CN115368779A - Coating slurry, coating preparation method and application thereof - Google Patents

Coating slurry, coating preparation method and application thereof Download PDF

Info

Publication number
CN115368779A
CN115368779A CN202211014567.5A CN202211014567A CN115368779A CN 115368779 A CN115368779 A CN 115368779A CN 202211014567 A CN202211014567 A CN 202211014567A CN 115368779 A CN115368779 A CN 115368779A
Authority
CN
China
Prior art keywords
coating
aqueous solution
aqueous
crucible
coating slurry
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202211014567.5A
Other languages
Chinese (zh)
Inventor
杨晓光
赖毅梅
关豪元
蓝威杰
杨立鹏
孙逢春
王文伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Automotive Research Institute of Beijing University of Technology
Original Assignee
Shenzhen Automotive Research Institute of Beijing University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen Automotive Research Institute of Beijing University of Technology filed Critical Shenzhen Automotive Research Institute of Beijing University of Technology
Priority to CN202211014567.5A priority Critical patent/CN115368779A/en
Publication of CN115368779A publication Critical patent/CN115368779A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
    • C09D101/08—Cellulose derivatives
    • C09D101/26—Cellulose ethers
    • C09D101/28—Alkyl ethers
    • C09D101/286—Alkyl ethers substituted with acid radicals
    • 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
    • C04B41/5001—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 carbon or carbonisable materials
    • 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
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C09D129/02—Homopolymers or copolymers of unsaturated alcohols
    • C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D139/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Coating compositions based on derivatives of such polymers
    • C09D139/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
    • C09D139/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D171/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crucibles And Fluidized-Bed Furnaces (AREA)

Abstract

The application discloses coating slurry, a coating preparation method and application thereof. The coating slurry comprises 80-90 parts by mass of aqueous solution of an aqueous polymer binder and 10-20 parts by mass of graphite powder. In the application, the coating slurry mainly comprises a water-based polymer, water and graphite powder, does not contain metal ions, and can be directly coated on the inner wall of the crucible. After the coating is formed by utilizing the coating slurry, the crucible inner wall can be isolated from the electrolyte material by utilizing the occupying effect of the coating, the electrolyte material is prevented from reacting with the crucible inner wall, and then the adhesion of phosphate solid electrolyte and the crucible inner wall is avoided, and the subsequent demoulding is convenient.

Description

Coating slurry, coating preparation method and application thereof
Technical Field
The invention relates to the field of coatings, in particular to coating slurry, a coating preparation method and application thereof.
Background
The all solid-state lithium battery is a focus of the next generation battery because of its high energy density and safety performance. As a core of the solid-state lithium battery technology, the solid-state electrolyte material determines the preparation cost and various performance parameters of the battery to a great extent. Phosphate-based lithium ion conductor of NASICON structure (e.g. Li) 1+x Al x Ti 2-x (PO 4 ) 3 、Li 1-x Al x Ge 2-x (PO 4 ) 3 ) The electrolyte is one of the most promising solid electrolyte materials due to its good comprehensive performance and wide raw material sources.
Currently, phosphate solid electrolytes are mainly prepared in the industry by a solid phase sintering process, and an alumina or mullite crucible is usually adopted, which generates H in the sintering process 3 PO 4 Liquid intermediate phase, liquid phase at high temperature and crucible (Al) 2 O 3 、SiO 2 Etc.) may react over time, causing crucible elements (Al, si, etc.) to enter the solid electrolyte. On the upper partThe problems are technical problems to be solved by the invention.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides: a coating slurry, a coating preparation method and application thereof.
According to a first aspect, there is provided in one embodiment a coating slurry comprising, in parts by mass:
80-90 parts of aqueous solution of aqueous polymer binder and 10-20 parts of graphite powder.
According to a second aspect, there is provided in an embodiment a method of preparing a coating layer using the above coating slurry, comprising the steps of:
preparing an aqueous solution of an aqueous polymer binder;
uniformly mixing the aqueous solution of the aqueous polymer binder with graphite powder to obtain the coating slurry;
and coating the coating slurry on a target surface and drying to obtain a coating.
According to a third aspect, an embodiment provides a crucible having an inner wall surface coated with a coating layer, the coating layer being obtained by coating the above coating slurry.
According to a fourth aspect, an embodiment provides the use of the above coating paste in a sintering process of a phosphate-based solid-state electrolyte.
In the application, the coating slurry mainly comprises a water-based polymer, water and graphite powder, does not contain metal ions, can be directly coated on the inner wall of a crucible, and does not cause element pollution to electrolyte materials.
After the coating is formed by utilizing the coating slurry, the crucible inner wall can be isolated from the electrolyte material by utilizing the occupying effect of the coating, the electrolyte material is prevented from reacting with the crucible inner wall, and then the adhesion of phosphate solid electrolyte and the crucible inner wall is avoided, and the subsequent demoulding is convenient.
Drawings
FIG. 1 is a schematic view of a crucible provided with a coating in an embodiment of the present application;
FIG. 2 is an XDR chart of samples 1 to 6 in example six of the present application;
the reference numbers indicate: crucible 1, coating 2.
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings. In the following description, numerous details are set forth in order to provide a better understanding of the present application. However, those skilled in the art will readily recognize that some of the features may be omitted in different instances or may be replaced by other materials, methods. In some instances, certain operations related to the present application have not been shown or described in detail in order to avoid obscuring the core of the present application from excessive description, and it is not necessary for those skilled in the art to describe these operations in detail, so that they may be fully understood from the description in the specification and the general knowledge in the art.
Furthermore, the features, operations, or characteristics described in the specification may be combined in any suitable manner to form various embodiments. Also, the various steps or actions in the method descriptions may be transposed or transposed in order, as will be apparent to one of ordinary skill in the art. Thus, the various sequences in the specification and drawings are for the purpose of describing certain embodiments only and are not intended to imply a required sequence unless otherwise indicated where such sequence must be followed.
When the crucible is used as a container for sintering the phosphate electrolyte, the phosphate electrolyte generally reacts with the inner wall of the crucible 1 at about 250-400 ℃, and the pollution to the electrolyte is caused. However, when the temperature is higher than 400 ℃, the electrolyte does not react with the inner wall of the crucible 1.
Therefore, the application provides a coating of a crucible for sintering phosphate solid electrolyte and a preparation method thereof, the raw material of the coating 2 is coating slurry, and the application is explained below.
The aqueous polymer binder presented in this application, i.e. the aqueous polymer used as binder.
In the examples of the present application, the coating slurry comprises, in parts by mass: 80-90 parts of aqueous solution of aqueous polymer binder and 10-20 parts of graphite powder.
Wherein, the aqueous solution of the aqueous polymer binder is used as the main body of the coating slurry, so as to form the coating slurry with a certain viscosity, so as to provide a certain adhesive force and adhesion force to the prepared coating slurry, and ensure that the coating 2 can be adhered to the target surface (for example, in the embodiment of the application, the target surface is the inner surface of the crucible 1), and specifically, the aqueous polymer binder can be selected from one or more of polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide, carboxymethyl cellulose and starch.
Wherein, the addition of graphite powder then can be favorable to increasing 2 thicknesses of coating, and simultaneously, the graphite powder is black component, adds in the coating thick liquids for the coating has darker colour, can conveniently observe the coating degree of coating, also conveniently observes the condition of electrolyte sintering simultaneously.
In an embodiment of the present application, in the aqueous solution of the aqueous polymer binder, the mass ratio of the aqueous polymer binder to water is 1.
In an embodiment of the present application, the mass ratio of the aqueous solution of the aqueous polymer binder to the graphite powder is 8:2 to 9:1.
Further, the application also provides a method for manufacturing a coating 2 by using the coating slurry, which specifically comprises the following steps:
step S1: preparing an aqueous solution of the aqueous polymer binder.
Specifically, in the step, 1 part by mass of the aqueous polymer binder is mixed with 11 to 80 parts by mass of deionized water until the aqueous polymer binder is completely dissolved in water to obtain an aqueous solution of the aqueous polymer.
Step S2: and uniformly mixing the aqueous solution of the aqueous polymer binder with graphite powder.
Specifically, in the step, the aqueous solution of the aqueous polymer binder and the graphite powder are mixed according to a mass ratio of 1.
And step S3: and coating the coating 2 on a target surface and drying to obtain the coating 2.
In this step, the coating method may be a spray coating method or a brush coating method, and the present application is not particularly limited as long as the method of uniformly coating the slurry on the target surface is applicable.
After coating is finished, transferring the target surface to an oven for baking until the coating slurry is dried and cured to obtain a coating 2, wherein the thickness of the dried coating 2 can be controlled to be 30-120 mu m, and in the more specific operation steps, the specific drying conditions are as follows: drying for 1-2 h at 60-120 ℃.
In the embodiment of the present application, the target surface is an inner wall of a container for sintering phosphate solid electrolyte, and in a common embodiment, the container may be an alumina crucible or a mullite crucible, but it should be understood that the target surface is not limited thereto, and the coating 2 may be prepared by the method of the present application in other containers for sintering phosphate solid electrolyte.
The crucible 1 finally prepared by the above method is structured as shown in fig. 1, and comprises a crucible 1, and a coating layer 2 is attached to the inner wall of the crucible 1.
In this application, the coating slurry mainly comprises water-based polymer, water and graphite powder, does not contain metal ions, can directly coat on the inner wall of the crucible 1, after the coating 2 is formed, in the high-temperature sintering process of phosphate solid electrolyte, the metal element permeation phenomenon can not occur, and even if the coating 2 falls off, the solid electrolyte material can not be polluted.
The research of the application finds that the raw material for synthesizing the phosphate electrolyte has a strong endothermic peak at 198 ℃, and is the first-stage decomposition of the raw material. In this process, intermediate products are formed: h in the liquid phase 3 PO 4 H in the liquid phase 3 PO 4 Will react with crucible components (Al) during sintering 2 O 3 Etc.) the following reactions occur:
Al 2 O 3 +6H 3 PO 4 ＝2Al(H 2 PO 4 ) 3 +6H 2 O；
Al 2 O 3 +3H 3 PO 4 ＝Al 2 (HPO 4 ) 3 +3H 2 O；
Al 2 O 3 +2H 3 PO 4 ＝2AlPO 4 +3H 2 O。
the temperature condition of the reaction is 280-320 ℃, wherein the generated 2Al (H) is 2 PO 4 ) 3 、Al 2 (HPO 4 ) 3 、2AlPO 4 The aluminum phosphate adhesives can be used for bonding metal and ceramic, so that the phosphate electrolyte is adhered to the crucible.
And utilize the disclosed coating thick liquids of this application, after container (for example crucible) inner wall is forming coating 2, utilize the occupy-place effect of coating 2, can keep apart 1 inner wall of crucible and electrolyte material, prevent that electrolyte material and 1 inner wall of crucible from taking place the reaction, can not produce aluminium phosphate system gluing agent, avoid the adhesion of phosphate solid electrolyte and 1 inner wall of crucible then, make things convenient for follow-up drawing of patterns.
Meanwhile, the sintering temperature of the electrolyte is usually about 700-800 ℃ as the final sintering temperature of the electrolyte, and the components of the coating slurry prepared by the method are all carbon-containing substances and can be completely sintered at 500-600 ℃, and the temperature exceeds Al 2 O 3 And H 3 PO 4 The temperature at which the reaction can take place, at which the coating can be converted into carbon dioxide, water and steam to volatilize away, so that after sintering, the coating can be completely decomposed without causing pollution to the electrolyte material, and the crucible can also be recycled.
To further illustrate the present application, the following more specific examples are provided to facilitate an understanding thereof.
The first embodiment is as follows:
in this example the aqueous polymer binder was carboxymethyl cellulose, available from alatin, graphite powder available from korea, and crucible 1 was an alumina crucible available from guangdong mountain mo new refractory limited.
The preparation method of the coating 2 comprises the following steps:
s1: preparing a carboxymethyl cellulose aqueous solution: at the temperature of 60 ℃, 1g of carboxymethyl cellulose is dissolved in 80g of deionized water, stirred for 240min and uniformly mixed to obtain carboxymethyl cellulose solution.
S2: and (2) taking 8g of the carboxymethyl cellulose aqueous solution prepared in the step (S1), adding 2g of graphite powder, and uniformly mixing by a homogenizer, wherein the mixing speed is 1600r/min, and the mixing time is 6min to obtain coating slurry.
S3, brushing the coating slurry on the inner wall of the crucible 1, and then placing the crucible 1 in an oven at 80 ℃ for drying for 1h to obtain a coating 2, wherein the thickness of the coating 2 is 52 microns.
Example two:
in this example, the aqueous polymeric binder was polyvinylpyrrolidone, which was obtained from Mecanne, graphite powder from Korea, and crucible 1 was an alumina crucible, which was obtained from Guangdong mountain Moore New refractory Co.
The preparation method of the coating 2 comprises the following steps:
s1: preparing a polyvinylpyrrolidone aqueous solution: at 60 ℃, 1g of polyvinylpyrrolidone is dissolved in 11g of deionized water, and the mixture is stirred for 360min and uniformly mixed to obtain the polyvinylpyrrolidone aqueous solution.
S2: and (2) taking 8.3g of the carboxymethyl cellulose aqueous solution prepared in the step (S1), adding 1.7g of graphite powder into the carboxymethyl cellulose aqueous solution, and uniformly mixing the mixture by a homogenizer at a mixing speed of 2000r/min for 8min to obtain coating slurry.
S3: brushing the coating slurry on the inner wall of the crucible 1, and then placing the crucible 1 in an oven at 80 ℃ for drying for 1h to obtain the coating 2, wherein the thickness of the coating 2 is 78 micrometers.
EXAMPLE III
In this example, the aqueous polymeric binder was polyethylene oxide, which was obtained from mclin, graphite powder from korea, and crucible 1 was a mullite crucible, which was obtained from guangdong mountain mo new refractory, inc.
S1: preparing a polyoxyethylene aqueous solution: 1g of polyethylene oxide was dissolved in 24g of deionized water at 25 ℃ and uniformly mixed with stirring for 180min to obtain an aqueous polyethylene oxide solution.
S2: and (3) taking 8g of the polyoxyethylene aqueous solution prepared in the step S1, adding 2g of graphite powder into the polyoxyethylene aqueous solution, and uniformly mixing the mixture by a homogenizer at a mixing speed of 2000r/min for 12min to obtain coating slurry.
S3: brushing the coating slurry on the inner wall of the crucible 1, and then placing the crucible 1 in an oven at 60 ℃ for drying for 1.5h to obtain the coating 2, wherein the thickness of the coating 2 is 72 mu m.
Example four:
in this example, the aqueous polymeric binder was polyvinyl alcohol, which was obtained from alatin, graphite powder from korea, and crucible 1 was a mullite crucible, which was obtained from new refractory, inc.
S1: preparing a polyvinyl alcohol aqueous solution: at 60 ℃, 1g of polyvinyl alcohol is dissolved in 12g of deionized water, stirred for 480min and uniformly mixed to obtain a polyvinyl alcohol aqueous solution.
S2: 9g of the aqueous polyvinyl alcohol solution obtained in step S1 were taken. Adding 1g of graphite powder into the mixture, and uniformly mixing the mixture by a homogenizer, wherein the mixing speed is 1800r/min, and the mixing time is 8min to obtain coating slurry;
s4: brushing the coating slurry on the inner wall of the crucible 1, and drying in an oven at 100 ℃ for 1h to obtain a coating 2, wherein the thickness of the coating 2 is 87 micrometers.
Example five:
in this example, the aqueous polymer binder was polyvinyl alcohol, which was obtained from alatin, graphite powder was obtained from korea, and crucible 1 was a mullite crucible, which was obtained from guangdong mountain mo new refractory, inc.
S1: preparing a polyvinyl alcohol aqueous solution: at 90 ℃, 0.8g of polyvinyl alcohol is dissolved in 9.2g of deionized water, stirred for 480min and uniformly mixed to obtain a polyvinyl alcohol aqueous solution.
S2: 9g of the aqueous polyvinyl alcohol solution prepared in step S1 were taken. Adding 1g of graphite powder into the mixture, and uniformly mixing the mixture by a homogenizer, wherein the mixing speed is 800r/min, and the mixing time is 15min to obtain coating slurry;
s4: brushing the coating slurry on the inner wall of the crucible 1, and placing the crucible in a drying oven at 120 ℃ for drying for 1h to obtain a coating 2, wherein the thickness of the coating 2 is 98 mu m.
Example six:
the crucible 1 prepared in the first to fifth embodiments of the invention is used for sintering phosphate solid electrolyte, and the specific sintering conditions are that the sintering temperature is 850-1000 ℃, and the heating rate is 2-10 ℃/min.
After completion of the sintering, the phosphate-based solid electrolytes obtained in the crucibles of examples one to five were respectively and correspondingly labeled as samples 1 to 5. In none of the samples 1 to 5 after sintering, the phenomenon of sticking to the crucible 1 was observed, and the samples 1 to 5 were easily released from the mold. The sintering of the phosphate-based solid electrolyte was carried out using an uncoated crucible (alumina crucible, available from new refractory, inc., san Moore, guangdong) and is labeled as sample 6. The sintered sample 6 was bonded to both the crucible wall and bottom.
Phase analysis was performed by XRD (X-ray diffraction) on each of the sintered samples 1 to 6, as shown in fig. 2, in which no significant impurity phase was found in any of the samples 1 to 5, and a significant impurity phase was present between 20 ° and 30 ° in the sample 6.
And respectively analyzing the content of the sintered solid electrolyte in the sintered samples 1 to 5 by adopting an ICP-MS (plasma Mass spectrometer), wherein no impurity element is found, and the content of the other elements accords with the molar ratio of the solid electrolyte material.
The present invention has been described in terms of specific examples, which are provided to aid understanding of the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.

Claims (10)

1. The coating slurry is characterized by comprising the following components in parts by mass:
80-90 parts of aqueous solution of aqueous polymer binder and 10-20 parts of graphite powder.
2. The coating slurry of claim 1 wherein the aqueous solution of the aqueous polymeric binder is one or more of polyvinyl alcohol, polyvinyl pyrrolidone, polyethylene oxide, carboxymethyl cellulose and starch.
3. The coating slurry according to claim 1, wherein the aqueous solution of the aqueous polymer binder has a mass ratio of aqueous polymer binder to water of 1.
4. The coating slip of claim 1, wherein the mass ratio of the aqueous solution of the aqueous polymeric binder to the graphite powder is 8:2 to 9:1.
5. A method for producing a coating using the coating slurry according to any one of claims 1 to 4, comprising the steps of:
preparing an aqueous solution of an aqueous polymer binder;
uniformly mixing the aqueous solution of the aqueous polymer binder with graphite powder to obtain the coating slurry;
and coating the coating slurry on a target surface and drying to obtain a coating.
6. The method of claim 5, wherein formulating the aqueous solution of the aqueous polymeric binder comprises:
mixing the aqueous polymer binder with water at the temperature of 0-100 ℃, and stirring for 180-480 min to obtain the aqueous solution of the aqueous polymer binder.
7. The method of claim 5, wherein uniformly mixing the aqueous solution of the aqueous polymeric binder with graphite powder comprises:
and mixing the aqueous solution of the aqueous polymer binder and graphite powder at a rotating speed of 800-2000 r/min for 5-15 min.
8. The method of claim 5, wherein applying the coating slurry to a target surface and drying to obtain a coating comprises:
and coating the coating slurry on the inner wall of a container for sintering phosphate solid electrolyte, and drying for 1-2 h at the temperature of 60-120 ℃ to obtain a coating with the thickness of 30-120 mu m.
9. A crucible comprising an inner wall, wherein the surface of the inner wall is coated with a coating layer, the coating layer being obtained by coating the coating slurry according to any one of claims 1 to 4.
10. Use of a coating slip as claimed in any one of claims 1 to 4 in a sintering process of phosphate-based solid-state electrolytes.
CN202211014567.5A 2022-08-23 2022-08-23 Coating slurry, coating preparation method and application thereof Pending CN115368779A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211014567.5A CN115368779A (en) 2022-08-23 2022-08-23 Coating slurry, coating preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211014567.5A CN115368779A (en) 2022-08-23 2022-08-23 Coating slurry, coating preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN115368779A true CN115368779A (en) 2022-11-22

Family

ID=84068353

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211014567.5A Pending CN115368779A (en) 2022-08-23 2022-08-23 Coating slurry, coating preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN115368779A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101498550A (en) * 2009-03-16 2009-08-05 北京航空航天大学 Crucible with Al2O3 anti-corrosion coating and method for producing Al2O3 anti-corrosion coating by slip-casting shaping process
CN101532776A (en) * 2009-03-16 2009-09-16 北京航空航天大学 Crucible with Y2O3 etching resistant coating and method for producing Y*O* etching resistant coating using slip casting moulding technique
CN102515847A (en) * 2011-11-25 2012-06-27 中原工学院 Method for preparing glass ceramics by graphite attached crucible
CN103183478A (en) * 2011-12-31 2013-07-03 浙江昱辉阳光能源有限公司 Silicon nitride crucible coating and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101498550A (en) * 2009-03-16 2009-08-05 北京航空航天大学 Crucible with Al2O3 anti-corrosion coating and method for producing Al2O3 anti-corrosion coating by slip-casting shaping process
CN101532776A (en) * 2009-03-16 2009-09-16 北京航空航天大学 Crucible with Y2O3 etching resistant coating and method for producing Y*O* etching resistant coating using slip casting moulding technique
CN102515847A (en) * 2011-11-25 2012-06-27 中原工学院 Method for preparing glass ceramics by graphite attached crucible
CN103183478A (en) * 2011-12-31 2013-07-03 浙江昱辉阳光能源有限公司 Silicon nitride crucible coating and preparation method thereof

Similar Documents

Publication Publication Date Title
Uhlenbruck et al. Cathode-electrolyte material interactions during manufacturing of inorganic solid-state lithium batteries
JP5854045B2 (en) All-solid-state lithium secondary battery and manufacturing method thereof
Zheng et al. Novel synthesis of LiVPO4F cathode material by chemical lithiation and postannealing
JP6189649B2 (en) Positive electrode active material powder and production method thereof
JP2017111954A (en) Metal oxide composition for film formation, positive electrode complex, method for manufacturing positive electrode complex, battery, and method for manufacturing battery
US20140008568A1 (en) Processes and compositions for multi-transition metal-containing cathode materials using molecular precursors
CN114605159A (en) Method and material for casting and sintering green garnet films
EP2717364A1 (en) Positive electrode active material particles, and positive electrode and all-solid-state battery using same
CN112243543A (en) Solid-state battery
JP2021509522A (en) LimMOxFy shell formation on cathode ceramic particles for Li-ion batteries via onium metal oxide fluoride precursor
JP6536141B2 (en) Method of manufacturing composite active material
CN102080197B (en) Method for coating surface of reinforcement in composite material
CN115368779A (en) Coating slurry, coating preparation method and application thereof
Shigeno et al. New lithium-conducting nitride glass Li3BN2
US9397359B2 (en) Method for preparing a material on a substrate by sol-gel means
Yamaguchi The development of low-temperature sintering techniques for functional ceramic devices using chemical reactions
WO2018088197A1 (en) All-solid-state battery and method for producing same
JP7050674B2 (en) Manufacturing method of ceramic cathode layer on current collector
CN116097469A (en) Positive electrode active material for lithium secondary battery, positive electrode for lithium secondary battery, and lithium secondary battery
JP2019507458A5 (en)
EP4246618A1 (en) Method for producing coated active material and method for producing electrode
US20070098905A1 (en) Method for preparing metal oxide layers
JP2019067572A (en) Manufacturing method of active material layer for all solid battery and manufacturing method of all solid battery
Shukla et al. Conformal coating of nanoscale features of microporous Anodisc™ membranes with zirconium and titanium oxides
EP4245726A1 (en) Method for producing coated active material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20221122

RJ01 Rejection of invention patent application after publication