CN103308415A - Preparation method of gas sensor array for detecting maotai-flavor liquor - Google Patents
Preparation method of gas sensor array for detecting maotai-flavor liquor Download PDFInfo
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- CN103308415A CN103308415A CN2013101928520A CN201310192852A CN103308415A CN 103308415 A CN103308415 A CN 103308415A CN 2013101928520 A CN2013101928520 A CN 2013101928520A CN 201310192852 A CN201310192852 A CN 201310192852A CN 103308415 A CN103308415 A CN 103308415A
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- gas sensor
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- maotai
- flavor liquor
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Abstract
The invention provides a preparation method of a gas sensor array for detecting maotai-flavor liquor. The preparation method comprises the steps of: (1) respectively steam-plating sodium polyacrylate, poly(1-(trimethylsilyl)-1-propyne), nylon 6 and organic glass on different quartz substrates by virtue of a vacuum film plating machine; and (2), welding the quartz substrates subjected to steam plating on a circuit board. The gas sensor array which is prepared by virtue of the method is small in size, low in cost and good in repeatability, can stably work in a long term, generates little influence on generation of coexistence gas and has high distinguishing performance to mixed gas. In addition, when an electronic nose system which is made by combining the gas sensor array and a piezoelectric system is used for detecting the maotai-flavor liquor, a fussy pretreatment process of a sample is not needed, the maotai-flavor liquor can be directly detected, the response speed is rapid, and the accuracy is high.
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 Maotai-flavor liquor.
Background technology
Food security has been global problems, and how problem such as especially at liquor industry, 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 emphasis and the difficult point of food products market management.Over past ten years, China has introduced external advanced instrument and equipment in succession, but as a whole, traditional method of inspection has not satisfied social demand, therefore, be badly in need of wanting new effective detection means, the nineties in 20th century, a kind of mode that combines by gas sensor and mode identification technology occurs and simulated biological olfactory system, thereby realize volatile matter is carried out the new equipment-Electronic Nose (claiming the smell scanner again) of detection and Identification function, its core component is gas sensor, has objective, quick, repeated advantage.
In the development of Electronic Nose, the selection of gas sensor array and application are key factors, and the right sensors array is most important to the performance that improves total 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 is affected by environment bigger, the cost height; 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 the manufacturing cost height, is unsuitable for portable electric nose.Therefore, need a kind of fast detecting, liquor pick-up unit 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 Maotai-flavor liquor, and size of the present invention is little, and cost is low, good reproducibility, and the energy long-term stable operation, the influence that coexistence gas produces is little, to the resolution performance height of mixed gas.
Realize the object of the invention: a kind of preparation method who detects the gas sensor array of Maotai-flavor liquor comprises step:
(1) with vacuum coating equipment respectively with sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation on different quartz substrates;
(2) evaporation is good quartz substrate is welded on the circuit board.
The vacuum tightness of vacuum coating equipment is 1 * 10 in the described step (1)
-6-1 * 10
-5Mbar.
The evaporation thickness of four kinds of thin polymer films is 50 μ m-100 μ m in the described step (1).
The evaporation temperature is 80-150 ℃ in the described step (1).
Use the beneficial effect of the gas sensor array that this method makes:
Size of the present invention is little, and cost is low, good reproducibility, and the energy long-term stable operation, the influence that coexistence gas produces is little, to the resolution performance height 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 pre-treatment process of sample when detecting Maotai-flavor liquor, can directly carry out, and response speed is fast the accuracy height.
Embodiment
For better explanation the present invention, below the technical scheme in the embodiment of the invention is clearly and completely described.
The characteristic volatile ingredient of analyzing in the Maotai-flavor liquor (be example with Maotai) by GC-MS in the laboratory is water, ethanol, acetic acid and lactic acid.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 compatibility preferably 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 compatibility preferably to ethanol; Acetic acid has strong electrophilic group, and (COOH), nylon 6 contains stronger electron donating group (NH-), so can judge that according to the solvation principle nylon 6 is soluble in acetic acid, namely 6 pairs of acetic acid of nylon has compatibility preferably; Lactic acid can form intramolecular hydrogen bond, exposed hydroxyl can with the organic glass structure in ester group form intermolecular ydrogen bonding, so organic glass can be dissolved in lactic acid, namely organic glass has compatibility preferably to lactic acid.Following table is characterization compound and the compatibility sensitive polymers resin structure formula thereof in the Maotai:
Therefore the characteristic odor water in the corresponding and Maotai-flavor liquor, ethanol, acetic acid, lactic acid etc. have compatibility preferably to four kinds of polymer films among the present invention respectively, when the mixed gas in the test sample 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 Maotai-flavor wine, to reach the qualitative analysis to the sample liquor that is detected.
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; Nylon 6 is bought in A Faaisha reagent company limited, and molecular weight is about 27000; Acetic acid is bought in lark prestige reagent company limited, and content is 99.8%; Organic glass is bought in lark prestige reagent company limited, and molecular weight is 15000; Lactic acid is bought in Aladdin reagent company limited, is AR level pure reagent.
2, be that its concrete steps are as follows on the circular quartz substrate of 1mm with sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation for 10mm thickness at diameter respectively on the UNIVEX-300 type vacuum coating equipment:
(1) selects suitable substrate frame, place quartz substrate and nylon 6;
(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, treats after instrument self checking normally bell jar to be 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 130 ℃, 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 was closed baffle plate automatically, and the control model of hot evaporation power-supply controller of electric is switched to external, cut off electric current.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 treating that 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, the high purity nitrogen of orderly close-down, primary power, recirculated cooling water and pressurized air;
(10) in like manner, with sodium polyacrylate, poly-trimethyl silicane-1-propine, organic glass respectively evaporation be on the circular quartz substrate of 1mm for 10mm thickness at diameter.
3, the model of buying in Beijing Orient De Fei Instr Ltd. is contact angle instrument every kind of reagent of measurement of OCA20 and the contact angle of its corresponding polymers film, 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 acetic acid and nylon 6 films is 25 °, shows that the compatibility of acetic acid and nylon 6 is better; The contact angle of lactic acid and organic glass film is 29.6 °, shows that the compatibility of lactic acid and organic glass 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, nylon 6, organic glass evaporation are being grown * wide=15 * 10mm on UNIVEX-300 type vacuum coating equipment, thickness is that its concrete steps are as follows on the rectangle quartz substrate of 1mm:
(1) selects suitable substrate frame, place quartz substrate and polyacrylic acid sodium polymer;
(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, treats after instrument self checking normally bell jar to be 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; Baffle controls interface at main screen
In change control mode into auto;
(6) reach 2 * 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 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 80 μ m, film-thickness monitoring was closed baffle plate automatically, and the control model of hot evaporation power-supply controller of electric is switched to external, cut off electric current.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 treating that 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, the high purity nitrogen of orderly close-down, primary power, recirculated cooling water and pressurized air;
(10) in like manner, will gather trimethyl silicane-1-propine, nylon 6, organic glass etc. respectively evaporation growing * wide=15 * 10mm, thickness is on the rectangle quartz substrate of 1mm.
3, the model of buying in Beijing Orient De Fei Instr Ltd. is the contact angle that the contact angle instrument of OCA20 is measured every kind of reagent and its corresponding polymers film, 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=65 * 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, respectively sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation are being grown * wide=12 * 12mm on UNIVEX-300 type vacuum coating equipment, thickness is that its concrete steps are as follows on the square quartz substrate of 1.0mm:
(1) selects suitable substrate frame, place quartz substrate and polyacrylic acid sodium polymer;
(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, treats after instrument self checking normally bell jar to be 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 100 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 100 μ m, film-thickness monitoring was closed baffle plate automatically, and the control model of hot evaporation power-supply controller of electric is switched to external, cut off electric current.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 treating that 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, the high purity nitrogen of orderly close-down, primary power, recirculated cooling water and pressurized air;
(10) in like manner, will gather trimethyl silicane-1-propine, nylon 6, organic glass respectively evaporation growing * wide=12 * 12mm, thickness is on the square quartz substrate of 1.0mm.
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 this 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, during smells of wine process gas sensor array, polymer film on the gas sensor array will adsorb the volatile ingredient of this wine, its quality is increased, 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 Maotai-flavor liquor, to reach the qualitative analysis to the sample liquor that is detected.
The present invention is by the physicochemical property of the feature volatile matter of analysis Maotai-flavor liquor, research and the suitable compatibility sensitive polymers film coating material of screening, the feature intelligent of research and collection Maotai-flavor liquor is smelt the news collection of illustrative plates, by the collection of illustrative plates comparison, whether the true and false of test sample liquor and quality 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 to the influence of its generation, to the resolution performance height of mixed gas.And its electric nasus system of making in conjunction with piezoelectric system does not need the loaded down with trivial details pre-treatment process of sample when detecting Maotai-flavor liquor, can directly carry out, and response speed is fast, the accuracy height.
The above; only for the preferable embodiment of the present invention, but protection scope of the present invention is not limited thereto, and 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 Maotai-flavor liquor is characterized in that, comprises step:
(1) with vacuum coating equipment respectively with sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation on different quartz substrates;
(2) evaporation is good quartz substrate is welded on the circuit board.
2. the preparation method of the gas sensor array of detection Maotai-flavor liquor according to claim 1 is characterized in that, the vacuum tightness of vacuum coating equipment is 1 * 10 in the described step (1)
-6-1 * 10
-5Mbar.
3. the preparation method of the gas sensor array of detection Maotai-flavor liquor according to claim 1 is characterized in that, the evaporation thickness of four kinds of thin polymer films is 50 μ m-100 μ m in the described step (1).
4. the preparation method of the gas sensor array of detection Maotai-flavor liquor according to claim 1 is characterized in that, the evaporation temperature is 80-150 ℃ in the described step (1).
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| CN201310192852.0A CN103308415B (en) | 2013-05-22 | 2013-05-22 | A kind of preparation method detecting the gas sensor array of Maotai-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 |
| CN103743951A (en) * | 2013-12-23 | 2014-04-23 | 中安高科检测科技（北京）有限公司 | Preparation method of gas-sensitive sensor array for dry salted and fermented soya paste from Six-necessity Store |
-
2013
- 2013-05-22 CN CN201310192852.0A patent/CN103308415B/en not_active Expired - Fee Related
Non-Patent Citations (3)
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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》, no. 4, 31 December 1980 (1980-12-31) * |
| 王传荣: "《白酒的香型及其风味特征研究》", 《酿酒科技》, no. 9, 31 December 2008 (2008-12-31) * |
| 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》, no. 9, 15 September 2011 (2011-09-15) * |
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 |
| CN103743951A (en) * | 2013-12-23 | 2014-04-23 | 中安高科检测科技（北京）有限公司 | Preparation method of gas-sensitive sensor array for dry salted and fermented soya paste from Six-necessity Store |
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