CN103675034A - Semiconductor resistance-type gas sensor and preparation method thereof - Google Patents
Semiconductor resistance-type gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a semiconductor resistance-type gas sensor and a preparation method thereof. The preparation method comprises the following steps: (1) coating a colloidal semiconductor quantum dot solution on an insulating substrate printed with electrodes, and forming a uniform film; (2) processing a quantum dot film by using a short-chain ligand solution; (3) removing the residual short-chain ligand and byproducts thereof; (4) repeating steps (1)-(3) for many times to obtain a colloidal semiconductor quantum dot film with a required thickness so as to complete preparation of the gas sensor. In the preparation method, the film can be formed on the insulating substrate directly, and the electrodes are prepared on the final colloidal semiconductor quantum dot film. The gas sensor comprises the insulating substrate, the electrodes and a gas-sensitive layer, wherein the gas-sensitive layer is the colloidal semiconductor quantum dot film. The gas sensor can detect instantaneous or subtle change of gas concentration at room temperature, and is high in response and restoration speed, high in sensitivity, safe and portable; therefore, the gas sensor 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 semi-conductor electricity resistive gas sensor that colloidal state quantum dot film is gas sensitive and preparation method thereof of take.
Background technology
Traditional semi-conductor electricity resistive gas sensor often adopts metal oxide (as SnO
2, ZnO, TiO
2deng) be gas sensitive, have metering system simple, highly sensitive, respond the features such as fast, easy to operate, good portability, cost be low, but such gas sensor must be heated to higher working temperature (200～600 ℃) in actual applications, power consumption is larger, reduced the portability of sensor, but also increased potential safety hazard, its application is very limited.In recent years, utilize the sp act of nano material to realize focus and the emphasis that room temperature air sensor is just becoming research, when traditional gas sensitive is made to the special constructions such as nano wire, nanotube, nanometer rods, nanobelt, also emerged the Novel Room Temperature gas sensitives such as Graphene, carbon nano-tube, silicon nanowires.
In addition,, in view of the tempting application prospect of flexible device, bigger serface and film formation at low temp process characteristic that existing researcher utilizes Graphene, carbon nano-tube to have, even successfully prepare room temperature flexible air body sensor in paper substrates at PET, PI.For example, the Luo Weier of masschusetts, u.s.a university branch school report in 2009 is successfully realized graphene oxide inkjet printing under room temperature NO on PET substrate
2detection, not enough is under the irradiation of 254nm ultraviolet light, can recover, and has greatly reduced the portable performance of sensor; 2012 Nian Gaigai seminars report again carbon nano-tube inkjet printing film forming on paper, the NO to 100ppm under room temperature
2and Cl
2sensitivity be respectively 2.4 and 2.7, yet its long response and release time, (3-5 minute, 7-12 minute) was still unfavorable for actual monitoring.
Colloidal state quantum dot adopts colloidal chemistry legal system standby, is that a kind of surface of quantum dot of growing with organic ligand molecule parcel is to control the wet chemical method of particle aggregation.Compare 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 temperature film-forming and the compatible feature such as good of flexible substrate, is the new type ideal material of preparation room tenderness gas sensor.The research of colloidal state quantum dot gas sensor can be traced back to calendar year 2001 the earliest, and researcher is by commercially available Sb doping SnO
2colloidal particles suspending liquid in the mode of spin coating at SiO
2film forming on substrate, produces resistance-type methanol gas sensor, and working temperature is low to moderate 150 ℃.Yet this device still need to be in high temperature (500 ℃) thermal treatment, cause particle size in true device up to tens nanometer, be unfavorable for giving full play to the feature of colloidal state quantum dot gas sensitive.Afterwards, in the research of colloidal state quantum dot gas sensor, the potpourri of main employing colloidal state quantum dot and organic polymer is gas sensitive, enable at room temperature film forming, so the particle size of colloidal state quantum dot has obtained good maintenance.But, owing to being dispersed in the organic polymer molecular network that conductivity is low, colloidal state quantum dot to the adsorption activity of gas and between electric transmission be restricted, cause such sensor air-sensitive performance at room temperature unsatisfactory, so working temperature is so higher.In addition, except resistance-type gas sensor, the room temperature air sensor that utilizes colloidal state quantum dot light photoluminescence (PL) to change also receives researcher's concern, but the latter cannot compare favourably with resistance-type gas sensor aspect portable.
2008, Wang seminar of Tsing-Hua University was with SnCl
45H
2o is the colloidal state SnO that raw material has synthesized oleic acid-oleyl amine parcel at 180 ℃
2quantum dot, the about 0.5-2.5nm of particle size, is dispersed in chloroformic solution, and is deposited in the ceramic die that is prefabricated with gold electrode to drip the mode being coated with, and utilizes N
2-H
2o carrier gas stream at room temperature be dried it and is made into resistance-type gas sensor, to the sensitivity of 100ppm alcohol vapour approximately 1.6, responds and is all less than 20 seconds release time at 300 ℃.Obviously, the working temperature of this sensor is higher, and sensitivity is on the low side.
Summary of the invention
Above defect or Improvement requirement for prior art, the invention provides a kind of semi-conductor electricity resistive gas sensor and preparation method thereof, moment or trace that this gas sensor can detect gas concentration at normal temperatures change, response resume speed is fast and highly sensitive, can adopt rigidity or flexible substrate, manufacture craft is simple, and cost is low, safe and portable, has a good application prospect.
For achieving the above object, according to one aspect of the present invention, a kind of preparation method of gas sensor is provided, it is characterized in that, comprise 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) with short chain ligand solution, process 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 the semiconductor colloidal state quantum dot film of desired thickness, completes the preparation of gas sensor.
According to another aspect of the present invention, a kind of preparation method of gas sensor is provided, it is characterized in that, comprise the steps: that (1) is coated in semiconductor colloidal state quantum dot solution in dielectric substrate, makes its even film forming; (2) with short chain ligand solution, process 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 the semiconductor colloidal state quantum dot film of desired thickness; (5) on the semiconductor colloidal state quantum dot film obtaining in step (4), prepare electrode, complete the preparation of gas sensor.
Preferably, described semiconductor colloidal state quantum dot solution is PbS colloidal state quantum dot solution or SnO
2colloidal state quantum dot solution.
Preferably, described dielectric substrate is paper, plastics, pottery, silicon chip or glass.
Preferably, described short chain ligand solution is NH
4cl or NaNO
2or Pb (NO
3)
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 quantum dot 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 SnO
2colloidal state quantum dot film.
In general, the above technical scheme of conceiving by the present invention compared with prior art, has following beneficial effect:
Moment or the trace that 1, can even detect gas concentration under normal temperature in lower working temperature change.On the one hand by choosing suitable material system, change component, structure and the size of process regulation quantum dot, the mode of replacing by part is on the other hand introduced ion or the group of specific function quantum dot surface is modified, and realizes the regulation and control to the chemical activity of colloidal state quantum dot film and conductive characteristic.
2, response resume speed is fast, without illumination or heating, gets final product fast quick-recovery, and highly sensitive, and selectivity is good, is beneficial to Real-Time Monitoring.
3, gas sensor not only can adopt the rigid substrate such as pottery, silicon chip or glass of conventional good heat resistance, can also adopt the relatively poor flexible substrate of thermotolerance such as plastics, paper, produce flexible air body sensor, obtain the advantages such as conventional rigid device incomparable light, thin, cost is low, pliability and good portability, and manufacture craft is simple, be expected to directly be mounted on the curved surfaces such as gas storage, various kinds of foods and biological skin surface and use, have a good application prospect.
Accompanying drawing explanation
Fig. 1 is the gas sensor response curve to 50ppm nitrogen dioxide at room temperature of the embodiment of the present invention 1 preparation.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.In addition,, in each embodiment of described the present invention, involved technical characterictic just can not combine mutually as long as do not form each other conflict.
Quanta point material prepared by carbon nano-tube, conducting polymer, Graphene and the alternate manner the most active with current room temperature air sensor field exploitation is compared, and colloidal state quantum dot has a series of other type gas sensitives and is difficult to alternative advantage.Colloidal state quantum dot not only size little (<10nm), specific surface area is large, active high, and physicochemical characteristic controllability is strong, can room temperature film-forming, be generally used in solar cell and photodetector.
Colloidal state quantum dot adopts solution chemical method synthetic, and its surface is wrapped up by long-chain organic ligands such as oleic acid, TOPO conventionally.The present invention is the air-sensitive film using colloidal state quantum dot as gas sensor creatively, on the one hand by changing the component of process regulation quantum dot, structure and size, regulate its energy gap width, the electronic states such as the size of exciton bind energy, ion or group that the mode of replacing by part is on the other hand introduced specific function carry out finishing to it, make gas molecule easily enter quantum dot film, the regulation and control of realization to the chemical activity of colloidal state quantum dot film and conductive characteristic, utilize its resistance value with the feature of ambient atmos concentration change, 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 the curved surfaces such as gas storage, various kinds of foods and biological skin surface and 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 SnO
2colloidal state quantum dot film.
The preparation method of the semi-conductor electricity resistive gas sensor of one embodiment of the invention comprises the steps:
(1) semiconductor colloidal state quantum dot solution is coated in the dielectric substrate that is printed on electrode, makes its even film forming.Particularly, colloidal state quantum dot can be at room temperature lifts to drip a painting, spin coating, immersion, sprays, the mode such as printing is coated in film forming on substrate.
(2) with short chain ligand solution, process quantum dot film, to displace the long-chain oleic acid on quantum dot surface, make 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 the semiconductor colloidal state quantum dot film of desired thickness, 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 the steps:
(1) semiconductor colloidal state quantum dot solution is coated in dielectric substrate, makes its even film forming.
(2) with short chain ligand solution, process quantum dot film, to displace the long-chain oleic acid on quantum dot surface, make 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 the semiconductor colloidal state quantum dot film of desired thickness.
(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, the preparation method of colloidal state quantum dot film gas sensor of the present invention 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 colloidal chemistry method to generate.
Particularly, under nitrogen environment by 0.9g(4mmol) PbO is dissolved in 3ml oleic acid (OA) and 17ml octadecylene (ODE) and is heated to 90 ℃ of precursors of preparing plumbi oleas, as plumbous source.Vacuumize and reach after 8 hours, this precursor temperature is risen to 120 ℃.By 180ul(1mmol) TMS is dissolved in 10ml ODE, as sulphur source.At 120 ℃, rapidly plumbous source is injected in sulphur source, after the complete blackening of question response system color, (approximately 15s) puts into cold water by solution and makes temperature be down to fast room temperature.In cooled solution, add proper amount of acetone, remove supernatant after centrifugal mixer, process toluene disperses then, acetone is centrifugal repeatedly circulates until supernatant is pure white.Final products therefrom is dried into powder and is dispersed in the vulcanized lead quantum dot solution that obtains 50mg/ml in normal octane.UV, visible light optical absorption spectra records the absorption peak of this quantum dot 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, with the speed spin coating 15s of 2500rpm; Sodium nitrite (the NaNO that is 10mg/ml by concentration
2) methanol solution be paved with whole quantum dot film, infiltrate 45s and dry, repeat twice; With absolute methanol, wash away remaining NaNO
2particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; Repeat above-mentionedly in steps twice, obtain three layers through NaNO
2the vulcanized lead quantum dot film of processing, completes the preparation of gas sensor.
Fig. 1 is the gas sensor response curve to 50ppm nitrogen dioxide gas at room temperature of the embodiment of the present invention 1 preparation, and as shown in Figure 1, the sensitivity of this gas sensor reaches 21.7, and response recovery time is respectively 12s and 37s.
Embodiment 2
The PbS colloidal state quantum dot solution of embodiment 1 preparation is evenly dropped in the PET plastic that is printed on electrode, with the speed spin coating 15s of 2500rpm; Sodium nitrite (the NaNO that is 10mg/ml by concentration
2) methanol solution be paved with whole quantum dot film, infiltrate 45s and dry, repeat twice; With absolute methanol, wash away remaining NaNO
2particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; Repeat above-mentionedly in steps twice, obtain three layers through NaNO
2the vulcanized lead quantum dot film of processing, completes the preparation of gas sensor.
The gas sensor of the test embodiment of the present invention 2 preparations is the response curve to 50ppm nitrogen dioxide at room temperature.
Embodiment 3
The PbS colloidal state quantum dot solution of embodiment 1 preparation is evenly dropped on the aluminium oxide ceramics substrate that is printed on electrode, with the speed spin coating 15s of 2500rpm; Sodium nitrite (the NaNO that is 10mg/ml by concentration
2) methanol solution be paved with whole quantum dot film, infiltrate 45s and dry, repeat twice; With absolute methanol, wash away remaining NaNO
2particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; Repeat above-mentionedly in steps twice, obtain three layers through NaNO
2the vulcanized lead quantum dot film of processing, completes the preparation of gas sensor.
The gas sensor of the test embodiment of the present invention 3 preparations is the response curve to 50ppm nitrogen dioxide at room temperature.
Embodiment 4
The PbS colloidal state quantum dot solution of embodiment 1 preparation is evenly dropped on the aluminium oxide ceramics substrate that is printed on electrode, with the speed spin coating 15s of 2500rpm; Ammonium chloride (the NH that is 10mg/ml by concentration
4cl) methanol solution is paved with whole quantum dot film, infiltrates 45s and dries, and repeats twice; With absolute methanol, wash away remaining NH
4cl particle and byproduct of reaction thereof, infiltrate 5s and dry, in triplicate; Repeat above-mentionedly in steps twice, obtain three layers through NH
4the vulcanized lead quantum dot film that Cl processes, completes the preparation of gas sensor.
The gas sensor of the test embodiment of the present invention 4 preparations is the response curve to 50ppm nitrogen dioxide at room temperature.
(1) prepare SnO
2colloidal state quantum dot solution.
By the SnCl of certain proportion amount
45H
2o, oleic acid and oleyl amine are heated to 100 ℃ and extremely clarification of vacuum drying reaction, are cooled to after 60 ℃ of a certain amount of ethanol of taking-up mix and add stainless steel autoclave, put into 180 ℃ of baking oven reaction 3h.Reacted rear taking-up, while being cooled to room temperature, solution taking-up in autoclave is centrifugal with ethanol mixed precipitation, subsequently precipitated product be scattered in solvent and again carry out ethanol centrifuge washing.After dry, by desired concn, be scattered in toluene and can obtain colloidal state quantum dot solution.
(2) the colloidal state quantum dot solution obtaining can be made to SnO according to the preparation method of above-mentioned colloidal state quantum dot film gas sensor
2colloidal state quantum dot film gas sensor.
The gas sensor that above-described embodiment is made and existing room temperature flexible air body sensor compare, 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 is compared with existing room temperature flexible air body sensor, when guaranteeing natural sensitivity, has greatly shortened response time and release time.To identical PbS colloidal state quantum dot, select paper as substrate, select NaNO simultaneously
2as short chain mineral solution, clean quantum dot film, the gas sensor obtaining has best combination property, i.e. higher sensitivity and shorter response recovery time.This is that gas molecule easily passes in and out colloidal state quantum dot film, thereby can reach higher sensitivity because paper substrates has loose and porous structure.
Semi-conductor electricity resistive gas sensor of the present invention and preparation method thereof is not limited to above-described embodiment, and particularly, the colloidal state quantum dot film in gas sensor is not limited to PbS colloidal state quantum dot film or SnO
2colloidal state quantum dot film can be also other semiconductor colloidal state quantum dot film; Colloidal state quantum dot solution in preparation method is not limited to PbS colloidal state quantum dot solution or SnO
2colloidal state quantum dot solution can be also other semiconductor colloidal state quantum dot solution; Dielectric substrate is not limited to paper, plastics or pottery, can be also other dielectric substrate; Short chain ligand solution is not limited to NH
4cl or NaNO
2solution can be also other short chain inorganics or organism ligand solution, as Pb (NO
3)
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 modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a preparation method for gas sensor, is characterized in that, comprises the steps:
(1) semiconductor colloidal state quantum dot solution is coated in the dielectric substrate that is printed on electrode, makes its even film forming;
(2) with short chain ligand solution, process 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 the semiconductor colloidal state quantum dot film of desired thickness, completes the preparation of gas sensor.
2. a preparation method for gas sensor, is characterized in that, comprises the steps:
(1) semiconductor colloidal state quantum dot solution is coated in dielectric substrate, makes its even film forming;
(2) with short chain ligand solution, process 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 the semiconductor colloidal state quantum dot film of desired thickness;
(5) on the semiconductor colloidal state quantum dot film obtaining in step (4), prepare electrode, complete the preparation of gas sensor.
3. the preparation method of gas sensor as claimed in claim 1 or 2, is characterized in that, described semiconductor colloidal state quantum dot solution is PbS colloidal state quantum dot solution or SnO
2colloidal state quantum dot solution.
4. the preparation method of gas sensor as claimed in claim 3, is characterized in that, described dielectric substrate is paper, plastics, pottery, silicon chip or glass.
5. the preparation method of the gas sensor as described in claim 3 or 4, is characterized in that, described short chain ligand solution is NH
4cl, NaNO
2or Pb (NO
3)
2solution.
6. a gas sensor of preparing by method described in claim 1 or 2, is characterized in that, comprises dielectric substrate, electrode and gas sensing layer, and described gas sensing layer is semiconductor colloidal state quantum dot film.
7. gas sensor as claimed in claim 6, is characterized in that, described dielectric substrate is paper, plastics, pottery, silicon chip or glass.
8. the gas sensor as described in claim 6 or 7, is characterized in that, described semiconductor colloidal state quantum dot film is PbS colloidal state quantum dot film or SnO
2colloidal state quantum dot film.
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