CN110285899B - Preparation method of ceramic pressure sensor - Google Patents
Preparation method of ceramic pressure sensor Download PDFInfo
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- CN110285899B CN110285899B CN201910227574.5A CN201910227574A CN110285899B CN 110285899 B CN110285899 B CN 110285899B CN 201910227574 A CN201910227574 A CN 201910227574A CN 110285899 B CN110285899 B CN 110285899B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B41/5072—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 oxides or hydroxides not covered by C04B41/5025
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/0041—Transmitting or indicating the displacement of flexible diaphragms
- G01L9/0051—Transmitting or indicating the displacement of flexible diaphragms using variations in ohmic resistance
- G01L9/006—Transmitting or indicating the displacement of flexible diaphragms using variations in ohmic resistance of metallic strain gauges fixed to an element other than the pressure transmitting diaphragm
Abstract
The invention relates to the technical field of sensors and discloses a preparation method of a ceramic pressure sensor. The preparation method comprises the following steps: 1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature, drying the ceramic base, placing the ceramic base in a high-temperature furnace for primary sintering after drying, and cooling the ceramic base to room temperature after sintering; 2) printing thick film slurry on the surface of an aluminum oxide ceramic substrate at a specified position of the aluminum oxide ceramic substrate by screen printing; 3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering, and cooling to obtain the ceramic. The invention greatly shortens the curing time of the resistance paste, and the resistance paste on the ceramic substrate can not deform in the curing process.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a preparation method of a ceramic pressure sensor.
Background
The sensor technology is one of the high and new technologies which are developed rapidly and is also an important mark for the development of modern science and technology. As an antenna for human to detect external information, the sensor technology is a technology for acquiring information in various forms with high precision, high efficiency and high reliability, converts non-electric quantity information into electric quantity information which is easy to process, creates necessary conditions for people to further know and reform the world, and provides a new method. The three major foundations of modern information technology are information pickup, information transmission and information processing, namely sensor technology, communication technology and computer technology, the sensor technology is located at the head of the information technology, is the source of the information technology and is the front-end foundation for acquiring information, and the development level of the sensor technology plays a decisive role in the development level and the function of an information technology system. As a source of the information detection system, the sensor is an indispensable part in analyzing, measuring, detecting and even controlling the system, and directly determines the quality of the system performance to some extent. The technologies of intelligent devices, mobile internet, computers and the like have made great progress at present, and people can more widely apply the technical achievements to the aspects of life, industrial production and the like.
Currently, pressure sensors are mainly classified into two types, a piezoresistive type and a pressure-capacitive type. The pressure-capacitance type sensor converts the variation of pressure into corresponding capacitance variation, and the capacitance variation can be converted into electrical signals of frequency, current, voltage and the like for output through a detection circuit. The high-power-factor LED driving circuit has good dynamic response and temperature stability, but high output impedance, poor load capacity and large influence of parasitic capacitance. The piezoresistive pressure sensor is characterized in that when an elastic diaphragm of the sensor is under the action of pressure, the resistance value of a force sensitive resistor on the diaphragm changes, and voltage output or current output in a linear relation with the pressure can be obtained through a measuring circuit. The temperature control device is simple in structure and easy to produce, but has the problem of temperature drift. Piezoresistive materials used in piezoresistive pressure sensors fall into three categories: semiconductors, metals, and thick film resistors. The performance of the thick film resistor material is between that of a semiconductor material and that of a metal material, the pressure sensor made of the semiconductor material takes a diffused silicon resistor as a force sensitive resistor, an elastomer of the pressure sensor is monocrystalline silicon and is easy to be influenced by temperature, the temperature drift of the sensor is large, and the corrosion resistance is poor; the pressure sensor made of metal materials generally comprises an elastic diaphragm and a metal strain gauge, and the metal strain gauge is bonded on the elastic diaphragm by adopting a bonding agent, so that the pressure sensor is easy to age. The thick film resistance material is a strain measurement material with better comprehensive performance. In addition, the thick film resistor is manufactured by printing thick film slurry on the ceramic elastic diaphragm by adopting a screen printing technology, and sintering the thick film resistor and the ceramic elastic diaphragm into a whole by high-temperature sintering.
The film thickness technology is mainly characterized in that a film is formed through screen printing and high-temperature sintering, and screen cloth made of different materials can meet the requirements of different printing processes. Since the 60 s, screen printing has been widely used in the electronics industries such as printed circuit boards, resistors, thick film integrated circuits, capacitors, etc., and in the screen material, stainless steel materials have been used as screens in the electronics manufacturing industry with high precision due to the unstable mesh size and low printing precision of the mesh material. Screen printing, leveling, drying and sintering are the key steps for manufacturing thick film circuits. After the slurry is deposited on the substrate, leveling and drying are needed, and after the slurry on the substrate is dried, sintering can be carried out.
Chinese patent publication No. CN107702788 discloses a ceramic high-temperature vibration sensor and a method for manufacturing the same, wherein a platinum paste is printed on a ceramic substrate by a screen printing method in the manufacturing process of the sensor, and then the sensor is placed in a drying furnace for drying treatment to dry the platinum paste, but the drying process is slow, and the platinum paste printed on the ceramic substrate has fluidity, so that the formed platinum paste is deformed.
Disclosure of Invention
The invention aims to solve the problem that the forming slurry platinum printed on a ceramic substrate is easy to deform in the drying process in the prior art, and provides a preparation method of a ceramic pressure sensor.
In order to achieve the purpose, the invention adopts the following technical scheme: a preparation method of a ceramic pressure sensor comprises the following steps:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 5-10min, drying the ceramic base, placing the ceramic base in a high-temperature furnace for primary sintering after drying, and cooling the ceramic base to room temperature after sintering;
2) printing thick film slurry on the surface of an aluminum oxide ceramic substrate at a specified position of the aluminum oxide ceramic substrate by screen printing;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering, and cooling to obtain the ceramic.
Preferably, the drying time in the step 1) is 10-15min, and the drying temperature is 120-150 ℃.
Preferably, the primary sintering temperature in the step 1) is 750-.
Preferably, the secondary sintering temperature in the step 3) is 800-850 ℃, and the sintering time is 2-5 h.
Preferably, the thick film slurry in the step 2) comprises the following components in parts by weight:
40-50 parts of molybdenum oxide, 5-10 parts of glass powder, 20-30 parts of modified phenolic resin binder and 10-20 parts of organic carrier.
Preferably, the preparation method of the modified phenolic resin binder comprises the following steps:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:5-10, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 2-5wt% of the phenol, heating to 80-85 ℃, adding formaldehyde, and reacting for 2-4 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 2-5; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:1-3, the addition amount of the dicyclohexylcarbodiimide is 2-5wt% of the carboxymethyl chitosan, and reacting for 1-2 hours; and adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:8-10, stirring and reacting for 30-50min, and cooling to obtain the modified phenolic resin binder.
The organic binder is adopted to replace the traditional inorganic binder, and the organic binder can ensure that the conductive phase and the ceramic are bonded more tightly and firmly; phenol and o-hydroxy phenol are subjected to condensation polymerization with formaldehyde to obtain phenolic resin, and in the sintering process, part of phenolic resin in the slurry on the ceramic substrate can be decomposed, the conductive phase is easy to fall off from the ceramic substrate, therefore, the invention modifies the phenolic resin to improve the heat resistance of the phenolic resin, adds a certain amount of o-hydroxyphenol in the preparation process of the phenolic resin, introduces hydroxyl with high reaction activity into the phenolic resin, carboxyl on the carboxymethyl chitosan and hydroxyl are subjected to condensation reaction, the carboxymethyl chitosan plays a role of a bridge, macromolecular chains of the phenolic resin are connected, the crosslinking degree of the phenolic resin is increased, therefore, the heat resistance of the phenolic resin is improved, hydroxyl and carboxyl on the carboxymethyl chitosan can form hydrogen bonds with conductive phase molybdenum oxide and hydroxyl on the surface of ceramic alumina, and the binding force of the phenolic resin with the ceramic alumina and the conductive phase molybdenum oxide is improved; tetravalent titanium ions in the titanium dioxide are complexed with hydroxyl on the carboxymethyl chitosan, so that the titanium dioxide is connected to a phenolic resin macromolecular chain, and the heat resistance of the phenolic resin can be further improved by the titanium dioxide; in addition, in the screen printing process, after the resistance paste is printed on the ceramic substrate, the resistance paste must be quickly cured at room temperature, otherwise the resistance paste printed on the ceramic substrate is easy to deform, and under the irradiation of infrared light, the titanium dioxide particles have a scattering effect on the infrared light, so that the curing time of the resistance paste is greatly shortened, and the resistance paste on the ceramic substrate is prevented from deforming.
Preferably, the titanium oxide is pretreated, and the pretreatment method comprises the following steps:
dropwise adding ammonia water into an ethanol aqueous solution with the mass concentration of 30-50% until the pH value is 9-9.5, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol aqueous solution is 1:5-10, heating to 75-85 ℃, uniformly stirring, adding amino trioxyethyl silane, wherein the mass ratio of the amino trioxyethyl silane to the titanium dioxide powder is 1:5-10, reacting for 1-3h under heat preservation, cooling, and then sequentially aging, filtering, washing and drying to obtain the catalyst.
The titanium dioxide is easy to agglomerate and is unevenly dispersed in the phenolic resin, the titanium dioxide is pretreated, and the amino trioxyethylsilane is bonded on the surface of the titanium dioxide, so that the lipophilicity of the titanium dioxide is improved, the dispersibility of the titanium dioxide in the phenolic resin is obviously improved, in addition, the amino on the amino trioxyethylsilane can form a hydrogen bond action with the hydroxyl and the carboxyl on the chitosan, and the titanium dioxide is not easy to separate out from slurry in the sintering process.
Therefore, the invention has the following beneficial effects: 1) under the irradiation of infrared light, the titanium dioxide particles have a scattering effect on the infrared light, so that the curing time of the resistance paste is greatly shortened, and the resistance paste on the ceramic substrate is prevented from deforming; 2) titanium dioxide can further improve the heat resistance of the phenolic resin; 3) the organic binder is adopted to replace the traditional inorganic binder, and the organic binder can enable the conductive phase and the ceramic to be bonded more tightly and firmly.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
In the present invention, unless otherwise specified, all the raw materials and equipment used are commercially available or commonly used in the art, and the methods in the examples are conventional in the art unless otherwise specified.
Example 1
Preparing a modified phenolic resin binder:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:8, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 3.5 wt% of the phenol, heating to 82 ℃, adding formaldehyde, and reacting for 3 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 3; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:2, the addition amount of the dicyclohexylcarbodiimide is 4 wt% of the carboxymethyl chitosan, and reacting for 1 h; adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:9, stirring for reaction for 40min, and cooling to obtain a modified phenolic resin binder; wherein the titanium dioxide is pretreated, and the pretreatment method comprises the following steps: dropwise adding ammonia water into 40% ethanol water solution until the pH value is 9.2, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol water solution is 1:8, heating to 80 ℃, uniformly stirring, adding amino trioxyethylsilane, wherein the mass ratio of the amino trioxyethylsilane to the titanium dioxide powder is 1:7, carrying out heat preservation reaction for 2 hours, cooling, and then sequentially carrying out aging, suction filtration, washing and drying to obtain the catalyst.
Preparing a ceramic pressure sensor:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 8min, drying the ceramic base at 130 ℃ for 12min, placing the ceramic base in a high-temperature furnace for primary sintering at 780 ℃ after drying, and cooling the ceramic base to room temperature after sintering for 2 h;
2) printing thick film paste on the surface of an alumina ceramic substrate at a specified position of the alumina ceramic substrate by screen printing, wherein the thick film paste comprises the following components in parts by weight: 45 parts of molybdenum oxide, 8 parts of glass powder, 25 parts of modified phenolic resin binder and 15 parts of organic carrier; the organic carrier comprises the following components in parts by weight: 18 parts of ethyl cellulose, 3 parts of furoic acid, 7 parts of polyacrylate and 60 parts of butyl carbitol acetate;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering at 820 ℃ for 3h, and cooling to obtain the ceramic.
Example 2
Preparing a modified phenolic resin binder:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:9, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 4 wt% of the phenol, heating to 85 ℃, adding formaldehyde, and reacting for 3 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 4; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:3, the addition amount of the dicyclohexylcarbodiimide is 4 wt% of the carboxymethyl chitosan, and reacting for 2 hours; adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:10, stirring for reaction for 45min, and cooling to obtain a modified phenolic resin binder; wherein the titanium dioxide is pretreated, and the pretreatment method comprises the following steps: dropwise adding ammonia water into an ethanol aqueous solution with the mass concentration of 50% until the pH value is 9.5, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol aqueous solution is 1:8, heating to 82 ℃, uniformly stirring, adding amino trioxyethylsilane, wherein the mass ratio of the amino trioxyethylsilane to the titanium dioxide powder is 1:9, carrying out heat preservation reaction for 2.5h, cooling, and then sequentially carrying out aging, suction filtration, washing and drying to obtain the titanium dioxide catalyst.
Preparing a ceramic pressure sensor:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 9min, drying the ceramic base at 125 ℃ for 13min, placing the ceramic base in a high-temperature furnace for primary sintering at 790 ℃ for 1h after drying, and cooling the ceramic base to room temperature after sintering;
2) printing thick film paste on the surface of an alumina ceramic substrate at a specified position of the alumina ceramic substrate by screen printing, wherein the thick film paste comprises the following components in parts by weight: 48 parts of molybdenum oxide, 9 parts of glass powder, 28 parts of modified phenolic resin binder and 17 parts of organic carrier; the organic carrier comprises the following components in parts by weight: 18 parts of ethyl cellulose, 4 parts of furoic acid, 9 parts of polyacrylate and 65 parts of butyl carbitol acetate;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering at 840 ℃ for 2.5h, and cooling to obtain the ceramic.
Example 3
Preparing a modified phenolic resin binder:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:6, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 2.5 wt% of that of the phenol, heating to 80 ℃, adding formaldehyde, and reacting for 2.5 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 2; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:2, the addition amount of the dicyclohexylcarbodiimide is 2 wt% of the carboxymethyl chitosan, and reacting for 1 h; adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:9, stirring for reaction for 35min, and cooling to obtain a modified phenolic resin binder; wherein the titanium dioxide is pretreated, and the pretreatment method comprises the following steps: dropwise adding ammonia water into an ethanol aqueous solution with the mass concentration of 30% until the pH value is 9.2, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol aqueous solution is 1:6, heating to 80 ℃, uniformly stirring, adding amino trioxyethylsilane, wherein the mass ratio of the amino trioxyethylsilane to the titanium dioxide powder is 1:6, carrying out heat preservation reaction for 1.5h, cooling, and then sequentially carrying out aging, suction filtration, washing and drying to obtain the titanium dioxide catalyst.
Preparing a ceramic pressure sensor:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 6min, drying the ceramic base at 125 ℃ for 12min, placing the ceramic base in a high-temperature furnace for primary sintering at 760 ℃ after drying, wherein the sintering time is 1h, and cooling the ceramic base to room temperature after sintering;
2) printing thick film paste on the surface of an alumina ceramic substrate at a specified position of the alumina ceramic substrate by screen printing, wherein the thick film paste comprises the following components in parts by weight: 42 parts of molybdenum oxide, 6 parts of glass powder, 23 parts of modified phenolic resin binder and 10 parts of organic carrier; the organic carrier comprises the following components in parts by weight: 16 parts of ethyl cellulose, 3 parts of furoic acid, 6 parts of polyacrylate and 55 parts of butyl carbitol acetate;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering, wherein the secondary sintering temperature is 810 ℃, the sintering time is 4 hours, and cooling to obtain the ceramic.
Example 4
Preparing a modified phenolic resin binder:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:10, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 5wt% of the phenol, heating to 85 ℃, adding formaldehyde, and reacting for 4 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 5; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:3, the addition amount of the dicyclohexylcarbodiimide is 5wt% of the carboxymethyl chitosan, and reacting for 2 hours; adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:10, stirring for reaction for 50min, and cooling to obtain a modified phenolic resin binder; wherein the titanium dioxide is pretreated, and the pretreatment method comprises the following steps: dropwise adding ammonia water into an ethanol aqueous solution with the mass concentration of 30-50% until the pH value is 9.5, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol aqueous solution is 1:10, heating to 85 ℃, uniformly stirring, adding amino trioxyethylsilane, wherein the mass ratio of the amino trioxyethylsilane to the titanium dioxide powder is 1:10, carrying out heat preservation reaction for 3 hours, cooling, and then sequentially carrying out aging, suction filtration, washing and drying to obtain the catalyst.
Preparing a ceramic pressure sensor:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 10min, drying the ceramic base at the drying temperature of 120 ℃ for 15min, placing the ceramic base in a high-temperature furnace for primary sintering at the primary sintering temperature of 800 ℃ for 1h after drying, and cooling the ceramic base to room temperature after sintering;
2) printing thick film paste on the surface of an alumina ceramic substrate at a specified position of the alumina ceramic substrate by screen printing, wherein the thick film paste comprises the following components in parts by weight: 50 parts of molybdenum oxide, 10 parts of glass powder, 30 parts of modified phenolic resin binder and 20 parts of organic carrier; the organic carrier comprises the following components in parts by weight: 20 parts of ethyl cellulose, 5 parts of furoic acid, 10 parts of polyacrylate and 70 parts of butyl carbitol acetate;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering at 850 ℃ for 2 hours, and cooling to obtain the ceramic.
Example 5
Preparing a modified phenolic resin binder:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:5, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 2 wt% of that of the phenol, heating to 80 ℃, adding formaldehyde, and reacting for 2 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 2; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:1, the addition amount of the dicyclohexylcarbodiimide is 2 wt% of the carboxymethyl chitosan, and reacting for 1 h; adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:8, stirring for reaction for 30min, and cooling to obtain a modified phenolic resin binder; wherein the titanium dioxide is pretreated, and the pretreatment method comprises the following steps: dropwise adding ammonia water into an ethanol aqueous solution with the mass concentration of 30% until the pH value is 9, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol aqueous solution is 1:5, heating to 75 ℃, uniformly stirring, adding amino trioxyethylsilane, wherein the mass ratio of the amino trioxyethylsilane to the titanium dioxide powder is 1:5, carrying out heat preservation reaction for 1h, cooling, and then sequentially carrying out aging, suction filtration, washing and drying to obtain the catalyst.
Preparing a ceramic pressure sensor:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 5min, drying the ceramic base at 150 ℃ for 10min, placing the ceramic base in a high-temperature furnace for primary sintering at 750 ℃ for 3h after drying, and cooling the ceramic base to room temperature after sintering;
2) printing thick film paste on the surface of an alumina ceramic substrate at a specified position of the alumina ceramic substrate by screen printing, wherein the thick film paste comprises the following components in parts by weight: 40 parts of molybdenum oxide, 5 parts of glass powder, 20 parts of modified phenolic resin binder and 10 parts of organic carrier; the organic carrier comprises the following components in parts by weight: 15 parts of ethyl cellulose, 2 parts of furoic acid, 5 parts of polyacrylate and 50 parts of butyl carbitol acetate;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering at the secondary sintering temperature of 800 ℃ for 5 hours, and cooling to obtain the ceramic.
Comparative example 1
Comparative example 1 differs from example 1 in that the modified phenolic resin binder is replaced by a commercially available ordinary phenolic resin binder.
The strain coefficients and temperature coefficients of the example and comparative example pressure sensors were measured and the curing time of the paste in the infrared was measured after printing the resistive paste on the ceramic substrate in the screen printing process.
| Example 1 | Example 3 | Example 5 | Comparative example 1 | |
| Coefficient of strain (GF) | 16 | 16 | 15 | 14 |
| Temperature coefficient of | 85 | 88 | 97 | 94 |
| Curing time(s) | 223 | 237 | 255 | 576 |
The comparative example and the example show that the resistance paste has shorter curing time under infrared ray and does not deform after being printed on the ceramic substrate in the silk-screen printing process.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The preparation method of the ceramic pressure sensor is characterized by comprising the following steps of:
1) selecting alumina ceramic as a base, cleaning and drying the alumina ceramic, printing silver palladium conductor slurry on an elastic membrane of the ceramic base, standing the ceramic base at room temperature for 5-10min, drying the ceramic base, placing the ceramic base in a high-temperature furnace for primary sintering after drying, and cooling the ceramic base to room temperature after sintering;
2) printing thick film slurry on the surface of an aluminum oxide ceramic substrate at a specified position of the aluminum oxide ceramic substrate by screen printing;
the thick film slurry in the step 2) comprises the following components in parts by weight:
40-50 parts of molybdenum oxide, 5-10 parts of glass powder, 20-30 parts of modified phenolic resin binder and 10-20 parts of organic carrier;
the preparation method of the modified phenolic resin binder comprises the following steps:
pre-melting phenol and o-hydroxyphenyl, adding the phenol and the o-hydroxyphenyl into a reaction kettle, wherein the molar ratio of the o-hydroxyphenyl to the phenol is 1:5-10, adding sodium hydroxide serving as a catalyst into the reaction kettle, wherein the addition amount of the sodium hydroxide is 2-5wt% of the phenol, heating to 80-85 ℃, adding formaldehyde, and reacting for 2-4 hours, wherein the molar ratio of the phenol to the formaldehyde is 1: 2-5; then adding carboxymethyl chitosan and a catalyst dicyclohexylcarbodiimide into the reaction kettle, wherein the molar ratio of the carboxymethyl chitosan to the o-hydroxyphenol is 1:1-3, the addition amount of the dicyclohexylcarbodiimide is 2-5wt% of the carboxymethyl chitosan, and reacting for 1-2 hours; adding titanium dioxide into the reaction kettle, wherein the mass ratio of the titanium dioxide to the carboxymethyl chitosan is 1:8-10, stirring and reacting for 30-50min, and cooling to obtain a modified phenolic resin binder;
3) and (3) placing the alumina ceramic printed with the thick film slurry as a substrate under an infrared lamp for drying, then placing the substrate in a high-temperature furnace for secondary sintering, and cooling to obtain the ceramic.
2. The method as claimed in claim 1, wherein the drying time in step 1) is 10-15min, and the drying temperature is 120-150 ℃.
3. The method as claimed in claim 1, wherein the primary sintering temperature in step 1) is 750-800 ℃, and the sintering time is 1-3 h.
4. The method as claimed in claim 1, wherein the secondary sintering temperature in step 3) is 800-.
5. The method of claim 1, wherein the titanium dioxide is pretreated, and the pretreatment comprises the following steps:
dropwise adding ammonia water into an ethanol aqueous solution with the mass concentration of 30-50% until the pH value is 9-9.5, adding titanium dioxide powder into the solution, wherein the mass ratio of the titanium dioxide powder to the ethanol aqueous solution is 1:5-10, heating to 75-85 ℃, uniformly stirring, adding amino trioxyethyl silane, wherein the mass ratio of the amino trioxyethyl silane to the titanium dioxide powder is 1:5-10, reacting for 1-3h under heat preservation, cooling, and then sequentially aging, filtering, washing and drying to obtain the catalyst.
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