CN105668613A - Fe-doped stannic oxide flower-like nanosphere material with ultrasensitive respiratory sensing performance - Google Patents
Fe-doped stannic oxide flower-like nanosphere material with ultrasensitive respiratory sensing performance Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01G19/00—Compounds of tin
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- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0081—Mixed oxides or hydroxides containing iron in unusual valence state [IV, V, VI]
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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
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- 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
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
Abstract
The invention discloses a Fe-doped stannic oxide flower-like nanosphere material with ultrasensitive respiratory sensing performance.The Fe-doped stannic oxide flower-like nanosphere material is characterized by being of a flower-like nanometer structure 200-250nm in diameter and large in void, and the diameter of nanorods ranges from 30nm to 50nm.A humidity sensor produced from the powdery material, namely the Fe-doped stannic oxide flower-like nanosphere material, has the advantages that when relative humidity changes between 11% and 95%, the humidity sensor is short in responding and recovering time (1s/4s, the sum of the responding and recovering time is less than 5s), high in sensitivity (about 6,500), quite wide in impedance change range (10<0>-10<4> kilohms) and capable of responding to human respiration quickly and keeping repeated measurement unattenuated while the high sensitivity is guaranteed.The Fe-doped stannic oxide flower-like nanosphere material with the ultrasensitive respiratory sensing performance is simple to prepare and excellent in humidity sensitivity, thereby being a satisfactory humidity and respiration sensor material.
Description
Technical field
The present invention relates to inorganic semiconductor sensor material preparing technical field, particularly relate to a kind of Fe2O3 doping tindioxide class flower-like nanometer ball material with super quick breathing sensitivities.
Background technology
Of a great variety for the metal-oxide semiconductor (MOS) gas sensor of gas-monitoring and warning at present, conventional has ZnO, SnO2、Fe2O3、SrTiO3、In2O3And WO3Deng. In these semiconductor transducers, tindioxide (SnO2) as n molded breadth forbidden band (Eg=3.6eV, temperature is 300K) semi-conductor, there is low-dimensional degree, low cost, less energy-consumption, hypersensitivity, high stability and highly selective and extensively studied, it is at present there is most the semiconductor type gas sensor commercially producing value, it is widely used in industry, agricultural, national defence, electronics, information and the every field closely bound up with people's lives, especially for the inflammable gas (as: CH of detection lower concentration4, LPG and H2Deng), toxic gas (as: CO, H2S and NOxDeng) and bio-medical aspect, take charge of a department especially.
In nanoscale field, the constitutional features of material and configuration of surface determine its physical and chemical performance to a great extent, therefore, in in the past few decades, Many researchers is devoted to the exploitation of new material structures, prepares the novel structures such as such as nano wire, nanometer rod, nanometer core-shell structure copolymer and nanometer box by various laboratory facilities. Relative to original block SnO2Material, novel nano structural material has better air-sensitive performance. Obviously, if a kind of material exists multiple SnO simultaneously2Nanometer new texture, will show more excellent performance in gas detection.
At actual SnO2In the research and development of base humidity-sensitive material, except there is new nanostructure, often to be carried out chemical doping, precious metal (as: Au, Pt, Pd and Rh etc.) doping right and wrong are usually shown in and quite ripe process means, form doped semiconductor nanocrystal film gas sensing material by doping, now can have than single made of new structural material and the SnO that do not adulterate2The gas sensing property that material is higher. But, precious metal is expensive so that produce in enormous quantities limited, and therefore, people naturally consider that common metal (as: Fe, Al and Cu etc.) adulterates. Being found by the effort of many investigators, common metal doping also can obtain moisture-sensitive preferably. The people such as Kim are by the flower-shaped SnO of class of Ni doped O2The air-sensitive performance research of nanometer ball finds, as Ni doped O, material has good CO gas-sensitive property under 25%RH humidity environment, traces it to its cause mainly: when sensor is in humidity environment, and NiO compares SnO2Easier adsorbed water molecule, such water molecules would not make SnO2Space is excessively saturated.(KimH-R, HaenschA, KimI-D, etal.TheRoleofNiODopinginReducingtheImpactofHumidityonth ePerformanceofSnO2-BasedGasSensors:SynthesisStrategies, andPhenomenologicalandSpectroscopicStudies [J] .AdvancedFunctionalMaterials, 2011,21 (23): 4456-4463.). The people such as XiGuangcheng synthesize ultra thin single crystalline SnO first2Nano-bar material, its diameter is only 2.0nm, for the detection of low-dimensional sensor provides new approaches. (GuangchengXiandJinhuaYe, UltrathinSnO2Nanorods:Template-andSurfactant-FreeSolutionPhaseSynthes is, GrowthMechanism, Optical, Gas-Sensing, andSurfaceAdsorptionProperties [J] .InorganicChemicals, 2010,49 (5): 2302-2309). But, in a lot of moisture-sensitive test, the breathing sensitivities of its sensor is unsatisfactory, and major cause has, and one is that scantling is big, and two is that sensor is long to the time of recovery of humidity. Therefore, excellent breathing sensing capabilities to be obtained, will break through from these two aspects.
Summary of the invention
The present invention is intended to for existing SnO2The weak point of base humidity-sensitive material muting sensitivity, high cost and preparation process complexity, by Template-free method, additive-free water heat transfer Fe2O3 doping tindioxide class flower-like nanometer ball humidity-sensitive material, hydrothermal method shortens the preparation cycle of material greatly. Improve humidity-sensitive material degree of crystallinity by lower concentration Fe2O3 doping, avoid high precious metal, and refinement crystal grain, little crystal grain class flower-like nanometer spherical structure enhances the susceptibility to detection humidity.
The present invention is achieved through the following technical solutions: a kind of Fe2O3 doping tindioxide class flower-like nanometer ball material with super quick breathing sensitivities, it is characterized in that: originate by metal ion of a certain proportion of stannic chloride pentahydrate and iron trichloride, with a certain amount of sodium hydroxide, the mixing solutions (deionized water and dehydrated alcohol volume ratio are 1:1) that deionized water and dehydrated alcohol are formed is hydrothermal system, proceed to after magnetic stirrer in the polytetrafluoroethyllining lining stainless steel cauldron (reactor volume is 50ml) with tindioxide crystal seed and carry out chemical reaction, room temperature is naturally cooled to after reacting certain time at a certain temperature, respectively with deionized water and dehydrated alcohol repeatedly centrifuge washing, white depositions is proceeded to air dry oven and is dried process, obtain the class flower-like nanometer ball SnO that diameter is 200-250nm subsequently2Original washing powder body.
Described medicine is all purchased in Shanghai Chemical Reagent Co., Ltd., Sinopharm Group (analytical pure AR).
In two kinds of described metallic cations, the molar fraction shared by iron trichloride is 0%, 0.5%, 1%, 2%, 5% and 10%.
Described hydrothermal system basicity (sodium hydroxide and stannic chloride pentahydrate mol ratio) is 10:1.
Described reaction system has isopyknic deionized water and dehydrated alcohol.
The described magnetic stirrer time is 20-30min, and speed is middling speed.
The described tindioxide crystal seed in described 50ml polytetrafluoroethyllining lining, adopts electronic balance weighing 0.351g stannic chloride pentahydrate to be dissolved in 20ml dehydrated alcohol; Weigh basicity be 10 sodium hydroxide (NaOH) be dissolved in 20ml deionized water; Under magnetic agitation effect, stannic chloride pentahydrate ethanolic soln is slowly added in aqueous sodium hydroxide solution, after continuing to stir 20min, obtain white opacity liquid;White opacity liquid is proceeded in 50ml polytetrafluoroethyllining lining stainless steel cauldron, it is heated to 140-180 DEG C, insulation 2h, to be cooled to room temperature, solution and throw out are poured out and obtained;
The described chemical reaction in reactor, temperature is 140-180 DEG C, and the time is 12h.
The drying of described white depositions in air dry oven, temperature is 70 DEG C, and the time is 5h.
Feature of the present invention is: material of the present invention is different from common SnO2The single nano structural material of base, it is a kind of class flower-like nanometer ball become by nanometer rod self-assembly, and space between spray forms bigger specific surface area, thus shows more excellent moisture-sensitive. Select common metal iron, improve crystal structure degree significantly reduce preparation cost simultaneously.
The present invention adopts humidity-sensitive material prepared by hydrothermal method, and technique is simple, when room temperature, human body respiration shows ultrafast superelevation response characteristic, can be used as the ideal material breathing sensor.
Accompanying drawing explanation
Fig. 1 is products therefrom XRD spectra of the present invention.
Fig. 2 is products therefrom transmission electron microscope (TEM) photo figure of the present invention. Wherein, the little figure in the upper right corner is high resolution picture figure.
Fig. 3 and Fig. 4 is 0%Fe doping SnO in the present invention2(iron ion molar fraction is 0%) and 2%Fe adulterate SnO2The surface film type sensing member wet sensitive performance map that (iron ion molar fraction is 2%) material makes. Wherein, 11%RH and 95%RH represents that relative humidity is 11% and 95% two kind of environment respectively. In Fig. 3,3s and 17s represents 0%Fe doping SnO respectively2The time of response of sensing member when changing in 11%RH and 95%RH two kinds of humidity environments and time of recovery. In Fig. 4,1s and 4s represents 2%Fe doping SnO respectively2The time of response of sensing member when changing in 11%RH and 95%RH two kinds of humidity environments and time of recovery.
Fig. 5 be product of the present invention make surface film type sensing member to human body respiration response figure. During the breathing measured, length is 120s.
Embodiment
Now specific embodiments of the invention are described below:
Embodiment 1:
The preparation of the tindioxide crystal seed in 50ml polytetrafluoroethyllining lining: adopt electronic balance weighing 0.351g stannic chloride pentahydrate to be dissolved in 20ml dehydrated alcohol; Weigh basicity be 10 sodium hydroxide (NaOH) be dissolved in 20ml deionized water; Under magnetic agitation effect, stannic chloride pentahydrate ethanolic soln is slowly added in aqueous sodium hydroxide solution, after continuing to stir 20min, obtain white opacity liquid; White opacity liquid is proceeded in 50ml polytetrafluoroethyllining lining stainless steel cauldron, it is heated to 140-180 DEG C, insulation 2h, to be cooled to room temperature, solution and throw out are poured out and obtained;
Embodiment 2:
0%Fe adulterates SnO2Prepared by powder body: adopt electronic balance weighing 0.351g stannic chloride pentahydrate (SnCl4·5H2O) it is dissolved in 20ml dehydrated alcohol; Weigh basicity be 10 sodium hydroxide (NaOH) be dissolved in 20ml deionized water; Under magnetic agitation effect, stannic chloride pentahydrate ethanolic soln is slowly added in aqueous sodium hydroxide solution, after continuing to stir 20min, obtain white opacity liquid; Being proceeded to by white opacity liquid in 50ml polytetrafluoroethyllining lining stainless steel cauldron, be heated to 140-180 DEG C, insulation 12h, naturally cools to room temperature subsequently; By the white depositions that obtains respectively with deionized water and dehydrated alcohol repeatedly centrifuge washing; By washing after throw out add a certain amount of dehydrated alcohol, shake even after be placed in air dry oven, at 70 DEG C, dry 5h.
Embodiment 3:
0.5%Fe adulterates SnO2Prepared by powder body: step and above-described embodiment 2 in the present embodiment are completely identical. The difference is that: weigh 0.351g stannic chloride pentahydrate (SnCl4·5H2And 0.0016g iron trichloride (FeCl O)3) be dissolved in 20ml dehydrated alcohol.
Embodiment 4:
1%Fe adulterates SnO2Prepared by powder body: step and above-described embodiment 3 in the present embodiment are completely identical. The difference is that: weigh 0.0033g iron trichloride (FeCl3) be dissolved in 20ml dehydrated alcohol.
Embodiment 5:
2%Fe adulterates SnO2Prepared by powder body: step and above-described embodiment 3 in the present embodiment are completely identical. The difference is that: weigh 0.0065g iron trichloride (FeCl3) be dissolved in 20ml dehydrated alcohol.
Embodiment 6:
5%Fe adulterates SnO2Prepared by powder body: step and above-described embodiment 3 in the present embodiment are completely identical. The difference is that: weigh 0.0163g iron trichloride (FeCl3) be dissolved in 20ml dehydrated alcohol.
Embodiment 7:
10%Fe adulterates SnO2Prepared by powder body: step and above-described embodiment 3 in the present embodiment are completely identical. The difference is that: weigh 0.0325g iron trichloride (FeCl3) be dissolved in 20ml dehydrated alcohol.
The final product Fe doping SnO obtained in the embodiment of the present invention2Powder body material, the wet sensitive of its XRD, tem analysis result and material/breathing the performance test results is described below:
FIGS, Fig. 1 is embodiment of the present invention 2-6 gained Fe-SnO2Product spectrogram. XRD analysis: adopt CuKα(wavelength is ray) diffraction, Dandong DX-2700 type X-ray diffractometer carries out. As we know from the figure, the present embodiment product diffraction peak and SnO2Standard peak matches (PDF#41-1445), it does not have impurity peaks signal occurs, and diffraction peak is wider, illustrates to have thinner crystal grain.
FIGS, Fig. 2 is the embodiment of the present invention 5 gained 2%Fe-SnO2Transmission electron microscope (TEM) the photo figure of product. Tem analysis: the microscopic appearance adopting Japan's JEM-2100 type transmission electron microscope observation material. As we know from the figure, the Fe2O3 doping SnO of gained2Powder body is self-assembled into class flower-like nanometer spherical structure by the nanometer rod that degree of crystallinity is good, wherein distance between nanometer rod is about 50nm, and spherical diameter is about 220nm, and the diameter of nanometer rod is about 40nm, therefore having bigger specific surface area, it is 38.622m that BET result shows its specific surface area2/g。
Wet sensitive the performance test results:
Humidity-sensitive element conventionally makes surface film type senser element. Concrete making step is:
Adulterate SnO by the Fe obtained in the embodiment of the present invention2Powder body and dehydrated alcohol and deionized water are that 8:1:1 adjusts form slurry according to mass ratio; Being dripped by slurry and be coated in prefabricated golden interdigital electrode, gold interdigital electrode take epoxy resin as substrate, and span is wide with referring to is 100 μm, and interdigital electrode is of a size of 10 × 10mm2, glued joint upper copper lead-in wire with low-temperature silver, form two electrode measurement systems; Then 120 DEG C, loft drier process 30 minutes it is placed in;
The evaluation of moisture sensor element function:
The accurate LCR digital electric bridge TH2828 of Changzhou Tong Hui Electronics Co., Ltd. is adopted to carry out the moisture-sensitive analysis of material. Wet sensitive environment is self-control humidity environment, it is defined as the humidity value that saturated salt solution is corresponding when room temperature reaches stable state, represents relative humidity respectively as 11%, 22%, 33%, 43%, 54%, 69%, 75%, 84% and 95% taking lithium chloride, potassium acetate, magnesium chloride, salt of wormwood, magnesium nitrate, potassiumiodide, sodium-chlor, Repone K and saltpetre.The Humidity Sensitivity adopted is defined as S=| ZRH11|/|ZRHy|, wherein, | ZRH11| with | ZRHy| represent the impedance value of sensor under relative humidity 11% and y% two kinds of environment respectively. In response and time of recovery calculate, it is defined as respectively, the time used when humidity reaches stationary value 90% and 10% from impedance when 11% humidity environment and y% environment facies change.
FIGS, Fig. 3 and Fig. 4 is SnO of the present invention2With 2%Fe doping SnO2The surface film type sensing member wet sensitive performance map that material makes. 2%Fe doping SnO prepared by the embodiment of the present invention2The surface film type senser element that class flower-like nanometer ball powder system is done, when 11% and 95% relative humidity variations, (impedance variations scope is four orders of magnitude 10 to show supper-fast response/time of recovery (being less than 1/4s), ultra-high sensitive degree (S=6500) and very wide impedance variations scope0–104K Ω), and pure SnO2The time of response of sensor is shorter is 3s, but time of recovery longer be 17s, illustrate that Fe's mixes the sensitivity that improve sensor.
FIGS, Fig. 5 be product of the present invention make surface film type sensing member to human body respiration response figure. Fe2O3 doping SnO prepared by the embodiment of the present invention2The surface film type senser element that class flower-like nanometer ball powder system is done, it is possible to respond human body respiration fast, while ensureing highly sensitive, does not decay in circulation measuring process, is a kind of good moisture sensor detecting material.
The present invention adopts humidity-sensitive material prepared by Template-free method, additive-free hydrothermal method, and technique is simple, and cost is low, and wet sensitive susceptibility is with the obvious advantage, it is possible to detection human body respiration, can become the ideal material breathing sensor.
Embodiment is to invention has been specific descriptions, but only for the invention will be further described, can not be interpreted as limiting the scope of the invention. Other change made when not deviating from spirit and protection domain for the technician of this area and amendment, if these amendments and modification are within the scope of the claims in the present invention, then the present invention also is intended to comprise these changes and amendment.
Claims (6)
1. one kind has the Fe2O3 doping tindioxide class flower-like nanometer ball material of super quick breathing sensitivities, it is characterised in that:
(1) the class flower-like nanometer spherical structure that there is nanometer rod self-assembly and become;
(2) diameter of class flower-like structure nanometer ball is 200-250nm, the diameter 30-50nm of nanometer rod;
(3) between class flower-like nanometer ball, space is relatively big, is about 50nm, has bigger specific surface area, and BET records value for 30-40m2/g。
2. the surface film type senser element that humidity-sensitive material according to claim 1 makes, it is characterized in that: the preparation method of gas sensitive is, electronic balance weighing 0.351g stannic chloride pentahydrate and molar fraction is adopted to be 0%, 0.5%, 1%, the iron trichloride (molar fraction relative to stannic chloride pentahydrate) of 2%, 5% and 10% is dissolved in 20ml dehydrated alcohol; Weigh basicity be 10 sodium hydroxide (NaOH) be dissolved in 20ml deionized water; Under magnetic agitation effect, stannic chloride pentahydrate ethanolic soln is slowly added in aqueous sodium hydroxide solution, after continuing to stir 20min, obtain white opacity liquid; Being proceeded to by white opacity liquid in the 50ml polytetrafluoroethyllining lining stainless steel cauldron with tindioxide crystal seed, be heated to 140-180 DEG C, insulation 12h, naturally cools to room temperature subsequently; By washing after throw out add a certain amount of dehydrated alcohol, shake even after be placed in air dry oven, at 70 DEG C, dry 5h.
3. the surface film type senser element obtained prepared by nanometer ball material according to claim 1, it is characterized in that: when 11% and 95% relative humidity variations, having quick response/time of recovery (1s/4s), this responds fast and is less than 5 seconds with sum time of recovery.
4. the tindioxide crystal seed in 50ml polytetrafluoroethyllining lining according to claim 2, it is characterised in that: adopt electronic balance weighing 0.351g stannic chloride pentahydrate to be dissolved in 20ml dehydrated alcohol; Weigh basicity be 10 sodium hydroxide (NaOH) be dissolved in 20ml deionized water; Under magnetic agitation effect, stannic chloride pentahydrate ethanolic soln is slowly added in aqueous sodium hydroxide solution, after continuing to stir 20min, obtain white opacity liquid; White opacity liquid is proceeded in 50ml polytetrafluoroethyllining lining stainless steel cauldron, it is heated to 140-180 DEG C, insulation 2h, to be cooled to room temperature, solution and throw out are poured out and obtained.
5. surface film type senser element according to claim 3, it is characterised in that: when 11% and 95% relative humidity variations, sensor has highly sensitive, and sensitivity is about S=6500, and impedance variations scope reaches four orders of magnitude (100–104kΩ)。
6. surface film type senser element according to claim 3, it is characterised in that: when detecting human body respiration, measuring through 20 circulations, impedance variations is undamped.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106564949A (en) * | 2016-11-01 | 2017-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Iron-doped nanometer tin antimony oxide nanometer powder, and preparation and application thereof |
| CN109738492A (en) * | 2018-12-20 | 2019-05-10 | 广州奥松电子有限公司 | A kind of production method of gas sensor sensitive material |
| CN110687185A (en) * | 2019-10-12 | 2020-01-14 | 河南师范大学 | Based on SnO2@Fe2O3Low-power-consumption acetone gas sensor of nano heterostructure sensitive material and preparation method thereof |
| CN113219006A (en) * | 2021-04-16 | 2021-08-06 | 华南理工大学 | Gas sensor, preparation method thereof and wearable electronic device |
| CN114166899A (en) * | 2021-11-24 | 2022-03-11 | 上海大学 | PdRh-based loaded SnO2Formaldehyde MEMS gas sensor with multi-shell structure and preparation method thereof |
| CN114414634A (en) * | 2022-01-20 | 2022-04-29 | 重庆工商大学 | Iron-doped cobalt hydroxystannate gas sensor material and preparation method thereof |
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| CN106564949A (en) * | 2016-11-01 | 2017-04-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Iron-doped nanometer tin antimony oxide nanometer powder, and preparation and application thereof |
| CN109738492A (en) * | 2018-12-20 | 2019-05-10 | 广州奥松电子有限公司 | A kind of production method of gas sensor sensitive material |
| CN110687185A (en) * | 2019-10-12 | 2020-01-14 | 河南师范大学 | Based on SnO2@Fe2O3Low-power-consumption acetone gas sensor of nano heterostructure sensitive material and preparation method thereof |
| CN113219006A (en) * | 2021-04-16 | 2021-08-06 | 华南理工大学 | Gas sensor, preparation method thereof and wearable electronic device |
| CN114166899A (en) * | 2021-11-24 | 2022-03-11 | 上海大学 | PdRh-based loaded SnO2Formaldehyde MEMS gas sensor with multi-shell structure and preparation method thereof |
| CN114414634A (en) * | 2022-01-20 | 2022-04-29 | 重庆工商大学 | Iron-doped cobalt hydroxystannate gas sensor material and preparation method thereof |
| CN117285069A (en) * | 2023-11-24 | 2023-12-26 | 山东乾能科技创新有限公司 | Lithium lanthanum titanate/tin dioxide nano material and MEMS methane sensor |
| CN117285069B (en) * | 2023-11-24 | 2024-03-22 | 山东乾能科技创新有限公司 | Lithium lanthanum titanate/tin dioxide nano material and MEMS methane sensor |
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