CN107827150A - A kind of nickel doped tin oxide nano material, formaldehyde gas sensor and preparation method - Google Patents
A kind of nickel doped tin oxide nano material, formaldehyde gas sensor and preparation method Download PDFInfo
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- CN107827150A CN107827150A CN201711341703.0A CN201711341703A CN107827150A CN 107827150 A CN107827150 A CN 107827150A CN 201711341703 A CN201711341703 A CN 201711341703A CN 107827150 A CN107827150 A CN 107827150A
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- nickel
- tin oxide
- nano material
- oxide nano
- gas sensor
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 294
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 238
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 119
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 90
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000002105 nanoparticle Substances 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 92
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 19
- 239000003153 chemical reaction reagent Substances 0.000 claims description 17
- 239000012043 crude product Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 239000012046 mixed solvent Substances 0.000 claims description 11
- 238000012544 monitoring process Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 235000013339 cereals Nutrition 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 235000011150 stannous chloride Nutrition 0.000 claims description 9
- 229910052571 earthenware Inorganic materials 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000012805 post-processing Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 229910018487 Ni—Cr Inorganic materials 0.000 claims description 3
- 238000003483 aging Methods 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 235000011868 grain product Nutrition 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical class Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- VRVAZSINCAZFLH-UHFFFAOYSA-N oxygen(2-) tin(4+) titanium(4+) Chemical compound [O--].[O--].[Ti+4].[Sn+4] VRVAZSINCAZFLH-UHFFFAOYSA-N 0.000 claims 1
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims 1
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims 1
- 230000004044 response Effects 0.000 abstract description 31
- 230000035945 sensitivity Effects 0.000 abstract description 20
- 238000001514 detection method Methods 0.000 description 15
- 239000007787 solid Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 229930040373 Paraformaldehyde Natural products 0.000 description 9
- 229920002866 paraformaldehyde Polymers 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000005352 clarification Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000002242 deionisation method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical class O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000011540 sensing material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 208000002454 Nasopharyngeal Carcinoma Diseases 0.000 description 1
- 206010061306 Nasopharyngeal cancer Diseases 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007799 dermal corrosion Effects 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000003 human carcinogen Toxicity 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 208000032839 leukemia Diseases 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 201000011216 nasopharynx carcinoma Diseases 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 231100000108 skin corrosion Toxicity 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- -1 the burn feeling of eye nose larynx Diseases 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Pathology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Combustion & Propulsion (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of nickel doped tin oxide nano material, the tin oxide nano particles of nickel doping are included, the atomicity percentage of nickel doping is 0.1%~10%, and the particle diameter of nano particle is not more than 250nm, and nano grain surface is into coarse ellipsoid.The invention provides the preparation method and its usage of nickel doped tin oxide nano material.Present invention also offers the formaldehyde gas sensor for including nickel doped tin oxide nano material, preparation method and the usage.The tin oxide base formaldehyde gas sensor of nickel doped tin oxide nano material and nickel doping prepared by the present invention has the characteristics of fast response time, high sensitivity, selectivity is good, operating temperature is low, ultralow detectable limit and long-time stability are good.
Description
Technical field
The present invention relates to gas sensing techniques field, more particularly to a kind of nickel doped tin oxide nano material, formaldehyde air-sensitive
Sensor and preparation method.
Background technology
Formaldehyde is a kind of colourless, flammable and strong smell material, often in construction material and family product.It is general to occupy
Formaldehyde source in room mainly includes punching press Wood products, smoking and combustion apparatus.When the aerial concentration of formaldehyde exceedes
During 0.1ppm (0.1 part of content of formaldehyde in every 1,000,000 parts of air), some people might have various short-term adverse reactions, such as flow
Tear, the burn feeling of eye nose larynx, cough, asthma, nausea and skin corrosion etc..And millworker, lab assistant and some medical treatment
Staff may be chronically exposed to the formaldehyde environment than general public higher concentration, face bigger health risk.At present,
Formaldehyde is classified as one of known human carcinogen by international cancer research institution (IARC), while some are directed in work and contacted
The research of the people of formaldehyde shows, formaldehyde induced with several cancers have it is close contact, including nasopharyngeal carcinoma and leukaemia.
Current existing formaldehyde sensor species, including the semiconductor gas sensor of the reproducibility based on formaldehyde gas,
Visualization fluorescence formaldehyde sensor, formaldehyde sonic surface wave gas sensors based on silica gel particle, based on molecular sieve adsorption mechanism
Formaldehyde gas molecular sieve sensor and formaldehyde gas electronic nose.Wherein, sensor is based on Metal Oxide Semiconductor Gas Sensing material
Material has the advantages that preparation is simple, cost is cheap, but for methanol, ethanol, benzene, toluene, hydrogen sulfide, ammonia in actual environment be present
Selectivity is not high during the interference of the gas molecule such as air-liquid gas and gasoline, and testing result has certain error.
Tin ash is applied earliest in one of the material in semiconductor gas sensor field, and it has preferable crystal knot
Structure, electrical conductivity and be applicable it is strong the advantages that, be always research and application focus.Tin ash Metal Oxide Semiconductor Gas Sensing material
Material, belongs to N-type semiconductor, the oxygen during it adsorbs air in 200~300 DEG C of temperature, forms the anion absorption of oxygen, makes semiconductor
In electron density reduce so that its resistance value increase, when detecting reducibility gas resistance with the increase of gas concentration and
Reduce.In actual applications pure tin dioxide gas-sensitive material have that PARA FORMALDEHYDE PRILLS(91,95) responsiveness is not high and selectivity it is bad etc. it is many not
Foot.In the prior art, other noble metals are doped to tin ash to improve the defects of it is as gas sensitive, such as platinum
(Pt), palladium (Pd) and golden (Au) etc., but doped precious metal is expensive to have the defects of serious pollution environment.In addition, existing partly lead
The shortcomings of body gas sensor also deposits temperature drift at work, and the response time is long, be badly in need of further exploitation performance it is more preferable, compared with
PARA FORMALDEHYDE PRILLS(91,95) molecules in response high sensitivity, the gas sensing material that the response time is short and selectivity is good, are solved existing under low temperature
The above-mentioned deficiency of semiconductor gas sensor in technology.
Therefore, those skilled in the art is directed to developing a kind of nickel doped tin oxide nano material, formaldehyde gas sensing
Device and preparation method.
The content of the invention
In view of the drawbacks described above of prior art, the technical problems to be solved by the invention are existing tin ash semiconductors
Gas sensor PARA FORMALDEHYDE PRILLS(91,95) response sensitivity is not high, selectivity is bad, detectable limit is not up to standard and operating temperature is higher.
To achieve the above object, the invention provides a kind of nickel doped tin oxide nano material, it includes the two of nickel doping
Tin oxide nanoparticles；Wherein, the atomicity percentage of nickel doping is 0.1%~10%, and the particle diameter of the nano particle is little
In 250nm.
Further, the nano grain surface is into coarse ellipsoid；
Further, the atomicity percentage of the nickel doping is 1%~10%；Preferably 2.5%~7.5%.
Present invention also offers a kind of preparation method of nickel doped tin oxide nano material, comprise the following steps：
Step 1-1, oxalic acid and tin source reagent are added in solvent, nickel source reagent and surfactant are added after stirring, is stirred
Mix to obtain mixed solution；
Step 1-2, the mixed solution that step 1-1 is obtained is prepared using a step solvent-thermal method, post processing obtains nickel doping
Tin oxide nanoparticles crude product；
Step 1-3, the tin oxide nanoparticles crude product that step 1-2 is obtained is dried, calcine obtain nickel doping two
Tin oxide nanoparticles product.
Further, in the step 1-1, tin source reagent is selected from two hydrated stannous chlorides, five hydrous tin chlorides or sulfuric acid
One or more combinations in stannous；
Further, in the step 1-1, nickel source reagent is selected from Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate or nickel sulfate
Middle one or more combinations；
Further, in the step 1-1, surfactant is polyvinylpyrrolidone；
Further, in the step 1-1, solvent is a kind of in water, ethanol or the mixed solvent of water and ethanol composition；
Further, in the step 1-1, the w/v (mg/ml) of tin source reagent and solvent is 2:1~4:
1；It is preferred that 3:1~4:1；
Further, in the step 1-2, a step solvent-thermal method is selected from hydro-thermal method or microwave-hydrothermal method；
Further, the reaction temperature of the hydro-thermal method is 160~240 DEG C, and the reaction time is 10~48h；The microwave
The reaction temperature of hydro-thermal method is 150~220 DEG C, and the microwave reaction time is 5~20min, and microwave pressure is not more than 20MPa；
Further, in the step 1-2, post processing includes washing, centrifugation；
Further, the solvent of the washing is a kind of in water, ethanol or the mixed solvent of water and ethanol composition；It is described
Centrifugal speed is 5000~10000rpm, and centrifugation time is 5~20min；
Further, in the step 1-3, drying temperature is 50~100 DEG C, and drying time is 5~24h；
Further, in the step 1-3, calcining heat is 300~500 DEG C, and calcination time is 1~5h.
Present invention also offers using nickel doped tin oxide nano material and any of the above-described system described in any of the above-described
The method that the nickel doped tin oxide nano material that Preparation Method is prepared prepares formaldehyde gas sensor, including nickel is adulterated and aoxidized
Tin nano material, which is coated on heater-type gas sensor, is made formaldehyde gas sensor.
Further, the method for preparing formaldehyde gas sensor, comprises the following steps：
Step 2-1, above-mentioned nickel doped tin oxide nano grain products are mixed with alcohol reagent and are coated in alumina tube
On outer surface, earthenware is inserted；
Step 2-2, by small Ni-Cr alloy heating coil inserting step 2-1 earthenware；
Step 2-3, step 2-2 earthenware is welded on hexagonal base and obtains a formaldehyde gas sensor unit；
Step 2-4, the sensor unit of manufacture is obtained into formaldehyde gas sensor in 180 DEG C of heat ageings.
Further, in the step 2-1, one or more of the alcohol reagent in methanol, ethanol, propyl alcohol, butanol.
In the better embodiment of the present invention, in the tin oxide nano particles of the nickel doping, the atom of nickel doping
Number percentage is 1%；
In another better embodiment of the present invention, in the tin oxide nano particles of the nickel doping, nickel doping
Atomicity percentage is 2.5%；
In another better embodiment of the present invention, in the tin oxide nano particles of the nickel doping, nickel doping
Atomicity percentage is 5%；
In another better embodiment of the present invention, in the tin oxide nano particles of the nickel doping, nickel doping
Atomicity percentage is 7.5%；
In another better embodiment of the present invention, in the tin oxide nano particles of the nickel doping, nickel doping
Atomicity percentage is 10%；
In another better embodiment of the present invention, in the step 1-1, tin source reagent is two hydrated stannous chlorides；
In another better embodiment of the present invention, in the step 1-1, nickel source reagent is Nickel dichloride hexahydrate；
In another better embodiment of the present invention, in the step 1-1, solvent is the mixed solvent of water and ethanol；
Wherein, the volume of water and ethanol (milliliter) is than being=1:1；
In another better embodiment of the present invention, in the step 1-1, the w/v of tin source reagent and solvent
(mg/ml) is 3.8:1；
In another better embodiment of the present invention, in the step 2-1, alcohol reagent is ethanol.
Present invention also offers nickel doped tin oxide nano material described in any of the above-described of the present invention, and any one to prepare
The purposes of nickel doped tin oxide nano material prepared by method in preparing for formaldehyde gas sensor.
Present invention also offers nickel doped tin oxide nano material described in any of the above-described of the present invention, and any one to prepare
The purposes of nickel doped tin oxide nano material prepared by method in preparing for Formaldehyde.
Present invention also offers formaldehyde air-sensitive prepared by nickel doped tin oxide nano material described in any of the above-described of the present invention
Purposes of the sensor in preparing for Formaldehyde；
Present invention also offers formaldehyde air-sensitive biography prepared by any of the above-described formaldehyde gas sensor preparation method of the present invention
Sensor is being prepared for the purposes in formaldehyde gas monitoring；
The formaldehyde gas monitoring carries out formaldehyde response using computer controlled measurement system WS-30A in surrounding air
Detection, object gas amount is injected in WS-30A closed chamber, by computer software monitoring record response condition, record sensor
Resistance, obtain monitoring the numerical value of formaldehyde gas.
Monitoring response sensitivity represents that S is defined as=R with Sa/Rg, wherein, RaAnd RgIt is in air respectively and object gas
In sensor resistance.
Using above scheme, nickel doped tin oxide nano material, formaldehyde gas sensor and preparation side disclosed by the invention
Method, there is advantages below：
The preparation technology of the tin oxide nanoparticles of nickel doping prepared by the present invention is simple, and raw material sources are extensive and price is low
It is honest and clean, easily realize industrialized production and application；
The present invention nickel doping stannic oxide nano material and its preparation formaldehyde gas sensor have fast response time,
High sensitivity, the beneficial effect that selectivity is good, operating temperature is low and long-time stability are good；
Nano material of the present invention optimizes metal-doped species, doping ratio, makes the semiconductor gas of tin oxide gas sensor
Body sensor material evades other precious metal dopings, reduces cost, opens up new doping direction, green, can be in reality
Reduced to greatest extent in the application of border and prepare cost, can be widely applied to low concentration formaldehyde air-sensitive monitoring field, have great
Application prospect.
Design, concrete technical scheme and the caused technique effect of the present invention are made into one below with reference to preferred embodiment
Step explanation, to be fully understood from the purpose of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph figure for the nickel doped tin oxide nano material that embodiment 1 is prepared；
Fig. 2 be the nickel doped tin oxide nano material of embodiment 1 prepare formaldehyde gas sensor at 200 DEG C to containing difference
The formaldehyde response-recovery performance map of concentration formaldehyde gas；
Fig. 3 be the nickel doped tin oxide nano material of embodiment 1 prepare formaldehyde gas sensor at 200 DEG C to various concentrations
The sensitivity curve of formaldehyde gas (illustration is the linear fit curve under low concentration)；
Fig. 4 is formaldehyde gas sensor prepared by the nickel doped tin oxide nano material of embodiment 1 and comparative example 6 undoped with nickel
Pure zirconia tin nano material prepare formaldehyde gas sensor 200 DEG C carry out 100ppm concentration under each gas air-sensitive selection
Performance map；
Fig. 5 be the nickel doped tin oxide nano material of embodiment 1 prepare formaldehyde gas sensor at 200 DEG C, 100ppm is dense
The formaldehyde gas long-time stability detection performance figure of degree.
Embodiment
Multiple preferred embodiments of the invention introduced below, make its technology contents more clear and readily appreciate.The present invention
It can be emerged from by many various forms of embodiments, these embodiments are exemplary description, protection model of the invention
Enclose the embodiment for being not limited only to mention in text.
If there is the experimental method of unreceipted actual conditions, generally according to normal condition, such as instructions book or handbook
Implemented.
The preparation of embodiment 1, nickel doped tin oxide nano material
Step 1, two hydrated stannous chlorides (1mmol) of two oxalic acid hydrates and 226mg that weigh 3.0g are added to water：It is anhydrous
Ethanol is 1:1 60mL in the mixed solvents, stir to solid dissolving, solution and become clarification；
Step 2,11.9mg Nickel dichloride hexahydrates (0.05mmol) are weighed to obtain with 1.0g polyvinylpyrrolidones addition step 1
To solution in, stir to obtain mixed solution；
Step 3, mixed solution above-mentioned steps obtained is warming up to 200 DEG C of heating 12h, is down to room temperature and uses deionization respectively
Water and ethanol alternately wash, and then centrifuge 10min in the case where centrifugal speed is 8000rpm, obtain the tin oxide nano of nickel doping
Grain crude product；
Step 4, by tin oxide nanoparticles crude product 60 DEG C of dry 24h in an oven of nickel doping, solid after drying is put
In high-temperature crucibles, Muffle furnace programming rate is set to carry out 400 DEG C of calcining 1h of Muffle furnace after 5 DEG C/min, cooling obtains nickel and mixed
Miscellaneous tin oxide nano particles product.
The tin oxide nano particles that obtained nickel adulterates are scanned testing electronic microscope, as shown in figure 1, this reality
It is uniform to apply the tin oxide nano particles appearance and size of the nickel doping of example, and pattern is shaggy " ellipsoid "；Grain size
Within 250nm.
The preparation of embodiment 2, nickel doped tin oxide nano material
Step 1, two hydrated stannous chlorides (1mmol) of two oxalic acid hydrates and 226mg that weigh 3.0g are added to water：It is anhydrous
Ethanol is 1:1 60mL in the mixed solvents, stir to solid dissolving, solution and become clarification；
Step 2,2.4mg Nickel dichloride hexahydrates (0.01mmol) are weighed to obtain with 1.0g polyvinylpyrrolidones addition step 1
To solution in, stir to obtain mixed solution；
Step 3, mixed solution above-mentioned steps obtained is warming up to 160 DEG C of heating 48h, is down to room temperature and uses deionization respectively
Water and ethanol alternately wash, and then centrifuge 20min in the case where centrifugal speed is 5000rpm, obtain the tin oxide nano of nickel doping
Grain crude product；
Step 4, by tin oxide nanoparticles crude product 80 DEG C of dry 18h in an oven of nickel doping, solid after drying is put
In high-temperature crucibles, Muffle furnace programming rate is set to carry out 300 DEG C of calcining 4h of Muffle furnace after 5 DEG C/min, cooling obtains nickel and mixed
Miscellaneous tin oxide nano particles product.
The preparation of embodiment 3, nickel doped tin oxide nano material
Step 1, two hydrated stannous chlorides (1mmol) of two oxalic acid hydrates and 226mg that weigh 3.0g are added to water：It is anhydrous
Ethanol is 1:1 60mL in the mixed solvents, stir to solid dissolving, solution and become clarification；
Step 2,6.00mg Nickel dichloride hexahydrates (0.025mmol) are weighed and add step 1 with 1.0g polyvinylpyrrolidones
In obtained solution, mixed solution is stirred to obtain；
Step 3, mixed solution above-mentioned steps obtained is warming up to 240 DEG C of heating 10h, is down to room temperature and uses deionization respectively
Water and ethanol alternately wash, and then centrifuge 5min in the case where centrifugal speed is 10000rpm, obtain the tin oxide nano of nickel doping
Grain crude product；
Step 4, by tin oxide nanoparticles crude product 100 DEG C of dry 5h in an oven of nickel doping, solid after drying is put
In high-temperature crucibles, Muffle furnace programming rate is set to carry out 500 DEG C of calcining 1h of Muffle furnace after 5 DEG C/min, cooling obtains nickel and mixed
Miscellaneous tin oxide nano particles product.
The preparation of embodiment 4, nickel doped tin oxide nano material
Step 1, two hydrated stannous chlorides (1mmol) of two oxalic acid hydrates and 226mg that weigh 3.0g are added to water：It is anhydrous
Ethanol is 1:1 60mL in the mixed solvents, stir to solid dissolving, solution and become clarification；
Step 2,17.9m Nickel dichloride hexahydrates (0.075mmol) are weighed to obtain with 1.0g polyvinylpyrrolidones addition step 1
To solution in, stir to obtain mixed solution；
Step 3, mixed solution above-mentioned steps obtained is warming up to 200 DEG C of heating 12h, is down to room temperature and uses deionization respectively
Water and ethanol alternately wash, and then centrifuge 10min in the case where centrifugal speed is 8000rpm, obtain the tin oxide nano of nickel doping
Grain crude product；
Step 4, by tin oxide nanoparticles crude product 50 DEG C of dry 24h in an oven of nickel doping, solid after drying is put
In high-temperature crucibles, Muffle furnace programming rate is set to carry out 400 DEG C of calcining 5h of Muffle furnace after 5 DEG C/min, cooling obtains nickel and mixed
Miscellaneous tin oxide nano particles product.
The preparation of embodiment 5, nickel doped tin oxide nano material
Step 1, two hydrated stannous chlorides (1mmol) of two oxalic acid hydrates and 226mg that weigh 3.0g are added to water：It is anhydrous
Ethanol is 1:1 60mL in the mixed solvents, stir to solid dissolving, solution and become clarification；
Step 2,23.8mg Nickel dichloride hexahydrates (0.1mmol) are weighed to obtain with 1.0g polyvinylpyrrolidones addition step 1
To solution in, stir to obtain mixed solution；
Step 3, mixed solution above-mentioned steps obtained is warming up to 200 DEG C of heating 12h, is down to room temperature and uses deionization respectively
Water and ethanol alternately wash, and then centrifuge 10min in the case where centrifugal speed is 8000rpm, obtain the tin oxide nano of nickel doping
Grain crude product；
Step 4, by tin oxide nanoparticles crude product 60 DEG C of dry 24h in an oven of nickel doping, solid after drying is put
In high-temperature crucibles, Muffle furnace programming rate is set to carry out 400 DEG C of calcining 1h of Muffle furnace after 5 DEG C/min, cooling obtains nickel and mixed
Miscellaneous tin oxide nano particles product.
The preparation of comparative example 6, stannic oxide nano material undoped with nickel
Step 1, two hydrated stannous chlorides (1mmol) of two oxalic acid hydrates and 226mg that weigh 3.0g are added to water：It is anhydrous
Ethanol is 1:1 60mL in the mixed solvents, stir to solid dissolving, solution and become clarification；
Step 2,1.0g polyvinylpyrrolidones are weighed to add in the solution that step 1 obtains, stir to obtain mixed solution；
Step 3, mixed solution above-mentioned steps obtained is warming up to 200 DEG C of heating 12h, is down to room temperature and uses deionization respectively
Water and ethanol alternately wash, and then centrifuge 10min in the case where centrifugal speed is 8000rpm, obtain the tin oxide nano undoped with nickel
Particle crude product；
Step 4, by the 60 DEG C of dry 24h in an oven of the tin oxide nanoparticles crude product undoped with nickel, by solid after drying
It is put in high-temperature crucibles, Muffle furnace programming rate is set to carry out 400 DEG C of calcining 1h of Muffle furnace after 5 DEG C/min, cooling obtains not
Adulterate the tin oxide nano particles product of nickel.
The preparation of embodiment 7, formaldehyde gas sensor
Step 1, nickel doped tin oxide nano grain products and comparative example 6 that above-described embodiment 1~5 obtains are obtained
Tin oxide nano particles product undoped with nickel is mixed and is coated on the outer surface of alumina tube with ethanol respectively, insertion pottery
Porcelain tube；
Step 2, by the earthenware of small Ni-Cr alloy heating coil inserting step 1；
Step 3, the earthenware of step 2 is welded on hexagonal base and obtains a formaldehyde gas sensor unit；
Step 4, the sensor unit of manufacture is obtained into formaldehyde gas sensor in 180 DEG C of heat ageings.
Test example 8, formaldehyde response detection
Detection method：
Formaldehyde response detection is carried out in surrounding air using computer controlled measurement system WS-30A, by object gas amount
Inject in WS-30A closed chamber, by computer software monitoring record response condition, sensitivity (S) is defined as S=Ra/Rg(RaAnd Rg
It is the resistance with the sensor in object gas in air respectively)
The formaldehyde gas monitoring carries out formaldehyde response using computer controlled measurement system WS-30A in surrounding air
Detection, object gas amount is injected in WS-30A closed chamber, by computer software monitoring record response condition, record sensor
Resistance, obtain monitoring the response numerical value of formaldehyde gas.
Monitoring response sensitivity represents that S is defined as=R with Sa/Rg, wherein, RaAnd RgIt is in air respectively and object gas
In sensor resistance.
Analysis of test results：
(1) formaldehyde gas sensor and comparative example 6 prepared by the nickel doped tin oxide nano material of embodiment 1~5 undoped with
It is sensitive that formaldehyde gas sensor prepared by the pure zirconia tin nano material of nickel carries out the response of 50ppm concentration formaldehyde at 200 DEG C respectively
Degree detection；
Result data is as shown in table 1：
The tin oxide gas sensitive of different nickel doping contrasts to the responsiveness of 50ppm formaldehyde at 1 200 DEG C of table
| Embodiment | Comparative example 6 | Embodiment 2 | Embodiment 3 | Embodiment 1 | Embodiment 4 | Embodiment 5 |
| Nickel doping concentration (at%) | 0 | 1 | 2.5 | 5 | 7.5 | 10 |
| Sensitivity (Ra/Rg) | 5.3 | 25.9 | 62.4 | 104.3 | 54.4 | 22.9 |
The data of table 1 show that the formaldehyde response sensitivity of pure zirconia tin nano material of the comparative example 6 undoped with nickel is 5.3, this
The formaldehyde response sensitivity of the nickel doped tin oxide nano material of inventive embodiments is more than 22, higher than the oxidation sijna undoped with nickel
The formaldehyde response sensitivity of rice material；The tin oxide gas that the nickel for being 2.5%~7.5% in the atomicity percentage of nickel doping adulterates
Quick material, formaldehyde response sensitivity reach more than 50.Show nickel doped tin oxide nano material of the embodiment of the present invention and preparation
Formaldehyde gas sensor, relative to pure zirconia tin nano material and the formaldehyde gas sensor of preparation undoped with nickel, tool
There is more excellent monitoring formaldehyde gas response performance.
(2) formaldehyde gas sensor prepared by the nickel doped tin oxide nano material of embodiment 1 at 200 DEG C to containing different dense
Spend the formaldehyde response-recovery performance detection of formaldehyde gas；
As a result as shown in Fig. 2 display the embodiment of the present invention 1 formaldehyde gas sensor PARA FORMALDEHYDE PRILLS(91,95) concentration for 1ppm~
The detection response of 50ppm formaldehyde gas recovers all within 30s, shows the nickel doped tin oxide nano of the embodiment of the present invention 1
Material and the formaldehyde gas sensor of preparation have more excellent response-recovery performance.
(3) formaldehyde gas sensor prepared by the nickel doped tin oxide nano material of embodiment 1 is at low concentration formaldehyde (50ppm)
Within, linear change is presented with detectable concentration in response sensitivity.This hair can be calculated according to the linear fit parameter of Fig. 3 illustration
The theoretical lowest detection limit of bright middle formaldehyde gas sensor：
The lowest detection limit (Limit of Detection, LOD)=3 × (Standard Deviation/Slope)
It is calculated as：The ≈ 0.121ppm ≈ 120ppb of LOD=3 × 0.07918 ÷ 1.9561
Result of calculation shows, the formaldehyde air-sensitive that in theory prepared by the nickel doped tin oxide nano material of the embodiment of the present invention 1
Sensor has ultralow detectable limit, is 120ppb, and such detectable limit can to greatest extent be ensured personal safety, had
Considerable application prospect.
(4) the formaldehyde gas sensor and comparative example 6 that prepared by the nickel doped tin oxide nano material of embodiment 1 are undoped with nickel
The response spirit of each gas under formaldehyde gas sensor prepared by pure zirconia tin nano material carries out 100ppm concentration at 200 DEG C respectively
Sensitivity detects；
As a result as shown in figure 4, the formaldehyde air-sensitive prepared using the nickel doped tin oxide nano material of the embodiment of the present invention 1 is passed
Sensor, the response sensitivity of PARA FORMALDEHYDE PRILLS(91,95) are significantly larger than the response sensitivity of other gases, show the nickel doping of the embodiment of the present invention 1
Stannic oxide nano material and the formaldehyde gas sensor PARA FORMALDEHYDE PRILLS(91,95) gas of preparation have excellent air-sensitive selectivity.
(5) formaldehyde gas sensor prepared by the nickel doped tin oxide nano material of embodiment 1 is at 200 DEG C, 100ppm concentration
The lower response sensitivity detection for carrying out long-term use of detection formaldehyde gas；
As a result as shown in figure 5, the formaldehyde air-sensitive prepared using the nickel doped tin oxide nano material of the embodiment of the present invention 1 is passed
Sensor, the response sensitivity of PARA FORMALDEHYDE PRILLS(91,95) still had the sensitive number of degrees more than 100 at 60 days under 200 DEG C, 100ppm concentration
Value, shows, the PARA FORMALDEHYDE PRILLS(91,95) gas of the nickel doped tin oxide nano material of the embodiment of the present invention 1 and the formaldehyde gas sensor of preparation
The detection long-time stability of body are good, the Formaldehyde being applicable in actual environment
In summary, the nickel doped tin oxide nano material of the embodiment of the present invention and the formaldehyde gas sensor first of preparation
Aldehyde response sensitivity is high, has excellent monitoring formaldehyde gas response performance and response-recovery performance, PARA FORMALDEHYDE PRILLS(91,95) gas has
Excellent air-sensitive selectivity, long-time stability are good.
Other embodiment technical scheme of the present invention also has beneficial effect similar to above.
Preferred embodiment of the invention described in detail above.It should be appreciated that the ordinary skill of this area is without wound
The property made work can makes many modifications and variations according to the design of the present invention.Therefore, all technician in the art
Pass through logic analysis, reasoning or the available technology of limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. a kind of nickel doped tin oxide nano material, it is characterised in that include the tin oxide nano particles of nickel doping；Wherein,
The atomicity percentage of nickel doping is 0.1%~10%, and the particle diameter of the nano particle is not more than 250nm.
2. nano material as claimed in claim 1, it is characterised in that the atomicity percentage of the nickel doping is 1%~10%；
The nano grain surface is into coarse ellipsoid.
3. a kind of preparation method of nickel doped tin oxide nano material, it is characterised in that comprise the following steps：
Step 1-1, oxalic acid and tin source reagent are added in solvent, nickel source reagent and surfactant are added after stirring, is stirred
Mixed solution；
Step 1-2, the mixed solution that step 1-1 is obtained is prepared using a step solvent-thermal method, post processing obtains the oxygen of nickel doping
Change tin nanoparticles crude product；
Step 1-3, the tin oxide nanoparticles crude product that step 1-2 is obtained is dried, calcine obtain nickel doping titanium dioxide
Tin nanoparticles product.
4. preparation method as claimed in claim 3, it is characterised in that in the step 1-1,
The one or more combinations in two hydrated stannous chlorides, five hydrous tin chlorides or stannous sulfate of tin source reagent；
The one or more combinations in Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate or nickel sulfate of nickel source reagent；
Surfactant is polyvinylpyrrolidone；
Solvent is a kind of in water, ethanol or the mixed solvent of water and ethanol composition；
The w/v of tin source reagent and solvent is 2:1~4:1.
5. preparation method as claimed in claim 3, it is characterised in that
In the step 1-2, a step solvent-thermal method is selected from hydro-thermal method or microwave-hydrothermal method；
Wherein, the reaction temperature of the hydro-thermal method is 160~240 DEG C, and the reaction time is 10~48h；The microwave-hydrothermal method
Reaction temperature is 150~220 DEG C, and the microwave reaction time is 5~20min, and microwave pressure is not more than 20MPa；
In the step 1-2, post processing includes washing, centrifugation；
Wherein, the solvent of the washing is a kind of in water, ethanol or the mixed solvent of water and ethanol composition；The centrifugal speed
For 5000~10000rpm, centrifugation time is 5~20min；
In the step 1-3, drying temperature is 50~100 DEG C, and drying time is 5~24h；
In the step 1-3, calcining heat is 300~500 DEG C, and calcination time is 1~5h.
6. the nickel doped tin oxide nano material that a kind of any one of claim 3~5 preparation method obtains, its feature exist
In the atomicity percentage that nickel adulterates in the nano material is 1%~10%, the particle diameter of nano particle in the nano material
No more than 250nm, nano grain surface is into coarse ellipsoid in the nano material.
7. a kind of formaldehyde gas sensor, it is characterised in that received including any one of the claim 1~2 nickel doped stannum oxide
Rice material, or the nickel doped tin oxide nano material that any one of claim 3~5 preparation method obtains；Wherein, the nickel
In doped tin oxide nano material, the atomicity percentage of nickel doping is 0.1%~10%, in the nano material, nanometer
The particle diameter of grain is not more than 250nm.
8. a kind of preparation method of formaldehyde gas sensor, it is characterised in that including nickel doped tin oxide nano material is coated
Formaldehyde gas sensor is made on to heater-type gas sensor.
9. preparation method as claimed in claim 8, it is characterised in that comprise the following steps：
Step 2-1, above-mentioned nickel doped tin oxide nano grain products are mixed with alcohol reagent and are coated in the appearance of alumina tube
On face, earthenware is inserted；
Step 2-2, by small Ni-Cr alloy heating coil inserting step 2-1 earthenware；
Step 2-3, step 2-2 earthenware is welded on hexagonal base and obtains a formaldehyde gas sensor unit；
Step 2-4, the sensor unit of manufacture is obtained into formaldehyde gas sensor in 160~200 DEG C of heat ageings.
10. any one of any one of the claim 1~2 nickel doped tin oxide nano material or claim 3~5 system
Formaldehyde gas sensor or claim 8~9 described in the nickel doped tin oxide nano material or claim 7 that Preparation Method obtains
The formaldehyde gas sensor that any one preparation method obtains is being prepared for the purposes in formaldehyde gas monitoring.
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