CN114400106A - Insulating layer slurry preparation material, insulating layer preparation method and gas sensor - Google Patents
Insulating layer slurry preparation material, insulating layer preparation method and gas sensor Download PDFInfo
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- CN114400106A CN114400106A CN202111613174.1A CN202111613174A CN114400106A CN 114400106 A CN114400106 A CN 114400106A CN 202111613174 A CN202111613174 A CN 202111613174A CN 114400106 A CN114400106 A CN 114400106A
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- insulating layer
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- 239000002002 slurry Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 48
- 238000009835 boiling Methods 0.000 claims abstract description 42
- -1 magnesium aluminate Chemical class 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000654 additive Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000007639 printing Methods 0.000 claims abstract description 12
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 11
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 11
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011029 spinel Substances 0.000 claims abstract description 11
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 11
- 239000000454 talc Substances 0.000 claims abstract description 11
- 235000012222 talc Nutrition 0.000 claims abstract description 11
- 229910052623 talc Inorganic materials 0.000 claims abstract description 11
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 239000011777 magnesium Substances 0.000 claims abstract description 10
- 235000001055 magnesium Nutrition 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 6
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000012245 magnesium oxide Nutrition 0.000 claims abstract description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
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- 238000010438 heat treatment Methods 0.000 claims description 26
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- 238000000498 ball milling Methods 0.000 claims description 18
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 18
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- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 12
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 12
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- 229940116411 terpineol Drugs 0.000 claims description 12
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- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 9
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- 238000003756 stirring Methods 0.000 claims description 9
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- 238000007650 screen-printing Methods 0.000 claims description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
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- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 150000003672 ureas Chemical class 0.000 claims description 5
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- 239000003792 electrolyte Substances 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
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- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 claims description 3
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 claims description 3
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 claims description 3
- QYMFNZIUDRQRSA-UHFFFAOYSA-N dimethyl butanedioate;dimethyl hexanedioate;dimethyl pentanedioate Chemical compound COC(=O)CCC(=O)OC.COC(=O)CCCC(=O)OC.COC(=O)CCCCC(=O)OC QYMFNZIUDRQRSA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- QQVIHTHCMHWDBS-UHFFFAOYSA-L isophthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC(C([O-])=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-L 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000005245 sintering Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 description 17
- 229910052760 oxygen Inorganic materials 0.000 description 17
- 239000007789 gas Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 12
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000000306 component Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 8
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 7
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- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
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- 235000010755 mineral Nutrition 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/10—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances metallic oxides
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B19/00—Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
An insulating layer slurry preparation material comprises the following components in percentage by mass: 25 to 71 percent of alpha-alumina powder; 5 to 20 percent of inorganic additive; 20.5 to 40 percent of organic solvent; 2.5 to 10 percent of organic carrier; 1% -5% of organic auxiliary agent; wherein the inorganic additive comprises at least one of magnesium aluminate spinel, kaolin, talc, silicon dioxide, magnesium oxide and calcium carbonate; the organic solvent comprises at least one of a high boiling point solvent and a low boiling point solvent, wherein the boiling point of the high boiling point solvent is more than 150 ℃, and the boiling point of the low boiling point solvent is less than 110 ℃. The insulating layer slurry prepared from the insulating layer slurry has good sintering compactness; by utilizing the characteristic that the high-boiling point solvent is not easy to volatilize, the solid content of the insulating layer slurry can be kept stable in the processes of storage and printing, the fluidity of the insulating layer slurry is stable, and the printing stability of the insulating layer slurry is favorably improved; the addition of the low boiling point solvent can increase the solubility and uniformity of the components of the insulating layer slurry.
Description
Technical Field
The invention relates to an insulating layer slurry preparation material, an insulating layer preparation method and a gas sensor.
Background
Yttria-stabilized zirconia (YSZ) is a solid electrolyte with high oxygen ion conductivity at high temperature, and is widely applied to the fields of oxygen sensors, nitrogen oxygen sensors, SOFC and the like. The chip of the nitrogen-oxygen sensor is internally provided with a heating wire, self-heating is realized under the condition of external heating voltage, the chip is heated to the working temperature, a large number of oxygen ion vacancies exist in the YSZ at high temperature, and the YSZ has high-temperature conductivity at the moment. When the automobile exhaust (contains O)2、NOXEtc.) after entering the internal cavity, under the action of the metal electrode and the voltage applied at the two ends of the metal electrode, gas is detected at the three-phase interface to obtain electrons, and oxygen ions are decomposed, because a large number of oxygen ion vacancies exist in the YSZ, the oxygen ions can be conducted to the common electrode, and the electrons are lost at the three-phase interface of the common electrode to generate oxygen which is released to the outside. In the process, the conduction of oxygen ions forms current, the magnitude of the current depends on the conduction quantity of the oxygen ions, and therefore, the automobile exhaust NO can be indirectly detected by detecting the magnitude of the currentXAnd the content provides a basis for the injection quantity of the SCR catalyst, so that the emission quantity control of the oxynitride in the automobile exhaust is realized. The working mechanism of the oxygen sensor is similar to that of the nitrogen-oxygen sensor, and the oxygen sensor utilizes the characteristic of high-temperature oxygen ion conductivity of YSZ solid electrolyte to treat O in automobile exhaust2The content is detected and then converted into an electric signal to be fed back to the ECU, so that a basis is provided for the injection quantity of the fuel oil.
A core component of an oxygen sensor and a nitrogen-oxygen sensor, namely a multilayer structure ceramic core body, belongs to a self-heating device, a heating wire with a specific shape is printed inside the core component, the heating of the ceramic core body is realized through an additional circuit, and the ceramic core body is heated to the optimal working temperature so as to realize the high-temperature oxygen ion conductivity of the ceramic core body. The heating wire of the ceramic core only plays a role of providing a heat source, and the external current cannot influence the detection current, so that the heating wire needs to be subjected to insulation treatment. The common practice is to print insulating layers on the upper and lower layers of the heater wire to realize the insulating treatment of the heater wire, and the commonly used insulating layer slurry is alumina-based slurry. However, the insulation layer slurry purchased in the market often has the following problems due to different systems and different formulas: (1) the matching with the heating wire is not matched, and cracking exists; (2) the slurry is not dense after sintering. Therefore, the insulation effect of the product is poor, and the detection precision is influenced.
It is to be noted that the information disclosed in the above background section is only for understanding the background of the present application and thus may include information that does not constitute prior art known to a person of ordinary skill in the art.
Disclosure of Invention
The invention mainly aims to overcome the defects of the background technology and provides an insulating layer slurry preparation material, an insulating layer preparation method and a gas sensor.
In order to achieve the purpose, the invention adopts the following technical scheme:
an insulating layer slurry preparation material comprises the following components in percentage by mass: .
Wherein the inorganic additive comprises at least one of magnesium aluminate spinel, kaolin, talc, silicon dioxide, magnesium oxide and calcium carbonate; the organic solvent comprises at least one of a high-boiling point solvent and a low-boiling point solvent, the boiling point of the high-boiling point solvent is more than 150 ℃, and the boiling point of the low-boiling point solvent is less than 110 ℃; preferably, the organic vehicle includes at least one of vinyl, cellulose, and acrylic resins.
Further:
the original grain size of the alpha-alumina powder is less than 1 mu m.
The mass ratio of the high-boiling-point solvent to the low-boiling-point solvent is 1: 3-3: 1.
the high boiling point solvent comprises at least one of terpineol, ethylene glycol butyl ether, dimethylformamide, dimethylacetamide, diethylene glycol monoethyl ether, dibasic ester, cyclohexanone, cyclohexanol and diethylene glycol; the low boiling point solvent comprises at least one of methanol, ethanol, isopropanol, isobutanol, ethyl acetate, propyl acetate, methyl ethyl ketone and chloroform.
The organic auxiliary agent comprises at least one of a dispersant, a plasticizer, a defoaming agent, a thixotropic agent and a flatting agent; preferably:
the dispersing agent comprises at least one of acrylate, alkyl, polyester copolymer and organic silicon;
the plasticizer comprises at least one of phthalate, isophthalate, terephthalate, benzoic acid and polyethylene glycol;
the defoaming agent comprises at least one of a defoaming polymer and a polysiloxane solution;
the thixotropic agent comprises at least one of a modified urea solution and a polyhydroxycarboxylic acid amide solution;
the leveling agent comprises at least one of polyether modified methyl alkyl polysiloxane copolymer, polymethyl alkyl-methyl aralkyl siloxane and polyether modified polydimethylsiloxane.
An insulating layer paste preparation method using the insulating layer paste preparation material, comprising the steps of:
(1) ball-milling the alpha-alumina powder, the inorganic additive, the high-boiling-point solvent, the low-boiling-point solvent and the dispersant for 12-36 hours to obtain a mixture;
(2) adding the organic carrier and the plasticizer into the mixture, continuing ball milling for 12-36 hours, and filtering through a filter screen to obtain pre-slurry;
(3) adding at least one of a defoaming agent, a thixotropic agent and a flatting agent into the pre-slurry, and stirring for 2-6 hours;
(4) and (4) carrying out viscosity modulation and homogenization treatment on the slurry obtained in the step (3), and standing to obtain the insulating layer slurry.
Further:
the ball milling is any one of planetary ball milling, roller ball milling and sand milling;
the filter screen is made of a nylon net or a stainless steel net with 100-400 meshes;
the homogenization treatment adopts a rolling and grinding mode;
the viscosity modulation adopts a heating evaporation or vacuum defoaming mode.
And (4) standing for 6-24 hours.
A preparation method of an insulating layer comprises the following steps: printing the insulating layer paste prepared by using the method of claim 6 on the surface of the YSZ electrolyte casting sheet and above the heating wire by a screen printing method and then drying.
Further, the screen printing method adopts 100-500 mesh nylon net or stainless steel net for printing.
The preparation method of the gas sensor comprises the step of preparing the heating wire insulating layer of the gas sensor by using insulating layer slurry, and is characterized in that the insulating layer slurry is prepared by using the insulating layer slurry preparation material.
A gas sensor comprises the insulating layer prepared by the preparation method.
The invention has the following beneficial effects:
the invention provides an insulating layer preparation material, which takes alumina as a main powder material, and also comprises an inorganic additive, an organic solvent, an organic carrier and an organic auxiliary agent, wherein the inorganic additive is added, so that the sintering temperature can be reduced during sintering, the sintering densification effect is achieved, the sintering temperature is closer to that of a ceramic core of a gas sensor, the problem that the existing insulating layer slurry is not densified during sintering is solved, and meanwhile, magnesia-alumina spinel, kaolin and talc are added in a mineral form, so that the dispersibility can be obviously improved, and the components are more uniform. At least one of a high boiling point solvent and a low boiling point solvent is added, the solid content of the insulating layer slurry can be kept stable in the processes of storage and printing by utilizing the characteristic that the high boiling point solvent is not easy to volatilize, the fluidity of the insulating layer slurry is stable, the printing stability of the insulating layer slurry is favorably improved, and the solubility and the uniformity of each component of the insulating layer slurry can be improved by adding the low boiling point solvent. The matching of the high boiling point solvent and the low boiling point solvent in the optimized scheme not only ensures the fluidity and the stability of the insulating layer slurry, but also ensures the solubility and the uniformity of each component. The addition of the organic carrier is beneficial to enabling the prepared insulating layer slurry to have good leveling property, adhesion and film forming property, and particularly, the insulating layer slurry can be well matched with a heating wire material, so that the problem of sintering cracking is solved.
The insulating layer paste prepared by the embodiment of the invention has good leveling property, adhesiveness and film-forming property, is suitable for screen printing, has flat appearance, no pinholes, shrinkage matching and compact sintering of an insulating layer prepared by the paste, can effectively solve the problems of non-compact sintering and cracking of the existing insulating layer paste when being applied to gas sensors such as oxygen sensors and nitrogen oxygen sensors, and improves the insulating property and the detection precision of the insulating layer paste.
Drawings
Fig. 1 is an SEM image of a non-dense insulating layer prepared by the conventional insulating layer slurry.
FIG. 2 is an SEM image showing that an insulating layer prepared from the conventional insulating layer slurry has cracks with a heating wire material after being sintered.
Fig. 3 is an insulating layer paste prepared in example 1 of the present invention.
FIG. 4 is an SEM image of a cross-section of an insulating layer prepared by using the insulating layer paste prepared in example 1 of the present invention.
Fig. 5 is an insulating layer paste prepared in example 2 of the present invention.
FIG. 6 is an SEM image of a cross section of an insulating layer prepared by using the insulating layer paste prepared in example 2 of the present invention.
Fig. 7 is an insulating layer paste prepared in example 3 of the present invention.
FIG. 8 is an SEM image of a cross-section of an insulating layer prepared by using the insulating layer paste prepared in example 3 of the present invention.
Detailed Description
The embodiments of the present invention will be described in detail below. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element. In addition, the connection may be for either a fixed or coupled or communicating function.
It is to be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for convenience in describing the embodiments of the present invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed in a particular orientation, and be in any way limiting of the present 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 one or more of that feature. In the description of the embodiments of the present invention, "a plurality" means two or more unless specifically limited otherwise.
The embodiment of the invention provides an insulating layer slurry preparation material which comprises the following components in percentage by mass:
wherein the inorganic additive comprises at least one of magnesium aluminate spinel, kaolin, talc, silicon dioxide, magnesium oxide and calcium carbonate; the organic solvent comprises at least one of a high boiling point solvent and a low boiling point solvent, wherein the boiling point of the high boiling point solvent is more than 150 ℃, and the boiling point of the low boiling point solvent is less than 110 ℃.
In a preferred embodiment, the mass ratio of the high-boiling point solvent to the low-boiling point solvent is 1: 3-3: 1. the high boiling point solvent comprises at least one of terpineol, ethylene glycol butyl ether, dimethylformamide, dimethylacetamide, diethylene glycol monoethyl ether, dibasic ester, cyclohexanone, cyclohexanol and diethylene glycol. The low boiling point solvent comprises at least one of methanol, ethanol, isopropanol, isobutanol, ethyl acetate, propyl acetate, methyl ethyl ketone and chloroform.
In a preferred embodiment, the organic vehicle includes at least one of vinyl, cellulose, and acrylic resins.
In a preferred embodiment, the primary grain size of the alpha-alumina powder is less than 1 μm.
In a preferred embodiment, the organic auxiliary agent includes at least one of a dispersant, a plasticizer, an antifoaming agent, a thixotropic agent, and a leveling agent.
In a preferred embodiment, the dispersant comprises at least one of acrylates, alkyls, polyester copolymers, silicones.
In a preferred embodiment, the plasticizer comprises at least one of phthalate, isophthalate, terephthalate, benzoic acid, polyethylene glycol.
In a preferred embodiment, the defoamer comprises at least one of a foam-breaking polymer, a polysiloxane solution.
In a preferred embodiment, the thixotropic agent comprises at least one of a modified urea solution, a polyhydroxycarboxylic acid amide solution.
In a preferred embodiment, the leveling agent comprises at least one of polyether modified methyl alkyl polysiloxane copolymer, polymethyl alkyl-methyl aralkyl siloxane and polyether modified polydimethylsiloxane.
The embodiment of the invention also provides an insulating layer slurry preparation method using the insulating layer slurry preparation material, which comprises the following steps:
(1) ball-milling the alpha-alumina powder, the inorganic additive, the high-boiling-point solvent, the low-boiling-point solvent and the dispersing agent for 12-36 hours to obtain a mixture;
(2) adding the organic carrier and the plasticizer into the mixture, continuing ball milling for 12-36 hours, and filtering through a filter screen to obtain pre-slurry;
(3) adding at least one of the defoaming agent, the thixotropic agent and the leveling agent into the pre-slurry, and stirring for 2-6 hours;
(4) and (4) carrying out viscosity modulation and homogenization treatment on the slurry obtained in the steps (1) to (3), and standing to obtain the insulating layer slurry.
In a preferred embodiment, the ball milling in the steps (1) and (2) is any one of planetary ball milling, roller ball milling and sand milling;
in a preferred embodiment, the filter screen in the step (2) adopts a nylon net or a stainless steel net with 100-400 meshes;
in a preferred embodiment, the homogenization treatment in the step (4) adopts a rolling and grinding mode;
in a preferred embodiment, the viscosity is adjusted by heating evaporation or vacuum defoaming in step (4).
In a preferred embodiment, the standing time in the step (4) is 6-24 hours.
The embodiment of the invention also provides a preparation method of the insulating layer, which comprises the following steps: the insulating layer paste prepared by using the foregoing examples was printed on the surface of the YSZ electrolyte tape and over the heating wire by screen printing and then dried.
In a preferred embodiment, the screen printing method uses 100-500 mesh nylon mesh or stainless steel mesh printing.
In a preferred embodiment, the YSZ electrolyte tape and the heating wire with the insulating layer paste printed on the surface are placed in an oven at 80-100 ℃ to be dried for 5-20 minutes.
The embodiment of the invention also provides a preparation method of the gas sensor, which comprises the step of preparing the heating wire insulating layer of the gas sensor by using the insulating layer paste, wherein the insulating layer paste is prepared by using the insulating layer paste preparation material in any one of the embodiments.
In some embodiments, the method for manufacturing a gas sensor further includes the step of preparing the insulating layer paste using the insulating layer paste preparation material.
In some embodiments, the gas sensor is a wide-area oxygen sensor or a nitrogen-oxygen sensor.
The insulating layer prepared by using the insulating layer slurry can well insulate the heating electrode of the gas sensor, so that the interference of a current signal input by a heating wire can be effectively avoided when the gas sensor works, and the detection precision of the gas sensor is improved.
Specific embodiments are described further below.
Example 1:
in this embodiment, the insulating layer slurry preparation material includes the following components by mass percent:
alpha-alumina powder: 47.05%, primary crystal D50: 0.623 mu m;
inorganic additives: 6.42 percent of magnesium aluminate spinel, kaolin and talc, wherein the mass ratio of the magnesium aluminate spinel is as follows: kaolin: talc 1: 1: 2;
organic solvent: 38.50% of a mixture of terpineol, butyl glycol, isobutanol, and propyl acetate, wherein the mass ratio of terpineol: ethylene glycol butyl ether: isobutanol: propyl acetate ═ 2: 2: 1: 1;
organic carrier: 4.28% polyvinyl butyral;
organic auxiliary agents: 0.70% of dispersing agent (acrylate), 1.55% of plasticizer (DBP), 0.50% of defoaming agent (polysiloxane solution), 0.50% of thixotropic agent (modified urea solution) and 0.50% of leveling agent (polyether modified methyl alkyl polysiloxane copolymer).
The method for preparing the insulating layer slurry and the insulating layer by using the materials comprises the following steps:
(1) weighing alpha-alumina powder and an inorganic additive according to a mass ratio, taking terpineol, butyl cellosolve, isobutyl alcohol and propyl acetate as solvents and taking acrylate as a dispersing agent, and ball-milling the mixture for 24 hours;
(2) weighing an organic carrier (polyvinyl butyral) and a plasticizer (DBP) according to the mass ratio, adding the organic carrier (polyvinyl butyral) and the plasticizer (DBP) into the mixture, and continuing to perform ball milling for 24 hours;
(3) and after discharging, continuously adding the defoaming agent, the thixotropic agent and the flatting agent into the slurry, and stirring for 2 hours by using a stirrer at the rotating speed of 120 revolutions per minute.
(4) And after stirring, performing oil bath on the slurry to remove redundant solvent, adjusting the viscosity, performing rolling and grinding for 3 times after the viscosity is adjusted, wherein the gap is 0.2mm, and standing for 12 hours after the rolling and grinding are finished to obtain the insulating layer slurry.
(5) Printing the insulating layer slurry on a YSZ tape casting sheet substrate and a heating wire by adopting a 300-mesh nylon wire mesh, drying in an oven at 85 ℃ for 10min, and then sintering in a box type furnace at 1450 ℃ for 2 h to obtain an insulating layer with the thickness of about 30 mu m.
Fig. 3 is an insulating layer paste prepared in example 1 of the present invention. FIG. 4 is an SEM image of a cross-section of an insulating layer prepared by using the insulating layer paste prepared in example 1 of the present invention.
Example 2:
in this embodiment, the insulating layer slurry preparation material includes the following components by mass percent:
alpha-alumina powder: 49.10%, primary crystal D50: 0.623 mu m;
inorganic additives: 8.32 percent of magnesium aluminate spinel, kaolin, talc, silicon dioxide, magnesium oxide and calcium carbonate, wherein the mass ratio of the magnesium aluminate spinel: kaolin: talc: silicon dioxide: magnesium oxide: calcium carbonate 1: 1: 2: 0.5: 0.5: 0.5;
organic solvent: 32.31% of a mixture of terpineol, dimethylacetamide, ethanol, and isobutanol, wherein the mass ratio of terpineol: dimethyl acetamide: ethanol: 1, isobutanol: 1: 1: 1;
organic carrier: 5.40% ethyl cellulose;
organic auxiliary agents: 0.92% of dispersant (polyester copolymer), 2.15% of plasticizer (polyethylene glycol), 0.50% of defoaming agent (polysiloxane solution), 0.50% of thixotropic agent (modified urea solution), and 0.80% of leveling agent (polymethyl alkyl-methyl aralkyl siloxane).
The method for preparing the insulating layer slurry and the insulating layer by using the materials comprises the following steps:
(1) weighing alpha-alumina powder and an inorganic additive according to a mass ratio, taking terpineol, dimethylacetamide, ethanol and isobutanol as solvents and taking a polyester copolymer as a dispersing agent, and ball-milling the mixture for 18 hours;
(2) weighing an organic carrier (ethyl cellulose) and a plasticizer (polyethylene glycol acid) according to the mass ratio, adding the organic carrier and the plasticizer into the mixture, and continuing to perform ball milling for 18 hours;
(3) and after discharging, continuously adding the defoaming agent, the thixotropic agent and the flatting agent into the slurry, and stirring for 4 hours by using a stirrer at the rotating speed of 120 revolutions per minute.
(4) And after stirring, performing oil bath on the slurry to remove redundant solvent, adjusting the viscosity, performing rolling and grinding for 3 times after the viscosity is adjusted, wherein the gap is 0.2mm, and standing for 6 hours after the rolling and grinding are finished to obtain the insulating layer slurry.
(5) Printing the insulating layer slurry on a YSZ tape casting sheet substrate and a heating wire by using a 200-mesh nylon wire mesh, drying in an oven at 85 ℃ for 10min, and sintering in a box type furnace at 1450 ℃ for 2 h to obtain an insulating layer with the thickness of about 30 mu m.
Fig. 5 is an insulating layer paste prepared in example 2 of the present invention. FIG. 6 is an SEM image of a cross section of an insulating layer prepared by using the insulating layer paste prepared in example 2 of the present invention.
Example 3:
in this embodiment, the insulating layer slurry preparation material includes the following components by mass percent:
alpha-alumina powder: 39.80%, primary crystal D50: 0.861 μm;
inorganic additives: 13.26 percent of magnesium aluminate spinel, kaolin and talc, wherein the mass ratio of the magnesium aluminate spinel: kaolin: talc 1: 1: 3;
organic solvent: 36.36% of a mixture of terpineol, butyl cellosolve, ethyl acetate and propyl acetate, wherein the mass ratio of terpineol: ethylene glycol butyl ether: ethyl acetate: propyl acetate ═ 1: 1: 2: 2;
organic carrier: 6.32% polyvinyl butyral;
organic auxiliary agents: 0.83% of dispersing agent (acrylate), 1.93% of plasticizer (DBP), 0.50% of defoaming agent (polysiloxane solution), 0.50% of thixotropic agent (polyhydroxycarboxylic acid amide solution) and 0.50% of leveling agent (polyether modified methyl alkyl polysiloxane copolymer).
The method for preparing the insulating layer slurry and the insulating layer by using the materials comprises the following steps:
(1) weighing alpha-alumina powder and an inorganic additive according to a mass ratio, taking terpineol, butyl cellosolve, ethyl acetate and propyl acetate as solvents and taking acrylate as a dispersing agent, and carrying out ball milling on the mixture for 24 hours;
(2) weighing an organic carrier (polyvinyl butyral) and a plasticizer (DBP) according to the mass ratio, adding the organic carrier (polyvinyl butyral) and the plasticizer (DBP) into the mixture, and continuing to perform ball milling for 24 hours;
(3) and after discharging, continuously adding the defoaming agent, the thixotropic agent and the flatting agent into the slurry, and stirring for 6 hours by using a stirrer at the rotating speed of 120 revolutions per minute.
(4) And after stirring, performing oil bath on the slurry to remove redundant solvent, adjusting the viscosity, performing rolling and grinding for 3 times after the viscosity is adjusted, wherein the gap is 0.2mm, and standing for 12 hours after the rolling and grinding are finished to obtain the insulating layer slurry.
(5) Printing the insulating layer slurry on a YSZ tape casting sheet substrate and a heating wire by adopting a 300-mesh nylon wire mesh, drying in an oven at 85 ℃ for 10min, and then sintering in a box type furnace at 1450 ℃ for 2 h to obtain an insulating layer with the thickness of about 30 mu m.
Fig. 7 is an insulating layer paste prepared in example 3 of the present invention. FIG. 8 is an SEM image of a cross-section of an insulating layer prepared by using the insulating layer paste prepared in example 3 of the present invention.
The insulating layer slurry prepared by the embodiment has good leveling property, adhesion property and film forming property, is compact after sintering, has no pin hole, is matched with a heating wire material, and does not crack. The preparation method is applied to preparation of the heating wire insulating layers of the oxygen sensor and the nitrogen-oxygen sensor, can improve the insulativity and the measurement precision of products, and effectively solves the problems of poor compactness, poor insulating effect and cracking caused by mismatching of sintering of the existing insulating layer slurry.
The background of the present invention may contain background information related to the problem or environment of the present invention and does not necessarily describe the prior art. Accordingly, the inclusion in the background section is not an admission of prior art by the applicant.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and these substitutions and modifications should be considered to fall within the scope of the invention. In the description herein, references to the description of the term "one embodiment," "some embodiments," "preferred embodiments," "an example," "a specific example," or "some examples" or the like are intended to 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, 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. Various embodiments or examples and features of various 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 and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the scope of the claims.
Claims (10)
1. The insulating layer slurry preparation material is characterized by comprising the following components in percentage by mass: .
Wherein the inorganic additive comprises at least one of magnesium aluminate spinel, kaolin, talc, silicon dioxide, magnesium oxide and calcium carbonate; the organic solvent comprises at least one of a high-boiling point solvent and a low-boiling point solvent, the boiling point of the high-boiling point solvent is more than 150 ℃, and the boiling point of the low-boiling point solvent is less than 110 ℃; preferably, the organic vehicle includes at least one of vinyl, cellulose, and acrylic resins.
2. The insulating layer slurry preparation material according to claim 1, wherein the α -alumina powder has a primary grain size of less than 1 μm.
3. The insulating layer slurry preparation material according to any one of claims 1 to 2, wherein the mass ratio of the high-boiling point solvent to the low-boiling point solvent is 1: 3-3: 1.
4. the insulation layer slurry preparation material according to claim 3, wherein the high boiling point solvent comprises at least one of terpineol, ethylene glycol butyl ether, dimethylformamide, dimethylacetamide, diethylene glycol monoethyl ether, dibasic ester, cyclohexanone, cyclohexanol, diethylene glycol; the low boiling point solvent comprises at least one of methanol, ethanol, isopropanol, isobutanol, ethyl acetate, propyl acetate, methyl ethyl ketone and chloroform.
5. The insulating layer slurry preparation material according to any one of claims 1 to 4, wherein the organic auxiliary agent comprises at least one of a dispersant, a plasticizer, an antifoaming agent, a thixotropic agent, and a leveling agent; preferably:
the dispersing agent comprises at least one of acrylate, alkyl, polyester copolymer and organic silicon;
the plasticizer comprises at least one of phthalate, isophthalate, terephthalate, benzoic acid and polyethylene glycol;
the defoaming agent comprises at least one of a defoaming polymer and a polysiloxane solution;
the thixotropic agent comprises at least one of a modified urea solution and a polyhydroxycarboxylic acid amide solution;
the leveling agent comprises at least one of polyether modified methyl alkyl polysiloxane copolymer, polymethyl alkyl-methyl aralkyl siloxane and polyether modified polydimethylsiloxane.
6. An insulation layer slurry preparation method using the insulation layer slurry preparation material according to any one of claims 1 to 5, comprising the steps of:
(1) ball-milling the alpha-alumina powder, the inorganic additive, the high-boiling-point solvent, the low-boiling-point solvent and the dispersant for 12-36 hours to obtain a mixture;
(2) adding the organic carrier and the plasticizer into the mixture, continuing ball milling for 12-36 hours, and filtering through a filter screen to obtain pre-slurry;
(3) adding at least one of a defoaming agent, a thixotropic agent and a flatting agent into the pre-slurry, and stirring for 2-6 hours;
(4) and (4) carrying out viscosity modulation and homogenization treatment on the slurry obtained in the step (3), and standing to obtain the insulating layer slurry.
7. The preparation method of the insulating layer is characterized by comprising the following steps of: printing the insulating layer paste prepared by using the method of claim 6 on the surface of the YSZ electrolyte casting sheet and above the heating wire by a screen printing method and then drying.
8. The method of preparing an insulating layer according to claim 7, wherein the screen printing method uses a 100-500 mesh nylon mesh or a stainless steel mesh for printing.
9. A method for manufacturing a gas sensor, comprising the step of forming an insulating layer of a heater wire of the gas sensor using an insulating layer paste, wherein the insulating layer paste is prepared using the insulating layer paste preparation material according to any one of claims 1 to 5.
10. A gas sensor comprising an insulating layer produced using the production method according to any one of claims 7 to 8.
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