CN110174449A - A kind of spherical thermal conductivity gas sensor of pearl and preparation method thereof - Google Patents
A kind of spherical thermal conductivity gas sensor of pearl and preparation method thereof Download PDFInfo
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- CN110174449A CN110174449A CN201910583260.9A CN201910583260A CN110174449A CN 110174449 A CN110174449 A CN 110174449A CN 201910583260 A CN201910583260 A CN 201910583260A CN 110174449 A CN110174449 A CN 110174449A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 107
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 68
- 239000002131 composite material Substances 0.000 claims abstract description 58
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 30
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 30
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 230000035699 permeability Effects 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract 8
- 239000011248 coating agent Substances 0.000 claims abstract 2
- 238000000576 coating method Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 63
- 238000007254 oxidation reaction Methods 0.000 claims description 33
- 230000003647 oxidation Effects 0.000 claims description 31
- 239000002002 slurry Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 26
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 239000002048 multi walled nanotube Substances 0.000 claims description 20
- 238000005245 sintering Methods 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000006255 coating slurry Substances 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 4
- 238000009388 chemical precipitation Methods 0.000 claims description 4
- 239000002079 double walled nanotube Substances 0.000 claims description 4
- 229910052741 iridium Inorganic materials 0.000 claims description 4
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052762 osmium Inorganic materials 0.000 claims description 4
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910052703 rhodium Inorganic materials 0.000 claims description 4
- 239000010948 rhodium Substances 0.000 claims description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052707 ruthenium Inorganic materials 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- 239000002109 single walled nanotube Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 239000002071 nanotube Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 5
- 230000004044 response Effects 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011206 ternary composite Substances 0.000 description 2
- 208000003351 Melanosis Diseases 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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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
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of spherical thermal conductivity gas sensors of pearl, comprising: resistance wire, the composite material being sintered simultaneously on the insulating layer and with insulating layer coated in the insulating layer on resistance wire, coating, with the shelter-clad of the pedestal of resistance wire welded connecting, the good air permeability being connect with base engagement.Resistance wire is in hollow ellipsoid shape, and there are the straightways at both ends；Insulating layer material isAluminum oxide nanometer scale ceramics superfines, composite material be carbon nano tube/graphene/The trielement composite material of aluminum oxide.Meanwhile the present invention also provides a kind of preparation methods of the spherical thermal conductivity gas sensor of pearl.The present invention makes full use of the large specific surface area of trielement composite material and the high characteristic of thermal stability, elliposoidal resistance wire are guided the forming of composite material and homogenizing agglomeration, make sensing element that there is uniform temperature field and good heat exchanger effectiveness, achievees the purpose that shorten the response time, improves detection accuracy and prolong the service life.
Description
Technical field
The invention belongs to gas detection technology field, it is related to a kind of spherical thermal conductivity gas sensor of pearl and its preparation side
Method, in particular to a kind of pearl based on carbon nano tube/graphene/α aluminum oxide trielement composite material spheroid shape resistance wire
Spherical thermal conductivity gas sensor and preparation method thereof.
Background technique
Thermal conductivity gas sensor is detected using the different characteristic of different types of various concentration gas conduction rate.?
In the industries such as medicine, food, tobacco, coal, petroleum, the concentration of various volatile organic compounds, detection pernicious gas is monitored
Aspect thermal conductivity sensor has a wide range of applications.In particular, thermal conductivity gas sensor is in terms of detecting flammable explosive gas
Compared with the other types gas sensor such as combustion type gas sensor, more securely and reliably, there is irreplaceable role.Pearl is spherical
Thermal conductivity gas sensor is the main Types of thermal conductivity gas sensor.
The apolegamy of sensor sensing material and the shape of resistance wire are to improve the key factor of gas sensor performance.Pearl ball
The sensing element of shape thermal conductivity sensor is mostly used is overmolding to that pearl is spherical and high temperature sintering sensitive material on cylindrical resistance wire
Mode prepare.During being overmolding to pearl, the cylinder of resistance wire lacks guiding function to sensitive material slurry, causes pearl ball
Shape sensitive component surfaces Forming Quality is not high and density of material is unevenly distributed；With cylindrical resistance wire sensitive material spherical to pearl
In the high-temperature sintering process of material, due to sensitive material be heated it is uneven so that sensitive material generate it is irregular reunite, cause in
Portion is also easy to produce the problem of micro-crack.In addition, the problem of the generally existing thermal stability deficiency of gas sensor, further improves heat
Stability is also the hot spot of research.
Graphene belongs to two-dimentional carbon nanomaterial, in the form of sheets structure, has specific surface area height, excellent thermal conductivity, mechanicalness
The characteristics such as energy is good, chemical property is stablized, but it is easy to assemble agglomeration, so as to cause the reduction of its specific surface area；Carbon nanotube is one
Carbon nanomaterial is tieed up, is in perforated tubular, being doped in graphene sheet layer can agglomerate to avoid the aggregation of graphene sheet layer；Tri- oxygen of α
Change two aluminium with indeformable thermal stability under the trace doped load capacity of uniqueness and high temperature of stable crystal form.
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 realized using the graphene satisfactory electrical conductivity compound with carbon nanotube
Gas concentration detection under room temperature, and there is faster response speed, but its recovery time senses compared with heat-conducted gas
The recovery time of device is long, and there is certain application limitations.Graphene/carbon nano-tube/metal oxide ternary composite material system
Standby resistor-type gas sensor has become the hot spot of research.
201510951882.4 patent of application number discloses a kind of gas sensor, the measuring cell for gas sensor
And its manufacturing method.The sensor of the invention includes shell and measuring cell, measuring cell by heating coil silk and be coated on plus
The bead-like body ceramics comprising fibrous material on hot taenidium, solve carrier when sensor is subject to big mechanical load and urge
Change the impaired problem of element bead-like body.Heating coil silk described in the patent is cylindric.Harbin Engineering University Zhang Hongquan
The sensing element of the micro-structure methane gas sensor of development is spherical in pearl, and what the resistance wire inside sensing element used is also round
Column.
It is retrieved by open source information as it can be seen that using graphene/carbon nano-tube/metal oxide ternary composite material preparation preparation
The sensitive material of the gas sensor of high-specific surface area belongs to research hotspot, but using carbon nano-tube material as porous logical
Road, graphene carry out tri compound as quick as thermal stability framework material as high conductivity material and α aluminum oxide
Feel material, and is had not been reported using the thermal conductivity gas sensor of spheroid shape resistance wire preparation.
Summary of the invention
The object of the present invention is to provide spherical thermal conductivity gas sensors of a kind of pearl and preparation method thereof, utilize tri compound
The high characteristic of the high-specific surface area and thermal stability of material, elliposoidal resistance wire is guided the forming of composite material and homogenizing is reunited
It acts on, surface forming is of low quality, density of material is unevenly distributed, there are micro-crack, high temperature are steady existing for solution sensing element
The problems such as qualitative difference, makes sensing element have uniform temperature field and good heat exchanger effectiveness, reaches shortening response and restores
Time, the purpose for improving detection accuracy and prolonging the service life.
Technical solution of the present invention: a kind of spherical thermal conductivity gas sensor of pearl, comprising: resistance wire is coated in resistance wire
On insulating layer, coated in the composite material being sintered simultaneously on the insulating layer and with the insulating layer, with resistance wire welding connect
The shelter-clad of the pedestal, the good air permeability being connect with base engagement that connect.Resistance wire is in hollow ellipsoid shape, and there are two
The straightway at end；Insulating layer material is α aluminum oxide nanometer scale ceramics superfines；Composite material is carbon nanotube/graphite
Alkene/α aluminum oxide trielement composite material.Insulating layer can be such that resistance wire keeps apart with composite material, between prevention the two
Shunting function.
Further, the resistance wire is one or more of platinum, palladium, rhodium, iridium, ruthenium, osmium, tungsten.
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 quantum dot, graphene nanometer sheet, graphene oxide, oxygen reduction fossil
One of black alkene or porous graphene.
Further, retain spacing between the coil of the resistance wire.
Further, the thermal conductivity gas sensor can detecte He, CO2、H2、CH4One or more of gas
Mixing.
The invention also discloses a kind of preparation methods of the spherical thermal conductivity gas sensor of pearl, comprising the following steps:
1) spheroid shape resistance wire is wound with coil winding machine；
2) tri compound sensitive material slurry is prepared；
3) resistance wire is welded on pedestal；
4) coating slurry on resistance wire；
5) energization high temperature sintering molding is carried out；
6) shield is coupled on pedestal.
Further, it is prepared described in step 2, 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 glycerol prepared by step (a)
It is mixed by weight 1:0.1~2, 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, xylene 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: by step
(c) carbon nano tube/graphene/α aluminum oxide trielement composite material prepared is mixed with glycerol by weight 1:0.1~2, is surpassed
Sound 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 4, comprising the following steps:
A) the α aluminum oxide slurry of one layer of preparation is coated on the resistance wire；
B) the trielement composite material slurry of preparation is coated outside α aluminum oxide pulp layer and in resistance wire ellipsoid inner cavity.
Further, the molding of high temperature sintering described in step 5 is realized using following procedure: under high pure nitrogen protection, to institute
Semi-finished product load DC voltage is stated, the sintering current of 160mA is passed to, temperature is controlled at 600 DEG C or so, remains powered on 60min.
Beneficial effects of the present invention:
1) carbon nanotube is one-dimensional porous carbon nanomaterial, when thermal conductivity gas sensor and gas are contacted as gas exchanges
Access；Graphene is two-dimentional carbon nanomaterial, has good heating conduction；α aluminum oxide has the only of stable crystal form
Indeformable physical performance under special trace doped load capacity and high temperature, the skeleton as sensitive material.The present invention will be with
Sensitive material of the upper triplicity as the spherical thermal conductivity gas sensor of pearl, so that sensitive material specific surface area with higher
And thermal stability, the heat exchanger effectiveness and thermal adaptability of sensor can be greatlyd improve.
2) resistance wire for using spheroid-like, can effectively improve the surface forming quality and material of the spherical sensing element of pearl
The uniformity coefficient of Density Distribution reduces the even degree of uneven heating of sensitive material when sintering at high temperature, reduces the micro- of internal generation
Crackle, meanwhile, make gas sensor that can form homogeneous temperature field at work, improves the reliability of gas sensor and use the longevity
Life.
3) for graphene sheet as black, carbon nanotube is compound with graphene, can omit the melanism of previous sensitive material preparation
Step enhances thermal energy utilization efficiency, improves radiating efficiency.
The present invention makes full use of the high-specific surface area of trielement composite material and the high characteristic of thermal stability, elliposoidal resistance wire
Forming guidance and homogenizing agglomeration to composite material, make sensing element that there is uniform temperature field and good heat exchange to imitate
Rate achievees the purpose that shorten the response time, improves detection accuracy and prolong the service life.
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 embodiment 1 of spherical thermal conductivity gas sensor of pearl of the present invention and the structural schematic diagram of embodiment 2；
Fig. 2-1 show a kind of sensing element structural schematic diagram of the embodiment 1 of the spherical thermal conductivity gas sensor of pearl of the present invention；
Fig. 2-2 show a kind of sensing element structural profile knot of the embodiment 1 of the spherical thermal conductivity gas sensor of pearl of the present invention
Structure partial enlargement diagram；
Fig. 3-1 show a kind of sensing element cross-section structure of the embodiment 2 of the spherical thermal conductivity gas sensor of pearl of the present invention and shows
It is intended to；
Fig. 3-2 show a kind of sensing element cross-section structure office of the embodiment 2 of the spherical thermal conductivity gas sensor of pearl of the present invention
Portion's enlarged diagram；
Fig. 4 show a kind of process of the embodiment 1 of the spherical thermal conductivity gas sensor preparation method of pearl and embodiment 2 of the present invention
Figure.
The wherein corresponding relationship in Fig. 1 to Fig. 4 between appended drawing reference and component names are as follows:
1, composite material；2, resistance wire；3, sensing element；4, pedestal；5, shelter-clad；6, α aluminum oxide insulating layer.
Specific embodiment
Below in conjunction with 2 the present invention is described in detail of specific embodiment 1 and embodiment.It should be noted that following embodiments
Described in technical characteristic or technical characteristic combination be not construed as it is isolated, they can by be combined with each other to
Reach superior technique effect.
Embodiment 1
The embodiment of the present invention 1 is described in conjunction with Fig. 1, Fig. 2-1 and Fig. 2-2: a kind of spherical thermal conductivity gas sensor of pearl, comprising:
Resistance wire 2, coated on the resistance wire insulating layer 6, coated in being burnt simultaneously on the insulating layer 6 and with the insulating layer 6
The composite material 1 of knot, with the resistance wire be welded to connect pedestal 4, the good air permeability being connect with the base engagement gold
Belong to shield 5.The resistance wire 2 is in hollow ellipsoid shape, and there are the straightways at both ends；6 material of insulating layer is tri- oxygen of α
Change two aluminium nanometer scale ceramics superfines；The composite material 1 is oxidation multi-wall carbon nano-tube tube/oxidation of graphene oxide/α tri- two
The trielement composite material of aluminium.The insulating layer 6 can be such that the resistance wire 2 keeps apart with the composite material 1, between prevention the two
Shunting function.
In embodiment 1, the resistance wire 2 is one or more of platinum, palladium, rhodium, iridium, ruthenium, osmium, tungsten.Preferential selection
Platinum.
In embodiment 1, 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 1, the graphene is graphene quantum dot, graphene nanometer sheet, graphene oxide, reduction-oxidation
One of graphene or porous graphene.Preferential selective oxidation graphene.
In embodiment 1, retain spacing between the coil of the resistance wire 2.
In embodiment 1, the thermal conductivity gas sensor can detecte He, CO2、H2、CH4One of gas or
A variety of mixing.
Referring to fig. 4, the present invention also provides a kind of embodiments: a kind of preparation side of the spherical thermal conductivity gas sensor of pearl
Method, comprising the following steps:
Step 100: being wound spheroid shape resistance wire with coil winding machine；
Step 200: preparing tri compound sensitive material slurry；
Step 300: resistance wire is welded on pedestal；
Step 400: the coating slurry on resistance wire；
Step 500: carrying out energization high temperature sintering molding；
Step 600: shield is coupled on pedestal.
In embodiment 1, it is prepared described in step 200, comprising the following steps:
A) the α aluminum oxide nanometer scale ceramics ultra-fine powder materials are prepared using chemical precipitation method；
B) oxidation multi-wall carbon nano-tube tube/graphene oxide/α aluminum oxide trielement composite material is prepared, process is as follows: by α
1:4~5:4~5 is mixed by volume for aluminum oxide, oxidation multi-wall carbon nano-tube tube, graphene oxide, and mixture is pressed volume
It is added in xylene solution than 1:100~300, stirring makes it be uniformly dispersed, and oxidation multi-wall carbon nano-tube tube/graphite oxide is made
Alkene/α aluminum oxide trielement composite material solution；Above-mentioned solution is centrifuged, washed and dried, oxidation multi wall is obtained
Carbon nanotube/graphene oxide/α aluminum oxide trielement composite material；
C) oxidation multi-wall carbon nano-tube tube/graphene oxide/α aluminum oxide trielement composite material slurry is prepared, process is as follows:
By oxidation multi-wall carbon nano-tube tube/graphene oxide/α aluminum oxide trielement composite material of step (b) preparation and glycerol by weight
Amount is mixed than 1:0.1~2, and ultrasonic disperse makes its mixing sufficiently, and the oxidation multi-wall carbon nano-tube tube/graphene oxide/α tri- is made
Al 2 O trielement composite material slurry.
In embodiment 1, it is coated described in step 400, comprising the following steps:
A) the α aluminum oxide slurry that one layer of preparation is coated on the resistance wire 2, forms insulating layer 6；
B) the trielement composite material slurry of preparation is coated outside α aluminum oxide pulp layer and in resistance wire ellipsoid inner cavity,
Form composite material 1；
In embodiment 1, the molding of high temperature sintering described in step 500 is realized using following procedure: under high pure nitrogen protection, to institute
Semi-finished product load DC voltage is stated, the sintering current of 160mA is passed to, temperature is controlled at 600 DEG C or so, remains powered on 60min.
Embodiment 2
The embodiment of the present invention 2 is described in conjunction with Fig. 1, Fig. 3-1 and Fig. 3-2: a kind of spherical thermal conductivity gas sensor of pearl, construction
Embodiment 1 is improved, comprising: resistance wire 2, coated on the resistance wire insulating layer 6, be coated in the insulating layer
The composite material 1 being sintered simultaneously on 6 and with the insulating layer 6, the pedestal 4 and the pedestal that are welded to connect with the resistance wire
The shelter-clad 5 of the good air permeability of mating connection.The resistance wire 2 is in hollow ellipsoid shape, and there are the straight lines at both ends
Section；The material of the insulating layer 6 is α aluminum oxide nanometer scale ceramics superfines；The composite material 1 is oxidation multi wall carbon
Nanotube/redox graphene/α aluminum oxide trielement composite material.The α aluminum oxide insulating layer 6 of sinter molding
Be divided into two parts: the α aluminum oxide insulating layer 6 coated on the resistance wire 2 can make the resistance wire 2 with it is compound
Material 1 is kept apart, and the shunting function between the two is prevented；The ellipsoid α aluminum oxide insulating layer of 2 inner core of resistance wire
6 prevent irregular flowing of the under test gas inside the resistance wire 2, improve the thermostabilization of thermal conductivity gas sensor
Property.
In example 2, the resistance wire 2 is one or more of platinum, palladium, rhodium, iridium, ruthenium, osmium, tungsten.Preferential selection
Platinum.
In example 2, 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 example 2, the graphene is graphene quantum dot, graphene nanometer sheet, graphene oxide, reduction-oxidation
One of graphene or porous graphene.Preferential selective reduction graphene oxide.
In example 2, retain spacing between the coil of the resistance wire 2.
In example 2, the thermal conductivity gas sensor can detecte He, CO2、H2、CH4One of gas or
A variety of mixing.
Referring to fig. 4, the present invention also provides a kind of embodiments: a kind of preparation side of the spherical thermal conductivity gas sensor of pearl
Method, comprising the following steps:
Step 100: being wound spheroid shape resistance wire with coil winding machine；
Step 200: preparing trielement composite material slurry；
Step 300: resistance wire is welded on pedestal；
Step 400: the coating slurry on resistance wire；
Step 500: carrying out energization high temperature sintering molding；
Step 600: shield is coupled on pedestal.
In example 2, it is prepared described in step 200, comprising the following steps:
A) α aluminum oxide nanometer scale ceramics ultra-fine powder materials are prepared using chemical precipitation method；
B) oxidation multi-wall carbon nano-tube tube/redox graphene/α aluminum oxide trielement composite material is prepared, process is as follows:
By α aluminum oxide, oxidation multi-wall carbon nano-tube tube, redox graphene, 1:4~5:4~5 is mixed by volume, by mixture
1:100~300 is added in xylene solution by volume, and stirring makes it be uniformly dispersed, and oxidation multi-wall carbon nano-tube tube/reduction is made
Graphene oxide/α aluminum oxide trielement composite material solution；Above-mentioned solution is centrifuged, washed and dried, is obtained
Oxidation multi-wall carbon nano-tube tube/redox graphene/α aluminum oxide trielement composite material；
C) prepare α aluminum oxide slurry, process is as follows: α aluminum oxide nanometer scale ceramics prepared by step (a) are ultra-fine
Dusty material is mixed with glycerol by weight 1:0.1~2, and ultrasonic disperse makes its mixing sufficiently, and α aluminum oxide slurry is made；
D) oxidation multi-wall carbon nano-tube tube/redox graphene/α aluminum oxide trielement composite material slurry, process are prepared
It is as follows: by step (b) preparation oxidation multi-wall carbon nano-tube tube/redox graphene/α aluminum oxide trielement composite material with
Glycerol is mixed by weight 1:0.1~2, and ultrasonic disperse makes its mixing sufficiently, and oxidation multi-wall carbon nano-tube tube/oxygen reduction fossil is made
Black alkene/α aluminum oxide trielement composite material slurry.
In example 2, on resistance wire 2 described in step 400 the step of coating slurry in two steps, specifically, first described
Upper suitable α aluminum oxide slurry is filled in resistance wire ellipsoid inner cavity, then is coated one layer of α tri- on the resistance wire and aoxidized
Two aluminum slurries；Oxidation multi-wall carbon nano-tube tube/oxidation of redox graphene/α tri- two is coated outside α aluminum oxide pulp layer again
Aluminium trielement composite material slurry.
In example 2, the molding of high temperature sintering described in step 500 is realized using following procedure: under high pure nitrogen protection,
DC voltage is loaded to the semi-finished product, passes to the sintering current of 160mA, temperature is controlled at 600 DEG C or so, remained powered on
60min。
The present invention makes full use of the high-specific surface area of trielement composite material and the high characteristic of thermal stability, elliposoidal resistance wire
Forming guidance and homogenizing agglomeration to composite material, make sensing element that there is uniform temperature field and good heat exchange to imitate
Rate achievees the purpose that shorten the response time, improves detection accuracy and prolong the service life.
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 (10)
1. a kind of spherical thermal conductivity gas sensor of pearl, comprising: resistance wire, coated on resistance wire insulating layer, be coated in institute
Composite material, the pedestal and base engagement with resistance wire welded connecting stated on insulating layer and be sintered simultaneously with the insulating layer
The shelter-clad of the good air permeability of connection；Resistance wire is in hollow ellipsoid shape, and there are the straightways at both ends；Insulating layer material
Material isAluminum oxide nanometer scale ceramics superfines, composite material be carbon nano tube/graphene/The three of aluminum oxide
First composite material；Insulating layer can be such that resistance wire keeps apart with composite material, prevent the shunting function between the two.
2. the spherical thermal conductivity gas sensor of pearl as described in claim 1, which is characterized in that the resistance wire be platinum, palladium,
One or more of rhodium, iridium, ruthenium, osmium, tungsten.
3. the spherical thermal conductivity gas sensor of pearl as described in claim 1, which is characterized in that the carbon nanotube is that oxidation is single
Wall carbon nano tube, oxidation one of double-walled carbon nano-tube or oxidation multi-wall carbon nano-tube tube.
4. the spherical thermal conductivity gas sensor of pearl as described in claim 1, which is characterized in that the graphene is graphene amount
One of sub- point, graphene nanometer sheet, graphene oxide, redox graphene or porous graphene.
5. the spherical thermal conductivity gas sensor of pearl as described in claim 1, which is characterized in that between the coil of the resistance wire
Retain spacing.
6. the spherical thermal conductivity gas sensor of pearl as described in claim 1, which is characterized in that the thermal conductivity gas sensor
It can detecte He, CO2、H2、CH4The mixing of one or more of gas.
7. the preparation method of the spherical thermal conductivity gas sensor of pearl as described in claim 1, which is characterized in that including following step
It is rapid:
1) spheroid shape resistance wire is wound with coil winding machine；
2) tri compound sensitive material slurry is prepared；
3) resistance wire is welded on pedestal；
4) coating slurry on resistance wire；
5) energization high temperature sintering molding is carried out；
6) shield is coupled on pedestal.
8. the preparation method of the spherical thermal conductivity gas sensor of pearl as claimed in claim 7, which is characterized in that described in step 2
Preparation, 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 glycerol
It is mixed by weight 1:0.1 ~ 2, 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, xylene 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 glycerol by weight 1:0.1 ~ 2, ultrasonic disperse
Make its mixing sufficiently, obtained carbon nano tube/graphene/Aluminum oxide trielement composite material slurry.
9. the preparation method of the spherical thermal conductivity gas sensor of pearl as claimed in claim 7, which is characterized in that described in step 4
Coating, comprising the following steps:
A) one layer of preparation is coated on the resistance wireAluminum oxide slurry；
B) existThe trielement composite material slurry of preparation is coated outside aluminum oxide pulp layer and in resistance wire ellipsoid inner cavity.
10. the preparation method of the spherical thermal conductivity gas sensor of pearl as claimed in claim 7, which is characterized in that described in step 5
High temperature sintering molding is realized using following procedure: under high pure nitrogen protection, being loaded DC voltage to the semi-finished product, is passed to
The sintering current of 160mA, temperature are controlled at 600 DEG C or so, remain powered on 60min.
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