CN101183086A - Preparation method of nanometer tin oxide fibre air-sensitive film - Google Patents
Preparation method of nanometer tin oxide fibre air-sensitive film Download PDFInfo
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- CN101183086A CN101183086A CNA2007101509413A CN200710150941A CN101183086A CN 101183086 A CN101183086 A CN 101183086A CN A2007101509413 A CNA2007101509413 A CN A2007101509413A CN 200710150941 A CN200710150941 A CN 200710150941A CN 101183086 A CN101183086 A CN 101183086A
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Abstract
The present invention relates to a preparation technique for preparing nanometer tin anhydride fiber gas sensor film material by using an electrostatic spinning method. The present invention comprises: 1, collosol gel static filature liquid allocation: polyethylene ketopyrrolidine is poured into dissolvent containing N, N-dimethyfomamide (DMF); the dissolvent is mixed at high speed to be completely dissolved; the polyethylene ketopyrrolidine/DMF dissolvent with the concentration of 5 wt percent to 8 wt percent is produced; and then, the dissolvent is mixed with qua-water stannic chloride water solution with the concentration of 10 wt percent to 40 wt percent; wherein, the weight ratio of the polyethylene ketopyrrolidine and the stannic chloride is between 3 to 1 and 3 to 4; the product is made after being mixed for 3 hours. 2. electrostatic spinning: The prepared collosol gel static filature liquid is injected into a electrostatic spinning device and transformed into aluminum chloride/ polyethylene ketopyrrolidine nanometer fibrous coat on the conditions that the voltage is between 25 Kv and 35 Kv; the extrusion speed is between 1 ml/min and 10 ml/min and the receive distance is between 10 cm and 20 cm through the electrostatic spinning. 3. calcination: finally, the prepared aluminum chloride/ polyethylene ketopyrrolidine nanometer fibrous coat is placed in a muffle furnace; the temperature is raised to 450 DEG C to 600 DEG C at the speed of 50 DEG C per hour; nanometer tin anhydride fibrous coat is gained after being calcined for 5 hours. The nanometer tin anhydride fibrous coat produced by the present invention is gas sensing material with high specific area and high sensitivity; in addition, the material can be widely applied to the field of catalyst, laser target material and so on.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic nanometer oxide tunica fibrosa, be specially a kind of electrostatic spinning preparation method of nanometer tin oxide fibre air-sensitive film.
Background technology
The industrial revolution has improved labour productivity greatly, when having enriched people's material and cultural life, has also brought serious environmental problem.Acid rain in recent years, greenhouse effect, depletions of the ozone layer etc. are threatening human existence, cause the concern of the whole society.For example: airborne NOx, SOx and HCl cause acid rain; CO
2, CH
4, NO
2, O
3And fluorocarbon (fluorine Lyons) produces greenhouse effect; Fluorocarbon and halocarbon cause depletion of the ozone layer; NH
3, H
2S produces pungent smell.Therefore, develop these environmental protection gas sensors, become the hot issue that everybody is concerned about, particularly function admirable, the research of high sensitivity air-sensitive sensing material are imperative.
Gas sensitive is a kind of functional material, and when this type of material runs into specific gas, its physicochemical property will certain variation take place with ambient atmos kind, concentration change under certain condition.The gas sensitive that begins one's study the external thirties, along with modern society to inflammable, explosive, poisonous, harmful gas detects, control, the requirement of reporting to the police are more and more higher, the performance of gas sensitive and kind have all obtained certain development.
The gas sensitive of research mainly is a metal-oxide semiconductor (MOS) at present, as zinc paste (ZnO), gamma-iron oxide (γ-Fe
2O
3), tin oxide (SnO
2) etc.Same SnO
2Compare γ-Fe
2O
3Chemical stability is relatively poor, can irreversiblely become α-Fe mutually at 350 ℃～450 ℃
2O
3, and that ZnO is the power consumption of element is bigger.Tin oxide (SnO
2) be a kind of n-N-type semiconductor N, its direct band gap can be for about 2.6ev for 3.9ev, indirect band gap, and is 2.0 in the refractive index of visible region, has the rutile-type crystal structure.SnO is found in the Tian Kou Shangyi of Japan in 1962
2Powder is very responsive to various inflammable gass, i.e. SnO in various inflammable gas
2The conductivity difference, made practical combustible gas sensor according to this characteristic; Nineteen sixty-eight, Japan Figaro company released first SnO
2Semiconductor combustible gas sensor commodity.
Have higher dividing potential drop when having the dispersed and high temperature in higher surface when the low temperature and cause hanging down densification owing to tin oxide, make it have the low frit performance, this just low frit performance makes them be mainly used in multi-aperture device and the catalyzer of making in the gas sensor, be used for the catalytic degradation and the atmosphere environment supervision, particularly SnO of reductibility toxic gas
2The sensor that nano material is made has highly sensitive, simplicity of design, in light weight and characteristics that cost is low.
Nano material is meant to have at least one dimension to be in nanoscale scope (1～100nm) or the material that is made of as elementary cell them in three dimensions.Under nanoscale, the ripple of electronics and the interaction between the atom will be subjected to the influence of scale size in the material, surface effect, small-size effect, quantum size effect and macro quanta tunnel effect occur.Utilize characteristics such as the huge surface area of nano material, higher surface activity, make it become the most promising material in the sensor manufacturing, can bring up to new height to the performance of sensor, not only volume is little, speed is fast, precision is high but also good reliability.
Current, mainly material is made nano particle both at home and abroad by physics and chemical means, wait as sol-gel process, hydro-thermal method, coprecipitation and microemulsion method and improve SnO
2Gas-sensitive property.Research to the one-dimensional tin oxide nano material is also less relatively.Up to nearly 3 years, a small amount of bibliographical information tin oxide nano rod [XuC K, Xu G D, Lju Y K.Preparation and characterization of SnO
2Nanorods bythermal decomposition of SnC
2O
4Precursor.Scripta Mater.2002,46 (11): 789～794], nano wire [Dai Z R, Gole J L, Stout J D, et al.Tin oxide nanowires, nanoribbons, and nanotubes.J.Phys.Chem.B, 2002,106 (10): 1274] and nano belt [Jian J K, Chen X L, Wang W J, el al.Appl Phy A.Synthesis of SnO
2Nanobelts and theirstructural characterization.2003,76:291～294] preparation.
Patent CN 1858308 adopts method of electrostatic spinning to prepare low-density tin ash laser target material, reported in this patent that employing polyvinylpyrrolidone/ethanolic solution and four water tin chloride/ethanolic solution blend high-speed stirred makes spinning liquid, there is the shortcoming of spinning liquid configuration difficulty in this method, and two kinds of solution blendings very easily cause polyvinylpyrrolidone to separate out and be difficult to dissolving again.
Summary of the invention
The technical matters that quasi-solution of the present invention is determined provides a kind of technology of preparing of nanometer tin oxide fibre membrane material.This membrane material is to adopt electrostatic spinning technique to spin out organic/inorganic pink salt nano fibrous membrane, makes the nanometer tin oxide fibre membrane material through high-temperature calcination.The fibre diameter of forming this membrane material is generally between 50～200nm, want little several magnitude than the fibre diameter (50 μ m～several millimeters) that conventional spinning process obtains, its specific surface area and volume ratio are 1000 times of conventional fibre approximately, fiber surface activity is big, absorption affinity is strong, is a kind of specific surface area height, highly sensitive gas sensitive; In addition, this material can also be widely used in fields such as catalyzer, laser target material.The present invention adopts polyvinylpyrrolidone/DMF and four water tin chloride/ethanolic solution blend to make that spinning liquid configuration technology is simple, efficient is high, is suitable for electrostatic spinning, and electrospinning device is not had specific (special) requirements, and spinnability is good.
The technical scheme that the present invention solves described nanometer tin oxide fibre air-sensitive film material technology problem is:
Design a kind of nanometer tin oxide fibre air-sensitive film material preparation method, comprise the steps:
(1) pour polyvinylpyrrolidone into N, in the dinethylformamide solvent, high-speed stirred is to dissolving fully, make polyvinylpyrrolidone/DMF solution, four water tin chloride ethanolic solutions with concentration 10～40wt% mix with it then, and stir about 3h can obtain collosol and gel electrostatic spinning liquid.
(2) the collosol and gel spinning liquid that makes being injected electrostatic spinning apparatus, is 25～35kV at voltage, and extruded velocity is 1～10mL/min, and receiving range is that electrostatic spinning becomes tin chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane under 10～20cm condition.
(3) at last tin chloride/the polyvinylpyrrolidonenanometer nanometer fiber membrane for preparing is positioned in the muffle furnace, is warming up to 450～600 ℃ with 50 ℃/h speed, calcining 5h obtains nanometer tin oxide fibre air-sensitive film.
Some other characteristics of the present invention are:
Described polyvinylpyrrolidone viscosity average molecular weigh scope is 600,000～1,300,000.
Described polyvinylpyrrolidone/DMF solution concentration is 5～8wt%.
Polyvinylpyrrolidone and four water tin chloride weight ratios are 3: 1～3: 4 in the described collosol and gel electrostatic spinning liquid.
Nanometer tin oxide fibre membrane material of the present invention according to the purposes needs, can adopt suitable process and controls the nanofiber yardstick.By adopting scanning electron microscope (U.S.), X-ray diffraction that nanometer tin oxide fibre is tested, the result shows, along with concentration of dope and extruded velocity increase, the diameter of microfibril received is big more, and voltage increases the diameter that helps reducing fiber; Tin chloride/polyvinylpyrrolidone organic inorganic hybridization fiber can obtain the tin dioxide nano fiber film at 600 ℃ of continuous calcining 5h.
Picture and text are simply described
Fig. 1 is a treatment of different temperature nanometer tin oxide fibre film scanning electron microscope synoptic diagram;
Fig. 2 is a treatment of different temperature nanometer tin oxide fibre film X diffraction light spectrogram.
Embodiment
Further narrate the present invention below in conjunction with embodiment, but the scope of application of the present invention is not limited:
Embodiment 1:
Getting sticking equal molecule molecular weight and be 600,000 polyvinylpyrrolidone 3g pours into and fills 57mL N, in the dinethylformamide solvent, high-speed stirred is to dissolving fully, make concentration and be polyvinylpyrrolidone/DMF solution of 5%, taking by weighing 1g four water tin chlorides is dissolved in the 9mL ethanol, then both solution are mixed and high-speed stirred 1 hour, obtain collosol and gel electrostatic spinning liquid; The collosol and gel spinning liquid that makes is injected electrostatic spinning apparatus, is 25kV at voltage, and extruded velocity is 10mL/min, and receiving range is that electrostatic spinning becomes aluminum chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane under the 10cm condition; Tin chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane with preparation is positioned in the muffle furnace at last, is warming up to 450 ℃ with 50 ℃/h speed, and oven dry 5h obtains dry tin chloride nanometer fibre gas-sensitive film.
Embodiment 2:
Getting sticking equal molecule molecular weight and be 900,000 polyvinylpyrrolidone 3g pours into and fills 47mLN, in the dinethylformamide solvent, high-speed stirred is to dissolving fully, make concentration and be polyvinylpyrrolidone ethanol/DMF solution of 6%, taking by weighing 2g four water tin chlorides is dissolved in the 8mL ethanol, then both solution are mixed and high-speed stirred 1 hour, obtain collosol and gel electrostatic spinning liquid; The collosol and gel spinning liquid that makes is injected electrostatic spinning apparatus, is 30kV at voltage, and extruded velocity is 5mL/min, and receiving range is that electrostatic spinning becomes aluminum chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane under the 10cm condition; Tin chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane with preparation is positioned in the muffle furnace at last, is warming up to 450 ℃ with 50 ℃/h speed, and calcining 5h obtains nanometer tin oxide fibre air-sensitive film.
Embodiment 3:
Getting sticking equal molecule molecular weight and be 1,100,000 polyvinylpyrrolidone 3g pours into and fills 40mLN, in the dinethylformamide solvent, high-speed stirred is to dissolving fully, make concentration and be polyvinylpyrrolidone/DMF solution of 7%, taking by weighing 2g four water tin chlorides is dissolved in the 10mL ethanol, then both solution are mixed and high-speed stirred 1 hour, obtain collosol and gel electrostatic spinning liquid; The collosol and gel spinning liquid that makes is injected electrostatic spinning apparatus, is 30kV at voltage, and extruded velocity is 8mL/min, and receiving range is that electrostatic spinning becomes aluminum chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane under the 15cm condition; Tin chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane with preparation is positioned in the muffle furnace at last, is warming up to 600 ℃ with 50 ℃/h speed, and calcining 5h obtains nanometer tin oxide fibre air-sensitive film.
Embodiment 4:
Getting sticking equal molecule molecular weight and be 1,300,000 polyvinylpyrrolidone 3g pours into and fills 34.5mLN, in the dinethylformamide solvent, high-speed stirred is to dissolving fully, make concentration and be polyvinylpyrrolidone/DMF solution of 8%, taking by weighing 4g four water tin chlorides is dissolved in the 6mL ethanol, then both solution are mixed and high-speed stirred 1 hour, obtain collosol and gel electrostatic spinning liquid; The collosol and gel spinning liquid that makes is injected electrostatic spinning apparatus, is 35kV at voltage, and extruded velocity is 1mL/min, and receiving range is that electrostatic spinning becomes aluminum chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane under the 20cm condition; Tin chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane with preparation is positioned in the muffle furnace at last, is warming up to 600 ℃ with 50 ℃/h speed, and calcining 5h obtains nanometer tin oxide fibre air-sensitive film.
Claims (4)
1. a nanometer tin oxide fibre air-sensitive film preparation methods is characterized in that it comprises the steps:
(1) pour polyvinylpyrrolidone into N, in the dinethylformamide solvent, high-speed stirred is to dissolving fully, make polyvinylpyrrolidone/DMF solution, four water tin chloride ethanolic solutions with concentration 10～40wt% mix with it then, and stir about 3h can obtain collosol and gel electrostatic spinning liquid.
(2) the collosol and gel spinning liquid that makes being injected electrostatic spinning apparatus, is 25～35kV at voltage, and extruded velocity is 1～10mL/min, and receiving range is that electrostatic spinning becomes tin chloride/polyvinylpyrrolidonenanometer nanometer fiber membrane under 10～20cm condition.
(3) at last tin chloride/the polyvinylpyrrolidonenanometer nanometer fiber membrane for preparing is positioned in the muffle furnace, is warming up to 450～600 ℃ with 50 ℃/h speed, calcining 5h obtains nanometer tin oxide fibre air-sensitive film.
2. nano-alumina fiber air-sensitive film preparation methods as claimed in claim 1 is characterized in that described polyvinylpyrrolidone viscosity average molecular weigh scope is 600,000～1,300,000.
3. nano-alumina fiber air-sensitive film preparation methods as claimed in claim 1 is characterized in that described polyvinylpyrrolidone/DMF solution concentration is 5～8wt%.
4. nano-alumina fiber air-sensitive film preparation methods as claimed in claim 1 is characterized in that polyvinylpyrrolidone and four water tin chloride weight ratios are 3: 1～3: 4 in the described collosol and gel electrostatic spinning liquid.
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| CN101368930B (en) * | 2008-09-02 | 2011-10-12 | 徐州市精英电器技术有限公司 | Production method for sensitive material and gas-sensitive element of halogen refrigerant detection sensor |
| CN102621198A (en) * | 2012-03-07 | 2012-08-01 | 福州大学 | Multi-element metal oxide gas-sensitive component of gas-sensitive sensor and preparation method thereof |
| CN101609059B (en) * | 2009-07-22 | 2013-04-03 | 西南科技大学 | Oxide/silicate mineral fiber nano composite air-sensitive film and preparation method thereof |
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Open date: 20080521 |