CN110865100A - Sheet-type structure integrated catalytic combustion type combustible gas sensor and preparation method thereof - Google Patents
Sheet-type structure integrated catalytic combustion type combustible gas sensor and preparation method thereof Download PDFInfo
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- CN110865100A CN110865100A CN201911313087.7A CN201911313087A CN110865100A CN 110865100 A CN110865100 A CN 110865100A CN 201911313087 A CN201911313087 A CN 201911313087A CN 110865100 A CN110865100 A CN 110865100A
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
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Abstract
The invention discloses a piece-structure integrated catalytic combustion type combustible gas sensor and a preparation method thereof, belongs to the technical field of sensors, and aims to solve the problems that the existing catalytic combustion type combustible gas sensor is complex in manufacturing process of a detection element and a compensation element, low in heat transfer efficiency and large in power consumption, and the size of the sensor is large and the packaging form is complex due to the separated detection element and the separated compensation element. The combustible gas sensor comprises two layers of ceramic chip substrates, wherein a signal transmission layer is arranged on the lower ceramic chip substrate, and four lead bonding pads, two signal transmission bonding pads and two resistance adjusting regions are arranged on the lower surface of the lower ceramic chip substrate; the upper surface is provided with four upper surface pads. The lower surface of the upper ceramic wafer substrate is provided with a resistance sensing layer which comprises two sensing resistors, the upper surface of the upper ceramic wafer substrate is provided with a catalytic combustion layer which comprises two catalytic units, and the two catalytic units respectively form a detection element and a compensation element. The detection of different combustible gases can be realized by changing the type of the catalyst. The invention is used for detecting and early warning combustible gas.
Description
Technical Field
The invention relates to a chip structure integrated catalytic combustion type combustible gas sensor and a preparation method thereof, belonging to the technical field of sensors.
Background
Combustible gas in the environment mainly comprises hydrogen, methane, propane, ethanol, acetylene, organic compounds and the like, when the combustible gas in the air is accumulated to a certain concentration, safety accidents such as combustion, explosion and the like are very easy to happen, so that great losses are caused to human health and public property, and especially the safety accidents are very easy to cause in the environments such as underground gas transmission pipe networks, coal mines, gas transmission stations and the like. In 2017, the natural gas pipeline in Guizhou sand town is combusted and exploded, so that a plurality of people are injured and killed; in 2019, a large gas explosion accident happens to Anhui Luling coal mines, which causes a plurality of miners to be in distress. Therefore, the concentration of the combustible gas needs to be monitored in real time in key places during the production, transportation and use processes of the combustible gas, and early warning is timely performed on places where accidents are likely to be induced, so that safety accidents are avoided. Therefore, a reliable combustible gas alarm or monitoring device is needed, and a combustible gas sensor in a combustible gas detection device becomes an industry standard tool with a huge use amount.
The combustible gas sensor can be divided into an electrochemical sensor, an optical sensor and a catalytic combustion sensor according to the principle, and compared with the electrochemical sensor and the optical sensor, the combustible gas sensor adopting the catalytic combustion principle has the advantages of sensitive reaction, simple structure, low circuit design difficulty, reliable use, low price, long service life and the like, is widely used for combustible gas early warning in the detection and monitoring industrial fields, and is known as an 'indiscriminate sensor'.
The catalytic combustion type combustible gas sensor utilizes the thermal effect principle of catalytic combustion, a measuring bridge is formed by pairing a detection element and a compensation element, under the condition of a certain temperature, combustible gas and oxygen are subjected to flameless combustion under the action of a catalyst on the surface of a carrier of the detection element, the temperature of the carrier is increased, the resistance value of a platinum wire resistor in the detection element is increased, so that the balance bridge is out of balance, an electric signal in direct proportion to the concentration of the combustible gas is output, and the concentration of the combustible gas is measured by measuring the resistance change of the platinum wire.
At present, the related technical products are introduced by science and technology companies such as FIGARO, NEMOTO, Henan Wei Sheng and the like in Japan and are used for detecting the concentration of combustible gas in the fields of industrial environment, gas transmission pipelines and the like, a detection element and a compensation element of a designed combustible gas sensor are separated from each other, and the detection element and the compensation element are designed and manufactured by adopting the traditional process and consist of a platinum wire wound coil and a catalyst carrier bead. Due to the design of a discrete structure, the sensor is large in size and complex in packaging; the detection element and the compensation element designed by the traditional process cause the complexity of the element manufacturing process, the low heat transfer efficiency causes the large power consumption and the reduction of indexes such as sensitivity, response speed and the like. The traditional manufacturing process is difficult to realize the miniaturization and low-power consumption manufacturing of the sensor, and limits the further development of the field of the catalytic combustion combustible gas sensor.
Disclosure of Invention
The invention aims to solve the problems that the existing catalytic combustion type combustible gas sensor is complex in manufacturing process, low in heat transfer efficiency and large in power consumption, and the sensor is large in size and complex in packaging form due to the fact that the detection element and the compensation element are separated, and provides a chip structure integrated catalytic combustion type combustible gas sensor.
The invention relates to a chip structure integrated catalytic combustion type combustible gas sensor, which comprises two layers of ceramic chip substrates, wherein a signal transmission layer is arranged on the lower ceramic chip substrate, a resistance value sensing layer is arranged on the lower surface of the upper ceramic chip substrate, and a catalytic combustion layer is arranged on the upper surface of the upper ceramic chip substrate;
the signal transmission layer comprises four lead bonding pads, two signal transmission bonding pads, four upper surface bonding pads and two resistance adjusting regions; the four lead bonding pads and the two signal transmission bonding pads are arranged on the lower surface of the lower ceramic chip substrate, and the four lead bonding pads are respectively a first lead bonding pad, a second lead bonding pad, a third lead bonding pad and a fourth lead bonding pad; a first signal transmission bonding pad is arranged between the first lead bonding pad and the second lead bonding pad, and a second signal transmission bonding pad is arranged between the third lead bonding pad and the fourth lead bonding pad;
the four upper surface bonding pads are arranged on the upper surface of the lower layer ceramic wafer substrate and are respectively a first upper surface bonding pad, a second upper surface bonding pad, a third upper surface bonding pad and a fourth upper surface bonding pad; the first upper surface bonding pad, the second upper surface bonding pad, the third upper surface bonding pad and the fourth upper surface bonding pad are respectively in mirror symmetry with the first signal transmission bonding pad, the second lead bonding pad, the second signal transmission bonding pad and the fourth lead bonding pad; the first upper surface bonding pad is communicated with the first signal transmission bonding pad through a first through hole penetrating through the lower ceramic wafer substrate; the second upper surface bonding pad and the second lead bonding pad are communicated through a second through hole penetrating through the lower ceramic wafer substrate; the third upper surface bonding pad and the second signal transmission bonding pad are communicated through a third through hole penetrating through the lower ceramic wafer substrate; the fourth upper surface bonding pad and the fourth lead bonding pad are communicated through a fourth through hole penetrating through the lower ceramic wafer substrate;
the lower surface of the lower ceramic wafer substrate is also provided with two resistance adjusting areas which are a first resistance adjusting area and a second resistance adjusting area respectively; the first resistance adjusting area is positioned between the first lead bonding pad and the first signal transmission bonding pad and is in contact communication with the first lead bonding pad and the first signal transmission bonding pad; the second resistance adjusting area is positioned between the second lead bonding pad and the second signal transmission bonding pad and is in contact communication with the second lead bonding pad and the second signal transmission bonding pad;
the resistance sensing layer comprises a first sensing resistor and a second sensing resistor; two ends of the first sensing resistor are respectively communicated with the first upper surface bonding pad and the second upper surface bonding pad, and two ends of the second sensing resistor are respectively communicated with the third upper surface bonding pad and the fourth upper surface bonding pad;
the catalytic combustion layer includes a first catalytic unit and a second catalytic unit; the first catalytic unit is positioned right above the first sensing resistor and comprises a catalyst carrier and a catalyst arranged on the catalyst carrier; the second catalytic unit is positioned right above the second sensing resistor and comprises a catalyst carrier.
Preferably, the signal transmission layer further includes four leads, which are a first lead, a second lead, a third lead and a fourth lead, respectively; the first lead, the second lead, the third lead and the fourth lead are respectively connected with the first lead bonding pad, the second lead bonding pad, the third lead bonding pad and the fourth lead bonding pad;
the first lead, the second lead, the third lead and the fourth lead are all made of Pt wires or alloy wires.
Preferably, the first resistance trimming region and the second resistance trimming region are both rectangular, the first resistance trimming region is provided with a long opening at one side communicated with the first lead bonding pad and the first signal transmission bonding pad, and the second resistance trimming region is provided with a long opening at one side communicated with the second lead bonding pad and the second signal transmission bonding pad;
the error of the resistance values of the first resistance adjusting area and the second resistance adjusting area is less than or equal to 0.1 omega;
the first resistance regulating area and the second resistance regulating area are made of Pt metal materials.
Preferably, the first sensing resistor and the second sensing resistor are annular or serpentine, the resistance values are adjusted through the length and the thickness, and the resistance value range is 10 omega-100 omega;
the first sensing resistor and the second sensing resistor are made of Pt metal materials.
Preferably, the first catalytic unit and the second catalytic unit of the catalytic combustion layer are both of a circular structure, and a circular thermal isolation suspension bridge is arranged outside the circular structure;
catalyst carriers of the first catalytic unit and the second catalytic unit are porous alumina ceramics, and the thickness of the catalyst carriers is 5-20 micrometers;
the catalyst of the first catalytic unit is formed by single-component or multi-component composition of Pt, Pd and Au.
Preferably, the first through hole, the second through hole, the third through hole and the fourth through hole are all filled with a Pt metal material.
Preferably, the four lead pads, the two signal transmission pads and the four upper surface pads are all made of Pt metal material.
The invention relates to a preparation method of a piece-structure integrated catalytic combustion type combustible gas sensor, which comprises the following specific processes:
s1, manufacturing a first through hole, a second through hole, a third through hole and a fourth through hole on the lower-layer ceramic wafer substrate by adopting a punching technology;
printing and filling Pt metal materials in the first through hole, the second through hole, the third through hole and the fourth through hole by a screen printing method;
printing four lead bonding pads, two signal transmission bonding pads and two resistance adjusting regions on the lower surface of the lower ceramic wafer substrate by using a silk-screen printing method and using a Pt metal material, and printing four upper surface bonding pads on the lower surface of the lower ceramic wafer substrate;
printing a first sensing resistor and a second sensing resistor on the lower surface of the upper ceramic chip substrate by using a Pt metal material by adopting a screen printing method;
printing catalyst carriers of a first catalytic unit and a second catalytic unit on the upper surface of the upper ceramic wafer substrate by using porous alumina ceramics by adopting a screen printing method;
s2, aligning and laminating the lower ceramic wafer substrate and the upper ceramic wafer substrate, and combining the two ceramic wafer substrates into an integral structure by adopting an isostatic pressing technology;
s3, obtaining an integral structure of the S2, and integrally forming by adopting a sintering technology;
s4, processing two resistance adjusting areas of the signal transmission layer by adopting a laser resistance adjusting technology, wherein the error of the resistance value is adjusted to be less than or equal to 0.1 omega;
s5, preparing a thermal isolation suspension bridge on the catalyst carriers of the first catalytic unit and the second catalytic unit by adopting a laser etching technology;
s6, respectively welding four leads on the four lead bonding pads by adopting a lead welding technology;
s7, coating glass slurry on the four lead pads and the two resistance adjusting areas by adopting a dispensing technology;
s8, sintering and molding the sample obtained in the S7 by adopting a sintering technology;
s9, dropping the solution of ions used by the catalyst onto the catalyst carrier of the first catalytic unit by adopting an impregnation technology, and drying and sintering to form a detection element on the first catalytic unit and a compensation element on the second catalytic unit;
and S10, separating the sensor core body containing the detection element and the compensation element by adopting a scribing technology to obtain the integrated catalytic combustion type combustible gas sensor.
Preferably, the ion solution used by the catalyst is dropped onto the catalyst carrier of the first catalytic unit by the dipping technique as described in S9, and the concentration and dropping volume of the solution are controlled by wetting the catalytic ion aqueous solution, so as to control the loading amount of the catalyst.
Preferably, the drying and sintering process of S9 is as follows:
drying the sample dropped with the catalyst at the temperature of 80-120 ℃, wherein the drying time is more than or equal to 9 h;
then calcining the dried sample, wherein the calcining temperature is controlled to be 500-900 ℃ according to the type of the catalyst, and the calcining time is 2-5 h.
The invention has the advantages that: the sheet-type structure integrated catalytic combustion type combustible gas sensor provided by the invention has a sheet-type structure, is small in size and simple in structure, the thin catalytic combustion layer increases the heat conduction efficiency, the power consumption of the sensor is effectively reduced, the catalytic combustion rate of combustible gas is improved, the performance indexes such as the sensitivity, the response speed and the like of the sensor are obviously improved, the reliability of a product is obviously enhanced by sintering and molding the catalyst carrier by adopting a porous ceramic material, and the detection of different types of combustible gas can be realized by changing the types of the catalyst. The combustible gas sensor is designed and manufactured based on HTCC technology, the manufacturing process is mature and controllable, the mass production of the sensor is easy to realize, and the miniaturization and integration design and manufacturing of the sensor are easy to realize.
Drawings
FIG. 1 is a schematic structural diagram of a combustible gas sensor with an integrated catalytic combustion type chip structure according to the invention;
FIG. 2 is a schematic structural view of the upper surface of an upper ceramic wafer substrate according to the present invention;
FIG. 3 is a schematic structural diagram of the lower surface of the upper ceramic wafer substrate according to the present invention;
FIG. 4 is a schematic structural view of a catalytic combustion layer according to the present invention;
FIG. 5 is a schematic diagram of the two trimming areas according to the present invention after trimming;
FIG. 6 is an SEM image of porous alumina ceramics used as catalyst carriers of two catalytic units according to the present invention;
FIG. 7 is a test curve diagram of a Pd catalyst methane combustible gas sensor adopting the sheet structure integrated catalytic combustion combustible gas sensor of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
The first embodiment is as follows: the following description of the present embodiment is made with reference to fig. 1 to 5, and the sensor of the present embodiment includes two ceramic wafer substrates, a signal transmission layer 1 is disposed on the lower ceramic wafer substrate, a resistance sensing layer 2 is disposed on the lower surface of the upper ceramic wafer substrate, and a catalytic combustion layer 3 is disposed on the upper surface of the upper ceramic wafer substrate;
the signal transmission layer 1 comprises four lead bonding pads, two signal transmission bonding pads, four upper surface bonding pads and two resistance adjusting regions; four lead bonding pads and two signal transmission bonding pads are arranged on the lower surface of the lower ceramic chip substrate, and the four lead bonding pads are a first lead bonding pad 1-1, a second lead bonding pad 1-2, a third lead bonding pad 1-3 and a fourth lead bonding pad 1-4 respectively; a first signal transmission bonding pad 1-5 is arranged between the first lead bonding pad 1-1 and the second lead bonding pad 1-2, and a second signal transmission bonding pad 1-6 is arranged between the third lead bonding pad 1-3 and the fourth lead bonding pad 1-4;
the four upper surface bonding pads are arranged on the upper surface of the lower layer ceramic wafer substrate and are respectively a first upper surface bonding pad 1-7, a second upper surface bonding pad 1-8, a third upper surface bonding pad 1-9 and a fourth upper surface bonding pad 1-10; the first upper surface bonding pad 1-7, the second upper surface bonding pad 1-8, the third upper surface bonding pad 1-9 and the fourth upper surface bonding pad 1-10 are respectively mirror-symmetrical to the first signal transmission bonding pad 1-5, the second lead bonding pad 1-2, the second signal transmission bonding pad 1-6 and the fourth lead bonding pad 1-4; the first upper surface bonding pads 1-7 are communicated with the first signal transmission bonding pads 1-5 through first through holes 1-13 penetrating through the lower ceramic chip substrate; the second upper surface bonding pad 1-8 and the second lead bonding pad 1-2 are communicated through a second through hole 1-14 penetrating through the lower ceramic chip substrate; the third upper surface bonding pads 1-9 and the second signal transmission bonding pads 1-6 are communicated through third through holes 1-15 penetrating through the lower ceramic chip substrate; the fourth upper surface bonding pad 1-10 and the fourth lead bonding pad 1-4 are communicated through a fourth through hole 1-16 penetrating through the lower ceramic chip substrate;
the lower surface of the lower ceramic wafer substrate is also provided with two resistance adjusting areas, namely a first resistance adjusting area 1-11 and a second resistance adjusting area 1-12; the first resistance trimming area 1-11 is positioned between the first lead bonding pad 1-1 and the first signal transmission bonding pad 1-5 and is in contact communication with the first lead bonding pad 1-1 and the first signal transmission bonding pad 1-5; the second resistance trimming area 1-12 is positioned between the second lead bonding pad 1-2 and the second signal transmission bonding pad 1-6 and is in contact communication with the second lead bonding pad 1-2 and the second signal transmission bonding pad 1-6;
the resistance sensing layer 2 comprises a first sensing resistor 2-1 and a second sensing resistor 2-2; two ends of the first sensing resistor 2-1 are respectively communicated with the first upper surface bonding pads 1-7 and the second upper surface bonding pads 1-8, and two ends of the second sensing resistor 2-2 are respectively communicated with the third upper surface bonding pads 1-9 and the fourth upper surface bonding pads 1-10;
the catalytic combustion layer 3 includes a first catalytic unit 3-1 and a second catalytic unit 3-2; the first catalytic unit 3-1 is positioned right above the first sensing resistor 2-1 and comprises a catalyst carrier and a catalyst arranged on the catalyst carrier; the second catalytic unit 3-2 is located right above the second sensing resistor 2-2 and includes a catalyst carrier.
In the embodiment, the first sensing resistor 2-1 is used for sensing the change of the resistance of the first sensing resistor 2-1 caused by the combustion of the combustible gas in the first catalytic unit 3-1 when the first catalytic unit 3-1 is heated to the working temperature; the second sensing resistor 2-2 is used for heating the second catalytic unit 3-2 to the working temperature; the first catalytic unit 3-1 serves as a detection element and the second sensing resistor 2-2 serves as a compensation element.
Further, the signal transmission layer 1 further includes four leads, which are respectively a first lead 1-17, a second lead 1-18, a third lead 1-19 and a fourth lead 1-20; the first lead 1-17, the second lead 1-18, the third lead 1-19 and the fourth lead 1-20 are respectively connected with the first lead pad 1-1, the second lead pad 1-2, the third lead pad 1-3 and the fourth lead pad 1-4;
the first leads 1-17, the second leads 1-18, the third leads 1-19 and the fourth leads 1-20 are all made of Pt wires or alloy wires.
Furthermore, the first resistance adjusting region 1-11 and the second resistance adjusting region 1-12 are both rectangular, a long opening is formed in one side, communicated with the first lead bonding pad 1-1 and the first signal transmission bonding pad 1-5, of the first resistance adjusting region 1-11, and a long opening is formed in one side, communicated with the second lead bonding pad 1-2 and the second signal transmission bonding pad 1-6, of the second resistance adjusting region 1-12;
the error of the resistance values of the first resistance adjusting area 1-11 and the second resistance adjusting area 1-12 is less than or equal to 0.1 omega;
the first resistance regulating area 1-11 and the second resistance regulating area 1-12 are made of Pt metal materials.
In this embodiment, the first resistance adjusting region 1-11 is opened to adjust resistance on the side communicating with the first lead pad 1-1 and the first signal transmission pad 1-5, and the second resistance adjusting region 1-12 is opened to adjust resistance on the side communicating with the second lead pad 1-2 and the second signal transmission pad 1-6.
Furthermore, the first sensing resistor 2-1 and the second sensing resistor 2-2 are annular or serpentine, and the resistance values are adjusted through the length and the thickness and range from 10 omega to 100 omega;
the first sensing resistor 2-1 and the second sensing resistor 2-2 are made of Pt metal materials.
Furthermore, the first catalytic unit 3-1 and the second catalytic unit 3-2 of the catalytic combustion layer 3 are both circular structures, and the outer sides of the circular structures are provided with circular thermal isolation suspension bridges 3-3;
catalyst carriers of the first catalytic unit 3-1 and the second catalytic unit 3-2 are porous alumina ceramics, and the thickness of the catalyst carriers is 5-20 micrometers;
the catalyst of the first catalytic unit 3-1 is formed by single-component or multi-component composition of Pt, Pd and Au.
In this embodiment, the thermal isolation suspension bridge 3-3 can prevent thermal interference between the first catalytic unit 3-1 and the second catalytic unit 3-2.
In this embodiment, the catalyst of the first catalytic unit 3-1 is a Pt, Pd, Au single component or multi-component composite composition, and selective catalytic combustion of combustible gas can be realized by controlling the composition of the catalyst, so as to realize selective detection of different combustible gases.
In the embodiment, the thickness of the catalyst carrier of the first catalytic unit 3-1 and the second catalytic unit 3-2 is 5-20 μm, the catalytic combustion efficiency and the heat conduction efficiency of the combustible gas are improved by controlling the thickness of the catalyst carrier, and the sensitivity and the response rate of the sensor are improved.
Further, Pt metal materials are filled in the first through holes 1-13, the second through holes 1-14, the third through holes 1-15 and the fourth through holes 1-16.
Furthermore, the four lead bonding pads, the two signal transmission bonding pads and the four upper surface bonding pads are all made of Pt metal materials.
The second embodiment is as follows: the following describes the present embodiment with reference to fig. 1 to 5, and the preparation method of the sheet-type structure integrated catalytic combustion combustible gas sensor according to the present embodiment is implemented based on the sheet-type structure integrated catalytic combustion combustible gas sensor, and the specific process of the preparation method is as follows:
s1, manufacturing a first through hole 1-13, a second through hole 1-14, a third through hole 1-15 and a fourth through hole 1-16 on a lower-layer ceramic sheet substrate by adopting a punching technology;
printing and filling Pt metal materials in the first through holes 1-13, the second through holes 1-14, the third through holes 1-15 and the fourth through holes 1-16 by adopting a screen printing method;
printing four lead bonding pads, two signal transmission bonding pads and two resistance adjusting regions on the lower surface of the lower ceramic wafer substrate by using a silk-screen printing method and using a Pt metal material, and printing four upper surface bonding pads on the lower surface of the lower ceramic wafer substrate;
printing a first sensing resistor 2-1 and a second sensing resistor 2-2 on the lower surface of the upper ceramic chip substrate by using a Pt metal material by adopting a screen printing method;
printing catalyst carriers of a first catalytic unit 3-1 and a second catalytic unit 3-2 on the upper surface of the upper ceramic chip substrate by using porous alumina ceramics by adopting a screen printing method;
s2, aligning and laminating the lower ceramic wafer substrate and the upper ceramic wafer substrate, and combining the two ceramic wafer substrates into an integral structure by adopting an isostatic pressing technology;
s3, obtaining an integral structure of the S2, and integrally forming by adopting a sintering technology;
s4, processing the two resistance adjusting areas of the signal transmission layer 1 by adopting a laser resistance adjusting technology, wherein the error of the resistance value is adjusted to be less than or equal to 0.1 omega;
s5, preparing a thermal isolation suspension bridge 3-3 on the catalyst carriers of the first catalytic unit 3-1 and the second catalytic unit 3-2 by adopting a laser etching technology;
s6, respectively welding four leads on the four lead bonding pads by adopting a lead welding technology;
s7, coating glass slurry on the four lead pads and the two resistance adjusting areas by adopting a dispensing technology;
s8, sintering and molding the sample obtained in the S7 by adopting a sintering technology;
s9, dropping a solution of ions used by the catalyst onto the catalyst carrier of the first catalytic unit 3-1 by adopting an impregnation technology, and drying and sintering to form a detection element on the first catalytic unit 3-1 and a compensation element on the second catalytic unit 3-2;
and S10, separating the sensor core body containing the detection element and the compensation element by adopting a scribing technology to obtain the integrated catalytic combustion type combustible gas sensor.
In the embodiment, a first lead 1-17 and a second lead 1-18 are respectively connected with a first lead bonding pad 1-1 and a second lead bonding pad 1-2, and a second upper surface bonding pad 1-8 is communicated with the second lead bonding pad 1-2 through a second through hole 1-14 penetrating through a lower ceramic chip substrate; the first resistance trimming area 1-11 is positioned between the first lead bonding pad 1-1 and the first signal transmission bonding pad 1-5 and is in contact communication with the first lead bonding pad 1-1 and the first signal transmission bonding pad 1-5; the first upper surface bonding pads 1-7 are communicated with the first signal transmission bonding pads 1-5 through first through holes 1-13 penetrating through the lower ceramic chip substrate; two ends of the first sensing resistor 2-1 are respectively communicated with the first upper surface bonding pad 1-7 and the second upper surface bonding pad 1-8; the first catalytic unit 3-1 is positioned right above the first sensing resistor 2-1; thus, the first lead 1-17 and the second lead 1-18 are used for sensing element signal transmission. While the third lead 1-19 and the fourth lead 1-20 are used for compensating element signal transmission.
Further, in S9, an ion solution used by the catalyst is dropped onto the catalyst carrier of the first catalytic unit 3-1 by using an impregnation technique, and the concentration and dropping volume of the solution are controlled by wetting the catalytic ion aqueous solution, so that the loading capacity of the catalyst can be controlled.
Still further, the specific process of drying and sintering in S9 is as follows:
drying the sample dropped with the catalyst at the temperature of 80-120 ℃, wherein the drying time is more than or equal to 9 h;
then calcining the dried sample, wherein the calcining temperature is controlled to be 500-900 ℃ according to the type of the catalyst, and the calcining time is 2-5 h.
As shown in fig. 6, in a test curve of the methane combustible gas sensor using the Pd catalyst, the catalyst carrier exhibits excellent porosity, which is beneficial for the catalyst to be soaked and adsorbed on the carrier material, and is beneficial for the combustible gas to perform catalytic combustion reaction on the catalyst, thereby increasing the corresponding speed of the sensor. The Pd-loaded detection unit is subjected to methane gas performance test, the test curve chart is shown in FIG. 7, the catalytic activity is higher at the working temperature of 500 ℃, and the highest conversion rate of methane reaches 95.9%. The sensor exhibits excellent detection performance for methane gas.
The High-Temperature Co-fired ceramic (HTCC) technology is an integrated assembly technology developed in recent years, mainly comprises the technical processes of punching, screen printing, lamination and the like, the HTCC technology is developed through the technical processes of many years, the technical process is mature, and because the HTCC technology is easy to realize multilayer wiring and an integrated structure, the product miniaturization and integrated design can be realized, the HTCC technology is widely applied to sensor manufacturing, and a new development direction is provided for the development of a new-generation combustible gas sensor. The invention adopts HTCC technology to complete the design and manufacture of the catalytic combustion type combustible gas sensor, the product is of an integrated structure, the size is small, the structure is simple, the heat transfer efficiency is increased, the power consumption of the sensor is effectively reduced, the performance indexes such as sensitivity, response speed and the like are obviously improved, the reliability of the product is obviously enhanced, the manufacturing process is mature and controllable, and the mass production of the sensor can be realized.
The method is based on HTCC technology, mainly comprises the technical processes of punching, screen printing, laminating, isostatic pressing and the like, is mature in technology, and can realize the mass production of the sensors. The sensor is designed by the integrated structure of the detection element and the compensation element, so that the sensor has small size and simple structure. The heat conduction efficiency of the detection element is effectively improved by controlling the thickness of the catalyst carrier, the power consumption of the sensor is reduced, the performance indexes such as sensitivity and response speed are obviously improved, and the use reliability of the product is obviously enhanced. The method can realize the selective detection of different combustible gases by optimizing the components and the compositions of the catalyst, and the product designed and developed by the method has the advantages of low cost, long service life and the like, and can be widely applied to the detection and early warning of the concentration of the combustible gas in production environments such as underground gas transmission pipe networks, coal mines, gas transmission stations and the like.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. It should be understood that features described in different dependent claims and herein may be combined in ways different from those described in the original claims. It is also to be understood that features described in connection with individual embodiments may be used in other described embodiments.
Claims (10)
1. The integrated catalytic combustion type combustible gas sensor with the chip structure is characterized by comprising two layers of ceramic chip substrates, wherein a signal transmission layer (1) is arranged on the lower ceramic chip substrate, a resistance value sensing layer (2) is arranged on the lower surface of the upper ceramic chip substrate, and a catalytic combustion layer (3) is arranged on the upper surface of the upper ceramic chip substrate;
the signal transmission layer (1) comprises four lead bonding pads, two signal transmission bonding pads, four upper surface bonding pads and two resistance adjusting regions; four lead bonding pads and two signal transmission bonding pads are arranged on the lower surface of the lower ceramic chip substrate, and the four lead bonding pads are a first lead bonding pad (1-1), a second lead bonding pad (1-2), a third lead bonding pad (1-3) and a fourth lead bonding pad (1-4) respectively; a first signal transmission bonding pad (1-5) is arranged between the first lead bonding pad (1-1) and the second lead bonding pad (1-2), and a second signal transmission bonding pad (1-6) is arranged between the third lead bonding pad (1-3) and the fourth lead bonding pad (1-4);
the four upper surface bonding pads are arranged on the upper surface of the lower layer ceramic chip substrate and are respectively a first upper surface bonding pad (1-7), a second upper surface bonding pad (1-8), a third upper surface bonding pad (1-9) and a fourth upper surface bonding pad (1-10); the first upper surface bonding pad (1-7), the second upper surface bonding pad (1-8), the third upper surface bonding pad (1-9) and the fourth upper surface bonding pad (1-10) are respectively in mirror symmetry with the first signal transmission bonding pad (1-5), the second lead bonding pad (1-2), the second signal transmission bonding pad (1-6) and the fourth lead bonding pad (1-4); the first upper surface bonding pads (1-7) are communicated with the first signal transmission bonding pads (1-5) through first through holes (1-13) penetrating through the lower ceramic chip substrate; the second upper surface bonding pad (1-8) is communicated with the second lead bonding pad (1-2) through a second through hole (1-14) penetrating through the lower ceramic chip substrate; the third upper surface bonding pads (1-9) are communicated with the second signal transmission bonding pads (1-6) through third through holes (1-15) penetrating through the lower ceramic chip substrate; the fourth upper surface bonding pad (1-10) is communicated with the fourth lead bonding pad (1-4) through a fourth through hole (1-16) penetrating through the lower ceramic chip substrate;
the lower surface of the lower ceramic wafer substrate is also provided with two resistance adjusting areas which are respectively a first resistance adjusting area (1-11) and a second resistance adjusting area (1-12); the first resistance trimming area (1-11) is positioned between the first lead bonding pad (1-1) and the first signal transmission bonding pad (1-5) and is in contact communication with the first lead bonding pad (1-1) and the first signal transmission bonding pad (1-5); the second resistance trimming area (1-12) is positioned between the second lead bonding pad (1-2) and the second signal transmission bonding pad (1-6) and is in contact communication with the second lead bonding pad (1-2) and the second signal transmission bonding pad (1-6);
the resistance sensing layer (2) comprises a first sensing resistor (2-1) and a second sensing resistor (2-2); two ends of the first sensing resistor (2-1) are respectively communicated with the first upper surface bonding pads (1-7) and the second upper surface bonding pads (1-8), and two ends of the second sensing resistor (2-2) are respectively communicated with the third upper surface bonding pads (1-9) and the fourth upper surface bonding pads (1-10);
the catalytic combustion layer (3) comprises a first catalytic unit (3-1) and a second catalytic unit (3-2); the first catalytic unit (3-1) is positioned right above the first sensing resistor (2-1) and comprises a catalyst carrier and a catalyst arranged on the catalyst carrier; the second catalytic unit (3-2) is positioned right above the second sensing resistor (2-2) and comprises a catalyst carrier.
2. The sheet structure integrated catalytic combustion type combustible gas sensor according to claim 1, wherein the signal transmission layer (1) further comprises four leads, a first lead (1-17), a second lead (1-18), a third lead (1-19) and a fourth lead (1-20); the first lead (1-17), the second lead (1-18), the third lead (1-19) and the fourth lead (1-20) are respectively connected with the first lead bonding pad (1-1), the second lead bonding pad (1-2), the third lead bonding pad (1-3) and the fourth lead bonding pad (1-4);
the first leads (1-17), the second leads (1-18), the third leads (1-19) and the fourth leads (1-20) are all made of Pt wires or alloy wires.
3. The chip structure integrated catalytic combustion type combustible gas sensor according to claim 2, wherein the first resistance trimming region (1-11) and the second resistance trimming region (1-12) are rectangular, the first resistance trimming region (1-11) is provided with a long opening at the side communicated with the first lead bonding pad (1-1) and the first signal transmission bonding pad (1-5), and the second resistance trimming region (1-12) is provided with a long opening at the side communicated with the second lead bonding pad (1-2) and the second signal transmission bonding pad (1-6);
the error of the resistance values of the first resistance trimming area (1-11) and the second resistance trimming area (1-12) is less than or equal to 0.1 omega;
the first resistance regulating area (1-11) and the second resistance regulating area (1-12) are made of Pt metal materials.
4. The chip structure integrated catalytic combustion type combustible gas sensor according to claim 3, wherein the first sensing resistor (2-1) and the second sensing resistor (2-2) are annular or serpentine, and the resistance value is adjusted by the length and the thickness and ranges from 10 Ω to 100 Ω;
the first sensing resistor (2-1) and the second sensing resistor (2-2) are made of Pt metal materials.
5. The sheet-type structure integrated catalytic combustion combustible gas sensor according to claim 4, wherein the first catalytic unit (3-1) and the second catalytic unit (3-2) of the catalytic combustion layer (3) are both circular structures, and the outer sides of the circular structures are provided with circular thermal isolation suspension bridges (3-3);
catalyst carriers of the first catalytic unit (3-1) and the second catalytic unit (3-2) are porous alumina ceramics, and the thickness of the catalyst carriers is 5-20 micrometers;
the catalyst of the first catalytic unit (3-1) is formed by single-component or multi-component composition of Pt, Pd and Au.
6. The sheet-type structure integrated catalytic combustion combustible gas sensor according to claim 5, wherein the first through hole (1-13), the second through hole (1-14), the third through hole (1-15) and the fourth through hole (1-16) are filled with Pt metal material.
7. The sheet structure integrated catalytic combustion type combustible gas sensor according to claim 6, wherein the four lead pads, the two signal transmission pads and the four upper surface pads are made of Pt metal material.
8. A preparation method of the sheet-type structure integrated catalytic combustion combustible gas sensor, which is realized based on the sheet-type structure integrated catalytic combustion combustible gas sensor of claim 7, and is characterized in that the preparation method comprises the following specific processes:
s1, manufacturing a first through hole (1-13), a second through hole (1-14), a third through hole (1-15) and a fourth through hole (1-16) on the lower-layer ceramic chip substrate by adopting a punching technology;
printing Pt-filled metal materials in the first through holes (1-13), the second through holes (1-14), the third through holes (1-15) and the fourth through holes (1-16) by adopting a screen printing method;
printing four lead bonding pads, two signal transmission bonding pads and two resistance adjusting regions on the lower surface of the lower ceramic wafer substrate by using a silk-screen printing method and using a Pt metal material, and printing four upper surface bonding pads on the lower surface of the lower ceramic wafer substrate;
printing a first sensing resistor (2-1) and a second sensing resistor (2-2) on the lower surface of the upper ceramic chip substrate by using a Pt metal material by adopting a screen printing method
Printing catalyst carriers of a first catalytic unit (3-1) and a second catalytic unit (3-2) on the upper surface of the upper ceramic chip substrate by using porous alumina ceramics by adopting a screen printing method;
s2, aligning and laminating the lower ceramic wafer substrate and the upper ceramic wafer substrate, and combining the two ceramic wafer substrates into an integral structure by adopting an isostatic pressing technology;
s3, obtaining an integral structure of the S2, and integrally forming by adopting a sintering technology;
s4, processing the two resistance adjusting areas of the signal transmission layer (1) by adopting a laser resistance adjusting technology, wherein the error of the resistance value is adjusted to be less than or equal to 0.1 omega;
s5, preparing a thermal isolation suspension bridge (3-3) on the catalyst carriers of the first catalytic unit (3-1) and the second catalytic unit (3-2) by adopting a laser etching technology;
s6, respectively welding four leads on the four lead bonding pads by adopting a lead welding technology;
s7, coating glass slurry on the four lead pads and the two resistance adjusting areas by adopting a dispensing technology;
s8, sintering and molding the sample obtained in the S7 by adopting a sintering technology;
s9, dropping a solution of ions used by the catalyst onto the catalyst carrier of the first catalytic unit (3-1) by adopting an impregnation technology, and drying and sintering to form a detection element on the first catalytic unit (3-1) and a compensation element on the second catalytic unit (3-2);
and S10, separating the sensor core body containing the detection element and the compensation element by adopting a scribing technology to obtain the integrated catalytic combustion type combustible gas sensor.
9. The method for preparing a combustible gas sensor with an integrated catalytic combustion chip structure according to claim 8, wherein the catalyst loading capacity can be controlled by dripping a solution of ions used by the catalyst onto the catalyst carrier of the first catalytic unit (3-1) by using an impregnation technique and controlling the concentration and dripping volume of the solution by wetting the catalytic ion aqueous solution in S9.
10. The method for preparing a combustible gas sensor with an integrated catalytic combustion chip structure according to claim 8, wherein the drying and sintering process of S9 is as follows:
drying the sample dropped with the catalyst at the temperature of 80-120 ℃, wherein the drying time is more than or equal to 9 h;
then calcining the dried sample, wherein the calcining temperature is controlled to be 500-900 ℃ according to the type of the catalyst, and the calcining time is 2-5 h.
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