CN102841077B - High-throughput screening platform for gas sensitive materials based on photo-thermal jointed excitation - Google Patents
High-throughput screening platform for gas sensitive materials based on photo-thermal jointed excitation Download PDFInfo
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Abstract
The invention discloses a high-throughput screening platform for gas sensitive materials based on photo-thermal jointed excitation. The high-throughput screening platform comprises a computer, a temperature control module, a gas circuit control module, a light source control module, a test chamber and a signal modulation module, wherein the test chamber is used for providing a testing environment including temperatures, gas categories, gas concentrations and light signals for the gas sensitive materials to be tested, and the test chamber is also used for educing test signals of the gas sensitive materials to be tested; and a material chip matched with the platform integrates signal electrodes and materials onto an alumina ceramic sheet by screen printing or other methods. The platform completes the high-throughout characterization of the gas sensitive materials at the conditions of specific temperatures, gas categories, concentrations and light excitation in a cooperation and modularized manner, the gas sensitive materials with practical application can be rapidly screened according to test results, and the platform can be used for detecting and warning hazardous gas in production and life of people.
Description
Technical field
The present invention relates to performance test and the screening of gas sensitive, specifically refer to the proving installation of the iron-enriched yeast material air-sensitive performance under a kind of photo-thermal associating shooting conditions, thus for the screening of material and the follow-up design instructing new material.
Background technology
Metal-oxide gas transducer has low price because of it, and susceptibility is high, and the response time is fast and be easy to the advantages such as production in enormous quantities and be widely used.Therefore exploitation has the metal oxide gas sensitive of hypersensitivity, high selectivity and good stability, for the preparation of gas sensor or sensor array, has great market using value.A kind of new gas sensitive of tradition exploitation generally will through the longer time cycle, and namely the performance of the preparing again of the performance evaluation-material-material of the preparation-material of material revalues, and so continuous circulation is explored, until the material of acquisition excellent performance.Such one side takes a large amount of time and efforts; Greatly slow down the speed of new material exploitation and gas sensor application on the other hand.Therefore develop a kind of can the Screening Platform of iron-enriched yeast gas sensitive performance, greatly can shorten performance evaluation time and the cost of new material system, reduce the error of Repeatability test, significant to the exploitation of gas sensor.
Summary of the invention
The object of the present invention is to provide and a kind ofly combine the gas sensitive high flux screening platform excited based on photo-thermal, the present invention accurately can control the temperature of material chip, the wavelength of laser exciter and intensity, and the test condition such as atmosphere, and then under the different photo-thermal shooting conditions of quick obtaining each gas sensitive film to the sensitive property of gas with various/smell.
Gas sensitive high flux screening platform under a kind of photo-thermal associating shooting conditions provided by the invention, comprises computing machine, temperature control modules, gas circuit control module, light source control module, test chamber and Signal-regulated kinase; It is characterized in that:
Computing machine passes through temperature control modules, gas circuit control module, and the control of light source control module regulates the test environment of test chamber, thus completes the high-throughout sign of gas sensitive;
Test chamber is used for providing for gas sensitive to be tested the test environment comprising temperature, gaseous species, gas concentration and light signal, and the extraction of the test signal of gas sensitive to be tested;
Temperature control modules controls for the temperature of test chamber;
Gas circuit control module is used for the test gas kind of test chamber and the control of concentration;
Optical excitation control module is used for the control of photo-excitation conditions needed for test chamber;
The test signal of Signal-regulated kinase to the gas sensitive to be tested of being drawn by test chamber is amplified, be supplied to computing machine after filtering operation carries out follow-up process.
As the improvement of technique scheme, described test chamber comprises epicoele and cavity of resorption, and the cavity of resorption of test chamber comprises middle substrate
and infrabasal plate, groove has been dug at middle substrate center place, for laying temperature control chip and material chip, and temperature control chip is positioned at below material chip, heating plate, between middle substrate and infrabasal plate, infrabasal plate has air intake opening, and middle substrate has gas outlet, gas is entered in the groove of middle substrate by air intake opening, and is discharged by gas outlet;
The epicoele of test chamber mainly comprises one piece of upper cover plate, signal probe, signal integrated circuit plate and laser exciter: in the middle part of upper cover plate, have window, transparent material installed by window, the window surrounding of upper cover plate has duct, the position consistency of its position and material chip electrode pin; Signal probe inserts in described duct, and laser exciter is positioned at above window, and signal integrated circuit plate is used for the test signal of signal probe to draw test chamber; The surrounding of upper cover plate has bosh, for the protection of laser exciter and the signal integrated circuit plate destruction from high temperature.
Digging the groove of an annular between the epicoele of test chamber and cavity of resorption, for placing red copper O-ring seal, ensureing the leakproofness after the pressing of test chamber upper and lower cavity.
As the further improvement of technique scheme, temperature control modules comprises heating control circuit and temperature control chip, wherein heating control circuit be connect with the heating plate in test chamber after, the heating power of heating plate is controlled by the output controlling heating duty ratio, temperature control chip is connected with the temperature signal end of heating control circuit, for the temperature feedback to material chip; Temperature control chip to be brushed on alumina ceramic substrate by Pt silk-screen by the mode of serigraphy to be made, and during use, is close to by temperature control chip and is placed on below material chip to be tested.
A more step as technique scheme is improved, and laser exciter is LED light source array; Gas circuit control module is made up of the flow controller of multiple parallel connection; First signal probe is inserted in the alumina ceramic tube of certain length and is glued together, and then vertically inserts in the duct of upper cover plate; Signal probe and ceramic pipe and and upper cover plate between all carry out adhesive seal by high temperature inorganic glue.
The multi-electrode material chip that the platform provided with invention mates, the multiple gas sensitive film of accessible site on it; Platform accurately can control the temperature of material chip, the wavelength of laser exciter and intensity in addition, and the test condition such as atmosphere, so under the different photo-thermal shooting conditions of quick obtaining each gas sensitive film to the sensitive property of gas with various/smell.The present invention has worked in coordination with the iron-enriched yeast of gas sensitive under photo-thermal associating shooting conditions in a modular manner, reach convenient and obtain the performance parameter of gas sensitive fast, thus filter out suitable material for specific application background, and database is provided to instruct for the design of follow-up new material.
Accompanying drawing explanation
Fig. 1 combines based on photo-thermal the gas sensitive high flux screening platform schematic diagram excited.
Fig. 2 is the test chamber schematic diagram removing top cage in example.
Fig. 3 is 36 array material chip schematic diagram in example.
Fig. 4 is the test platform of this example of employing take tin ash as base material, and the mode surface modification noted by droplet under the condition of thermal excitation obtains the air-sensitive performance the selection result of 34 kinds of different materials system PARA FORMALDEHYDE PRILLS(91,95)s, toluene, benzene, dimethylbenzene, sulphuric dioxide, nitrogen dioxide, carbon monoxide and ammonias.300 DEG C, Fig. 4 (a) formaldehyde; Fig. 4 (b) toluene 300 DEG C; Fig. 4 (c) benzene 300 DEG C; Fig. 4 (d) dimethylbenzene 300 DEG C; Fig. 4 (e) carbon monoxide 200 DEG C; Fig. 4 (f) ammonia 200 DEG C; Fig. 4 (g) sulphuric dioxide 200 DEG C; Fig. 4 (h) nitrogen dioxide 200 DEG C.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be not intended to limit the present invention.
Provided by the inventionly a kind ofly combine the gas sensitive high flux screening platform excited based on photo-thermal, for the performance characterization of many arrays gas sensitive and screening.
As shown in Figure 1, the gas sensitive high flux screening platform that this example provides comprises computing machine 1, temperature control modules 2, gas circuit control module 3, optical excitation control module 4, test chamber 5, and Signal-regulated kinase 6.
As shown in Figure 2, the test chamber 5 that this example adopts is for providing for gas sensitive to be tested the test environment comprising temperature, gaseous species, gas concentration and light signal, and the extraction of the test signal of gas sensitive to be tested.
Test chamber 5 is primarily of epicoele and cavity of resorption composition, the cavity of resorption of test chamber 5 forms primarily of middle substrate 5B and infrabasal plate 5C, be embedded with the heating plate 51 into cavity heating two pieces of substrate 5B, 5C middles, in addition, between two cover plates 5B, 5C, also dig air intake opening 52 and gas outlet 53.Wherein air intake opening 52 is positioned at the side of infrabasal plate 5C heating plate 51, is a vertical through hole.Enter in test chamber after air drain after gas is entered by air intake opening 52 below middle substrate 5B, the tail gas tested leaves test chamber 5 and discharges through gas outlet 53, and gas outlet 53 is arranged in the side of substrate 5B; Dug groove in middle substrate 5B centre, for laying temperature control chip 54 and material chip 50, and temperature control chip 54 is positioned at below material chip 50, just can be controlled the probe temperature of gas sensitive like this by temperature control modules 2 accurately.Here material chip 50 can adopt multiple material (as pottery, silicon chip etc.) to be obtained by the fabrication techniques such as serigraphy, photoetching, and the electrode wiring mode of material chip 50 can design according to the demand of user.
The epicoele of test chamber 5 mainly comprises one piece of upper cover plate 5A, signal probe 55, signal integrated circuit plate 56 and laser exciter 59: have bosh 57 in the inner direction along rib of upper cover plate 5A surrounding, for the protection of laser exciter 59 and signal integrated circuit plate 56 destruction from high temperature; First signal probe 55 is inserted in the alumina ceramic tube of certain length and is glued together, then vertically insert in the duct of upper cover plate 5A (on upper cover plate 5A, the position in duct and the position of material chip 50 electrode pin are consistent), after the degree of depth inserted ensures epicoele and cavity of resorption pressing, signal probe 55 can with material chip 50 close contact in cavity of resorption, signal probe 55 and ceramic pipe and all carry out adhesive seal by high temperature inorganic glue afterwards and between upper cover plate 5A in whole process; Signal integrated circuit plate 56 signal probe is stretched out the partly integrated of epicoele upper cover plate 5A then by data connector 58, test signal is drawn test chamber; The position of laser exciter 59 is positioned at the centre of epicoele upper cover plate 5A: it digs a foursquare window in the centre of upper cover plate 5A, window quartz glass seals, then put on the Centromedian window of upper cover plate 5A after packaged for laser exciter 59, be positioned at directly over material chip 50, ensure that the material on material chip 50 is positioned within the illumination range of laser exciter 59.Corresponding position is also dug in the middle of the signal integrated circuit plate 56 replacing that a square hole identical with laser exciter 59 size is convenient to laser exciter 59.
Dig the groove of an annular between the epicoele of test chamber and cavity of resorption, for placing red copper O-ring seal 5D, then epicoele and cavity of resorption are fixed up by the screw pressing on four angles, ensure the leakproofness after test chamber upper and lower chamber pressing.
Computing machine 1 is central controller and the data processing of whole platform and stores terminal, its test environment needed for material, by exporting the control of temperature control modules 2, gas circuit control module 3 and light source control module 4, complete material at specified temp, iron-enriched yeast under gaseous species and concentration and photo-excitation conditions, finally realizes the collection to material electric signal, pre-service and storage.
Temperature control modules 2 controls for the heating of gas sensitive and temperature.The temperature control modules 2 that this example adopts mainly comprises heating control circuit and temperature control chip 54.Wherein heating control circuit be connect with the heating plate 51 in test chamber 5 after, the heating power of heating plate 51 is controlled by the output controlling heating duty ratio, temperature control chip 54 is connected with the temperature signal end of heating control circuit, for the temperature feedback to material chip 50.Temperature control chip 54 to be brushed on alumina ceramic substrate by Pt silk-screen by the mode of serigraphy to be made, during use, temperature control chip 54 is close to and is placed on below material chip 50 to be tested, so just accurately can control the temperature of gas sensitive (i.e. material chip to be tested).Whole temperature control modules 2 is controlled by computing machine 1.Temperature controlling range is room temperature ~ 600 DEG C.
Gas circuit control module 3 is for the control of gas sensitive test gas kind and concentration.Gas circuit control module 3 in this example is formed primarily of the flow controller of multiple parallel connection, and by the accurate control of flow controller to each component gas flow, the gas blending desired concn is sent in test chamber by the air intake opening 52 in test chamber 5.
Optical excitation control module 4 is for the control of photo-excitation conditions needed for gas sensitive.Optical excitation control module 4 in this example is for controlling laser exciter 59, and computing machine 1, by optical excitation control module 4, controls the light signal of laser exciter 59, to complete the photoexcitation process to gas sensitive on material chip 50.The LED light source array that the laser exciter 59 that this platform current uses is mainly commercially available;
The test signal of Signal-regulated kinase 6 to the gas sensitive to be tested of being drawn by test chamber 5 carries out pre-service, and is supplied to computing machine 1.
The course of work of test platform provided by the invention is:
(1) corresponding bid value is inputted under the control panel of the modules in a computer of the external field environment first needed for testing of materials;
(2) each control module is started working after receiving the order that computing machine transmits: temperature control modules 2 according to bid value by heating materials to corresponding temperature value, gas circuit control module 3 starts according to bid value the mode selecting the kind of measurement atmosphere and mixed gas, and optical excitation control module 4 controls wavelength and the intensity of cut-offfing of laser exciter 59 and laser exciter according to bid value.Whole effective object is all the material chip 50 in test chamber 5;
(3), after treating that each control module reaches stable output according to bid value, computing machine completes the iron-enriched yeast to material chip 50 by corresponding testing process again;
(4), after having tested, computing machine 1 completes pre-service and the storage of test data.
Example 1:
Adopt and provided by the inventionly combine the gas sensitive high flux screening platform that excites to SnO based on photo-thermal
2base gas sensitive has carried out the high flux screening under thermal excitation condition.In this example, material chip 50 adopts 36 array material chips, and as shown in Figure 3, be printed on 36 parallel poles 33 by the mode of serigraphy in the centre of alumina ceramic substrate 31, electrode pin 32 cloth is to the surrounding of potsherd.For the material chip designed, first we print identical SnO by the method for serigraphy on the parallel pole 33 of 36 array material chips
2base material, then notes the mode of surface modification at 36 SnO by droplet
2base material film instils the ionizable metal salt solution of 3 kinds of concentration of upper Ca, Ti, Cr, Mn, Fe, Co, Pd, Cu, Zn, Y, Ce 11 kinds of different elements.Mode finally by high temperature sintering obtains the 36 array material chips prepared.
After preparing 36 array material chips, we are from room temperature, and the temperature of test chamber 5 is controlled to 300 DEG C, to SnO
2sill chip carries out air-sensitive performance test, test gas to as if eight kinds of main room air pollution gas formaldehyde, toluene, benzene, dimethylbenzene, nitrogen dioxide, sulphuric dioxide, carbon monoxide and ammonias, test concentrations is 18.7ppm respectively, 11.7ppm, 8.6ppm, 10.6ppm, 29ppm, 44ppm, 2142.5ppm and 33ppm.
By high-throughout performance characterization, we filter out respectively for doping process and the working temperature of eight kinds of gas the bests, and test screen result is as shown in table 1:
Table 1SnO
2the air-sensitive performance test screen result of sill chip
As can be seen here, in this example, under utilizing photo-thermal provided by the invention to combine shooting conditions, gas sensitive high flux screening platform can characterize the air-sensitive performance of a large amount of material systems under the modulating action of light and heat fast, then from these characterization results, we can filter out gas sensitive specific gas to hypersensitivity and high selectivity fast, thus for the making of gas sensor.
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 done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. the gas sensitive high flux screening platform under photo-thermal associating shooting conditions, is characterized in that: it comprises computing machine (1), temperature control modules (2), gas circuit control module (3), light source control module (4), test chamber (5) and Signal-regulated kinase (6);
Computing machine (1) passes through temperature control modules (2), gas circuit control module (3), and the control of light source control module (4) regulates the test environment of test chamber (5), thus completes the high-throughout sign of gas sensitive;
Test chamber (5) is for providing for gas sensitive to be tested the test environment comprising temperature, gaseous species, gas concentration and light signal, and the extraction of the test signal of gas sensitive to be tested;
Temperature control modules (2) controls for the temperature of test chamber (5);
The test gas kind of gas circuit control module (3) for test chamber (5) and the control of concentration;
Optical excitation control module (4) is for the control of the required photo-excitation conditions of test chamber (5);
The test signal of Signal-regulated kinase (6) to the gas sensitive to be tested of being drawn by test chamber (5) is amplified, be supplied to computing machine (1) after filtering operation carries out follow-up process, test chamber (5) comprises epicoele and cavity of resorption, the cavity of resorption of test chamber (5) comprises middle substrate 5B and infrabasal plate (5C), groove has been dug in middle substrate (5B) centre, for laying temperature control chip (54) and material chip (50), and temperature control chip (54) is positioned at material chip (50) below, heating plate (51) is arranged between substrate (5B) and infrabasal plate (5C), infrabasal plate (5C) has air intake opening (52), middle substrate (5B) has gas outlet (53), gas enters in the groove of middle substrate (5B) by air intake opening (52), and discharged by gas outlet (53),
The epicoele of test chamber (5) mainly comprises one piece of upper cover plate (5A), signal probe (55), signal integrated circuit plate (56) and laser exciter (59): have window at upper cover plate (5A) middle part, transparent material installed by window, the window surrounding of upper cover plate (5A) has duct, the position consistency of its position and material chip (50) electrode pin; Signal probe (55) first inserts in alumina ceramic tube, more vertically inserts in the described duct of upper cover plate (5A), and after the degree of depth of insertion ensures epicoele and cavity of resorption pressing, signal probe (55) can with material chip (50) close contact in cavity of resorption; Signal probe (55) and ceramic pipe and and upper cover plate (5A) between all carry out adhesive seal by high temperature inorganic glue; Laser exciter (59) is positioned at above window, and signal integrated circuit plate (56) is for drawing test chamber by the test signal of signal probe (55); The surrounding of upper cover plate (5A) has bosh (57), for the protection of laser exciter (59) and signal integrated circuit plate (56) destruction from high temperature;
Dig the groove of an annular between the epicoele of test chamber and cavity of resorption, for placing red copper O-ring seal (5D), and between epicoele and cavity of resorption, pressing is fixed;
Temperature control modules (2) comprises heating control circuit and temperature control chip (54), wherein heating control circuit be connect with the heating plate (51) in test chamber (5) after, the heating power of heating plate (51) is controlled by the output controlling heating duty ratio, temperature control chip (54) is connected with the temperature signal end of heating control circuit, for the temperature feedback to material chip (50); Temperature control chip (54) to be brushed on alumina ceramic substrate by Pt silk-screen by the mode of serigraphy to be made, and during use, is close to by temperature control chip (54) and is placed on below material chip to be tested (50);
Described laser exciter (59) is LED light source array;
Described gas circuit control module (3) is made up of the flow controller of multiple parallel connection.
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| CN104076122A (en) * | 2014-05-26 | 2014-10-01 | 电子科技大学 | Temperature continuously-adjustable point-contact gas-sensitive humidity-sensitive test cavity |
| CN104807786A (en) * | 2015-05-14 | 2015-07-29 | 中国科学院新疆理化技术研究所 | Method for photo-electrically detecting trinitrotoluene steam by utilizing catalytic-gas sensitive mechanism |
| EP3417271A4 (en) * | 2016-02-16 | 2019-11-13 | Weiss Technik North America, Inc. | Environmental test chamber |
| CN106226356A (en) * | 2016-08-16 | 2016-12-14 | 成都市和平科技有限责任公司 | A kind of Intelligent indoor formaldehyde gas detecting system and method |
| CN109900749A (en) * | 2019-03-13 | 2019-06-18 | 华中科技大学 | A kind of micro-hotplate Gas Sensor Array device and manufacturing method based on ceramic substrate |
| CN110646468B (en) * | 2019-09-29 | 2022-02-11 | 天津职业技术师范大学(中国职业培训指导教师进修中心) | Method for characterizing high-throughput materials |
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