CN105603713A - Preparation method and applications of SnO2/ZnO nano composite fiber material with coaxial heterostructure - Google Patents
Preparation method and applications of SnO2/ZnO nano composite fiber material with coaxial heterostructure Download PDFInfo
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Abstract
The invention provides a preparation method and applications of a SnO2/ZnO nano composite fiber material with a coaxial heterostructure, and belongs to the technical field of metal oxide semiconductor sensor material preparation. The preparation method comprises following steps: PVP is taken as an organic solvent; SnCl2.2H2O, ethyl alcohol, and DMF are mixed fully so as to obtain a Sn salt spinning precursor liquid, and electrostatic spinning and high temperature oxygen-containing calcining are adopted so as to obtain SnO2 nano fiber; the SnO2 nano fiber is prepared into a slurry, is dried, and is delivered into an ethanol solution of zinc acetate, and an obtained mixture is heated in thermostatic waterbath at 80 to 90 DEG C so as to obtain the hollow SnO2/ZnO nano composite fiber material with a coaxial heterostructure. The SnO2/ZnO nano composite fiber material with a coaxial heterostructure, novel morphology, and a stable structure is obtained at a reasonable ratio via two-step-method of electrostatic spinning and thermostatic waterbath. The preparation method is simple; the raw materials are cheap and easily available; the preparation method is suitable for large scale production; and at the same time, indirectly heated gas sensors prepared from the SnO2/ZnO nano composite fiber material possesses more excellent and higher sensitivity on methanol.
Description
Technical field
The present invention relates to a kind of SnO of coaxial heterogeneous structure2The preparation of/ZnO nano complex fiber materialMethods and applications, belong to metal oxide semiconductor sensor material preparation process technical field.
Background technology
Tin ash is to study one of semiconductor gas sensor material the earliest. Because it has higherElectrical conductivity, the advantage such as crystal structure is stable, with low cost and broad applicability, makes it at semiconductorGas sensor field is the focus of research and application always. But single metal oxide is partly ledBody material, due to the defect of its performance, often can not meet the requirement of multiple application.
The sensitiveness of Semiconductor gas sensors material not only depends on the composition of material, the structure of material itself,Pattern also can make a big impact to performance. Although Chinese patent CN101144789A discloses oneHighly sensitive gas sensor, sol-gal process obtains nanometer grade powder SnO2/ ZnO, due to nanometerLevel Specific Surface Area Measurement is large, easily reunites, dispersed bad, causes gas sensing property to be difficult to reach requirement. PeaceThe paddy Cuiping of emblem normal university is taking copper chloride, two hydrated stannous chlorides, thiocarbamide, ethylene glycol as raw material,Make copper tin sulphur, through calcining, obtain a kind of porous flower-like tin dioxide material after pickling, to toluene,The gases such as formaldehyde have higher sensitive property, and response sensitivity less than 6.5 to 100ppm acetone.Existing Semiconductor gas sensors material preparation method is generally comparatively complicated, requires harshness for manufacturing conditions,And cost of material is high, be not suitable for large-scale production. How in Semiconductor gas sensors material preparation process, to mixAssorted different elements, the synthetic composite with heterojunction structure is still this to obtain the air-sensitive performance of helping each otherThe study hotspot that field is current and difficult point.
Summary of the invention
The present invention, for making up the deficiencies in the prior art, provides a kind of SnO of coaxial heterogeneous structure2/ZnOThe preparation method of nanometer composite fiber material. The complex fiber material Stability Analysis of Structures obtaining by the method,Air-sensitive performance excellence, can be preparing extensive use in gas sensor, and the heater-type prepared of this materialGas sensor PARA FORMALDEHYDE PRILLS(91,95) shows better, sensitiveer sensitivity.
Technical conceive of the present invention is: design a kind of nanometer composite fiber material with new structure,By raw material rational proportion, utilize method of electrostatic spinning and water bath with thermostatic control two-step method, at hollow multilevel hierarchySnO2Even growth ZnO nano spherolite on nanofiber, has obtained the coaxial heterogeneous structure of hollowSnO2/ ZnO nano complex fiber material.
The present invention is achieved in that a kind of SnO of coaxial heterogeneous structure2/ ZnO nano composite fibreThe preparation method of material, comprises following processing step:
1. taking PVP as organic solvent, by SnCl2·2H2O, ethanol and DMF are fully mixedThe spinning precursor liquid of Sn salt, adopts method of electrostatic spinning to obtain intermediate product, forges containing oxygen through 600 DEG C of high temperatureBurn, obtain the SnO of hollow multilevel hierarchy2Nanofiber;
Wherein, SnCl2·2H2The mass ratio of O and PVP is (0.5～1.1): (0.8～1.5)
Ethanol and SnCl2·2H2The ratio of O is (0.8～2) ml:(100～200) mg; DMF andThe volume ratio of ethanol is (0.5～0.8): 1;
For reaching best experiment effect, the technological parameter of described electrostatic spinning is: spinning voltage is22 DEG C of 24KV, temperature, humidity is 40RH;
High temperature of the present invention refers to having high-temperature calcination in the atmosphere that oxygen exists containing oxygen calcining, asAir calcination, preferably it carries out in uncovered Muffle furnace.
2. by SnO2Nanofiber furnishing pasty state, is applied on glassware, and thickness is 0.1～0.5mm,Be dried 1～1.5 hour in 200～250 DEG C of drying boxes, by the aqueous zinc acetate solution of 0.02～0.06mol/LEvenly drop in SnO2On nanofiber surface, be placed in 200～250 DEG C of drying box inner dryings 30～40 minutes;Dried glassware is placed in the ethanolic solution of zinc acetate of 0.02～0.06mol/L,In the water bath with thermostatic control of 80～90 DEG C, heat 2～4 hours to obtain product I, product I separated with glassware,At 40～60 DEG C, be dried 2～4 hours, obtain the SnO of the coaxial heterogeneous structure of hollow2/ ZnO answersClose nano material. The glassware of step described in 2., according to the difference of experimental size, can be taked notSame container is as sheet glass, slide or surface plate etc.
Preferably, step 2. described smearing be to be spun on glassware with 2400HZ on gel machineOn.
The present invention also asks protection to have the SnO of coaxial heterogeneous structure prepared by said method2/ ZnO nanoComplex fiber material.
Another object of the present invention is the coaxial heterogeneous structure prepared by said method of request protectionSnO2/ ZnO nano complex fiber material is in the application of preparing in gas sensor, preferably in formaldehyde air-sensitiveApplication in element, utilize heater-type gas sensor PARA FORMALDEHYDE PRILLS(91,95) prepared by this material show better,Sensitiveer sensitivity.
The SnO of gained coaxial heterogeneous structure of the present invention2/ ZnO composite nano materials is a kind of many in hollowThe SnO of level structure2The ZnO nano ball that the particle diameter of evenly having grown on nanofiber is 200～400nmGrain. SnO2Nanofiber wall thickness is about 15-20nm, and fibre wall is by the SnO of particle diameter 5～20nm2ReceiveRice grain rearranges, at SnO2The epontic ZnO nano ball of nanofiber, its nanometer spheroliteFootpath is about 200～40nm, forms the SnO of coaxial multistage hollow2With ZnO heterojunction structure.
Compared with prior art, the invention has the beneficial effects as follows: by rational proportioning by SnO2WithZnO carries out compound, makes SnO2Learn from other's strong points to offset one's weaknesses with ZnO, performance synergy, has overcome single goldBelong to oxide and apply limited defect in gas sensor field. Adopt method of electrostatic spinning and water bath with thermostatic controlMethod two-step method acquisition pattern novelty, Stability Analysis of Structures have the SnO of coaxial heterogeneous structure2/ ZnO nano is multipleCondensating fiber material, nanometer composite fiber material preparation technology of the present invention is simple, and raw material is cheap and easy to get, suitableClose large-scale production. The SnO of the coaxial heterogeneous structure that meanwhile, prepared by the present invention2/ ZnO nano is compoundFibrous material can be used widely in gas sensor, the heater-type that particularly uses this material to prepareIt is better that gas sensor shows PARA FORMALDEHYDE PRILLS(91,95), sensitiveer sensitivity.
Brief description of the drawings
Accompanying drawing of the present invention is totally 6 width.
Fig. 1 is SnO2, ZnO and SnO2The X-ray diffractogram of/ZnO nano complex fiber material;
Wherein: a, SnO2，b、ZnO，c、SnO2/ ZnO nano complex fiber material;
Fig. 2 is the SnO of the hollow multilevel hierarchy prepared of method of electrostatic spinning2Nanofiber microstructureField transmitting electron-microscope scanning figure (amplifying 30,000 times);
Fig. 3 is the SnO of the coaxial heterogeneous structure prepared of the present invention2/ ZnO nano complex fiber material is micro-See the field transmitting electron-microscope scanning figure (amplifying 3.5 ten thousand times) of structure;
Fig. 4 is the SnO of the coaxial heterogeneous structure prepared of the present invention2/ ZnO nano complex fiber material is micro-See the field transmitting electron-microscope scanning figure (amplifying 50,000 times) of structure;
Fig. 5 adopts SnO of the present invention2Sensor prepared by/ZnO nano complex fiber material exists350 DEG C of curve maps that response sensitivity changes with concentration of formaldehyde; Wherein, concentration of formaldehyde scope is0.1-500ppm；
Fig. 6 adopts SnO of the present invention2Sensor prepared by/ZnO nano complex fiber material existsThe response sensitivity of 350 DEG C of PARA FORMALDEHYDE PRILLS(91,95)s and five kinds of interference gas benzene, toluene, methyl alcohol, acetone and ammoniasComparison diagram.
Detailed description of the invention
Following non-limiting example can make those of ordinary skill in the art's comprehend originallyInvention, but do not limit the present invention in any way. In following embodiment, if no special instructions, institute adoptsExperimental technique be conventional method, material therefor, reagent Deng Junkecong biological or chemical company are bought.
Embodiment 1
Two-step method is prepared the SnO of coaxial heterogeneous structure2/ ZnO nano composite
A kind of SnO of coaxial heterogeneous structure2The preparation method of/ZnO composite nano-fiber material, comprisesFollowing processing step:
1. take 0.5gSnCl2·2H2O is dissolved in 4ml absolute ethyl alcohol, and magnetic agitation is to dissolving completely, moltenLiquid is water white transparency shape, takes 0.8gPVP and 2mlDMF, is dissolved in SnCl2Ethanolic solutionIn, after magnetic agitation 8h, form the thick spinning precursor liquid of water white transparency. By the SnO preparing2Spinning precursor liquid injects the 10ml glass needle tubing that is connected to No. 7 syringe needles, access electrostatic spinning apparatus. QuietElectric spinning device is mainly made up of three partial devices, high voltage source, the container with shower nozzle and receiving systemThree part compositions. Container with shower nozzle is made up of the 10ml glass needle tubing that is connected to No. 7 syringe needles, shower nozzleConnect respectively the positive and negative polarities of high voltage source with receiving system, under the effect of high voltage source, shower nozzle withBetween receiving system, form high-voltage electrostatic field. In spinning process, the spinning precursor liquid in glass needle tubing existsUnder the effect of high-voltage electrostatic field, the solution of shower nozzle place positively charged forms " taylor cone " at spinning nozzle place, andForm and spray thread, to negative pole motion, on receiving system, collect white scraps of paper shape product. StaticSpinning process, high voltage source arranges 24KV, and spinning the temperature inside the box is 22 DEG C, and humidity is 40%RH.By the white scraps of paper shape intermediate product of collecting logical oxygen high-temperature calcination in Muffle furnace, obtain as accompanying drawing 2Shown white SnO2Nanofiber.
2. by 1. gained SnO of step2Nanofiber weighs 0.20g, by agate mortar pulverize state,By ground SnO2Powder adds appropriate ethanol dilution, furnishing pasty state; Choose 5cm × 1cm and carry glassSheet, by the SnO having diluted2Be spun on 0.1mm on slide, be placed in interior 200 DEG C dry 1 of drying boxHour, then the aqueous zinc acetate solution of 0.03mol/L is dropped on slide with dropper to the acetic acid of droppingThe amount of the zinc aqueous solution is not limited, to cover SnO2Be as the criterion, and be placed in 200 DEG C of drying boxes dryDry 30～40 minutes. Dried slide is placed in the ethanolic solution of zinc acetate of 0.03mol/L,The concentration of ethanolic solution is 99.9%, heats 4 hours in the water bath with thermostatic control of 90 DEG C, last, extractsSlide can have the SnO of the coaxial heterogeneous structure of hollow after dry 4 hours in 60 DEG C2/ ZnO'sComposite.
Embodiment 2
1. take 1.1gSnCl2·2H2O is dissolved in 1.5ml absolute ethyl alcohol, and magnetic agitation is extremely dissolved completely,Solution is water white transparency shape, takes 1.5gPVP and 1.2mlDMF, is dissolved in SnCl2EthanolIn solution, after magnetic agitation 8h, form the thick spinning precursor liquid of water white transparency, adopt Static SpinningSilk method obtains containing SnCl2White scraps of paper shape intermediate product,, obtain containing oxygen calcining through 600 DEG C of high temperatureThe SnO of hollow multilevel hierarchy2Nanofiber;
2. by SnO2Nanofiber furnishing pasty state, is spun on 0.1～0.5mm on slide, in 250 DEG CDry 1.5 hours of drying box, evenly drops in SnO by the acetic acid zinc solution of 0.06mol/L2Fiber tableOn face, be placed in 250 DEG C of drying box inner dryings 40 minutes; Dried slide is placed on to 0.06mol/LThe ethanolic solution of zinc acetate in, in the water bath with thermostatic control of 90 DEG C, heat 4 hours, finally extract and carry a glassSheet, in 60 DEG C dry 4 hours, obtain the SnO of the coaxial heterogeneous structure of hollow2The compound of/ZnO receivesRice material.
Embodiment 3
1. take 0.8gSnCl2·2H2O is dissolved in 8ml absolute ethyl alcohol, and magnetic agitation is to dissolving completely, moltenLiquid is water white transparency shape, takes 1gPVP and 4.8mlDMF, is dissolved in SnCl2Ethanolic solutionIn, after magnetic agitation 8h, form the thick spinning precursor liquid of water white transparency, adopt method of electrostatic spinningObtain containing SnCl2White scraps of paper shape intermediate product, containing oxygen calcining, obtain hollow through 600 DEG C of high temperatureThe SnO of multilevel hierarchy2Nanofiber;
2. by SnO2Nanofiber furnishing pasty state, is spun on 0.5mm on slide, dry in 200 DEG CDry 1 hour of dry case, evenly drops in SnO by the acetic acid zinc solution of 0.02mol/L2On fiber surface,Be placed in 200 DEG C of drying box inner dryings 30 minutes; Dried slide is placed on to the second of 0.02mol/LIn the ethanolic solution of acid zinc, in the water bath with thermostatic control of 80 DEG C, heat 2 hours, finally extract slide,In 40 DEG C dry 2 hours, obtain the SnO of the coaxial heterogeneous structure of hollow2The composite Nano material of/ZnOMaterial.
Application examples
1, prepare sensor
By embodiment 1 gained SnO2/ ZnO nano composite mixes furnishing pasty state with deionized water,Be coated on earthenware with fine, soft fur brush, to be dried after, heat treatment 90 minutes under 500 DEG C of conditions; WillEarthenware is welded on hexagonal pedestal, obtains heater-type gas sensor.
2, sensor test
Sensor is placed in to static test system. The operating temperature of sensor element is 350 DEG C. SoThe formaldehyde gas molecule of rear introducing variable concentrations (concentration range is 0.1-500ppm), or 10ppm orBenzene, toluene, methyl alcohol, acetone and the ammonia interference gas molecule of 50ppm. Pass by capture card collectionIn the Circuits System of sensor under air and the formaldehyde atmosphere at the variable concentrations taking air as backgroundThe variation of voltage partial pressure value, as the signal of sensor. Calculate the response of sensor by PCSensitivity.
Gas response sensitivity (S) is defined as element resistance value R in airaWith element adsorbed gasRear resistance value RgRatio, i.e. S=Ra/Rg. Wherein, Ra＝RL(Vc-Vair)/Vair，Rg＝RL(Vc-Vgas)/Vgas，
VairAnd VgasBe respectively the aerial dividing potential drop of gas sensor and the dividing potential drop in tested gas,RLFor the resistance of the divider resistance of connecting in bleeder circuit, VcFor the total voltage providing to bleeder circuit.
The sensor response sensitivity computing formula that PC calculates is S=Vgas(Vc-Vair)/Vair(Vc-Vgas)。
Accompanying drawing 5 provided 350 DEG C at formaldehyde sensor to the response spirit in time of the formaldehyde of variable concentrationsSensitivity change curve. The formaldehyde least concentration measuring is 0.1ppm, and response sensitivity can reach 1.67.
Accompanying drawing 6 has provided sensor PARA FORMALDEHYDE PRILLS(91,95) and five kinds of interference gas benzene, toluene, first at 350 DEG CThe response sensitivity comparison diagram of alcohol, acetone and ammonia. Adopt coaxial heterogeneous structure of the present inventionSnO2Sensor prepared by/ZnO nano complex fiber material shows good formaldehyde at 350 DEG CSensitivity and the selectivity to benzene, toluene, methyl alcohol, acetone and ammonia.
Claims (4)
1. the SnO of a coaxial heterogeneous structure2The preparation method of/ZnO nano complex fiber material, itsBe characterised in that, comprise following processing step:
1. taking PVP as organic solvent, by SnCl2·2H2O, ethanol and DMF are fully mixedThe spinning precursor liquid of Sn salt, adopts method of electrostatic spinning to obtain intermediate product, forges containing oxygen through 600 DEG C of high temperatureBurn, obtain the SnO of hollow multilevel hierarchy2Nanofiber;
Wherein, SnCl2·2H2The mass ratio of O and PVP is (0.5～1.1): (0.8～1.5)
Ethanol and SnCl2·2H2The ratio of O is (0.8～2) ml:(100～200) mg; DMF andThe volume ratio of ethanol is (0.5～0.8): 1;
2. by SnO2Nanofiber furnishing pasty state, is applied on glassware, and thickness is 0.1～0.5mm,Be dried 1～1.5 hour in 200～250 DEG C of drying boxes, by the aqueous zinc acetate solution of 0.02～0.06mol/LEvenly drop in SnO2On nanofiber surface, be placed in 200～250 DEG C of drying box inner dryings 30～40 minutes;Dried glassware is placed in the ethanolic solution of zinc acetate of 0.02～0.06mol/L,In the water bath with thermostatic control of 80～90 DEG C, heat 2～4 hours to obtain product I, product I separated with glassware,At 40～60 DEG C, be dried 2～4 hours, obtain the SnO of the coaxial heterogeneous structure of hollow2/ ZnO answersClose nano material.
2. the SnO of a coaxial heterogeneous structure2The preparation method of/ZnO nano complex fiber material, itsBe characterised in that, step 2. described smearing is to be spun on glassware with 2400HZ on gel machine.
3. the SnO of a coaxial heterogeneous structure2/ ZnO nano complex fiber material is according to claimPrepared by the method described in 1.
4. the SnO of the coaxial heterogeneous structure that as claimed in claim 1 prepared by method2/ ZnO nano is compoundFibrous material is in the application of preparing in gas sensor.
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