CN103308415B - A kind of preparation method detecting the gas sensor array of Maotai-flavor liquor - Google Patents
A kind of preparation method detecting the gas sensor array of Maotai-flavor liquor Download PDFInfo
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- CN103308415B CN103308415B CN201310192852.0A CN201310192852A CN103308415B CN 103308415 B CN103308415 B CN 103308415B CN 201310192852 A CN201310192852 A CN 201310192852A CN 103308415 B CN103308415 B CN 103308415B
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- flavor liquor
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Abstract
The invention provides a kind of preparation method detecting the gas sensor array of Maotai-flavor liquor, comprise step: (1) with vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation on different quartz substrates; (2) by quartz substrate good for evaporation welding on circuit boards; Apply gas sensor array size prepared by method of the present invention little, cost is low, reproducible, can long-term stable operation, and the impact that co-existing gases produces is little, high to the resolution performance of mixed gas.And with the electric nasus system that it is made in conjunction with piezoelectric system, the pretreatment process not needing sample loaded down with trivial details when detecting Maotai-flavor liquor, can directly carry out, and fast response time, accuracy is high.
Description
Technical field
The invention belongs to gas sensor technology field, especially relate to a kind of preparation method detecting the gas sensor array of Maotai-flavor liquor.
Background technology
Food security has been global problems, especially at liquor industry, there is the problems such as lower, the quick detectability deficiency of quality and safety control level, correlation technique and equipment fall behind, how to differentiate that white wine quality becomes the Focal point and difficult point of food products market management.Nearly ten years, China has introduced external more advanced instrument and equipment in succession, but as a whole, traditional method of inspection can not meet the demand of society, therefore, be badly in need of wanting new effective detection means, the nineties in 20th century, occur that a kind of mode combined by gas sensor and mode identification technology simulates Biologic Olfaction system, thus realize the new equipment-Electronic Nose (also known as smell scanner) of volatile matter being carried out to detection and Identification function, its core component is gas sensor, has objective, quick, repeated advantage.
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 improving whole system.The kind of gas sensor array is a lot, and conventional has 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 galvanochemistry type gas sensor array etc.But these gas sensor array all also exist some unavoidable defects, as: the working temperature of MOS type gas sensor is high and must heat, and easily drifts about, to the sulfide occurred in the mixed gas easily reaction in " poisoning "; CP conductivity type gas sensor active material electropolymerization process is more difficult and time-consuming, and exist with VOC contact response and drift about, very responsive to humidity, release time is long; QCM gas sensor test specification is less, and affected by environment comparatively large, 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 not easily encapsulates with integrated, there is 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, market needs a kind of quick detection, liquor determination device that resolution is high.
Summary of the invention
The object of the invention is to provide a kind of preparation method detecting the gas sensor array of Maotai-flavor liquor, and size of the present invention is little, and cost is low, reproducible, and energy long-term stable operation, the impact that co-existing gases produces is little, high to the resolution performance of mixed gas.
Realize the object of the invention: a kind of preparation method detecting the gas sensor array of Maotai-flavor liquor, comprises step:
(1) with vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation on different quartz substrates;
(2) by quartz substrate good for evaporation welding on circuit boards.
In described step (1), the vacuum tightness of vacuum coating equipment is 1 × 10
-6-1 × 10
-5mbar.
In described step (1), the evaporation thickness of four kinds of thin polymer films is 50 μm-100 μm.
In described step (1), evaporation temperature is 80-150 DEG C.
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, reproducible, and energy long-term stable operation, the impact that co-existing gases produces is little, high to the resolution performance of mixed gas.The electric nasus system that this gas sensor array is made in conjunction with piezoelectric system, the pretreatment process not needing sample loaded down with trivial details when detecting Maotai-flavor liquor, can directly carry out, and fast response time, accuracy is high.
Embodiment
For better the present invention being described, below the technical scheme in the embodiment of the present invention is clearly and completely described.
Be water, ethanol, acetic acid and lactic acid by the GC-MS characteristic volatile ingredient analyzed in Maotai-flavor liquor (for Maotai) in the lab.Have carboxyl according in the structural formula of sodium polyacrylate, easily and between hydrone form stronger hydrogen bond action, so sodium polyacrylate is soluble in water, namely it has good compatibility to water; Form stronger hydrogen bond action according to the oxygen atom of the hydrogen atom on silicon methyl in poly-trimethyl silicane-1-propine structure easily and in ethanol molecule, judge that it is soluble in ethanol, namely it has good compatibility to ethanol; Acetic acid is with strong electrophilic group (-COOH), and nylon 6 is containing stronger electron donating group (-NH-), so can judge that nylon 6 is soluble in acetic acid according to solvation principle, namely nylon 6 pairs of acetic acid have good compatibility; Lactic acid can form intramolecular hydrogen bond, and exposed hydroxyl can form intermolecular ydrogen bonding with the ester group in organic glass structure, so organic glass can be dissolved in lactic acid, namely organic glass has good compatibility to lactic acid.Following table is the fluoropolymer resin structural formula of characteristic compounds in Maotai and compatibility sensitivity thereof:
Therefore the characteristic odor water, ethanol, acetic acid, lactic acid etc. of four kinds of polymer films in the present invention respectively in corresponding and Maotai-flavor liquor have good compatibility, when detecting the mixed gas in sample by this gas sensor array, polymer film can to there being higher responsiveness, the electric signal collection of illustrative plates of comprehensive response is obtained by piezoelectric system, namely the characteristic spectrum storehouse reflecting this sample is obtained, by contrasting with the standard diagram of Maotai-flavor liquor, to reach the qualitative analysis to detected sample white wine.
Embodiment 1:
1, testing sodium polyacrylate used buys 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 AlfaAesar 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, on UNIVEX-300 type vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation on the circular quartz substrate of diameter to be 10mm thickness be 1mm, its concrete steps are as follows:
(1) select 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) 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 interface of bleeding, starts to bleed, after starting to bleed, forbid power-off;
(5) on thickness setting instrument, setting evaporation thickness is 50 μm; Control mode is changed into auto in the baffle controls interface of main screen;
(6) when vacuum tightness reaches 1 × 10
-5during mbar, start evaporation;
(7) hot evaporated segment: the hot evaporation power-supply controller of electric opening bottom, changes control model into internal, give tacit consent to No. 1 (inner side) heated by electrodes.Regulate electric current to rise to 130 DEG C to vacuum the temperature inside the box, observe heating boat situation by view window.Baffle plate opened by the open button pressing film-thickness monitoring, starts evaporation.When thickness reaches 50 μm, the automatic closing baffle plate of film-thickness monitoring, by the control mode switch of hot evaporation power-supply controller of electric to external, cuts off electric current.This layer material evaporation completes;
(8) evaporation continues after completing to vacuumize about 10 minutes, stops bleeding after waiting plating material to cool completely again;
(9) be switched to interface of bleeding when closing vacuum pump, after pressing switch, first molecular pump starts stall, now molecular pump power source controller shows the load of molecular pump.After load pilot lamp extinguishes, main screen is switched to inflation interface, presses inflation button and start inflation.Now need the reduction valve opening High Purity Nitrogen, back pressure is forbidden more than an atmospheric pressure.Open bell jar after having exitted, take out sample and plating material, evaporation process completes, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) in like manner, by sodium polyacrylate, poly-trimethyl silicane-1-propine, organic glass respectively evaporation on the circular quartz substrate of diameter to be 10mm thickness be 1mm.
3, the model bought in Beijing Orient De Fei Instrument Ltd. be OCA20 contact angle instrument on measure the contact angle of the thin polymer film of often kind of reagent and its correspondence, the contact angle of measurement result display 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 film 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 of preparation in step 2 are welded on circuit board respectively, make gas sensor, be finally arranged in a row in the plastics box being fixed on long × wide × height=45 × 3 × 12mm, made gas sensor array.
Embodiment 2:
1, agents useful for same and polymkeric substance in the same manner as in Example 1.
2, on UNIVEX-300 type vacuum coating equipment, respectively sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation are being grown × wide=15 × 10mm, thickness is that on the rectangle quartz substrate of 1mm, its concrete steps are as follows:
(1) select suitable substrate frame, place quartz substrate and sodium polyac rylate 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) 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 interface of bleeding, starts to bleed, after starting to bleed, forbid power-off;
(5) on thickness setting instrument, setting evaporation thickness is 80 μm; At the baffle controls interface of main screen
Middlely change control mode into auto;
(6) when vacuum tightness reaches 2 × 10
-6during mbar, start evaporation;
(7) hot evaporated segment: the hot evaporation power-supply controller of electric opening bottom, changes control model into internal, give tacit consent to No. 1 (inner side) heated by electrodes.Regulate electric current to rise to 120 DEG C to vacuum the temperature inside the box, observe heating boat situation by view window.Baffle plate opened by the open button pressing film-thickness monitoring, starts evaporation.When thickness reaches 80 μm, the automatic closing baffle plate of film-thickness monitoring, by the control mode switch of hot evaporation power-supply controller of electric to external, cuts off electric current.This layer material evaporation completes;
(8) evaporation continues after completing to vacuumize about 10 minutes, stops bleeding after waiting plating material to cool completely again;
(9) be switched to interface of bleeding when closing vacuum pump, after pressing switch, first molecular pump starts stall, now molecular pump power source controller shows the load of molecular pump.After load pilot lamp extinguishes, main screen is switched to inflation interface, presses inflation button and start inflation.Now need the reduction valve opening High Purity Nitrogen, back pressure is forbidden more than an atmospheric pressure.Open bell jar after having exitted, take out sample and plating material, evaporation process completes, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) in like manner, by poly-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 bought in Beijing Orient De Fei Instrument Ltd. be OCA20 contact angle instrument on measure the contact angle of the thin polymer film of often kind of reagent and its correspondence, measurement result is identical with in embodiment 1.
4, four kinds of polymer film piezoids of preparation in step 2 are welded on circuit board respectively, make gas sensor, be finally arranged in a row in the plastics box being fixed on long × wide × height=65 × 3 × 12mm, just made gas sensor array.
Embodiment 3:
1, agents useful for same and polymkeric substance in the same manner as in Example 1.
2, on UNIVEX-300 type vacuum coating equipment, respectively sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation are being grown × wide=12 × 12mm, thickness is that on the square quartz substrate of 1.0mm, its concrete steps are as follows:
(1) select suitable substrate frame, place quartz substrate and sodium polyac rylate 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) 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 interface of bleeding, starts to bleed, after starting to bleed, forbid power-off;
(5) on thickness setting instrument, setting evaporation thickness is 100 μm; Control mode is changed into auto in the baffle controls interface of main screen;
(6) when vacuum tightness reaches 1 × 10
-6during mbar, start evaporation;
(7) hot evaporated segment: the hot evaporation power-supply controller of electric opening bottom, changes control model into internal, give tacit consent to No. 1 (inner side) heated by electrodes.Regulate electric current to rise to 100 DEG C to vacuum the temperature inside the box, observe heating boat situation by view window.Baffle plate opened by the open button pressing film-thickness monitoring, starts evaporation.When thickness reaches 100 μm, the automatic closing baffle plate of film-thickness monitoring, by the control mode switch of hot evaporation power-supply controller of electric to external, cuts off electric current.This layer material evaporation completes;
(8) evaporation continues after completing to vacuumize about 10 minutes, stops bleeding after waiting plating material to cool completely again;
(9) be switched to interface of bleeding when closing vacuum pump, after pressing switch, first molecular pump starts stall, now molecular pump power source controller shows the load of molecular pump.After load pilot lamp extinguishes, main screen is switched to inflation interface, presses inflation button and start inflation.Now need the reduction valve opening High Purity Nitrogen, back pressure is forbidden more than an atmospheric pressure.Open bell jar after having exitted, take out sample and plating material, evaporation process completes, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) in like manner, by poly-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 bought in Beijing Orient De Fei Instrument Ltd. be OCA20 contact angle instrument on measure the contact angle of often kind of reagent and its correspondence, measurement result is identical with in embodiment 1.
4, four kinds of polymer film piezoids of preparation in step 2 are welded on circuit board respectively, make gas sensor, be finally arranged in a row in the plastics box being fixed on long × wide × height=55 × 3 × 15mm, just made gas sensor array.
With the gas sensor array that the method is made, electric nasus system is can be made in conjunction with piezoelectric system, when detecting sample, gas sensor array is placed in the bottleneck of sample white wine, bottleneck is opened, smells of wine are through gas sensor array, polymer film on gas sensor array is by the volatile ingredient of this wine of absorption, its quality is increased, this phenomenon obtains the electric signal spectrogram of comprehensive response by piezoelectric system, namely the feature spectrogram that can reflect sample white wine is obtained, this spectrogram contrasts with the standard control spectrogram as identification Maotai-flavor liquor, to reach the qualitative analysis to detected sample white wine.
The present invention is by analyzing the physicochemical property of the feature volatile matter of Maotai-flavor liquor, study and screen the polymer thin film coating materials of suitable compatibility sensitivity, to study and the feature intelligent gathering Maotai-flavor liquor smells news collection of illustrative plates, by collection of illustrative plates comparison, whether the true and false and the quality that detect sample white wine reach a standard.
The gas sensor array that application the present invention makes, size is little, and cost is low, reproducible, and energy long-term stable operation, the impact that co-existing gases produces it is little, high to the resolution performance of mixed gas.And its electric nasus system made in conjunction with piezoelectric system, the pretreatment process not needing sample loaded down with trivial details when detecting Maotai-flavor liquor, can directly carry out, fast response time, accuracy is high.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change 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 (1)
1. detect a preparation method for the gas sensor array of Maotai-flavor liquor, it is characterized in that, comprise step:
(1) with vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 6, organic glass evaporation on different quartz substrates;
(2) by quartz substrate good for evaporation welding on circuit boards;
In described step (1), the vacuum tightness of vacuum coating equipment is 1 × 10
-6-1 × 10
-5mbar;
In described step (1), the evaporation thickness of four kinds of thin polymer films is 50 μm-100 μm;
In described step (1), evaporation temperature is 80-150 DEG C.
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| 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 |
| 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 |
| 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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Non-Patent Citations (3)
| Title |
|---|
| 《国外半导体气体传感器件发展概况》;孙良彦;《仪表技术与传感器》;19801231(第4期);第1-5页 * |
| 《基于气体传感器阵列的白酒分类与识别》;王立川;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20110915(第9期);第2-4章 * |
| 《白酒的香型及其风味特征研究》;王传荣;《酿酒科技》;20081231(第9期);第49-52页 * |
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