CN108169287A - A kind of hot-wire gas sensor and preparation method thereof - Google Patents
A kind of hot-wire gas sensor and preparation method thereof Download PDFInfo
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- CN108169287A CN108169287A CN201711368762.7A CN201711368762A CN108169287A CN 108169287 A CN108169287 A CN 108169287A CN 201711368762 A CN201711368762 A CN 201711368762A CN 108169287 A CN108169287 A CN 108169287A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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Abstract
The invention discloses a kind of hot-wire gas sensor and preparation method thereof, the gas sensor includes sensitive chip, 3 foot tube seat of standard, wherein：The sensitive chip includes ceramic substrate, signal electrode pad, signal electrode, heating electrode pad, heating electrode, metal lead wire, sensitive material and noble metal lead；The ceramic substrate uses triangular structure, and for heating electrode arrangement in the top of triangle base, signal electrode is arranged in the lower section of triangular apex；The both ends of the signal electrode are connected with signal electrode pad, heat and heating electrode pad is connected with above electrode；The metal lead wire is connect with signal electrode pad, and noble metal lead is connect with heating electrode pad, and sensitive material is attached on signal electrode and heating electrode；The metal lead wire and noble metal lead are connect with the stem of 3 foot tube seat of standard.The hot-wire gas sensor configuration of the present invention is compact, can effectively reduce the heat power consumption of sensor, increase the yield of unit area.
Description
Technical field
The invention belongs to sensor technical fields, are related to a kind of gas sensor and preparation method thereof more particularly to one kind
Detect hot-wire gas sensor of low concentration flammable explosive gas and preparation method thereof.
Background technology
Gas sensor refers to whether there is specific gas in certain area coverage for detection and/or can continuously measure
The primary instrument of gas composition concentration.In security protections sides such as coal mine, oil, chemical industry, municipal administration, medical treatment, communications and transportation, families
Face, gas sensor are usually used in detecting flammable, inflammable, toxic gas concentration or its presence or absence etc..Calorifics formula gas sensing
Device is an important branch in gas sensor family.
Calorifics formula gas sensor mainly has heat-conducted and two major class of thermo-chemical type.Heat-conducted is the thermal conductivity using gas
Rate, by measuring one or more of gas component concentrations to the variation of wherein temperature-sensitive element resistance, in answering for industrial quarters
With the history of existing decades, the gas that can be analyzed is also wide.Thermo-chemical type is the heat reacted based on analyzed aerochemistry
Effect, such as catalytic combustion method gas sensor, semiconductor-type gas sensor, hot-wire gas sensor.
At present, hot-wire gas sensor is widely used in industry and field of traffic.Such as：Traffic police detects the wine of drunk driving
Smart detector, using hot-wire gas sensor；The portable leakage detector of Household gas pipeline, use is also hot line
Formula gas sensor；Coal mining mine is used to analyze the CH in tunnel4Content, the alkanes gas content that oil exploitation is sewed are changed
Organic vapor in work workshop analysis air etc..Hot-wire gas sensor is used to detect flammable explosive gas concentration range several
Within ten ppm, hundreds of ppm are limited to compared with high detection.Traditional method is using filament-winding method coiling heater strip, and heater strip is simultaneously as letter
Number electrode is coated on heater strip using tin oxide powdery pulp and forms sensitive material.Traditional hot wire sensor way is most
Big problem is that heater strip has the function of also to there is signal testing outside heating function, is that follow-up modulate circuit connection uses
When, measuring signal is adjusted to the heated voltage fluctuation influence of meeting and the interference of environment temperature factor, and is not easy to compensate, measurement accuracy phase
To relatively low；Another problem is that traditional method is hand-made, and sensor performance dispersibility is larger, it is difficult to realize batch micro operations.
CN200580009988.7 disclose a kind of heater coil for gas sensor, detection element for gas sensor,
The manufacturing method of catalytic combustion type gas sensor and catalytic combustion type gas sensor, the heater coil for gas sensor
It is the heating coil for catalytic combustion type gas sensor, which has weldering pearl portion and leading part, and weldering pearl portion is by n weights
Convolute coil is formed.
CN201510945458.9 discloses a kind of gas sensor element and gas of the plate extended along long side direction
Body sensor, the gas sensor element have plate composite ceramic layer；Electrode portion is in the interarea of the side of composite ceramic layer
Side is contiguously configured with the solid electrolyte section；Leading part is in the interarea side of the side of composite ceramic layer.
CN201210286970.3 discloses a kind of elongated sensor element in Semiconductor substrate, the elongated sensing
Device element extends across opening and with opposite first surface and second surface, first surface and second surface are exposed with wanting
The gas of sensing is in contact, and it is sensitive that the conductivity of elongated sensor element, which can externally reveal gas composition concentration,.
Invention content
In order to solve, the hand-made large dispersion brought of existing hot-wire gas sensor, power consumption are high, yield rate is low, difficult
To realize the general considerations such as batch micro operations, while solve that sensor bulk is big, operating temperature control accuracy is low, gas accuracy of detection
The Key technique problems such as low, response time is slow, the present invention provides it is a kind of can batch micro operations hot-wire gas sensor and its
Preparation method.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of hot-wire gas sensor, including sensitive chip, 3 foot tube seat of standard, wherein：
The sensitive chip includes ceramic substrate, signal electrode pad, signal electrode, heating electrode pad, heating electrode, metal
Lead, sensitive material and noble metal lead；
The heating electrode and signal electrode are arranged on ceramic substrate the same face；
The ceramic substrate uses triangular structure, and in the top of triangle base, signal electrode is arranged in heating electrode arrangement
The lower section of triangular apex；
The both ends of the signal electrode are connected with signal electrode pad, heat and heating electrode pad is connected with above electrode；
The metal lead wire is connect with signal electrode pad, and noble metal lead is connect with heating electrode pad, sensitive material attachment
On signal electrode；
The metal lead wire and noble metal lead are connect with the stem of 3 foot tube seat of standard.
A kind of preparation method of above-mentioned hot-wire gas sensor, includes the following steps：Nanohole array Al2O3Ceramic base
Piece cleaning oil removing → physical deposition platinum film → high-temperature heat treatment platinum film → mask → dry etching platinum film → go photoresist →
Prepare sensitive material → printing thick film sensitive material → sintering → mask graphics chip → wet etching substrate → dissolving base
Piece metallic aluminium substrate → lead is bonded → encapsulates sealing cap.Specific implementation step is as follows：
A, ceramic substrate is cleaned, oil removing, dedusting；
B, platinum film is prepared in ceramic substrate surface using physical deposition process, vacuum evaporation coating film method or spatter film forming method；
C, the ceramic substrate for having deposited platinum film is heat-treated using high-temperature heat treatment process；
D, using photoetching process mask lithography, heating electrode and signal electrode figure are formed；
E, platinum film is etched using dry etch process, ion beam etch process, plasma etching industrial or laser etching process, directly
Platinum film to non-mask all etches completion；
F, remove photoresist, clean, after drying, in detecting electrode exit thick-film technique printing signal electrode pad and heating
Electrode pad；
G, thick film ink is made by organic bond in sensitive material, prints thickness on signal electrode using thick film print technology
Film sensitive material, and be put into sintering furnace and be sintered；
H, using photoetching process mask lithography, ceramic base sensitive chip figure is formed；
E, ceramic substrate is etched using wet-etching technology, forms ceramic base sensitive chip triangular structure；
M, ceramic base sensitive chip monomer is removed using dissolving substrate metal substrate approach；
N, metal lead wire and noble metal lead are stained with high temperature conductive silver slurry, are bonded in signal electrode pad and heating electrode weldering
Pan Chu is put into sintering furnace and is sintered；
P, sensitive chip is encapsulated on the stem of 3 foot tube seat of standard, sealing cap, forms hot-wire gas sensor.
In the present invention, the sensitive material uses the alumina nano tube framework material of graduation nano tin dioxide modification.
In the present invention, the ceramic substrate has the characteristics that the penetrating of micro Process using what electrochemical in-situ growing method was formed
Type nanohole array Al2O3Ceramic substrate.
In the present invention, the signal electrode is " multiple twin bow " font structure.
The invention has the advantages that：
1st, hot-wire gas sensor configuration of the invention is compact, and it is same that heating electrode and signal electrode are produced on ceramic substrate
On face, and heating electrode and temperature detecting unit are combined into one, realize that the temperature of working sensor occurs, Detection ＆ Controling；
It is grown using electrochemical in-situ, while there is open type nano-pore array structure Al2O3Ceramic substrate, it is nano oxidized with classifying
There is the sensitive material of tin modification alumina nano tube framework material preferable adhesive force to not readily disengage from, simultaneously because substrate has
There is open type nanohole array so that sensor has the fast-response characteristic that excellent gas detects.
2nd, hot-wire gas sensor of the invention can form gas detection and warning instrument with signal conditioning circuit, just
Under normal environmental condition, detection gas, hydrogen, alkane, eneyne, liquefied gas, oil vapour, organic solvent etc., suitable for environmental protection,
The trace detection of the pollutions such as air, water source；Analysis, monitoring, the research of poisonous substance；Biochemistry；Clinical practice；Pathology and virus are ground
Study carefully；Food fermentation；Petrochemical industry；PETROLEUM PROCESSING；Analysis of oil；Geology, mine locating research；Organic chemistry；Study on the synthesis；Health inspection
Epidemic disease；Public hazards test and analyze and research.
Description of the drawings
Fig. 1 is heating electrode and signal electrode distribution schematic diagram on sensitive chip；
Fig. 2 is structure diagram of the sensitive chip with lead and sensitive material；
Fig. 3 is encapsulated in standard base schematic diagram for sensor chip；
Fig. 4 is the manufacturing process block flow diagram of hot-wire gas sensor of the present invention；
In figure：1- ceramic substrates, 2- signal electrodes pad, 3- signal electrodes, 4- heating electrode pad, 5- heating electrode, 6- gold
Belong to lead, 7- sensitive materials, 8- noble metals lead, 9- sensitive chips, 10- stems, 3 foot tube seat of 11- standards.
Specific embodiment
Technical scheme of the present invention is further described below in conjunction with the accompanying drawings, however, it is not limited to this, every to this
Inventive technique scheme is modified or replaced equivalently, and without departing from the spirit and scope of technical solution of the present invention, should all be covered
In protection scope of the present invention.
As shown in Figs. 1-3, hot-wire gas sensor provided by the invention includes sensitive chip 9,3 foot tube seat 11 of standard,
Wherein：
The sensitive chip 9 includes ceramic substrate 1, signal electrode pad 2, signal electrode 3, heating electrode pad 4, heating electrode
5th, metal lead wire 6, sensitive material 7 and noble metal lead 8；
The ceramic substrate 1 uses triangular structure, heats electrode 5 and signal electrode 3 is arranged on 1 the same face of ceramic substrate,
Heating electrode 5 is arranged in the top of triangle base, and signal electrode 3 is arranged in the lower section of triangular apex, heating electrode 5 and letter
Number electrode 3 forms the coplanar structure form of separation, and heats electrode 5 and have thermometric and temperature controlling function simultaneously；
The both ends of the signal electrode 3 are connected with signal electrode pad 4, and the top of heating electrode 5 is connected with heating electrode pad
4；
The metal lead wire 6 is connect with signal electrode pad 2, and noble metal lead 8 is connect with heating electrode pad 4, sensitive material 7
It is attached on signal electrode 3；
The metal lead wire 6 and noble metal lead 8 are connect with the stem 10 of 3 foot tube seat of standard.
As shown in figure 4, the preparation method of above-mentioned hot-wire gas sensor includes the following steps：It can micro-machined Al2O3Pottery
Ceramic chip-sputtering platinum film-high-temperature heat treatment-mask-dry etching-printing silver soldering disk-be heat-treated-prepare sensitive material-
Make thick film sensitivity slurry-printing thick film sensitive material-sintering-mask-wet etching-stripping substrate-solder taul-chip
Encapsulation-formation hot-wire gas sensor, the manufacturing method between each work step can carry out arbitrary combination according to specific requirement.Tool
Body implementation steps are as follows：
A, with organic solvent cleaning ceramic substrate, oil removing dedusting, the ceramic substrate is using the growth of metal aluminum foil electrochemical in-situ
Formed 0.06 ~ 0.25mm thickness can the micro-machined Al with open type nano-pore array structure2O3Ceramic substrate, it is organic
Solvent is one or more of toluene, acetone, ethyl alcohol；
B, platinum film is deposited in ceramic substrate surface using sputtering technology, the platinum film thickness is 0.3 ~ 1.5um；
C, the ceramic substrate for having deposited platinum film is heat-treated using high-temperature heat treatment process, heat treatment temperature is 600 ~ 1200
℃；
D, using photoetching process mask lithography, heating electrode and signal electrode figure are formed；
E, platinum film is etched using dry etch process, is completed until the platinum film of non-mask all etches；
F, remove photoresist, clean, after drying, in detecting electrode exit thick-film technique printing signal electrode pad and heating
Electrode pad, printing pad heat treatment temperature are 600 ~ 750 DEG C；
G, by the use of alumina nano tube as framework material, using classifying, nano tin dioxide modifies framework material, obtains
To sensitive material；
H, thick film ink is made by organic bond in sensitive material, prints thickness on signal electrode using thick film print technology
Film sensitive material, sensitive material film forming thickness are 10 ~ 25 microns；And be put into sintering furnace and be sintered, sintering temperature is 550 ~ 700
℃；
E, using photoetching process mask lithography, sensitive chip figure is formed；
M, using sulfuric acid and hydrochloric acid solution as etching agent, wet etching ceramic substrate forms ceramic base sensitive chip three
Angular structure；
N, using the metallic aluminium under displacement reaction method dissolving substrate, ceramic base sensitive chip monomer is removed in stripping；
P, metal lead wire and noble metal are stained with high temperature conductive silver slurry, are bonded in signal electrode pad and heating electrode pad
Place, is put into sintering furnace and is sintered, and sintering temperature is 550 ~ 700 DEG C；
Q, sensitive chip is encapsulated on the stem of 3 foot tube seat of standard, sealing cap, forms hot-wire gas sensor.
Hot-wire gas sensor operation principle provided by the invention is as follows：
Sensor chip is heated to a certain range of high temperature by heating electrode, once the sensitive material quilt being printed on signal electrode
It heats, the oxygen in air will seize electronics from the donor level of the semiconducting crystal particle in sensitive material, and crystallize
Adsorption on Surface negative electron, increases surface potential, so as to hinder the movement of conduction electrons, so, gas sensor is in air
In be constant resistance value.At this moment oxidation reaction occurs for reducibility gas and the oxygen of semiconductor surface absorption, due to gas molecule
From suction effect make its surface potential height change, therefore, the resistance value of sensor will change.For reproducibility gas
Body, resistance value reduce；For oxidizing gas, then resistance value increase.The variation of sensitive material resistance value is coupled on signal electrode,
Parallel relationship is formed with the resistance value of signal electrode, by being tested the calibration of gas, according to the resistance value at measurement signal electrode both ends
Variation can perceive the concentration of tested gas.
The hot-wire gas sensor configuration of the present invention is compact, and three end deriving structures of hot line gas sensor are realized
Triangular apex position is drawn, and than the volume that traditional square structure reduces half, is effectively reduced the heat power consumption of sensor, is increased single
The yield of plane product.
The present invention hot-wire gas sensor signal electrode is designed to " multiple twin bow " font structure, can improve with it is quick
Feel material area, greatly improve transducer sensitivity.
The hot-wire transducer of the present invention can detect flammable explosive gas and organic solvent volatilization steam etc., suitable for stone
The application fields such as oil, chemical industry, the energy.
Claims (10)
1. a kind of hot-wire gas sensor, it is characterised in that the gas sensor includes sensitive chip, 3 foot tube seat of standard,
Wherein：
The sensitive chip includes ceramic substrate, signal electrode pad, signal electrode, heating electrode pad, heating electrode, metal
Lead, sensitive material and noble metal lead；
The heating electrode and signal electrode are arranged on ceramic substrate the same face；
The ceramic substrate uses triangular structure, and in the top of triangle base, signal electrode is arranged in heating electrode arrangement
The lower section of triangular apex；
The both ends of the signal electrode are connected with signal electrode pad, heat and heating electrode pad is connected with above electrode；
The metal lead wire is connect with signal electrode pad, and noble metal lead is connect with heating electrode pad, sensitive material attachment
On signal electrode；
The metal lead wire and noble metal lead are connect with the stem of 3 foot tube seat of standard.
2. hot-wire gas sensor according to claim 1, it is characterised in that the sensitive material is received using graduation
The alumina nano tube framework material of rice tin oxide modification.
3. hot-wire gas sensor according to claim 1, feature uses electrochemical in-situ in the ceramic substrate
The Al with open type nanohole array that growing method is formed2O3Ceramic substrate, thickness are 0.06 ~ 0.25mm.
4. hot-wire gas sensor according to claim 1, feature is " multiple twin bow " font in the signal electrode
Structure.
5. a kind of preparation method of the hot-wire gas sensor described in claim 1-4 any claims, it is characterised in that
The method step is as follows：
A, ceramic substrate is cleaned, oil removing, dedusting；
B, platinum film is prepared in ceramic substrate surface using physical deposition process, vacuum evaporation coating film method or spatter film forming method；
C, the ceramic substrate for having deposited platinum film is heat-treated using high-temperature heat treatment process；
D, using photoetching process mask lithography, heating electrode and signal electrode figure are formed；
E, platinum film is etched using dry etch process, ion beam etch process, plasma etching industrial or laser etching process, directly
Platinum film to non-mask all etches completion；
F, remove photoresist, clean, after drying, in detecting electrode exit thick-film technique printing signal electrode pad and heating
Electrode pad；
G, thick film ink is made by organic bond in sensitive material, prints thickness on signal electrode using thick film print technology
Film sensitive material, and be put into sintering furnace and be sintered；
H, using photoetching process mask lithography, ceramic base sensitive chip figure is formed；
E, ceramic substrate is etched using wet-etching technology, forms ceramic base sensitive chip triangular structure；
M, ceramic base sensitive chip monomer is removed using dissolving substrate metal substrate approach；
N, metal lead wire and noble metal lead are stained with high temperature conductive silver slurry, are bonded in signal electrode pad and heating electrode weldering
Pan Chu is put into sintering furnace and is sintered；
P, sensitive chip is encapsulated on the stem of 3 foot tube seat of standard, sealing cap, forms hot-wire gas sensor.
6. the preparation method of hot-wire gas sensor according to claim 5, it is characterised in that in the step b, platinum
Film thickness is 0.3 ~ 1.5um.
7. the preparation method of hot-wire gas sensor according to claim 5, it is characterised in that in the step c, pottery
Ceramic chip heat treatment temperature is 600 ~ 1200 DEG C.
8. the preparation method of hot-wire gas sensor according to claim 5, it is characterised in that in the step f, print
The heat treatment temperature of brush signal electrode pad and heating electrode pad is 600 ~ 750 DEG C.
9. the preparation method of hot-wire gas sensor according to claim 5, it is characterised in that quick in the step h
It is 10 ~ 25 microns to feel material filming thickness, and sintering temperature is 550 ~ 700 DEG C.
10. the preparation method of hot-wire gas sensor according to claim 5, it is characterised in that in the step p, burn
Junction temperature is 550 ~ 700 DEG C.
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