CN103675034B - A kind of semi-conductor electricity resistive gas sensor and preparation method thereof - Google Patents
A kind of semi-conductor electricity resistive gas sensor and preparation method thereof Download PDFInfo
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- CN103675034B CN103675034B CN201310634216.9A CN201310634216A CN103675034B CN 103675034 B CN103675034 B CN 103675034B CN 201310634216 A CN201310634216 A CN 201310634216A CN 103675034 B CN103675034 B CN 103675034B
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Abstract
The invention discloses a kind of semi-conductor electricity resistive gas sensor and preparation method thereof. Preparation method comprises the steps: that (1) is coated in semiconductor colloidal state quantum dot solution in the dielectric substrate that is printed on electrode, makes its even film forming; (2) process quantum dot film with short chain ligand solution; (3) remove remaining short chain part and accessory substance thereof; (4) repeatedly repeated execution of steps (1), to step (3), obtains having the semiconductor colloidal state quantum dot film of desired thickness, completes the preparation of gas sensor. In said method, also direct film forming in dielectric substrate, prepares electrode on the semiconductor colloidal state quantum dot film in the end obtaining. Gas sensor comprises dielectric substrate, electrode and gas sensing layer, and gas sensing layer is semiconductor colloidal state quantum dot film. Moment or trace that this gas sensor can detect gas concentration at normal temperatures change, and response resume speed is fast and highly sensitive, and safe and portable, has a good application prospect.
Description
Technical field
The invention belongs to gas sensitive and Element Technology field, more specifically, relate to a kind of with colloidal state amountSemi-conductor electricity resistive gas sensor that son point film is gas sensitive and preparation method thereof.
Background technology
Traditional semi-conductor electricity resistive gas sensor often adopts metal oxide (as SnO2、ZnO、TiO2Deng) be gas sensitive, have metering system simple, highly sensitive, respond fast, easy to operate,The feature such as good portability, cost are low, but such gas sensor must be heated in actual applicationsHigh operating temperature (200～600 DEG C), power consumption is larger, has reduced the portability of sensor, but alsoIncrease potential safety hazard, its application is very limited. In recent years, utilize the special of nano materialActivity realizes room temperature air sensor is just becoming focus and the emphasis of research, and traditional gas sensitive is being doneWhen becoming the special constructions such as nano wire, nanotube, nanometer rods, nanobelt, also emerged Graphene,The Novel Room Temperature such as CNT, silicon nanowires gas sensitive.
In addition,, in view of the tempting application prospect of flexible device, existing researcher utilizes Graphene, carbon to receiveThe bigger serface that mitron has and film formation at low temp process characteristic, at PET, PI even in paper substratesSuccessfully prepare room temperature flexible air body sensor. For example, the Luo Weier of masschusetts, u.s.a university branch school in 2009Report is successfully realized graphene oxide inkjet printing under room temperature NO on PET substrate2Detection,Not enough is under the irradiation of 254nm ultraviolet light, can recover, and has greatly reduced sensorPortable performance; 2012 Nian Gaigai seminars report again CNT inkjet printing film forming on paper, chamberNO to 100ppm under temperature2And Cl2Sensitivity be respectively 2.4 and 2.7, but its long responseAnd (3-5 minute, 7-12 minute) is still unfavorable for actual monitoring recovery time.
Colloidal state quantum dot adopts colloid chemistry legal system standby, is a kind of raw with organic ligand molecule parcelThe surface of long quantum dot is to control the wet chemical method of particle aggregation. Compared with common nano material,There is the controlled and good uniformity of size, activity is high, physicochemical characteristic is controlled, be easy to finishing, room temperatureThe features such as film forming and flexible substrate compatibility are good are the new type ideal of preparation room tenderness gas sensorMaterial. The research of colloidal state quantum dot gas sensor can be traced back to calendar year 2001 the earliest, and researcher is by commercially availableSb doping SnO2Colloidal particles suspension in the mode of spin coating at SiO2Film forming on substrate, producesResistance-type methanol gas sensor, operating temperature is low to moderate 150 DEG C. But this device still need to be at high temperature(500 DEG C) heat treatment, causes particle size in true device up to tens nanometer, is unfavorable for fullyThe feature of performance colloidal state quantum dot gas sensitive. Afterwards, main in the research of colloidal state quantum dot gas sensorAdopting the mixture of colloidal state quantum dot and organic polymer is gas sensitive, enables at room temperatureFilm forming, therefore the particle size of colloidal state quantum dot has obtained good maintenance. But, owing to being dispersed inIn the low organic polymer molecular network of electrical conductivity, the adsorption activity of colloidal state quantum dot to gas and itBetween electric transmission be restricted, cause such sensor air-sensitive performance at room temperature unsatisfactory,Therefore operating temperature is so higher. In addition,, except resistance-type gas sensor, utilize colloidal state quantum dot lightThe room temperature air sensor that photoluminescence (PL) changes also receives researcher's concern, but the latter is portableProperty aspect cannot compare favourably with resistance-type gas sensor.
2008, Wang seminar of Tsing-Hua University was with SnCl4·5H2O is that raw material closes at 180 DEG CBecome the colloidal state SnO of oleic acid-oleyl amine parcel2Quantum dot, the about 0.5-2.5nm of particle size, by its dispersionIn chloroformic solution, and be deposited in the ceramic die that is prefabricated with gold electrode to drip the mode being coated with, utilizeN2-H2O carrier gas stream is at room temperature dried it and is made into resistance-type gas sensor, at 300 DEG CTo the sensitivity of 100ppm alcohol vapour approximately 1.6, respond and be all less than 20 seconds recovery time. Obviously,The operating temperature of this sensor is higher, and sensitivity is on the low side.
Summary of the invention
For above defect or the Improvement requirement of prior art, the invention provides a kind of semiconductor resistorFormula gas sensor and preparation method thereof, this gas sensor can detect the wink of gas concentration at normal temperaturesBetween or trace change, response resume speed fast and highly sensitive, can adopt rigidity or flexible substrate,Manufacture craft is simple, and cost is low, and safe and portable has a good application prospect.
For achieving the above object, according to one aspect of the present invention, provide a kind of gas sensorPreparation method, is characterized in that, comprises the steps: that (1) is coated with semiconductor colloidal state quantum dot solutionOverlay in the dielectric substrate that is printed on electrode, make its even film forming; (2) by short chain ligand solution treating capacitySon point film; (3) remove remaining short chain part and accessory substance thereof; (4) repeatedly repeat stepSuddenly (1), to step (3), obtains having the semiconductor colloidal state quantum dot film of desired thickness, completesThe preparation of gas sensor.
According to another aspect of the present invention, provide a kind of preparation method of gas sensor, its featureBe, comprise the steps: that (1) is coated in semiconductor colloidal state quantum dot solution in dielectric substrate,Make its even film forming; (2) process quantum dot film with short chain ligand solution; (3) remove remnants'Short chain part and accessory substance thereof; (4) repeatedly repeated execution of steps (1), to step (3), obtains toolThere is the semiconductor colloidal state quantum dot film of desired thickness; (5) semi-conductor adhesive obtaining in step (4)On state quantum dot film, prepare electrode, complete the preparation of gas sensor.
Preferably, described semiconductor colloidal state quantum dot solution is PbS colloidal state quantum dot solution or SnO2Colloidal state quantum dot solution.
Preferably, described dielectric substrate is paper, plastics, pottery, silicon chip or glass.
Preferably, described short chain ligand solution is NH4Cl or NaNO2Or Pb (NO3)2Solution.
According to another aspect of the present invention, a kind of gas sensor of preparing with said method is provided,It is characterized in that, comprise dielectric substrate, electrode and gas sensing layer, described gas sensing layer is semiconductor colloidal state amountSon point film.
Preferably, described dielectric substrate is paper, plastics, pottery, silicon chip or glass.
Preferably, described semiconductor colloidal state quantum dot film is PbS colloidal state quantum dot film or SnO2GlueState quantum dot film.
In general, the above technical scheme of conceiving by the present invention compared with prior art, hasFollowing beneficial effect:
Moment or the trace that 1, can even detect gas concentration under normal temperature in lower operating temperature change. OneAspect is by choosing suitable material system, change process regulation quantum dot component, structure andSize, the mode of replacing by part is on the other hand introduced the ion of specific function or group to quantum dotSurface is modified, and realizes chemism to colloidal state quantum dot film and the regulation and control of conductive characteristic.
2, response resume speed is fast, gets final product fast quick-recovery without illumination or heating, and highly sensitive, choosingSelecting property is good, is beneficial to Real-Time Monitoring.
3, it is firm that gas sensor not only can adopt pottery, silicon chip or the glass etc. of conventional good heat resistanceProperty substrate, can also adopt the relatively poor flexible substrate of the heat resistance such as plastics, paper, produces flexibilityGas sensor, obtain conventional rigid device incomparable light, thin, cost is low, pliability and justThe advantages such as the property taken is good, and manufacture craft is simple, is expected to directly be mounted on gas storage, all kinds of foodOn the curved surfaces such as thing and biological skin surface, use, have a good application prospect.
Brief description of the drawings
Fig. 1 is that the gas sensor prepared of the embodiment of the present invention 1 is at room temperature to 50ppm nitrogen dioxideResponse curve.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with accompanying drawingAnd embodiment, the present invention is further elaborated. Should be appreciated that described herein concreteEmbodiment only, in order to explain the present invention, is not intended to limit the present invention. In addition described,Involved technical characterictic in each embodiment of the present invention just can as long as do not form to conflict each otherMutually to combine.
With the most active CNT of current room temperature air sensor field exploitation, conducting polymer,Quanta point material prepared by Graphene and alternate manner is compared, colloidal state quantum dot have a series of otherType gas sensitive is difficult to alternative advantage. Colloidal state quantum dot is size little (< 10nm), specific surface not onlyLong-pending large, active high, and physicochemical characteristic controllability is strong, can room temperature film-forming, be generally used for solar-electricityIn pond and photodetector.
Colloidal state quantum dot adopts solution chemical method synthetic, and its surface is had by the long-chain such as oleic acid, TOPO conventionallyMachine part parcel. The present invention is the air-sensitive film using colloidal state quantum dot as gas sensor creatively, and oneAspect is by changing component, structure and the size of process regulation quantum dot, regulate its energy gap width,The electronic states such as the size of exciton bind energy, the mode of replacing by part is on the other hand introduced specific meritIon or the group of energy carry out finishing to it, make gas molecule easily enter quantum dot film, realThe now regulation and control of the chemism to colloidal state quantum dot film and conductive characteristic, utilize its resistance value with the external worldThe feature that gas concentration changes, the moment or the trace that detect at normal temperatures gas concentration change. In addition,Utilize its room temperature film-forming feature by element manufacturing in the flexible substrate such as paper, be expected to directly be mounted on gasOn the curved surfaces such as memory device, various kinds of foods and biological skin surface, use.
Semi-conductor electricity resistive gas sensor of the present invention comprises: dielectric substrate, electrode and gas sensing layer.Gas sensing layer is semiconductor colloidal state quantum dot film, is specially PbS colloidal state quantum dot film or SnO2GlueState quantum dot film.
The preparation method of the semi-conductor electricity resistive gas sensor of one embodiment of the invention comprises following stepRapid:
(1) semiconductor colloidal state quantum dot solution is coated in the dielectric substrate that is printed on electrode, makes it equalEven film forming. Particularly, colloidal state quantum dot can be at room temperature lift to drip a painting, spin coating, immersion, spray,The modes such as printing are coated in film forming on substrate.
(2) process quantum dot film with short chain ligand solution, to displace the long-chain oil on quantum dot surfaceAcid, makes gas molecule easily enter quantum dot film.
(3) remove remaining short chain part and accessory substance thereof.
(4) repeatedly repeated execution of steps (1), to step (3), obtains having partly leading of desired thicknessBody colloidal state quantum dot film, completes the preparation of gas sensor.
The preparation method of the semi-conductor electricity resistive gas sensor of another embodiment of the present invention comprises as followsStep:
(1) semiconductor colloidal state quantum dot solution is coated in dielectric substrate, makes its even film forming.
(2) process quantum dot film with short chain ligand solution, to displace the long-chain oil on quantum dot surfaceAcid, makes gas molecule easily enter quantum dot film.
(3) remove remaining short chain part and accessory substance thereof.
(4) repeatedly repeated execution of steps (1), to step (3), obtains having partly leading of desired thicknessBody colloidal state quantum dot film.
(5) on semiconductor colloidal state quantum dot film, prepare electrode, complete the preparation of gas sensor.
For making those skilled in the art understand better the present invention, below in conjunction with specific embodiment to thisThe preparation method of bright colloidal state quantum dot film gas sensor is elaborated.
Embodiment 1
(1) prepare PbS colloidal state quantum dot solution. With PbO as plumbous source, two trimethyl silicane sulfanes(TMS), as sulphur source, adopt the reaction of colloid chemistry method to generate.
Particularly, under nitrogen environment by 0.9g(4mmol) PbO is dissolved into 3ml oleic acid (OA)And in 17ml octadecylene (ODE) and be heated to 90 DEG C of predecessors of preparing plumbi oleas, as plumbous source. Take outVacuum reached after 8 hours, and this predecessor temperature is risen to 120 DEG C. By 180ul(1mmol) TMSBe dissolved in 10mlODE, as sulphur source. At 120 DEG C, rapidly plumbous source is injected in sulphur source, treat anti-Answering after the complete blackening of system color (approximately 15s) that solution is put into cold water makes temperature be down to fast room temperature.In cooled solution, add proper amount of acetone, after centrifugal mixer, remove supernatant, then pass through tolueneDispersion, the centrifugal repeatedly circulation of acetone are until supernatant is pure white. Final products therefrom is dried into powder alsoBe dispersed in the vulcanized lead quantum dot solution that obtains 50mg/ml in normal octane. UV, visible light optical absorption spectra is surveyedAbsworption peak that must this quantum dot is in the position of 1178nm.
(2) vulcanized lead colloidal state quantum dot solution is evenly dropped in the paper substrates that is printed on electrode, withThe speed spin coating 15s of 2500rpm; Natrium nitrosum (the NaNO that is 10mg/ml by concentration2) methyl alcohol moltenLiquid is paved with whole quantum dot film, infiltrates 45s and dries, and repeats twice; Wash away remnants with absolute methanolNaNO2Particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; Repeat above-mentioned allStep twice, obtains three layers through NaNO2The vulcanized lead quantum dot film of processing, completes gas sensorPreparation.
Fig. 1 is that the gas sensor prepared of the embodiment of the present invention 1 is at room temperature to 50ppm nitrogen dioxideThe response curve of gas, as shown in Figure 1, the sensitivity of this gas sensor reaches 21.7, and response recoversTime is respectively 12s and 37s.
Embodiment 2
PbS colloidal state quantum dot solution prepared by embodiment 1 evenly drops in the PET plastics that are printed on electrodeOn substrate, with the speed spin coating 15s of 2500rpm; Natrium nitrosum (the NaNO that is 10mg/ml by concentration2)Methanol solution be paved with whole quantum dot film, infiltrate 45s and dry, repeat twice; Use absolute methanolWash away remaining NaNO2Particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; RepeatAbove-mentioned in steps twice, obtain three layers through NaNO2The vulcanized lead quantum dot film of processing, completes gasThe preparation of body sensor.
The gas sensor prepared of the test embodiment of the present invention 2 is at room temperature to 50ppm nitrogen dioxideResponse curve.
Embodiment 3
PbS colloidal state quantum dot solution prepared by embodiment 1 evenly drops in the aluminium oxide pottery that is printed on electrodeOn at the bottom of ceramic liner, with the speed spin coating 15s of 2500rpm; The natrium nitrosum that is 10mg/ml by concentration(NaNO2) methanol solution be paved with whole quantum dot film, infiltrate 45s and dry, repeat twice; WithAbsolute methanol washes away remaining NaNO2Particle and byproduct of reaction thereof, infiltrate 5s and dry, and repeats threeInferior; Repeat above-mentionedly in steps twice, obtain three layers through NaNO2The vulcanized lead quantum dot film of processing,Complete the preparation of gas sensor.
The gas sensor prepared of the test embodiment of the present invention 3 is at room temperature to 50ppm nitrogen dioxideResponse curve.
Embodiment 4
PbS colloidal state quantum dot solution prepared by embodiment 1 evenly drops in the aluminium oxide pottery that is printed on electrodeOn at the bottom of ceramic liner, with the speed spin coating 15s of 2500rpm; Ammonium chloride (the NH that is 10mg/ml by concentration4Cl)Methanol solution be paved with whole quantum dot film, infiltrate 45s and dry, repeat twice; Use absolute methanolWash away remaining NH4Cl particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; RepeatAbove-mentioned in steps twice, obtain three layers through NH4The vulcanized lead quantum dot film that Cl processes, completes gasThe preparation of body sensor.
The gas sensor prepared of the test embodiment of the present invention 4 is at room temperature to 50ppm nitrogen dioxideResponse curve.
Embodiment 5
(1) prepare SnO2Colloidal state quantum dot solution.
By the SnCl of certain proportion amount4·5H2O, oleic acid and oleyl amine are heated to 100 DEG C, and also vacuum drying is anti-Should be to clarification, be cooled to after 60 DEG C of a certain amount of ethanol of taking-up mix and add stainless steel autoclave, putEnter reaction 3h in 180 DEG C of baking ovens. Reacted rear taking-up, while being cooled to room temperature by solution in autoclaveTake out centrifugally with ethanol mixed precipitation, subsequently precipitated product be scattered in solvent and again carry out ethanolCentrifuge washing. After dry, be scattered in toluene and can obtain colloidal state quantum dot solution by desired concn.
(2) by the colloidal state quantum dot solution obtaining according to above-mentioned colloidal state quantum dot film gas sensorPreparation method can make SnO2Colloidal state quantum dot film gas sensor.
The gas sensor that above-described embodiment is made compares with existing room temperature flexible air body sensor, as shown in table 1 to the various performance parameters of nitrogen dioxide.
The gas sensor that table 1 embodiment makes and the Performance Ratio of existing gas sensor are
Gas sensor prepared by various embodiments of the present invention and existing room temperature flexible air body sensor phaseRatio has greatly shortened response time and recovery time in ensureing natural sensitivity. To identicalPbS colloidal state quantum dot, select paper as substrate, select NaNO simultaneously2Molten as short chain inorganic matterLiquid cleans quantum dot film, and the gas sensor obtaining has best combination property, i.e. higher spiritSensitivity and shorter response recovery time. This is that gas divides because paper substrates has loose and porous structureSon is turnover colloidal state quantum dot film easily, thereby can reach higher sensitivity.
Semi-conductor electricity resistive gas sensor of the present invention and preparation method thereof is not limited to above-mentioned enforcementExample, particularly, it is thin that the colloidal state quantum dot film in gas sensor is not limited to PbS colloidal state quantum dotFilm or SnO2Colloidal state quantum dot film can be also other semiconductor colloidal state quantum dot film; Preparation sideColloidal state quantum dot solution in method is not limited to PbS colloidal state quantum dot solution or SnO2Colloidal state quantum dot is moltenLiquid can be also other semiconductor colloidal state quantum dot solution; Dielectric substrate is not limited to paper, plasticsOr pottery, can be also other dielectric substrate; Short chain ligand solution is not limited to NH4Cl or NaNO2Solution can be also other short chain inorganic matter or organic matter ligand solution, as Pb (NO3)2Solution.
Those skilled in the art will readily understand, the foregoing is only preferred embodiment of the present invention,Not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, etc.With replacement and improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. a preparation method for gas sensor, is characterized in that, comprises the steps:
(1) by PbS colloidal state quantum dot solution or SnO2Colloidal state quantum dot solution is coated in and is printed on electrodeDielectric substrate on, make its even film forming;
(2) process quantum dot film with short chain ligand solution, to displace the long-chain oil on quantum dot surfaceAcid, makes gas molecule easily enter quantum dot film; Described short chain ligand solution is NaNO2OrPb(NO3)2Solution;
(3) remove remaining short chain part and accessory substance thereof;
(4) repeatedly repeated execution of steps (1), to step (3), obtains having partly leading of desired thicknessBody colloidal state quantum dot film, completes the preparation of gas sensor.
2. a preparation method for gas sensor, is characterized in that, comprises the steps:
(1) by PbS colloidal state quantum dot solution or SnO2Colloidal state quantum dot solution is coated in dielectric substrateUpper, make its even film forming;
(2) process quantum dot film with short chain ligand solution, to displace the long-chain oil on quantum dot surfaceAcid, makes gas molecule easily enter quantum dot film; Described short chain ligand solution is NaNO2OrPb(NO3)2Solution;
(3) remove remaining short chain part and accessory substance thereof;
(4) repeatedly repeated execution of steps (1), to step (3), obtains having partly leading of desired thicknessBody colloidal state quantum dot film;
(5) on the semiconductor colloidal state quantum dot film obtaining in step (4), prepare electrode, complete gasThe preparation of body sensor.
3. the preparation method of gas sensor as claimed in claim 1 or 2, is characterized in that, instituteStating dielectric substrate is paper, plastics, pottery, silicon chip or glass.
4. a gas sensor of preparing by method described in claim 1 or 2, is characterized in that,Comprise dielectric substrate, electrode and gas sensing layer, described gas sensing layer is PbS colloidal state quantum dot film or SnO2Colloidal state quantum dot film.
5. gas sensor as claimed in claim 4, is characterized in that, described dielectric substrate be paper,Plastics, pottery, silicon chip or glass.
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