CN110174448A - A kind of electromagnetism interference type thermal conductivity gas sensor chip and preparation method thereof - Google Patents
A kind of electromagnetism interference type thermal conductivity gas sensor chip and preparation method thereof Download PDFInfo
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- CN110174448A CN110174448A CN201910583252.4A CN201910583252A CN110174448A CN 110174448 A CN110174448 A CN 110174448A CN 201910583252 A CN201910583252 A CN 201910583252A CN 110174448 A CN110174448 A CN 110174448A
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- 239000002131 composite material Substances 0.000 claims abstract description 49
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 45
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- 238000002604 ultrasonography Methods 0.000 claims description 3
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- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 239000002120 nanofilm Substances 0.000 description 1
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Classifications
-
- 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
- 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
- G01N27/18—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 caused by changes in the thermal conductivity of a surrounding material to be tested
- G01N27/185—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 caused by changes in the thermal conductivity of a surrounding material to be tested using a catharometer
Abstract
The invention discloses a kind of electromagnetism interference type thermal conductivity gas sensor chips, comprising: substrate, the resistor stripe being deposited in substrate, the insulating layer coated on resistor stripe, the sensitive composite material of coating on the insulating layer, the lead with resistor stripe welded connecting.Substrate is the cellular aluminum oxide of growth in situ；Resistor stripe is in two-wire spiral；Insulating layer material isAluminum oxide nanometer scale ceramics superfines, sensitive composite material be carbon nano tube/graphene/Aluminum oxide trielement composite material.Meanwhile the present invention also provides a kind of preparation methods of electromagnetism interference type thermal conductivity gas sensor chip.The present invention makes full use of the specific surface area height of trielement composite material and the strong characteristic of thermal stability, two-wire spiral resistor stripe to have the function of that cutting down external electromagnetic field interferes chip current, make sensor chip that there is good heat exchanger effectiveness and stability, achievees the purpose that shorten the response time, improves detection accuracy.
Description
Technical field
The invention belongs to gas detection technology field, be related to a kind of electromagnetism interference type thermal conductivity gas sensor chip and
Preparation method, in particular to it is a kind of dry based on the anti-electromagnetism of carbon nano tube/graphene/α aluminum oxide trielement composite material
Disturb type thermal conductivity gas sensor chip and preparation method thereof.
Background technique
Thermal conductivity gas sensor is that according to gas with various there is the principle of different thermal conductivity to be detected, mainly by heating
Resistor stripe and gas sensitive material are constituted, and adding thermal resistance item generally uses single line bending, inserts the shapes such as finger.Thermal conductivity gas sensor
It is extensive in the industrial applications such as industry, agricultural, petroleum, coal.But under interference of electromagnetic field environment, due to the magnetic line of force in magnetic field
Active cutting to adding thermal resistance item, generates interference electric current, interference electric current seriously affects heat-conducted gas in adding thermal resistance item
The stability of sensor is not available or detection accuracy is not high so that thermal conductivity gas sensor exists under interference of electromagnetic field environment
The problem of.In addition, thermal conductivity sensor is also in the prevalence of the problem of thermal stability difference.Improve the diamagnetic of thermal conductivity gas sensor
Property and thermal stability for expand thermal conductivity gas sensor application range have positive meaning.
Graphene and carbon nanotube are the new materials of rapid rising, and graphene is two-dimensional layered structure, and carbon nanotube is one
Pipe cavernous structure is tieed up, α aluminum oxide has high thermal stability, triplicity can get large specific surface area, thermostabilization
The strong trielement composite material of property.Meanwhile two-wire spiral fashion conducting wire has the noninductive property for weakening external magnetic field interference, by itself and three
First composite material organically combines, and can effectively improve the thermal stability and diamagnetism of sensor.
201410128545.0 patent of application number disclose binary carbon material-conductive composite nano-polymers air-sensitive film and
Preparation method, the binary carbon material are grapheme material and carbon nanotube, carbon nano-fiber, nanoporous carbon or nanometer stone
Any combination in ink.The patent plays the synergistic effect and complementation generated between different materials, prepares with excellent
The composite nano film of gas-sensitive property.
201510272072.6 patent of application number discloses a kind of graphene/multi-walled carbon nanotube/zinc oxide composite
Resistor-type gas sensor and production method, the patent realize gas concentration under room temperature detection, and have compared with
Fast response speed, but its recovery time is long compared with the recovery time of thermal conductivity gas sensor, and there is certain application limitations.
201611123371.4 patent of application number discloses a kind of wire wrap nickel current sensing element and production method, including
Skeleton, conducting ring, supporting element, nickel wire and manganese-copper filament；Skeleton is the rotary body with threaded hole.Nickel wire, nickel are wound on skeleton
Silk uses noninductive two-wire winding process coiling on skeleton.The working sensor performance of the invention is stablized, and may replace platinum resistance sensitivity
Warm element applies in the product for civilian use.
201711241843.0 patent of application number discloses a kind of hot physical property probe, comprising: has the heated filament spiral shell of insulating film layer
Body is visited made of rotation shape coiling；It is attached to the protective layer for visiting external wall；Connect two terminals for visiting two lead-out wires of body
Son.The spy body of elongated cylindrical structure is two-wire coiling after heated filament doubling.The hot physical property sonde configuration arrangement is accurate, measuring accuracy
Probe size is effectively reduced in height.
Open source information retrieval is as it can be seen that prepare Gao Bibiao using graphene/carbon nano-tube/metal oxide ternary composite material
The sensitive material of the gas sensor of area belongs to research hotspot, but utilizes porous access, the graphene of carbon nano-tube material
The high-termal conductivity of material and the thermal stability of α aluminum oxide material carry out tri compound as sensitive material, and using double
Line spiral resistor stripe has not been reported to improve the diamagnetic thermal conductivity sensor of sensor chip.
Summary of the invention
The object of the present invention is to provide a kind of electromagnetism interference type thermal conductivity gas sensor chips and preparation method thereof.Benefit
Have with the strong characteristic of the specific surface area height and thermal stability of trielement composite material, two-wire spiral resistor stripe and cuts down external electromagnetic
Effect of the field to chip current interference, makes the good heat exchanger effectiveness of sensing element and stability, is made with solving traditional sensors
With the problem of occasion limitation and thermal stability difference, enables the sensor to work normally under interference of electromagnetic field environment, expand
The use scope of sensor, while shortening the response time, improve detection accuracy.
A kind of technical solution of the present invention: electromagnetism interference type thermal conductivity gas sensor chip, comprising: include: substrate,
Deposition resistor stripe on the substrate, coated on the resistor stripe and the substrate sensitive composite material, with the electricity
Hinder the lead that item is welded to connect, which is characterized in that the substrate is the cellular aluminum oxide of growth in situ；The resistor stripe
In two-wire spiral；The insulating layer material is α aluminum oxide nanometer scale ceramics superfines, and insulating layer can make the electricity
Resistance item is kept apart with the composite material, prevents the shunting function between the two；The sensitive composite material is carbon nanotube/graphite
Alkene/α aluminum oxide trielement composite material.
Further, the carbon nanotube is oxidized single-walled carbon nanotubes, oxidation double-walled carbon nano-tube or oxidation multi wall carbon
One of nanotube.
Further, the graphene is graphene nanometer sheet, graphene oxide, redox graphene or porous graphite
One of alkene.
Further, the thermal conductivity gas sensor, which can detecte, differs biggish gas with air conduction coefficient, such as
CO2、CH4、H2。
The invention also discloses a kind of preparation method of electromagnetism interference type thermal conductivity gas sensor chip, including it is following
Step:
1) growth in situ prepares aluminum oxide substrate, and technique processing micro structure body is cut by laser；
2) deposition forms two-wire spiral resistor stripe；
3) α aluminum oxide slurry and trielement composite material slurry are prepared；
4) resistor stripe welding lead；
5) coating slurry forms semi-finished product；
6) slurry high temperature sintering；
7) detection and rating test.
Further, it deposits, includes the following steps described in step 2；
A) aluminum oxide substrate is cut by laser to obtain electromagnetic disturbance sensor base；
B) sensor base is cleaned；
C) platinum product is deposited to by magnetron sputtering technique by substrate surface；
D) by photo etched mask, ion beam etching method processes platinum film, obtains the resistor stripe.
Further, it is prepared described in step 3, comprising the following steps:
A) α aluminum oxide nanometer scale ceramics ultra-fine powder materials are prepared using chemical precipitation method；
B) α aluminum oxide ternary slurry is prepared, process is as follows: α aluminum oxide material and pine tar prepared by step (a)
Alcohol is mixed by weight 1:0.1~2, and ultrasonic disperse makes its mixing sufficiently, and α aluminum oxide slurry is made；
C) carbon nano tube/graphene/α aluminum oxide trielement composite material is prepared, process is as follows: by α aluminum oxide, carbon
1:4~5:4~5 is mixed by volume for nanotube, graphene, and by mixture, terpineol solution is added in 1:100~300 by volume
In, stirring makes it be uniformly dispersed, and carbon nano tube/graphene/α aluminum oxide trielement composite material solution is made；It will be above-mentioned molten
Liquid is centrifuged, washes and dries, and obtains carbon nano tube/graphene/α aluminum oxide trielement composite material；
D) carbon nano tube/graphene/α aluminum oxide trielement composite material slurry is prepared, process is as follows: step (c) is made
Standby carbon nano tube/graphene/α aluminum oxide trielement composite material is mixed with terpinol by weight 1:0.1~2, ultrasound
Dispersion makes its mixing sufficiently, and carbon nano tube/graphene/α aluminum oxide trielement composite material slurry is made.
Further, it is coated described in step 5, comprising the following steps:
A) the α aluminum oxide slurry of one layer of preparation is coated on the resistor stripe；
B) the trielement composite material slurry of preparation is coated on the α aluminum oxide pulp layer.
Further, high temperature sintering described in step 6 is using directly to the load DC voltage realization of semi-finished product described in step 5.
Specifically, under high pure nitrogen protection, DC voltage is loaded to the semi-finished product, passes to the sintering current of 120mA-260mA, temperature
Degree control remains powered on 30min-60min at 550 DEG C -700 DEG C or so.
The invention has the advantages that:
1) carbon nanotube is one-dimensional carbon nano material, and graphene is two-dimentional carbon nanomaterial, and α aluminum oxide has stable crystal form
The trace doped load capacity of uniqueness and high temperature under indeformable physical performance, using the above triplicity as heat-conducted gas
The sensitive material of body sensor, so that sensitive material specific surface area with higher and thermal stability, can greatly improve sensing
The heat exchanger effectiveness and thermal adaptability of device.
2) can effectively weaken high-intensitive dynamic outer magnetic field using the resistor stripe of two-wire spiral to produce adding thermal resistance item
Raw interference electric current improves the applicability, stability and detection accuracy of gas sensor.
The present invention makes full use of the specific surface area height of trielement composite material and the strong characteristic of thermal stability, two-wire spiral electricity
Resistance item have the function of cut down external electromagnetic field to chip current interfere, make sensor chip have good heat exchanger effectiveness with
Stability, even if remaining to achieve the purpose that shorten the response time, improving detection accuracy under interference of electromagnetic field environment.
Detailed description of the invention
The advantages of above-mentioned and/or additional aspect of the invention, will be apparent from the description of the embodiment in conjunction with the following figures
Be readily appreciated that, in which:
Fig. 1 show a kind of structural representation of the embodiment of electromagnetism interference type thermal conductivity gas sensor chip of the invention
Figure；
Fig. 2 show a kind of resistor stripe structure of the embodiment of electromagnetism interference type thermal conductivity gas sensor chip of the invention
Schematic diagram；
Fig. 3 show a kind of stream of the embodiment of electromagnetism interference type thermal conductivity gas sensor chip preparation method of the invention
Cheng Tu.
Wherein corresponding relationship of the Fig. 1 into Fig. 3 between appended drawing reference and component names are as follows:
1, aluminum oxide substrate；2, resistor stripe；3, insulating materials；4, sensitive composite material；5, lead.
Specific embodiment
Below in conjunction with specific embodiment the present invention is described in detail.It should be noted that skill described in following embodiments
The combination of art feature or technical characteristic is not construed as isolated, they can be combined with each other to reaching better
Technical effect.
The embodiment of the present invention is described in conjunction with Fig. 1 and Fig. 2: a kind of electromagnetism interference type thermal conductivity gas sensor chip,
Include: substrate 1, deposition resistor stripe 2 on the substrate, coated on resistor stripe insulating layer 3, be coated in the resistor stripe
With the sensitive composite material 4 in the substrate, the lead 5 with resistor stripe welded connecting.The substrate 1 is growth in situ
Cellular aluminum oxide；The resistor stripe 2 is in two-wire spiral；The insulating layer 3 is super for α aluminum oxide nanometer scale ceramics
Fine powder, the insulating layer can be such that the resistor stripe keeps apart with the composite material, prevent the shunting function between the two；Institute
Stating sensitive composite material 4 is carbon nano tube/graphene/α aluminum oxide trielement composite material.
In embodiment, the resistor stripe 2 is one or more of platinum, palladium, rhodium, iridium, ruthenium, osmium, tungsten.Preferential selection
Platinum.
In embodiment, the carbon nanotube is oxidized single-walled carbon nanotubes, oxidation double-walled carbon nano-tube or oxidation multi wall
One of carbon nanotube.Preferential selective oxidation multi-walled carbon nanotube.
In embodiment, the graphene is graphene nanometer sheet, graphene oxide, redox graphene or porous stone
One of black alkene.Preferential selective oxidation graphene.
In embodiment, the thermal conductivity gas sensor, which can detecte, differs biggish gas with air conduction coefficient,
Such as CO2、CH4、H2。
Referring to Fig. 3, the present invention also provides a kind of embodiments: disclosing a kind of electromagnetism interference type heat-conducted gas biography
The preparation method of sensor chip, comprising the following steps:
Step 100: growth in situ prepares aluminum oxide substrate, and technique processing micro structure body is cut by laser；
Step 200: deposition forms two-wire spiral resistor stripe；
Step 300: preparation α aluminum oxide slurry and trielement composite material slurry；
Step 400: resistor stripe welding lead；
Step 500: coating slurry forms semi-finished product；
Step 600: slurry high temperature sintering；
Step 700: detection and rating test.
In embodiment, it deposits, includes the following steps described in step 200；
A) aluminum oxide substrate is sliced and is grown (1.5mm-3mm) × wide (1.2mm-5mm) × height (0.01mm-
Electromagnetic disturbance sensor base 0.1mm)；
B) sensor base is cleaned；
C) platinum product is deposited to by magnetron sputtering technique by substrate surface, forms 0.5 μm of -0.9 μ m thick film；
D) by photo etched mask, ion beam etching method processes platinum film, obtains resistor stripe as shown in Figure 2.
In embodiment, it is prepared described in step 300, comprising the following steps:
A) α aluminum oxide nanometer scale ceramics ultra-fine powder materials are prepared using chemical precipitation method；
B) α aluminum oxide ternary slurry is prepared, process is as follows: α aluminum oxide material and pine tar prepared by step (a)
Alcohol is mixed by weight 1:0.1~2, and ultrasonic disperse makes its mixing sufficiently, and α aluminum oxide slurry is made；
C) carbon nano tube/graphene/α aluminum oxide trielement composite material is prepared, process is as follows: by α aluminum oxide, carbon
1:4~5:4~5 is mixed by volume for nanotube, graphene, and by mixture, terpineol solution is added in 1:100~300 by volume
In, stirring makes it be uniformly dispersed, and carbon nano tube/graphene/α aluminum oxide trielement composite material solution is made；It will be above-mentioned molten
Liquid is centrifuged, washes and dries, and obtains carbon nano tube/graphene/α aluminum oxide trielement composite material；
D) carbon nano tube/graphene/α aluminum oxide trielement composite material slurry is prepared, process is as follows: step (c) is made
Standby carbon nano tube/graphene/α aluminum oxide trielement composite material is mixed with terpinol by weight 1:0.1~2, ultrasound
Dispersion makes its mixing sufficiently, and carbon nano tube/graphene/α aluminum oxide trielement composite material slurry is made.
In embodiment, it is coated described in step 500, comprising the following steps:
A) the α aluminum oxide slurry that one layer of preparation is coated on the resistor stripe 2, as the insulating layer 3；
B) the trielement composite material slurry 4 of the upper coating preparation at described 3 layers of α aluminum oxide slurry insulating layer.
In embodiment, high temperature sintering described in step 600 is using directly to the load DC voltage of semi-finished product described in step 500
It realizes.Specifically, under high pure nitrogen protection, DC voltage is loaded to the semi-finished product, passes to the sintering electricity of 120mA-260mA
Stream, temperature are controlled at 550 DEG C -700 DEG C or so, remain powered on 30min-60min.
The present invention makes full use of the specific surface area height of trielement composite material and the strong characteristic of thermal stability, two-wire spiral electricity
Resistance item have the function of cut down external electromagnetic field to chip current interfere, make sensor chip have good heat exchanger effectiveness with
Stability, even if remaining to achieve the purpose that shorten the response time, improving detection accuracy under interference of electromagnetic field environment.
Although the embodiment of the present invention is had been presented for herein, for it will be appreciated by those skilled in the art that this hair
Bright patent is not limited to the details of above-mentioned exemplary embodiment, and in the feelings of the spirit or essential attributes without departing substantially from the invention patent
Under condition, the invention patent can be realized with other assembling forms.Above-described embodiment is only exemplary, the model of the invention patent
It encloses and is indicated by the appended claims rather than the foregoing description, it is intended that by the meaning and model of the condition of equivalent for falling in claim
All changes in enclosing are included in the invention patent.It should not be using the embodiments herein as the restriction of interest field of the present invention.
Claims (8)
1. a kind of electromagnetism interference type thermal conductivity gas sensor chip, comprising: substrate, applies the resistor stripe being deposited in substrate
The insulating layer that overlays on resistor stripe and substrate, coating sensitive composite material on the insulating layer draws with resistor stripe welded connecting
Line, which is characterized in that the substrate is the cellular aluminum oxide of growth in situ；The resistor stripe is in two-wire spiral；Institute
Stating insulating layer material isAluminum oxide nanometer scale ceramics superfines, insulating layer can make the resistor stripe with it is described compound
Material is kept apart, and the shunting function between the two is prevented；The sensitive composite material be carbon nano tube/graphene/Aluminum oxide
Trielement composite material.
2. electromagnetism interference type thermal conductivity gas sensor chip as described in claim 1, which is characterized in that the carbon nanometer
Pipe is oxidized single-walled carbon nanotubes, oxidation one of double-walled carbon nano-tube or oxidation multi-wall carbon nano-tube tube.
3. electromagnetism interference type thermal conductivity gas sensor chip as described in claim 1, which is characterized in that the graphene
For one of graphene nanometer sheet, graphene oxide, redox graphene or porous graphene.
4. the preparation method of electromagnetism interference type thermal conductivity gas sensor chip as described in claim 1, which is characterized in that
The following steps are included:
1) growth in situ prepares aluminum oxide substrate, and technique processing micro structure body is cut by laser；
2) deposition forms two-wire spiral resistor stripe；
3) it preparesAluminum oxide slurry and trielement composite material slurry；
4) resistor stripe welding lead；
5) coating slurry forms semi-finished product；
6) slurry high temperature sintering；
7) detection and rating test.
5. the preparation method of electromagnetism interference type thermal conductivity gas sensor chip as claimed in claim 4, which is characterized in that
It is deposited described in step 2, comprising the following steps:
A) aluminum oxide substrate is cut by laser to obtain electromagnetic disturbance sensor base；
B) sensor base is cleaned；
C) platinum product is deposited to by magnetron sputtering technique by substrate surface；
D) by photo etched mask, ion beam etching method processes platinum film, obtains the resistor stripe.
6. the preparation method of electromagnetism interference type thermal conductivity gas sensor chip as claimed in claim 4, which is characterized in that
It is prepared described in step 3, comprising the following steps:
A) it is prepared using chemical precipitation methodAluminum oxide nanometer scale ceramics ultra-fine powder materials；
B) it preparesAluminum oxide ternary slurry, process are as follows: by step (a) preparationAluminum oxide material and pine tar
Alcohol is mixed by weight 1:0.1 ~ 2, and ultrasonic disperse makes its mixing sufficiently, is madeAluminum oxide slurry；
C) prepare carbon nano tube/graphene/Aluminum oxide trielement composite material, process are as follows: willAluminum oxide, carbon
1:4 ~ 5:4 ~ 5 is mixed by volume for nanotube, graphene, and by mixture, terpineol solution is added in 1:100 ~ 300 by volume
In, stirring makes it be uniformly dispersed, and obtained carbon nano tube/graphene/Aluminum oxide trielement composite material solution；It will be above-mentioned molten
Liquid is centrifuged, washes and dries, and acquisition carbon nano tube/graphene/Aluminum oxide trielement composite material；
D) prepare carbon nano tube/graphene/Aluminum oxide trielement composite material slurry, process are as follows: step (c) is made
Standby carbon nano tube/graphene/Aluminum oxide trielement composite material is mixed with terpinol by weight 1:0.1 ~ 2, ultrasound point
Dissipating makes its mixing sufficiently, and obtained carbon nano tube/graphene/Aluminum oxide trielement composite material slurry.
7. the preparation method of the spherical thermal conductivity gas sensor of pearl as claimed in claim 4, which is characterized in that described in step 5
Coating, comprising the following steps:
A) one layer of preparation is coated on the resistor stripeAluminum oxide slurry；
B) existThe trielement composite material slurry of preparation is coated on aluminum oxide pulp layer.
8. the preparation method of electromagnetism interference type thermal conductivity gas sensor chip as claimed in claim 4, which is characterized in that
High temperature sintering described in step 6 is using directly to the load DC voltage realization of semi-finished product described in step 5；Specifically, in high pure nitrogen
Under protection, DC voltage is loaded to the semi-finished product, passes to the sintering current of 120mA-260mA, temperature is controlled at 550 DEG C -700
DEG C or so, remain powered on 30min-60min.
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