CN103323362A - Method for preparing gas-sensitive sensor array for detecting rice-flavor liquor - Google Patents
Method for preparing gas-sensitive sensor array for detecting rice-flavor liquor Download PDFInfo
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- CN103323362A CN103323362A CN2013102020062A CN201310202006A CN103323362A CN 103323362 A CN103323362 A CN 103323362A CN 2013102020062 A CN2013102020062 A CN 2013102020062A CN 201310202006 A CN201310202006 A CN 201310202006A CN 103323362 A CN103323362 A CN 103323362A
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Abstract
The invention provides a method for preparing a gas-sensitive sensor array for detecting rice-flavor liquor, comprising the following steps of: (1) vapor-plating sodium polyacrylat, poly[1-(trimethylsilyl)-1-propyne, nylon 66, polystyrene and polyurethane on different quartz substrates by a vacuum coating machine respectively; and (2) welding the vapor-plated quartz substrates on a circuit board. The gas-sensitive sensor array prepared by the method has advantages of small dimension, low cost, good repeatability, long-term stable work, small influence caused by concomitant gases, and high resolution ratio on mixed gases. An electric noise system prepared by combination of the gas-sensitive sensor array and a piezoelectric system, can detect true and false of the rice-flavor liquor without a complex pretreatment process on a sample, can directly be used, and has advantages of fast response speed and high accuracy.
Description
Technical field
The invention belongs to the gas sensor technical field, especially relate to a kind of its preparation method that detects the gas sensor array of rice spirit.
Background technology
Concern have in the liquor industry of broad masses of the people life that the quality and safety control level is lower, fast detecting scarce capacity, correlation technique and the problems such as equipment falls behind, how to differentiate that the liquor quality becomes the Focal point and difficult point that food products market is managed.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 gas sensor of using at present mainly is that electricity is led control sensor (having the body electricity to lead two kinds of control type and surface conductance control types), be the gas sensor of CN114655A such as publication number, its structure mainly comprises layer of metal oxide gas sensory (such as ZnO, SnO2 etc.) and a well heater.This class gas sensor need to be heated to carrying out smoothly of about 300 ℃ of guarantee redox reactions, therefore there is following drawback in it: one, need heating and temperature controlling device, increased the volume of sensor, power consumption and complexity, inconvenience is made of existing microelectronic technique; Two, integrated level is not high; Three, not high to the weak organic gas sensitivity of most of oxidation-reduction quality.Therefore, with development a kind of can fast detecting, liquor determination device that resolution is high, the effective development of China's food service industry is significant.
Summary of the invention
The object of the invention provides a kind of preparation method who detects the gas sensor array of rice 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 rice spirit comprises step:
(1) with vacuum coating equipment respectively with sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 66, 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)
-6-1 * 10
-5Mbar.
The evaporation thickness of five kinds of thin polymer films is 80 μ m-120 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 rice 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 rice spirit (take the Guilin three-flower wine as example) by GC-MS in the laboratory is water, ethanol, bata-phenethyl alcohol, ethyl acetate and 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; Hydroxyl in the bata-phenethyl alcohol (OH) easily and the hydrogen on the amide group form hydrogen bond, be soluble in bata-phenethyl alcohol so can judge nylon 66, namely 66 pairs of bata-phenethyl alcohols of nylon have the compatibility of getting well; 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 three-flower wine of Guilin and the fluoropolymer resin structural formula of compatibility sensitivity thereof:
Therefore five kinds of polymer films among the present invention respectively characteristic odor water, ethanol, bata-phenethyl alcohol, ethyl acetate, the ethyl lactate in the corresponding and rice spirit preferably compatibility is arranged, 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 liquor, 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 66 is bought in A Faaisha reagent company limited, and molecular weight is about 27000; Bata-phenethyl alcohol is bought in lark prestige reagent company limited, purity 95%; 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, nylon 66, polystyrene, polyurethane evaporation at diameter respectively on the UNIVEX-300 type vacuum coating equipment:
(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
-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 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, nylon 66, polyurethane 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 bata-phenethyl alcohol and nylon 66 films is 23.3 °, shows that the compatibility of bata-phenethyl alcohol and nylon 66 is better; The contact angle of ethyl acetate and plasticon is 25.5 °, shows that the compatibility of ethyl acetate and polystyrene is better; The contact angle of ethyl lactate and polyurethane film is 24 °, shows that the compatibility of ethyl lactate and polyurethane is better.
4, five 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=60 * 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 66, polystyrene, polyurethane 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 0.8mm:
(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 100 μ m; Baffle controls interface at main screen
Middlely 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 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 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, nylon 66, polyurethane philosophy evaporation are being grown * wide=12 * 12mm, thickness is on the square quartz substrate of 0.8mm.
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 thin polymer film, and is identical among measurement result and the embodiment 1.
4, five 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=70 * a 3 * 15mm, 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 66, polystyrene, polyurethane evaporation are being grown * wide=12 * 8mm on UNIVEX-300 type vacuum coating equipment, thickness is that its concrete steps are as follows on the rectangle quartz substrate of 1.2mm:
(1) selects suitable substrate frame, place quartz substrate and poly styrene 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, 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 120 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 120 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, nylon 66, polystyrene, polyurethane respectively evaporation growing * wide=12 * 8mm, thickness is on the rectangle quartz substrate of 1.2mm.
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 thin polymer film, and is identical among measurement result and the embodiment 1.
4, five 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=70 * a 3 * 10mm, 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, during smells of wine process gas sensor array, polymer film on the gas sensor array will adsorb the feature volatile ingredient of this wine, 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 spectrogram of identification rice spirit, 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 rice spirit, the thin polymer film coating material of the compatibility sensitivity that research and screening are suitable, the feature intelligent of research and collection rice spirit 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 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 rice 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 rice spirit is characterized in that, comprises step:
(1) with vacuum coating equipment respectively with sodium polyacrylate, poly-trimethyl silicane-1-propine, nylon 66, 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 rice spirit 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 rice spirit according to claim 1 is characterized in that, the evaporation thickness of five kinds of thin polymer films is 80 μ m-120 μ m in the described step (1).
4. the preparation method of the gas sensor array of detection rice spirit according to claim 1 is characterized in that, the evaporation temperature is 80-150 ℃ in the described step (1).
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| CN2013102020062A CN103323362A (en) | 2013-05-27 | 2013-05-27 | Method for preparing gas-sensitive sensor array for detecting rice-flavor liquor |
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| CN2013102020062A CN103323362A (en) | 2013-05-27 | 2013-05-27 | Method for preparing gas-sensitive sensor array for detecting rice-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
- 2013-05-27 CN CN2013102020062A patent/CN103323362A/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 (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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Application publication date: 20130925 |