CN103323361A - Making method of gas-sensitive sensor array for detecting Fen-flavor liquor - Google Patents
Making method of gas-sensitive sensor array for detecting Fen-flavor liquor Download PDFInfo
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- CN103323361A CN103323361A CN2013101924873A CN201310192487A CN103323361A CN 103323361 A CN103323361 A CN 103323361A CN 2013101924873 A CN2013101924873 A CN 2013101924873A CN 201310192487 A CN201310192487 A CN 201310192487A CN 103323361 A CN103323361 A CN 103323361A
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Abstract
The invention provides a making method of a gas-sensitive sensor array for detecting a Fen-flavor liquor. The method comprises the following steps: respectively vapor-plating sodium polyacrylate, polytrimethylsilylpropyne, polystyrene and polyurethane on different quartz substrates through using a vacuum coating machine; and welding the vapor-plated quartz substrates onto a circuit board. The gas-sensitive sensor array made through using the method has the advantages of small dimension, low cost, good repeatability, long-term stable working, small influences of coexistence gases, and high resolution performance to a mixed gas. An electronic nose system made through combining the array with a piezoelectric system has the advantages of direct implementation without a tedious sample preprocessing process during the detection of the Fen-flavor liquor, fast response speed and high accuracy.
Description
Technical field
The invention belongs to the gas sensor technical field, especially relate to a kind of preparation method who detects the gas sensor array of fen-flavor type white spirit.
Background technology
At present in liquor industry, how the problem such as have that the quality and safety control level is lower, fast detecting scarce capacity, correlation technique and equipment fall behind differentiates that the liquor quality becomes the Focal point and difficult point of food products market management.The food connoisseur observes, analyzes, describes, defines the level according to color, the lattice of product by vision, sense of smell, the sense of taste, makes comprehensive evaluation, as the Main Basis of determining the liquor grade.This method is quick, easy, and evaluation has globality, comprehensive advantage.Yet different people has different impressions to the same smell, thereby different evaluations is just arranged; People's sensory sensitivity is vulnerable to the interference of extraneous factor, even same person also has different impressions and evaluation to the same smell when different environment, different mood, so sensory evaluation exists certain limitation and uncertainty.The nineties in 20th century, a kind of mode that combines by gas sensor and mode identification technology occurs and simulated the Biologic Olfaction system, thereby realize volatile matter is carried out the new equipment-Electronic Nose (claiming again the smell scanner) of detection and Identification function, its core component is gas sensor, and it is objective, quick, repeated to have advantages of.
In the development of Electronic Nose, the choice and application of gas sensor array is key factor, and suitable sensor array is most important to the performance that improves whole system.The kind of gas sensor array is a lot, and commonly used have metal-oxide semiconductor (MOS) (MOS) conductivity type gas sensor array, organic polymer films (CP) conductivity type gas sensor array, QCM (Quartz Crystal Microbalance) (QCM) gas sensor array, surface acoustic wave (SAW) gas sensor array, L B film gas sensor array and a galvanochemistry type gas sensor array etc.Yet these gas sensor array all exist some unavoidable defectives, as: the high and necessary heating of the working temperature of MOS type gas sensor, easily drift about, the sulfide that occurs in the mixed gas easily is " poisoning " reaction; CP conductivity type gas sensor active material electropolymerization process is difficulty and time-consuming relatively, has drift with the VOC contact response, and very responsive to humidity, release time is long; QCM gas sensor test specification is less, and affected by environment larger, cost is high; The poor signal to noise of SAW gas sensor, sensitivity is lower; The chip of L B film gas sensor MOSFET vessel sensor is difficult for encapsulation with integrated, have the reference value drift, and kind is less; Galvanochemistry type gas sensor easy to leak, complicated in mechanical structure, the life-span is not long, and the gaseous species of detection is limited, and manufacturing cost is high, is unsuitable for portable electric nose.Therefore, need a kind of fast detecting, liquor determination device that resolution is high on the market.
Summary of the invention
The object of the invention provides a kind of preparation method who detects the gas sensor array of fen-flavor type white spirit, and size of the present invention is little, and cost is low, good reproducibility, and the energy long-term stable operation, the impact of coexistence γ-ray emission is little, and is high to the resolution performance of mixed gas.
Realize the object of the invention: a kind of preparation method who detects the gas sensor array of fen-flavor type white spirit comprises step:
(1) with vacuum coating equipment respectively with sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, polyurethane evaporation on different quartz substrates;
(2) quartz substrate that evaporation is good is welded on the circuit board.
The vacuum tightness of vacuum coating equipment is 1 * 10 in the described step (1)
-7-1 * 10
-5Mbar.
The evaporation thickness of four kinds of thin polymer films is 50 μ m-80 μ m in the described step (1).
The evaporation temperature is 80-150 ℃ in the described step (1).
The beneficial effect of the gas sensor array that application the method is made:
Size of the present invention is little, and cost is low, good reproducibility, and the energy long-term stable operation, the impact of coexistence γ-ray emission is little, and is high to the resolution performance of mixed gas.The electric nasus system that this gas sensor array is made in conjunction with piezoelectric system does not need the loaded down with trivial details pretreatment process of sample when detecting fen-flavor type white spirit, can directly carry out, and fast response time, accuracy is high.
Embodiment
Be better explanation the present invention, the below is clearly and completely described the technical scheme in the embodiment of the invention.
The characteristic volatile ingredient of analyzing in the fen-flavor type white spirit (take Fenyang wine as example) by GC-MS in the laboratory is water, ethanol, ethyl acetate, ethyl lactate.In the structural formula according to sodium polyacrylate carboxyl is arranged, easily and form more intense hydrogen bond action between the hydrone, so sodium polyacrylate is soluble in water, namely it has preferably compatibility to water; According to the hydrogen atom on the silicon methyl in poly-trimethyl silicane-1-propine structure easily and the stronger hydrogen bond action of the formation of the oxygen atom in the ethanol molecule, judge that it is soluble in ethanol, namely it has preferably compatibility to ethanol; The solubility parameters (δ=9.1) of the solubility parameters of polystyrene (δ=8.9) and ethyl acetate is very approaching, and the degree of their polarity and formation hydrogen bond about equally, so polystyrene is soluble in ethyl acetate, namely ethyl acetate p-poly-phenyl ethene has good compatibility; Judge that according to rule of similarity polyurethane can be dissolved in ethyl lactate, namely polyurethane has preferably compatibility to ethyl lactate.Following table is characterization compound in the Fenyang wine and the fluoropolymer resin structural formula of compatibility sensitivity thereof:
Therefore four kinds of polymkeric substance among the present invention respectively in corresponding and the fen-flavor type white spirit principal ingredient water, ethanol, ethyl acetate, ethyl lactate etc. preferably compatibility is arranged.When the mixed gas in the test sample liquor passes through this gas sensor array, polymer film can be to there being higher responsiveness, the electric signal collection of illustrative plates that is comprehensively responded by piezoelectric system, namely obtain to reflect the characteristic spectrum storehouse of this sample, contrast by the standard diagram with delicate fragrance type wine, to reach the qualitative analysis to test sample liquor.
Embodiment 1:
1, the used sodium polyacrylate of experiment is bought in Aladdin reagent company limited, and molecular weight is 4,000,000; Water is secondary deionized water; Poly-trimethyl silicane-1-propine is bought in Aladdin reagent company limited, and molecular weight is 500,000; Ethanol is bought in Aladdin reagent company limited, is AR level pure reagent; Polystyrene is bought in lark prestige reagent company limited, and molecular weight is 15000; Ethyl acetate is bought in lark prestige reagent company limited, and content is 99.8%; Polyurethane is bought in lark prestige reagent company limited, and molecular weight is 35000; Ethyl lactate is bought in Aladdin reagent company limited, is AR level pure reagent.
2, be that 10mm thickness is that its concrete steps are as follows on the circular quartz substrate of 1mm with sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, polyurethane evaporation at diameter respectively on the UNIVEX-300 type vacuum coating equipment:
(1) selects suitable substrate frame, place quartz substrate and polyurethane;
(2) check recirculated cooling water, pressurized air and high pure nitrogen state, check the oil level of mechanical pump and outlet oil mist filter;
(3) the primary power knob is threaded to vertical position, after instrument self checking is normal, bell jar is buckled, note the connecting rod position in left side;
(4) by F1 and F5 display screen is switched to the interface of bleeding, begin to bleed, forbid outage after beginning to bleed;
(5) setting instrument setting evaporation thickness at thickness is 50 μ m; In the baffle controls interface of main screen, change control mode into auto;
(6) reach 1 * 10 when vacuum tightness
-5During mbar, the beginning evaporation;
(7) hot evaporated segment: open the hot evaporation power-supply controller of electric of bottom, change control model into internal, give tacit consent to (inboard) heated by electrodes No. 1.Regulate electric current to vacuum the temperature inside the box and rise to 120 ℃, observe heating boat situation by view window.Press the open button of film-thickness monitoring and open baffle plate, the beginning evaporation.When thickness reached 50 μ m, film-thickness monitoring autoshutdown baffle plate to external, cut off electric current with the control mode switch of hot evaporation power-supply controller of electric.This layer material evaporation is finished;
(8) continue to vacuumize about 10 minutes after evaporation is finished, wait to plate to stop again bleeding after material cools off fully;
Switch to the interface of bleeding when (9) closing vacuum pump, press switch after molecular pump at first begin stall, show the load of molecular pump this moment on the molecular pump power source controller.After the load pilot lamp extinguishes, main screen is switched to the inflation interface, press the inflation button and begin inflation.Need open the reduction valve of High Purity Nitrogen this moment, and back pressure forbids surpassing an atmospheric pressure.Open bell jar after venting is finished, take out sample and plating material, evaporation process is finished, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) in like manner, with sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene respectively evaporation be that 10mm thickness is on the circular quartz substrate of 1mm at diameter.
3, the model of buying in Beijing Orient De Fei Instr Ltd. is that the contact angle instrument of OCA20 is measured every kind of reagent and its corresponding contact angle, measurement result shows that the contact angle of water and sodium polyacrylate film is 17.5 °, much smaller than 90 °, show that the compatibility of water and sodium polyacrylate is fine; The contact angle of ethanol and poly-trimethyl silicane-1-propine film is 20.6 °, shows that the compatibility of ethanol and poly-trimethyl silicane-1-propine is fine; The contact angle of ethyl acetate and plasticon is 25.5 °, shows that the compatibility of ethyl acetate and polyurethane is better; The contact angle of ethyl lactate and polyurethane is 24 °, shows that the compatibility of ethyl lactate and polyurethane is better.
4, four kinds of polymer film piezoids with preparation in the step 2 are welded in respectively on the circuit board, make gas sensor, at last it are arranged in a row in the plastics box that is fixed in long * wide * height=45 * a 3 * 12mm, have made gas sensor array.
Embodiment 2:
1, identical among agents useful for same and polymkeric substance and the embodiment 1.
2, respectively sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, polyurethane evaporation are being grown * wide=10 * 10mm on UNIVEX-300 type vacuum coating equipment, thickness is that its concrete steps are as follows on the square quartz substrate of 1mm:
(1) selects suitable substrate frame, place quartz substrate and polyurethane;
(2) check recirculated cooling water, pressurized air and high pure nitrogen state, check the oil level of mechanical pump and outlet oil mist filter;
(3) the primary power knob is threaded to vertical position, after instrument self checking is normal, bell jar is buckled, note the connecting rod position in left side;
(4) by F1 and F5 display screen is switched to the interface of bleeding, begin to bleed, forbid outage after beginning to bleed;
(5) setting instrument setting evaporation thickness at thickness is 70 μ m; In the baffle controls interface of main screen, change control mode into auto;
(6) reach 1 * 10 when vacuum tightness
-6During mbar, the beginning evaporation;
(7) hot evaporated segment: open the hot evaporation power-supply controller of electric of bottom, change control model into internal, give tacit consent to (inboard) heated by electrodes No. 1.Regulate electric current to vacuum the temperature inside the box and rise to 100 ℃, observe heating boat situation by view window.Press the open button of film-thickness monitoring and open baffle plate, the beginning evaporation.When thickness reached 70 μ m, film-thickness monitoring autoshutdown baffle plate to external, cut off electric current with the control mode switch of hot evaporation power-supply controller of electric.This layer material evaporation is finished;
(8) continue to vacuumize about 10 minutes after evaporation is finished, wait to plate to stop again bleeding after material cools off fully;
Switch to the interface of bleeding when (9) closing vacuum pump, press switch after molecular pump at first begin stall, show the load of molecular pump this moment on the molecular pump power source controller.After the load pilot lamp extinguishes, main screen is switched to the inflation interface, press the inflation button and begin inflation.Need open the reduction valve of High Purity Nitrogen this moment, and back pressure forbids surpassing an atmospheric pressure.Open bell jar after venting is finished, take out sample and plating material, evaporation process is finished, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) in like manner, sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene philosophy evaporation are being grown * wide=10 * 10mm, thickness is on the square quartz substrate of 1mm.
3, the model of buying in Beijing Orient De Fei Instr Ltd. is that the contact angle instrument of OCA20 is measured every kind of reagent and its corresponding contact angle, and is identical among measurement result and the embodiment 1.
4, four kinds of polymer film piezoids with preparation in the step 2 are welded in respectively on the circuit board, make gas sensor, at last it are arranged in a row in the plastics box that is fixed in long * wide * height=45 * a 3 * 12mm, have just made gas sensor array.
Embodiment 3:
1, identical among agents useful for same and polymkeric substance and the embodiment 1.
2, on UNIVEX-300 type vacuum coating equipment respectively sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, polyurethane evaporation is being grown * wide=12 * 12mm, thickness is that its concrete steps are as follows on the square quartz substrate of 1.2mm:
(1) selects suitable substrate frame, place quartz substrate and polystyrene;
(2) check recirculated cooling water, pressurized air and high pure nitrogen state, check the oil level of mechanical pump and outlet oil mist filter;
(3) the primary power knob is threaded to vertical position, after instrument self checking is normal, bell jar is buckled, note the connecting rod position in left side;
(4) by F1 and F5 display screen is switched to the interface of bleeding, begin to bleed, forbid outage after beginning to bleed;
(5) setting instrument setting evaporation thickness at thickness is 80 μ m; In the baffle controls interface of main screen, change control mode into auto;
(6) reach 1 * 10 when vacuum tightness
-7During mbar, the beginning evaporation;
(7) hot evaporated segment: open the hot evaporation power-supply controller of electric of bottom, change control model into internal, give tacit consent to (inboard) heated by electrodes No. 1.Regulate electric current to vacuum the temperature inside the box and rise to 80 ℃, observe heating boat situation by view window.Press the open button of film-thickness monitoring and open baffle plate, the beginning evaporation.When thickness reached 80 μ m, film-thickness monitoring autoshutdown baffle plate to external, cut off electric current with the control mode switch of hot evaporation power-supply controller of electric.This layer material evaporation is finished;
(8) continue to vacuumize about 10 minutes after evaporation is finished, wait to plate to stop again bleeding after material cools off fully;
Switch to the interface of bleeding when (9) closing vacuum pump, press switch after molecular pump at first begin stall, show the load of molecular pump this moment on the molecular pump power source controller.After the load pilot lamp extinguishes, main screen is switched to the inflation interface, press the inflation button and begin inflation.Need open the reduction valve of High Purity Nitrogen this moment, and back pressure forbids surpassing an atmospheric pressure.Open bell jar after venting is finished, take out sample and plating material, evaporation process is finished, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) in like manner, with sodium polyacrylate, poly-trimethyl silicane-1-propine, polyurethane respectively evaporation growing * wide=12 * 12mm, thickness is on the square quartz substrate of 1.2mm.
3, the model of buying in Beijing Orient De Fei Instr Ltd. is that the contact angle instrument of OCA20 is measured every kind of reagent and its corresponding contact angle, and is identical among measurement result and the embodiment 1.
4, four kinds of polymer film piezoids with preparation in the step 2 are welded in respectively on the circuit board, make gas sensor, at last it are arranged in a row in the plastics box that is fixed in long * wide * height=55 * a 3 * 15mm, have just made gas sensor array.
The gas sensor array made from the method, can be made into electric nasus system in conjunction with piezoelectric system, during test sample, gas sensor array is placed the bottleneck of sample liquor, bottleneck is opened, when the characteristic odor of sample liquor passes through gas sensor array, polymer film on the gas sensor array is with the feature volatile ingredient of adsorption sample liquor, make its mass penalty, the electric signal spectrogram that this phenomenon is comprehensively responded by piezoelectric system, namely obtain reflecting the feature spectrogram of sample liquor, this spectrogram with compare as the standard control spectrogram of identification fen-flavor type white spirit, to reach the qualitative analysis to sample liquor.
The present invention is by the physicochemical property of the feature volatile matter of analysis fen-flavor type white spirit, the thin polymer film coating material of the compatibility sensitivity that research and screening are suitable, the feature intelligent of research and collection fen-flavor type white spirit is smelt the news collection of illustrative plates, by the collection of illustrative plates comparison, whether the true and false and the quality that detect fen-flavor type white spirit reach a standard.
Use the gas sensor array that the present invention makes, size is little, and cost is low, good reproducibility, and the energy long-term stable operation, coexistence gas is little on the impact of its generation, and is high to the resolution performance of mixed gas.And its electric nasus system of making in conjunction with piezoelectric system does not need the loaded down with trivial details pretreatment process of sample when detecting fen-flavor type white spirit, can directly carry out, and fast response time, accuracy is high.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (4)
1. a preparation method who detects the gas sensor array of fen-flavor type white spirit is characterized in that, comprises step:
(1) with vacuum coating equipment respectively with sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, polyurethane evaporation on different quartz substrates;
(2) quartz substrate that evaporation is good is welded on the circuit board.
2. the preparation method of the gas sensor array of detection fen-flavor type white spirit according to claim 1 is characterized in that, the vacuum tightness of vacuum coating equipment is 1 * 10 in the described step (1)
-7-1 * 10
-5Mbar.
3. the preparation method of the gas sensor array of detection fen-flavor type white spirit according to claim 1 is characterized in that, the evaporation thickness of four kinds of thin polymer films is 50 μ m-80 μ m in the described step (1).
4. the preparation method of the gas sensor array of detection fen-flavor type white spirit according to claim 1 is characterized in that, the evaporation temperature is 80-150 ℃ in the described step (1).
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| CN2013101924873A CN103323361A (en) | 2013-05-22 | 2013-05-22 | Making method of gas-sensitive sensor array for detecting Fen-flavor liquor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103543176A (en) * | 2013-10-16 | 2014-01-29 | 北京交通大学 | Preparation method of gas sensor array for detecting feng-flavor type white spirit |
| CN103543177A (en) * | 2013-10-16 | 2014-01-29 | 北京交通大学 | Preparation method of gas sensor array for detecting all-aroma type white spirit |
| CN103755153A (en) * | 2014-01-22 | 2014-04-30 | 南通天盛新能源科技有限公司 | Method for preparing substrate for high formyl group functional group density biological chip |
-
2013
- 2013-05-22 CN CN2013101924873A patent/CN103323361A/en active Pending
Non-Patent Citations (3)
| Title |
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| 孙良彦: "国外半导体气体传感器件发展概况", 《仪表技术与传感器》 * |
| 王传荣: "白酒的香型及其风味特征研究", 《酿酒科技》 * |
| 王立川: "基于气体传感器阵列的白酒分类与识别", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103543176A (en) * | 2013-10-16 | 2014-01-29 | 北京交通大学 | Preparation method of gas sensor array for detecting feng-flavor type white spirit |
| CN103543177A (en) * | 2013-10-16 | 2014-01-29 | 北京交通大学 | Preparation method of gas sensor array for detecting all-aroma type white spirit |
| CN103755153A (en) * | 2014-01-22 | 2014-04-30 | 南通天盛新能源科技有限公司 | Method for preparing substrate for high formyl group functional group density biological chip |
| CN103755153B (en) * | 2014-01-22 | 2016-03-30 | 南通天盛实验器材有限公司 | A kind of method preparing high aldehyde functions's density biochip substrate |
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Application publication date: 20130925 |