background
The polymer sealing gasket generally adopted by 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 electrolyzed water, so that the polymer sealing gasket can only be applied to normal-temperature water electrolysis equipment, and has certain limitation in the application of high-temperature water electrolysis equipment.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
To this end, an embodiment of the present invention provides a method for manufacturing a ceramic sheet, and the ceramic sheet manufactured according to the method has high-temperature sealing performance.
The embodiment of the invention also provides a sealing assembly 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 for more than 20 hours at the temperature of 20-70 ℃ to evaporate the solvent, cooling the model to room temperature, and forming the slurry into a ceramic wafer, wherein pores are formed in the ceramic wafer, the porosity of the ceramic wafer is more than or equal to 30%, and the pore diameter of the pores is 0.1-1 micron;
and step 3: obtaining molten salt, and soaking the ceramic plate prepared in the step 2 in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic plate for more than 10 hours;
and 4, step 4: and taking out the ceramic wafer, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic wafer into salt particles.
According to the preparation method of the ceramic chip provided by the embodiment of the invention, salt particles are filled in pores of the ceramic chip, the salt particles have a melting temperature, and when the use temperature of the ceramic chip is higher than the melting temperature of the salt particles, the salt particles can be melted to form molten salt. Under the capillary effect, the molten salt remains filled in the pores, forming a wet seal. Therefore, the ceramic sheet prepared by the preparation method of the ceramic sheet 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 sheet cannot be changed at high temperature due to the inherent high-temperature resistance of the ceramic sheet.
In some embodiments, step 2 further comprises: and carrying out hot pressing on the formed ceramic wafer.
In some embodiments, the molten salt comprises 60% to 70% by mole lithium carbonate and 30% to 40% by mole potassium carbonate.
In some embodiments, the additive comprises a binder, a dispersant, a plasticizer, the binder being polyvinyl alcohol, the dispersant being lactic acid, and the plasticizer being a mixture of glycerol, glyceryl triacetate, and ethylene glycol.
In some embodiments, the weight fraction of the frit is 20.0 parts to 40.0 parts, and the weight fraction of the solvent is 1.0 to 5.0 times the weight fraction of the frit.
In some embodiments, the molten salt has a melting temperature of 180 ℃ to 920 ℃.
According to another aspect of the present invention, there is provided a sealing assembly, including a ceramic sheet, the ceramic sheet being prepared according to the method for preparing a ceramic sheet according to any one of the above embodiments; the ceramic chip clamp is arranged between the first flange and the second flange, and the gas through hole, the first opening and the second opening oppositely form a communicated channel in a first direction.
In some embodiments, the sealing assembly further comprises a solid-liquid sealing medium, an annular first sealing chamber is defined between the ceramic plate and the first flange, an annular second sealing chamber is defined between the ceramic plate and the second flange, the first sealing chamber and the second sealing chamber both surround the channel, and the solid-liquid sealing medium is filled in the first sealing chamber and the second sealing chamber.
In some embodiments, a portion of the solid-liquid sealing medium in a liquid state can enter and fill a gap between the first flange and the ceramic sheet and a gap between the second flange and the ceramic sheet.
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 diagram of a ceramic sheet according to an embodiment of the present application.
Fig. 3 is a schematic structural diagram of a first flange according to an embodiment of the present application.
Reference numerals:
the mounting structure comprises a mounting screw rod 1, a screw cap 2, a first flange 3, a ceramic sheet 4, a first sealing chamber 5, a second mounting hole 6, a gas through hole 7, a first opening 8, a second opening 9, a second flange 10, a second sealing chamber 11, a first connecting pipe 12, a second connecting pipe 13, an annular groove 14 and a 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 with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
The application discloses a preparation method of a ceramic chip, which comprises the following steps:
step 1: obtaining a slurry, wherein the slurry is a mixture containing a solvent, a 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 for more than 20 hours at the temperature of 20-70 ℃ to evaporate the solvent, cooling the model to room temperature, and forming the slurry into a ceramic wafer, wherein pores are formed in the ceramic wafer, the porosity of the ceramic wafer is more than or equal to 30%, and the pore diameter of the pores is 0.1-1 micron;
and step 3: obtaining molten salt, and soaking the ceramic plate prepared in the step 2 in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic plate for more than 10 hours;
and 4, step 4: and taking out the ceramic wafer, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic wafer into salt particles.
Optionally, the powder lot in step 1 comprises one or more of lithium aluminum oxide powder, magnesium oxide powder, lithium cobaltate powder, lithium manganate powder, and aluminum oxide powder. And 3, obtaining the molten salt from the melted salt mixture, soaking the ceramic plate with the pores in the liquid molten salt, and gradually introducing the molten salt into the pores of the ceramic plate and filling the molten salt in the pores of the ceramic plate according to a capillary effect. After cooling and drying in the step 4, the liquid molten salt in the pores of the ceramic wafer is solidified into solid, namely salt particles.
In some embodiments, the method for preparing the ceramic sheet further comprises a hot pressing step, i.e., step 3: the step 2 further comprises: and carrying out hot pressing on the formed ceramic wafer.
According to the preparation method of the ceramic chip provided by the embodiment of the invention, salt particles are filled in pores of the ceramic chip, the salt particles have a melting temperature, and when the use temperature of the ceramic chip is higher than the melting temperature of the salt particles, the salt particles can be melted to form molten salt. Under the capillary effect, the molten salt remains filled in the pores, forming a wet seal. Therefore, the ceramic sheet prepared by the preparation method of the ceramic sheet 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 sheet cannot be changed at high temperature due to the inherent high-temperature resistance of the ceramic sheet.
Alternatively, the salt particles have a melting temperature of 180 ℃ to 920 ℃. That is, when the temperature of the working condition of the ceramic sheet exceeds the melting temperature of the salt particles, the salt particles can be melted into molten salt, and the molten salt is filled in the pores of the ceramic sheet to form wet sealing. It should be noted that the melting temperature of the salt particles is related to the composition of the salt particles, and those skilled in the art can select the salt particles with an appropriate melting temperature as the filling material of the ceramic sheet according to the use condition of the ceramic sheet when selecting the salt particles.
Optionally, the molten salt comprises 60-70% by mole lithium carbonate and 30-40% by mole 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 of the powder. 7.0 to 12.0 portions of adhesive, 1.5 to 3.0 portions of dispersant and 4.0 to 8.0 portions of plasticizer.
Specific examples of the method for producing the ceramic sheet of the present invention are provided below.
The first embodiment is as follows:
step 1: preparing materials, wherein the powder material is lithium aluminum oxide powder, wherein 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 dispersant is lactic acid; the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol, wherein the ratio of glycerol: glyceryl triacetate: the ratio of ethylene glycol is 1:1: 1; the solvent is water;
the weight fraction of the powder is 20.0 parts; 7.0 parts of binder; the weight fraction of the dispersant is 1.5 parts; the weight fraction of the plasticizer is 4.0 parts; the weight fraction of the solvent is 1.0 time 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, placing the model in an environment with the temperature of 20-70 ℃ for drying for more than 20 hours to evaporate the solvent, and after cooling to the room temperature, forming the slurry into a ceramic wafer with the porosity of 34.65%;
and step 3: obtaining molten salt, wherein the molten salt comprises 60% of lithium carbonate and 40% of potassium carbonate in mol content; the adhesive is polyvinyl alcohol, and the ceramic plate prepared in the step 2 is soaked in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic plate for more than 10 hours;
and 4, step 4: and taking out the ceramic wafer, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic wafer into salt particles.
Example two:
step 1: preparing materials, wherein the powder material is lithium aluminum oxide powder, wherein 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 dispersant is lactic acid; the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol, wherein the ratio of glycerol: glyceryl triacetate: the ratio of 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; the weight fraction of the dispersant is 3.0 parts; 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, placing the model in an environment with the temperature of 20-70 ℃ for drying for more than 20 hours to evaporate the solvent, and after cooling to room temperature, forming the slurry into a ceramic wafer with the porosity of 56.89%;
and step 3: obtaining molten salt, wherein the molten salt comprises 70% of lithium carbonate and 30% of potassium carbonate in mol content; the adhesive is polyvinyl alcohol, and the ceramic plate prepared in the step 2 is soaked in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic plate for more than 10 hours;
and 4, step 4: and taking out the ceramic wafer, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic wafer into salt particles.
Example three:
step 1: preparing materials, wherein the powder material is lithium aluminum oxide powder, wherein 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 dispersant is lactic acid; the plasticizer is a mixture of glycerol, glyceryl triacetate and ethylene glycol, wherein the ratio of glycerol: glyceryl triacetate: the ratio of 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, placing the model in an environment with the temperature of 20-70 ℃ for drying for more than 20 hours to evaporate the solvent, and after cooling to the room temperature, forming the slurry into a ceramic wafer with the porosity of 49.76%;
and step 3: obtaining molten salt, wherein the molten salt comprises 65% of lithium carbonate and 35% of potassium carbonate in molar content; the adhesive is polyvinyl alcohol, and the ceramic plate prepared in the step 2 is soaked in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic plate for more than 10 hours;
and 4, step 4: and taking out the ceramic wafer, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic wafer 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 produced by the method for producing a ceramic sheet according to any one of the above embodiments. The ceramic plate 4 is sandwiched between the first flange 3 and the second flange 10.
The ceramic plate 4 is provided with a gas through hole 7, the first flange 3 and the second flange 10 are provided with a first opening hole 8 and a second opening hole 9, and the gas through hole 7 and the first opening hole 8 and the second opening hole 9 form a communicated channel in the first direction. The channel is used for the passage of a sealing medium (gas).
When the sealing assembly provided by the embodiment of the invention is applied to a high-temperature working condition, the phase change of the salt particles in the pores is converted from a solid state to a 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 plays a role in preventing the gas in the channel from leaking through the pores. Therefore, the sealing assembly 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 reduced to be lower than the melting temperature, the molten salt filled in the pores of the ceramic sheet 4 is converted into solid salt particles, is filled in the pores of the ceramic sheet 4 as filler, and is melted into liquid molten salt again in the next high-temperature application, so that wet sealing is realized.
In some embodiments, the seal assembly further comprises a solid-liquid sealing medium, the solid-liquid sealing 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. An annular first sealed chamber 5 is defined between the first flange 3 and the ceramic plate 4, and an annular second sealed chamber 11 is defined between the second flange 10 and the ceramic plate 4. The first 5 and second 11 sealed chambers are both arranged around the passage.
In some embodiments, the solid-liquid sealing medium is filled in the first sealed chamber 5 and the second sealed chamber 11 and can perform a phase change reaction in the first sealed chamber 5 and the second sealed chamber 11 to convert from a solid state to a liquid state. As an example, below the phase transition temperature, a solid-liquid sealing medium in solid form is contained in the first and second sealing chambers 5, 11 when the sealing assembly is assembled. The assembled sealing assembly is applied to a high-temperature working condition, and along with the gradual rise of the working condition temperature of the sealing assembly, solid-liquid sealing media in the first sealing cavity 5 and the second sealing cavity 11 undergo phase change and are changed from a solid state to a liquid state.
The liquid solid-liquid sealing medium in the first and second seal chambers 5, 11 forms a wet seal in the seal chambers, preventing gas in the channels from leaking through the assembly gap. In this way, the liquid molten salt in the pores of the ceramic plate 4 and the liquid solid-liquid sealing medium 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 particularly 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 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 a capillary effect.
It should be noted that 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. Optionally, 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 sheet 4 and the gap between the second flange 10 and the ceramic sheet 4 can further prevent gas from leaking through the assembly gap.
As the working time is prolonged, the solid-liquid sealing medium in a partially liquid state still remains in the first sealing chamber 5 and the second sealing chamber 11, so that a wet sealing line in the first sealing chamber 5 and the second sealing chamber 11 can be ensured. Therefore, sufficient solid-liquid sealing medium should be contained in the first and second seal chambers 5 and 11 when the seal assembly is assembled.
Therefore, the liquid solid-liquid sealing medium retained 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 plate 4 and the gap between the second flange 10 and the ceramic plate 4, and the liquid molten salt in the pores of the ceramic plate 4 form a multiple sealing line, and the sealing performance of the sealing assembly is further improved.
In some embodiments, the solid-liquid sealing medium is a salt mixture that melts to form a molten salt, the molten salt being a melt formed after the salt melts, the molten salt being in a liquid mode.
Alternatively, the salt mixture comprises at least two salt species, each having a eutectic point, i.e., having the same (or relatively similar) phase transition temperature.
Optionally, the salt mixture in this embodiment is 60 to 70 mole% lithium carbonate and 30 to 40 mole% potassium carbonate.
Optionally, the phase transition temperature of the solid-liquid sealing medium is 180 ℃ to 920 ℃.
Fig. 1 is a cross-sectional view of the 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 respectively disposed on both sides of the ceramic sheet 4.
Fig. 2 is a schematic structural diagram of a ceramic plate according to an embodiment of the present application, and fig. 3 is a schematic structural diagram of a first flange according to an embodiment of the present application. As shown in fig. 1 and 2, the ceramic plate 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, and the axes of the gas through hole 7, the first opening 8 and the second opening 9 are coincident, 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 passage of a sealing medium (gas).
In the embodiment, an annular first sealed chamber 5 is formed between the ceramic plate 4 and the first flange 3, an annular second sealed chamber 11 is formed between the ceramic plate 4 and the second flange 10, and the first sealed chamber 5 and the second sealed chamber 11 are respectively arranged around the channel. That is, a first sealed chamber 5 and a second sealed chamber 11 are formed between both sides of the ceramic sheet 4 and the first flange 3 and the second flange 10, respectively.
In the present embodiment, as shown in fig. 1, the side of the first flange 3 close to the ceramic plate 4 is provided with an annular groove 14 surrounding the channel, and a first sealed chamber 5 is defined between the annular groove 14 and the side of the ceramic plate 4 close to the first flange 3. That is, an annular groove 14 centered on the channel is formed on the first flange 3 and on a side close to the ceramic plate 4, and an annular first sealed chamber 5 is formed between the annular groove 14 and the ceramic plate 4.
Similarly to the first flange 3, the second flange 10 is provided with an annular groove surrounding the channel on the side close to the ceramic plate 4, and the second sealed chamber 11 is defined between the annular groove and the side of the ceramic plate 4 close to the second flange 10. That is, an annular groove centered on the channel is formed on the second flange 10 and on the other side close to the ceramic plate 4, and an annular second sealed chamber 11 is formed between the annular groove and the ceramic plate 4.
In other embodiments, the side of the ceramic plate 4 close 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 close to the ceramic plate 4. The side of the ceramic plate 4 close to the second flange 10 may be provided with an annular groove surrounding the channel, defining a second sealed chamber 11 between the annular groove and the side of the second flange close to the ceramic plate 4.
Still alternatively, in other embodiments, the side of the first flange 3 close to the ceramic plate 4 is provided with a first annular groove surrounding the channel, and the side of the ceramic plate 4 close to the first flange 3 is provided with a second annular groove surrounding the channel, the first annular groove and the second annular groove being opposite and defining the first sealed chamber 5. That is to say, a first annular groove is formed in one side of the first flange 3, a second annular groove is formed in one side of the ceramic plate 4 corresponding to the first flange 3, the first annular groove and the second annular groove are both arranged with the channel as the center, and an annular first sealing chamber 5 is formed between the first annular groove and the second annular groove.
Similarly to the first flange 3, the second flange 10 is provided with a third annular groove surrounding the channel on the side close to the ceramic plate 4, and the ceramic plate 4 is provided with a fourth annular groove surrounding the channel on the side close to the second flange 10, the third annular groove being opposite to the fourth annular groove and defining a second sealed chamber 11. That is to say, a third annular groove is formed in one side of the second flange 10, a fourth annular groove is formed in one side of the ceramic plate 4 corresponding to the second flange 10, the third annular groove and the fourth annular groove are both arranged with the channel as the center, and an annular second sealing chamber 11 is formed between the third annular groove and the fourth annular groove.
In some embodiments, the first sealed chamber 5 may include a plurality of first sealed chambers 5, and a plurality of first sealed chambers 5 are sequentially sleeved. That is, a plurality of concentric annular first sealed chambers 5 may be disposed between the first flange 3 and the ceramic plate 4 with the channel as the center, that is, the plurality of first sealed chambers 5 are disposed along the radial direction of the ceramic plate 4 with different radii. It should be noted that a plurality of second sealed chambers 11 may also be arranged, the plurality of second sealed chambers 11 are arranged along the radial direction of the ceramic plate according to different radii, and the plurality of second sealed chambers 11 may be arranged sequentially according to a certain interval, or may be arranged according to different intervals.
The arrangement of the first sealing chambers 5 and the 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 is communicated with the first opening 8, the second flange 10 is connected to the second connection pipe 13, and the second connection pipe 13 is communicated with the second opening 9. The first connection pipe 12 is communicated with the second connection pipe 13 through the first opening 8, the gas passing hole 7 and the second opening 9, and integrally forms a passage extending in the first direction. It should be noted that the first connection pipe 12 and the second connection pipe 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, with an end of the first connecting pipe 12 communicating with an end of the first opening 8 and an end of the second connecting pipe 13 communicating with an 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 mounting hole 15, the second mounting hole 6 and the third mounting hole to connect the ceramic plate 4, the first flange 3 and the second flange 10. That is to say, the first flange 3, the second flange 10 and the ceramic plate 4 are respectively provided with a second mounting hole 6, a third mounting hole and a first mounting hole 15, the centers of the first mounting hole 15, the second mounting hole 6 and the third mounting hole are positioned on the same straight line, the mounting screw 1 penetrates through the second mounting hole 6, the first mounting hole 15 and the third mounting hole, and the nut 2 is screwed down, 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 is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer 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, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (10)

1. The preparation method of the ceramic chip is characterized by comprising 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 for more than 20 hours at the temperature of 20-70 ℃ to evaporate the solvent, cooling the model to room temperature, and forming the slurry into a ceramic wafer, wherein pores are formed in the ceramic wafer, the porosity of the ceramic wafer is more than or equal to 30%, and the pore diameter of the pores is 0.1-1 micron;
and step 3: obtaining molten salt, and soaking the ceramic plate prepared in the step 2 in the molten salt so that the molten salt is soaked and filled in the pores of the ceramic plate for more than 10 hours;
and 4, step 4: and taking out the ceramic wafer, drying at room temperature for more than 20 hours, and solidifying the molten salt in the pores of the ceramic wafer into salt particles.
2. The method for preparing ceramic sheets according to claim 1, wherein step 2 further comprises: and carrying out hot pressing on the formed ceramic wafer.
3. The ceramic sheet preparation method according to claim 1, wherein the molten salt comprises 60-70% by mole of lithium carbonate and 30-40% by mole of potassium carbonate.
4. The method for manufacturing the ceramic sheet according to claim 1, wherein the additives comprise 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, triacetin and ethylene glycol.
5. The method for preparing ceramic sheet according to claim 4 wherein the powder is 20.0-40.0 parts by weight and the solvent is 1.0-5.0 times the powder.
6. Method for manufacturing a ceramic sheet according to any of claims 1-5, wherein the temperature of the molten salt is 180-920 ℃.
7. A seal assembly, comprising:
a ceramic sheet prepared by the method according to any one of claims 1 to 6;
the ceramic chip clamp is arranged between the first flange and the second flange, and the gas through hole, the first opening and the second opening oppositely form a communicated channel in a first direction.
8. The seal assembly of claim 7, further comprising a solid-liquid sealing medium, wherein an annular first seal chamber is defined between the ceramic plate and the first flange, an annular second seal chamber is defined between the ceramic plate and the second flange, the first seal chamber and the second seal chamber both surround the channel, and the solid-liquid sealing medium is filled in the first seal chamber and the second seal chamber.
9. The seal assembly according to claim 8, wherein a portion of the solid-liquid sealing medium in a liquid state can enter and fill in a gap between the first flange and the ceramic sheet and a gap between the second flange and the ceramic sheet.
10. The seal assembly of claim 8 or 9, wherein the solid-liquid sealing medium is a salt mixture.
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