CN111855068A - Ceramic sensor and preparation method thereof - Google Patents
Ceramic sensor and preparation method thereof Download PDFInfo
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- 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
- G01L9/12—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 by making use of variations in capacitance, i.e. electric circuits therefor
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- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/18—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a linear resistance, e.g. platinum resistance thermometer
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures
Abstract
The invention discloses a ceramic sensor and a preparation method thereof, wherein the ceramic sensor comprises a ceramic bolerous thin sheet, a ceramic base and a conductive channel which are formed into an integrated structure, a cavity is formed between the ceramic bolerous thin sheet and the ceramic base, and the thickness of the ceramic bolerous thin sheet is smaller than that of the ceramic base; the bottom surface of the ceramic bolerous sheet is provided with a common electrode, a pressure sensing electrode and a reference electrode are arranged in the central area of the top surface of the ceramic base, the conductive channel is arranged on the ceramic base and consists of a channel hole and a conductive electrode filled in the channel hole, the conductive channel comprises a first conductive channel connected with the common electrode, a second conductive channel connected with the pressure sensing electrode and a third conductive channel connected with the reference electrode, and each conductive electrode penetrates through the bottom of the ceramic base and is provided with a leading-out end. The ceramic sensor can effectively solve the problems of low air tightness yield, poor reliability and the like of the conventional ceramic sensor.
Description
Technical Field
The invention relates to the field of sensors, in particular to a ceramic sensor and a preparation method thereof.
Background
In the conventional ceramic sensor, for example, a ceramic capacitive pressure sensor, electrodes are respectively disposed on opposite surfaces of a ceramic elastic sheet and a ceramic base, and the ceramic elastic sheet and the ceramic base are sealed by a sealing material (e.g., glass paste) to form a cavity structure between the opposite surfaces. The existing ceramic capacitance pressure sensor has the problems of poor sealing performance, poor reliability and the like.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a ceramic sensor and a preparation method thereof.
The technical problem of the invention is solved by the following technical scheme:
a ceramic sensor comprises a ceramic bolerous thin sheet, a ceramic base and a conductive channel; a cavity is formed between a middle region of the bottom surface of the ceramic elastic sheet and a middle region of the top surface of the ceramic base, and the thickness of the ceramic elastic sheet is smaller than that of the ceramic base; the bottom surface of the ceramic bolerous thin sheet corresponding to the cavity is provided with a common electrode, the central area of the top surface of the ceramic base corresponding to the cavity is provided with a pressure sensing electrode and a reference electrode, and the reference electrode is annular and concentric with the pressure sensing electrode and surrounds the outside of the pressure sensing electrode to be spaced from the pressure sensing electrode; the projection of the common electrode on the top surface of the ceramic base corresponding to the cavity completely covers the pressure sensing electrode and the reference electrode; the conductive channel is arranged on the ceramic base, consists of a channel hole and a conductive electrode filled in the channel hole, and comprises a first conductive channel connected with the common electrode, a second conductive channel connected with the pressure sensing electrode and a third conductive channel connected with the reference electrode, and each conductive electrode penetrates through the bottom of the ceramic base and is provided with a leading-out end; the ceramic elastic sheet, the ceramic base and the conductive channel are sintered to form an integral structure.
Preferably, the temperature sensing device further comprises a temperature sensing electrode formed in the ceramic base, and the conductive channel further comprises a fourth conductive channel and a fifth conductive channel connected with the temperature sensing electrode.
Preferably, a soldering layer is formed on each of the terminals of the conductive electrodes after the plating process.
Preferably, the interval between the pressure sensing electrode and the reference electrode is 0.1 mm-0.8 mm.
A preparation method of a ceramic sensor comprises the following steps:
(1) preparing a plurality of first green tapes, a second green tape, a plurality of third green tapes and a fourth green tape, and forming a channel hole of the conductive channel by opening a hole on each third green tape;
the plurality of first green belts and the plurality of third green belts are obtained by casting and drying first ceramic slurry, and the second green belt is obtained by printing the common electrode in the middle area of the surface of one of the first green belts;
wherein the forming of the fourth green tape comprises the steps of:
A. printing the reference electrode and the pressure-sensitive electrode on a central region of a surface of one of the third green tapes;
B. printing a second ceramic slurry on the surface of the green tape formed in the step A, wherein the reference electrode and the pressure sensing electrode are arranged on the surface of the green tape, and the positions of the green tape are except the channel hole and the middle area;
C. printing a slurry decomposable at a medium and low temperature on the middle area of the green tape formed in the step B to obtain a fourth green tape, wherein the printing thicknesses of the step B and the step C are the same;
(2) filling a conductive paste into each channel hole in each third green tape and each fourth green tape and drying;
(3) laminating the first green tape, the second green tape, the fourth green tape and the third green tape in sequence to form a green body, wherein one side of the second green tape, on which the common electrode is arranged, is adjacent to one side of the fourth green tape, on which the slurry decomposable at the medium and low temperature is printed, the first green tape and the second green tape are laminated to form the ceramic raw sheet, and the third green tape and the fourth green tape are laminated to form the ceramic base;
(4) carrying out isostatic pressing treatment on the green body formed in the step (3), and then cutting to form a sensor green body;
(5) and (4) carrying out gel discharging sintering on the sensor green body formed in the step (4), wherein in the gel discharging sintering process, all decomposable slurry at a medium and low temperature is firstly decomposed to form the cavity, then after sintering is continued, the conductive slurry is formed into a conductive electrode which is filled in the channel hole, the conductive electrode is provided with a leading-out end on the bottom surface of the ceramic base, and the ceramic paleoplastic sheet, the ceramic base and the conductive channel are in an integrated structure.
Preferably, the method further comprises the step of forming the temperature sensing electrode: and printing a temperature sensing electrode on any one of the third green belts or the fourth green belt, and forming a conductive channel corresponding to the temperature sensing electrode on the ceramic base.
Preferably, the method further comprises the step (6): and (5) respectively electroplating the leading-out ends of the conductive electrodes in the step (5) to form welding layers.
Preferably, the paste for printing and forming the temperature sensing electrode is metal paste with TCR > 2000 ppm/DEG C, sheet resistance > 20m omega/□, sintering temperature > 1500 ℃, and printing thickness is 5-20 mu m.
Preferably, the aperture of the channel hole is 50-1000 μm; the printing thicknesses of the common electrode, the reference electrode and the pressure sensing electrode are respectively and independently 1-5 mu m; in the step B, the printing thickness of the second ceramic slurry is 20-100 mu m; and the printing thickness of the slurry decomposable at the medium and low temperature in the step C is 20-100 mu m.
Preferably, the first ceramic slurry comprises the following components in parts by mass: 45-60% of main powder, 0.5-5% of sintering aid, 20-35% of casting organic solvent, 0.5-2% of dispersant and 5-15% of adhesive; the second ceramic slurry comprises the following components in percentage by mass: 55-75% of main powder, 0.5-6% of sintering aid, 8-20% of organic solvent for printing, 1-5% of surfactant and 5-15% of adhesive; the slurry decomposable at the medium and low temperature comprises the following components in parts by mass: 60-80% of carbon powder, 8-20% of organic solvent, 5-15% of binder and 1-5% of surfactant.
Compared with the prior art, the invention has the advantages that: according to the ceramic sensor, the ceramic bolerous thin sheet, the ceramic base and the conductive channel are integrated, the sealing connection of the ceramic bolerous thin sheet and the ceramic base is guaranteed, the good sealing connection between the conductive channel and each electrode is also guaranteed, a welding layer can be further electroplated at the leading-out end of the conductive electrode in the conductive channel subsequently, the ceramic sensor is effectively welded with an external circuit subsequently, the conductive channel is formed in the process of forming the ceramic sensor and is in direct contact connection with each electrode, and the conductive channel is not required to be connected subsequently through a contact pin, so that the problems of poor air tightness and poor reliability of the existing ceramic sensor due to poor sealing and contact pin are solved, the sealing property and the reliability of the ceramic sensor are greatly improved, and the service life of the sensor is prolonged.
Further, the temperature sensing electrode is also integrated in the ceramic sensor, so that the ceramic sensor can be used for detecting pressure and temperature simultaneously on the basis of not increasing the volume.
Drawings
FIG. 1 is a schematic cross-sectional view of a ceramic capacitive pressure and temperature sensor in an embodiment of the invention;
FIG. 2 is a schematic diagram of the top surface of the ceramic base of the ceramic capacitive pressure and temperature sensor in an embodiment of the invention;
FIG. 3 is a schematic view of the bottom surface of a ceramic bolerous sheet of the ceramic capacitive pressure and temperature sensor in an embodiment of the invention;
FIG. 4 is a schematic diagram of step (7) of a method of making a ceramic capacitive pressure and temperature sensor in an embodiment of the present invention;
FIG. 5 is a graph showing the output relationship between the resistance R and the temperature T of the ceramic capacitor pressure and temperature sensor according to the embodiment of the present invention;
FIG. 6 is a graph of the output of the ceramic capacitance pressure and temperature sensors versus capacitance in an embodiment of the present invention.
Detailed Description
The invention will be further described with reference to the accompanying drawings and preferred embodiments. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
It should be noted that the terms of orientation such as left, right, up, down, top and bottom in the present embodiment are only relative concepts to each other or are referred to the normal use state of the product, and should not be considered as limiting.
The invention provides a ceramic sensor which comprises a ceramic bole thin sheet, a ceramic base and a conductive channel; a cavity is formed between a middle region of the bottom surface of the ceramic elastic sheet and a middle region of the top surface of the ceramic base, and the thickness of the ceramic elastic sheet is smaller than that of the ceramic base; the bottom surface of the ceramic bolerous thin sheet corresponding to the cavity is provided with a common electrode, the central area of the top surface of the ceramic base corresponding to the cavity is provided with a pressure sensing electrode and a reference electrode, and the reference electrode is annular (annular with an opening), is concentric with the pressure sensing electrode and surrounds the outside of the pressure sensing electrode to be spaced from the pressure sensing electrode; the projection of the common electrode on the top surface of the ceramic base corresponding to the cavity completely covers the pressure sensing electrode and the reference electrode; the conductive channel is arranged on the ceramic base, consists of a channel hole and a conductive electrode filled in the channel hole, and comprises a first conductive channel connected with the common electrode, a second conductive channel connected with the pressure sensing electrode and a third conductive channel connected with the reference electrode, and each conductive electrode penetrates through the bottom of the ceramic base and is provided with a leading-out end; the ceramic elastic sheet, the ceramic base and the conductive channel are sintered to form an integral structure.
The ceramic sensor formed by the scheme is used for detecting pressure and is a ceramic capacitance pressure sensor, wherein a common electrode and a pressure sensing electrode form a measuring capacitor Cp, the common electrode and a reference electrode form a reference capacitor Cr, when a ceramic elastic sheet is pressed and deformed, the common electrode is also deformed, so that the gap of a cavity is reduced, the capacitance is changed, the variation of Cp and Cr is converted into direct current voltage respectively for output, the magnitude of applied pressure is measured by a difference signal of two output voltages, and the larger the pressure is, the larger the capacitance variation is.
The ceramic capacitive pressure sensor is generally used in automobiles and industrial systems, and the sensor is required to have high reliability and long service life under severe working environments, while most of the existing ceramic capacitive pressure sensors adopt glass slurry as a sealing material between a ceramic elastic sheet and a ceramic base to form a cavity structure, and in addition, a through hole is reserved on the ceramic base, and the leading-out of an internal electrode is realized in a mode of inserting a pin into the through hole; in the invention, the ceramic elastic sheet, the ceramic base and the conductive channel are formed into an integrated structure, the formed ceramic elastic sheet and the ceramic base are made of the same material, the problem of mismatching of different materials is solved, meanwhile, the ceramic elastic sheet and the ceramic base are sintered into an integrated structure, the conductive channel is also sintered with the ceramic elastic sheet and the ceramic base into an integrated structure, and the conductive channel is well connected with the electrodes on the ceramic base and the ceramic elastic sheet in a sealing manner (the conductive electrode in the conductive channel is directly connected with the electrodes in a contact manner), the conductive channel is formed in the process of forming the ceramic capacitor pressure sensor and is in direct contact connection with each electrode, and the conductive channel is not required to be connected through a contact pin subsequently, so that the problems of poor air tightness and poor reliability of the conventional ceramic capacitor pressure sensor caused by sealing and poor contact pin are solved, the sealing property and the reliability of the ceramic capacitor pressure sensor are greatly improved, and the service life of the sensor is prolonged.
In some preferred embodiments, the ceramic base further comprises a temperature sensing electrode formed in the ceramic base, and the conductive path further comprises a fourth conductive path and a fifth conductive path connected to the temperature sensing electrode. More preferably, the temperature sensing electrode is also formed on the top surface of the ceramic base, is on the same surface as the reference electrode and the pressure sensing electrode, but is not in the cavity, the temperature sensing electrode is in a ring shape with an opening, surrounds the periphery of the reference electrode, and is provided with a fourth conductive channel and a fifth conductive channel at two ends of the ring shape respectively.
The ceramic capacitor pressure sensor is widely applied to pressure detection of water, gas, liquid and various media, pressure and temperature values are often required to be simultaneously tested in corresponding application environments, and the synergistic effect of temperature and pressure is also required to be simultaneously considered when the sensor is calibrated, so that the output precision of the sensor is improved. In the preferred scheme of the application, the temperature sensing electrode is also integrated in the ceramic sensor, so that the ceramic sensor can be used for measuring pressure and temperature simultaneously on the basis of not increasing the volume, and the ceramic sensor can be called as a ceramic capacitance pressure and temperature sensor.
After having increased the temperature measurement function, can further optimize the precision of sensor, because under the different temperatures (no pressure), the capacitance value of sensor is difference a bit, if there is not temperature sensor, the poor meeting misunderstanding of electric capacity is pressure variation, the relatively poor problem of the measuring accuracy who leads to the sensor from this, and be in the same place temperature and pressure sensor integration, through the change of temperature, the change condition of capacitance value difference, back-end circuit chip is through demarcating the relation of record difference in temperature and capacitance difference, can improve the precision of sensor with this.
In some preferred embodiments, a welding layer is formed on each lead-out end of each conductive electrode after electroplating treatment, and the formed welding layer can be subsequently and effectively welded with an external circuit, preferably, a nickel layer is plated on each lead-out end, and then a tin layer is plated on the surface of each nickel layer to wrap the nickel layer, wherein the thickness of each nickel layer is preferably 2-5 μm, and the thickness of each tin layer is preferably 3-10 μm.
In some preferred embodiments, the pressure sensing electrode and the reference electrode are spaced apart by 0.1mm to 0.8 mm.
The invention also provides a preparation method of the ceramic sensor, which comprises the following steps:
(1) preparing a plurality of first green tapes, a second green tape, a plurality of third green tapes and a fourth green tape, and forming a channel hole of the conductive channel by opening a hole on each third green tape;
the plurality of first green belts and the plurality of third green belts are obtained by casting and drying first ceramic slurry, and the second green belt is obtained by printing the common electrode in the middle area of the surface of one of the first green belts;
wherein the forming of the fourth green tape comprises the steps of:
A. printing the reference electrode and the pressure-sensitive electrode on a central region of a surface of one of the third green tapes;
B. printing a second ceramic slurry on the surface of the green tape formed in the step A, wherein the reference electrode and the pressure sensing electrode are arranged on the surface of the green tape, and the positions of the green tape are except the channel hole and the middle area;
C. printing a slurry decomposable at a medium and low temperature on the middle area of the green tape formed in the step B to obtain a fourth green tape, wherein the printing thicknesses of the step B and the step C are the same;
(2) filling and filling the conductive slurry into each channel hole in the third green tape and the fourth green tape and drying;
(3) laminating the first green tape, the second green tape, the fourth green tape and the third green tape in sequence to form a green body, wherein one side of the second green tape, on which the common electrode is arranged, is adjacent to one side of the fourth green tape, on which the slurry decomposable at the medium and low temperature is printed, the first green tape and the second green tape are laminated to form the ceramic raw sheet, and the third green tape and the fourth green tape are laminated to form the ceramic base; the preferable lamination pressure is 20-40 t, and the pressing temperature is as follows: 30 to 70 ℃.
(4) Carrying out isostatic pressing treatment on the green body formed in the step (3), and then cutting to form a sensor green body; preferably, the static pressure treatment is carried out at a water temperature of 60 to 70 ℃ and a pressure of 10 to 100 MPa.
(5) And (4) carrying out gel discharging sintering on the sensor green body formed in the step (4), wherein in the gel discharging sintering process, all decomposable slurry at a medium and low temperature is firstly decomposed to form the cavity, then after sintering is continued, the conductive slurry is formed into a conductive electrode which is filled in the channel hole, the conductive electrode is provided with a leading-out end on the bottom surface of the ceramic base, and the ceramic paleoplastic sheet, the ceramic base and the conductive channel are in an integrated structure. Preferably, the sintering temperature is: 1350-1600 ℃ in air or reducing atmosphere.
In some preferred embodiments, the preparation method further includes the step of forming a temperature-sensitive electrode: and printing a temperature sensing electrode on any one of the third green belts or the fourth green belt, and forming a conductive channel corresponding to the temperature sensing electrode on the ceramic base. More preferably, the temperature sensing electrode is formed on the same surface of the fourth green tape as the reference electrode and the pressure sensing electrode, but not in the cavity, that is, when the reference electrode and the pressure sensing electrode are printed on the middle region of the surface of one of the third green tapes in step a, the temperature sensing electrode is also printed, and when the second ceramic paste is printed in step B, the temperature sensing electrode may be covered with the second ceramic paste or may not be covered with the second ceramic paste.
In some preferred embodiments, the method further comprises the step (6): and (5) respectively electroplating the leading-out ends of the conductive electrodes in the step (5) to respectively form welding layers. Preferably, a nickel layer is plated on the leading-out end, and then a tin layer is plated on the surface of the nickel layer to wrap the nickel layer, wherein the thickness of the nickel layer is preferably 2-5 μm, and the thickness of the tin layer is preferably 3-10 μm.
In some preferred embodiments, the pore diameter of the channel pore is 50-1000 μm; the printing thicknesses of the common electrode, the reference electrode and the pressure sensing electrode are respectively and independently 1-5 mu m.
In some preferred embodiments, the paste for forming the temperature sensing electrode is printed with a metal paste having a TCR > 2000 ppm/DEG C, a sheet resistance > 20m omega/□, a sintering temperature > 1500 ℃, and a printing thickness of 5 to 20 μm.
In some preferred embodiments, the pastes for printing the common electrode, the reference electrode and the pressure sensing electrode are each independently made of metal powder that can withstand high-temperature sintering, such as Pt, Ag-Pt, Pd, Ag-Pd, W, Ni alloy, and the like. More preferably, the three are selected from the same material and the same thickness.
In some preferred embodiments, in the step B, the printing thickness of the second ceramic slurry is 20-100 μm; and C, printing the thickness of the slurry decomposable at the medium and low temperature in the step C to be 20-100 mu m, and finally sintering to form a cavity with the depth of 10-80 mu m.
In some preferred embodiments, the first ceramic slurry comprises the following components in parts by mass: 45-60% of main powder, 0.5-5% of sintering aid, 20-35% of casting organic solvent, 0.5-2% of dispersant and 5-15% of adhesive; wherein the main powder in the first ceramic slurry is Al2O3Powder, ZrO2One of powder or mixture of two kinds of powder, and sintering aid of ZnO, CaO, MgO, SiO2At least one of the organic solvent for casting is at least one of toluene, propyl acetate, isobutanol and ethanol, the grade of the dispersing agent is BYK-110, and the adhesive is acrylic resin, butyraldehyde resin and the like; mixing the components of the first ceramic slurry in proportion, adding zirconia balls as a medium, and continuously performing ball milling for 15-30 h to form casting slurry.
In some preferred embodiments, the second ceramicThe slurry comprises the following components in parts by mass: 55-75% of main powder, 0.5-6% of sintering aid, 8-20% of printing organic solvent, 1-5% of surfactant and 5-15% of adhesive; wherein the main powder in the second ceramic slurry is Al2O3Powder, ZrO2One of powder or mixture of two kinds of powder, and sintering aid of ZnO, CaO, MgO, SiO2At least one of terpineol, butyl carbitol and butyl carbitol acetate as an organic solvent for printing, at least one of lecithin and bis (3-trimethoxysilylpropyl) amine (trade name KH170) as a surfactant, and at least one of ethyl cellulose, acrylic resin and butyral resin as a binder; and mixing the components of the second ceramic slurry according to a ratio, adding zirconia balls as a medium, and continuously performing ball milling for 15-30 h to form the printing slurry. More preferably, the main powder of the first ceramic slurry and the main powder of the second ceramic slurry are made of the same material.
In some preferred embodiments, the slurry decomposable at the medium-low temperature comprises the following components in parts by mass: 60-80% of carbon powder, 8-20% of organic solvent, 5-15% of binder and 1-5% of surfactant; wherein the organic solvent is at least one of terpineol, butyl carbitol and butyl carbitol acetate, the binder is at least one of ethyl cellulose, acrylic resin and butyraldehyde resin, and the surfactant is at least one of lecithin and bis (3-trimethoxysilylpropyl) amine (trade name KH 170); mixing the components of the slurry which can be decomposed at medium and low temperature in proportion, adding zirconia balls as a medium, and continuously ball-milling for 15-30 h to form the printing slurry.
The present invention is illustrated in detail by the following more specific examples.
As shown in fig. 1 to 3, the example is a ceramic capacitive pressure and temperature sensor, and the sensor includes a ceramic bolerous thin sheet 1, a ceramic base 2, a conductive channel and a welding layer 11, a cavity 12 is formed between a middle region of a bottom surface of the ceramic bolerous thin sheet 1 and a middle region of a top surface of the ceramic base 2, and a thickness of the ceramic bolerous thin sheet 1 is smaller than that of the ceramic base 2; the bottom surface of the ceramic bolerous thin sheet corresponding to the cavity 12 is provided with a common electrode 3, the central area of the top surface of the ceramic base 2 corresponding to the cavity 12 is provided with a pressure sensing electrode 5 and a reference electrode 4, the reference electrode 4 is in an annular shape with an opening, is concentric with the pressure sensing electrode 5 and surrounds the outer surface of the pressure sensing electrode 5 to be spaced from the pressure sensing electrode (in the example, the spacing is 0.6 mm); the projection of the common electrode 3 on the top surface of the ceramic base corresponding to the cavity completely covers both the pressure-sensitive electrode 5 and the reference electrode 4; the periphery of the cavity on the top surface of the ceramic base 2 is also provided with a temperature sensing electrode 6, the temperature sensing electrode 6 is also in an annular shape with an opening and surrounds the periphery of the pressure sensing electrode 5, a conductive channel is arranged on the ceramic base 2 and consists of channel holes 13, 14, 15, 16 and 17 and conductive electrodes filling the channel holes 13, 14, 15, 16 and 17, the conductive channel comprises a first conductive channel 10 connected with the common electrode 3, a second conductive channel 8 connected with the pressure sensing electrode 5 and a third conductive channel 9 connected with the reference electrode 4, and the fourth conductive channel 7-1 and the fifth conductive channel 7-2 are connected with the temperature sensing electrodes, each conductive electrode penetrates through the bottom of the ceramic base to be provided with a leading-out end, each leading-out end is subjected to electroplating treatment to form a welding layer 11, and the ceramic bole sheet 1, the ceramic base 2 and each conductive channel are sintered to form an integrated structure.
The preparation method of the ceramic capacitance pressure and temperature sensor comprises the following steps:
(1) preparing a first ceramic slurry (slurry for casting): the first ceramic slurry comprises the following components in percentage by mass: main powder (Al)2O350% of powder), 5% of sintering aid (ZnO), 28% of organic solvent (ethanol), 2% of dispersant (BYK-110) and 15% of adhesive (acrylic resin), mixing the components in proportion, adding zirconia balls as a medium, and continuously performing ball milling for 30 hours to form casting slurry.
(2) Preparing a second ceramic paste (as a printing paste): the second ceramic slurry comprises the following components in percentage by mass: main powder (Al)2O3Powder) 75%, sintering aid (ZnO) 5%, organic solvent (terpineol) 8%, surfactant (KH170) 2% and adhesive (ethyl cellulose) 10%; mixing the components in proportion, adding zirconia balls as a mediumAnd ball milling is continued for 30h to form printing slurry.
(3) Preparation of a paste decomposable at medium and low temperatures (as a printing paste): the medium-low temperature in the slurry decomposable at the medium-low temperature is 200-1000 ℃, and comprises the following components in percentage by mass: 75% of carbon powder, 12% of organic solvent (terpineol), 10% of binder (ethyl cellulose) and 3% of surfactant (KH 170); mixing the components in proportion, adding zirconia balls as a medium, and continuously performing ball milling for 30 hours to form printing slurry.
(3) Casting: and (2) carrying out casting and drying on the first ceramic slurry prepared in the step (1), wherein the casting thickness after drying is 50 microns, and a plurality of raw belts are obtained through multiple manufacturing, wherein some raw belts are used as first raw belts for subsequent manufacturing of ceramic elastic sheets, and other raw belts are used as third raw belts for subsequent manufacturing of ceramic bases.
(4) Opening a hole: for each third green tape, the green tape is holed at the electrode leading-out position by adopting a mechanical or laser holing mode to form channel holes 13, 14, 15, 16 and 17, and the preferable hole diameter is as follows: 50 to 1000 μm, in this case, the diameter of the opening is 500 μm.
(5) Printing: and printing the common electrode 3 on the middle area of the surface of one of the first green tapes to obtain a second green tape, wherein the paste for printing the common electrode 3 is Pt paste, and the printing thickness is 4 mu m.
(6) Printing: printing a reference electrode 4 and a pressure sensing electrode 5 on the middle area of the surface of one third green tape, wherein the reference electrode 4 is in an annular shape with an opening, is concentric with the pressure sensing electrode 5 and is arranged outside the pressure sensing electrode 5 in a surrounding mode and is spaced from the pressure sensing electrode, and the spacing distance is 0.6 mm; and continuously printing a temperature sensing electrode 6 on the periphery of the pressure sensing electrode 5, wherein the pastes for printing the reference electrode 4 and the pressure sensing electrode 5 are both Pt paste, and the printing thicknesses are both 4 μm, in other examples, the materials of the common electrode 3, the reference electrode 4 and the pressure sensing electrode 5 can be different, and are preferably the same; the paste for printing the temperature sensing electrode 6 is metal paste (Ag-Pd paste is selected in the example) with the resistance Temperature Coefficient (TCR) > 2000 ppm/DEG C, the sheet resistance (resistivity of the paste) > 20m omega/□ and the sintering temperature > 1500 ℃, the printing thickness is 15 mu m, and the resistance value of the temperature sensing electrode is linearly changed along with the change of the peripheral temperature of the sensor. (in other examples, the temperature-sensitive electrode 6 may be printed separately on another third green sheet, not in the same layer as the reference electrode 4 and the pressure-sensitive electrode 5).
(7) Printing: on the green tape obtained in step (6), the second ceramic paste prepared in step (2) is printed according to the position area 18 (area filled with dots) shown in fig. 4 (i.e., the second ceramic paste is printed on the surface having the reference electrode, the pressure-sensitive electrode, and the temperature-sensitive electrode, except for the channel hole and the middle area (i.e., the central blank area except for the channel hole in fig. 4, where the reference electrode and the pressure-sensitive electrode are provided, and the middle area is subsequently used to form a cavity)), that is, the middle area and the channel hole, which are to be subsequently formed with a cavity, are avoided during printing, and the printing thickness is 25 μm.
(8) Printing: continuously printing the green tape formed in the step (7) by adopting the slurry decomposable at the medium-low temperature in the step (3), wherein the printing area is the middle area not covered by the second ceramic slurry in the step (7), the printing thickness is kept consistent with that in the step (7) and is 25 mu m, and a fourth green tape is obtained after the treatment in the steps (6) to (8);
(9) printing: printing conductive paste into corresponding channel holes of a third green tape and a fourth green tape with the channel holes, filling the channel holes with the conductive paste, and then drying, wherein after the conductive paste filled in the channel holes 13 and 14 is sintered to form a fourth conductive channel 7-1 and a fifth conductive channel 7-2, the two ends of the temperature sensing electrode 6 are correspondingly connected, after the conductive paste filled in the channel hole 15 is sintered to form a second conductive channel 8, the pressure sensing electrode 5 is correspondingly connected, after the conductive paste filled in the channel hole 16 is sintered to form a third conductive channel 9, the reference electrode 4 is correspondingly connected, and after the conductive paste filled in the channel hole 17 is sintered to form a conductive channel 10, the common electrode 3 is correspondingly connected; the conductive paste is preferably, but not limited to, a conductive silver paste made of metal powder capable of resisting high-temperature sintering, such as Pt, Ag-Pt, Pd, Ag-Pd, W, Ni alloy and the like, and in this case, the conductive silver paste is Pt paste.
(10) Laminating: and (3) laminating and pressing the obtained first green tape, second green tape, fourth green tape and third green tape into a blank according to the structural design sequence, wherein the laminating pressure is 35t, and the laminating temperature is as follows: at 60 ℃. The surface, provided with the common electrode, of the second green tape and the surface, printed with the slurry decomposable at medium and low temperatures, of the fourth green tape are closely attached to each other face to face, the first green tape and the second green tape are stacked and then used for forming the ceramic bolete sheet, and the third green tape and the fourth green tape are stacked and then used for forming the ceramic base.
(11) Warm water pressure: and (3) clamping the upper surface and the lower surface of the blank in the step (10) by using flat steel plates, placing the blank on a sealing bag for vacuumizing treatment, and carrying out isostatic pressing treatment at the water temperature of 70 ℃ and the pressure of 60 MPa.
(12) Cutting: and (3) cutting the green body processed in the step (11) according to the product size design to form an independent sensor green body, wherein the ceramic elastic sheet and the ceramic base can be one of square, round or oval.
(13) And (3) binder removal and sintering: and (3) carrying out glue discharging on the green body obtained in the step (12), and sintering in air or reducing atmosphere after glue discharging, wherein the sintering temperature is 1450 ℃. After sintering, the ceramic bolerous thin sheet, the ceramic base and the conductive channel form an integrated structure, the reference electrode, the pressure sensing electrode, the common electrode and the temperature sensing electrode form good direct contact with the conductive electrodes in the corresponding conductive channels, and a contact pin leading-out electrode is not needed in the subsequent use process.
(14) Electroplating: and (3) putting the sintered ceramic body obtained in the step (13) and media such as electroplating pellets into a basket, electroplating nickel at the leading-out end of each conductive electrode, electroplating tin on the surface of the nickel to wrap the nickel, wherein the thickness of the nickel layer is 3 microns, and the thickness of the tin layer is 6 microns, and forming a welding layer 11 for subsequent effective welding with an external circuit.
In the finally formed ceramic capacitive pressure and temperature sensor, the thickness of the ceramic elastic sheet is between 0.3mm and 1.2mm, and the thickness of the ceramic base is greater than that of the ceramic elastic sheet and is about 4-5 mm.
As shown in fig. 5-6, fig. 5 is a graph of the output relationship between the resistance R and the temperature T of the ceramic capacitor pressure and temperature sensor in this example, wherein the solid line represents the measured value and the dotted line represents the fitted linear curve, which shows that the temperature and the output resistance are linear, and the corresponding temperature can be determined by the output resistance; fig. 6 is a graph showing the relationship between the pressure of the ceramic capacitor and the pressure of the temperature sensor and the output of the capacitor in this example, and it can be seen that the capacitance changes linearly with the change in pressure.
The following table shows the sealing performance test results of the ceramic capacitor pressure sensor (the sealing material between the ceramic elastic sheet and the ceramic base is made of glass slurry and the internal electrode is led out in a pin inserting mode) manufactured by the prior art and the ceramic capacitor pressure and temperature sensor (the example is shown in the table) manufactured by the method of the application.
According to the preparation method, the raw belt is obtained by adopting a tape casting method, holes are formed in the raw belt by adopting a mechanical or laser mode, electrodes and cavities are formed by adopting a screen printing process, and the processes of laminating, sintering, electroplating and the like are adopted, so that the temperature and pressure testing function can be integrated in the ceramic core body, and the problems of low air tightness yield, poor reliability and the like of the conventional ceramic sensor can be effectively solved.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several equivalent substitutions or obvious modifications can be made without departing from the spirit of the invention, and all the properties or uses are considered to be within the scope of the invention.
Claims (10)
1. A ceramic sensor is characterized by comprising a ceramic bole thin sheet, a ceramic base and a conductive channel;
a cavity is formed between a middle region of the bottom surface of the ceramic elastic sheet and a middle region of the top surface of the ceramic base, and the thickness of the ceramic elastic sheet is smaller than that of the ceramic base;
the bottom surface of the ceramic bolerous thin sheet corresponding to the cavity is provided with a common electrode, the central area of the top surface of the ceramic base corresponding to the cavity is provided with a pressure sensing electrode and a reference electrode, and the reference electrode is annular and concentric with the pressure sensing electrode and surrounds the outside of the pressure sensing electrode to be spaced from the pressure sensing electrode; the projection of the common electrode on the top surface of the ceramic base corresponding to the cavity completely covers the pressure sensing electrode and the reference electrode;
the conductive channel is arranged on the ceramic base, consists of a channel hole and a conductive electrode filled in the channel hole, and comprises a first conductive channel connected with the common electrode, a second conductive channel connected with the pressure sensing electrode and a third conductive channel connected with the reference electrode, and each conductive electrode penetrates through the bottom of the ceramic base and is provided with a leading-out end;
the ceramic elastic sheet, the ceramic base and the conductive channel are sintered to form an integral structure.
2. The ceramic sensor of claim 1, wherein: the temperature sensing electrode is formed in the ceramic base, and the conductive channel further comprises a fourth conductive channel and a fifth conductive channel which are connected with the temperature sensing electrode.
3. The ceramic sensor of claim 1 or 2, wherein: the leading-out ends of the conductive electrodes are respectively provided with a welding layer after being electroplated.
4. The ceramic sensor of claim 1, wherein: the interval between the pressure sensing electrode and the reference electrode is 0.1 mm-0.8 mm.
5. A method of manufacturing a ceramic sensor according to claim 1, comprising the steps of:
(1) preparing a plurality of first green tapes, a second green tape, a plurality of third green tapes and a fourth green tape, and forming a channel hole of the conductive channel by opening a hole on each third green tape;
the plurality of first green belts and the plurality of third green belts are obtained by casting and drying first ceramic slurry, and the second green belt is obtained by printing the common electrode in the middle area of the surface of one of the first green belts;
wherein the forming of the fourth green tape comprises the steps of:
A. printing the reference electrode and the pressure-sensitive electrode on a central region of a surface of one of the third green tapes;
B. printing a second ceramic slurry on the surface of the green tape formed in the step A, wherein the reference electrode and the pressure sensing electrode are arranged on the surface of the green tape, and the positions of the green tape are except the channel hole and the middle area;
C. printing a slurry decomposable at a medium and low temperature on the middle area of the green tape formed in the step B to obtain a fourth green tape, wherein the printing thicknesses of the step B and the step C are the same;
(2) filling a conductive paste into each channel hole in each third green tape and each fourth green tape and drying;
(3) laminating the first green tape, the second green tape, the fourth green tape and the third green tape in sequence to form a green body, wherein one side of the second green tape, on which the common electrode is arranged, is adjacent to one side of the fourth green tape, on which the slurry decomposable at the medium and low temperature is printed, the first green tape and the second green tape are laminated to form the ceramic raw sheet, and the third green tape and the fourth green tape are laminated to form the ceramic base;
(4) carrying out isostatic pressing treatment on the green body formed in the step (3), and then cutting to form a sensor green body;
(5) and (4) carrying out gel discharging sintering on the sensor green body formed in the step (4), wherein in the gel discharging sintering process, all decomposable slurry at a medium and low temperature is firstly decomposed to form the cavity, then after sintering is continued, the conductive slurry is formed into a conductive electrode which is filled in the channel hole, the conductive electrode is provided with a leading-out end on the bottom surface of the ceramic base, and the ceramic paleoplastic sheet, the ceramic base and the conductive channel are in an integrated structure.
6. The method of claim 5, further comprising the step of forming a temperature sensing electrode: and printing a temperature sensing electrode on any one of the third green belts or the fourth green belt, and forming a conductive channel corresponding to the temperature sensing electrode on the ceramic base.
7. The production method according to claim 5 or 6, further comprising the step (6): and (5) respectively electroplating the leading-out ends of the conductive electrodes in the step (5) to form welding layers.
8. The method of claim 6, wherein the paste for printing the temperature sensing electrode is a metal paste having a TCR of more than 2000 ppm/c, a sheet resistance of more than 20m Ω/□, a sintering temperature of more than 1500 c, and a printing thickness of 5 to 20 μm.
9. The method according to claim 5, wherein the pore diameter of the channel pore is 50 to 1000 μm; the printing thicknesses of the common electrode, the reference electrode and the pressure sensing electrode are respectively and independently 1-5 mu m; in the step B, the printing thickness of the second ceramic slurry is 20-100 mu m; and the printing thickness of the slurry decomposable at the medium and low temperature in the step C is 20-100 mu m.
10. The method according to claim 5,
the first ceramic slurry comprises the following components in percentage by mass: 45-60% of main powder, 0.5-5% of sintering aid, 20-35% of casting organic solvent, 0.5-2% of dispersant and 5-15% of adhesive;
the second ceramic slurry comprises the following components in percentage by mass: 55-75% of main powder, 0.5-6% of sintering aid, 8-20% of organic solvent for printing, 1-5% of surfactant and 5-15% of adhesive;
the slurry decomposable at the medium and low temperature comprises the following components in parts by mass: 60-80% of carbon powder, 8-20% of organic solvent, 5-15% of binder and 1-5% of surfactant.
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