CN103543176A - Preparation method of gas sensor array for detecting feng-flavor type white spirit - Google Patents
Preparation method of gas sensor array for detecting feng-flavor type white spirit Download PDFInfo
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- CN103543176A CN103543176A CN201310484559.1A CN201310484559A CN103543176A CN 103543176 A CN103543176 A CN 103543176A CN 201310484559 A CN201310484559 A CN 201310484559A CN 103543176 A CN103543176 A CN 103543176A
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Abstract
The invention provides a preparation method of a gas sensor array for detecting feng-flavor type white spirit. The preparation method comprises the following steps: (1) respectively evaporating and plating sodium polyacrylate, polytrimethyl silicon-1-propyne, polystyrene and alkyd resin on different quartz substrates by adopting a vacuum coating machine; and (2) welding the evaporated and plated quartz substrates on a circuit board. The gas sensor array prepared by applying the preparation method disclosed by the invention is small in dimension, low in cost, good in repeatability, capable of stably working for a long time, small in influences generated by coexisted gases and high in resolution performance of a gas mixture. An electronic noise system manufactured by combining the gas sensor array with a voltage system can directly detect without a fussy sample pre-treatment process while detecting whether the feng-flavor type white spirit is true or false; and moreover, the preparation method is quick in response speed and high in degree of accuracy.
Description
Technical field
The invention belongs to gas sensor technical field, especially relate to a kind of preparation method who detects the gas sensor array of phoenix aromatic white spirit.
Background technology
At present, food security has been global problems, especially in being related to the liquor industry of broad masses of the people's life, how the problem such as have that quality and safety control level is lower, fast detecting scarce capacity, correlation technique and equipment fall behind, differentiate that white wine quality becomes the Focal point and difficult point of food products market management.The nineties in 20th century, occurred that a kind of mode combining by gas sensor and mode identification technology simulates Biologic Olfaction system, thereby realize the new equipment-Electronic Nose (claiming again smell scanner) of volatile matter being carried out to detection and Identification function, its core component is gas sensor, has advantages of objective, quick, repeated.
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 of raising whole system.At present the gas sensor of application is mainly that electricity is led and controlled sensor (having body electricity to lead two kinds of control type and surface conductance control types), as the publication number gas sensor that is CN114655A, its structure mainly comprise layer of metal oxide gas sensory (as ZnO, SnO
2deng) 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, by development a kind of can fast detecting, the effective development of liquor determination device ，Dui China food service industry that resolution is high is significant.
Summary of the invention
The object of the invention is to provide a kind of preparation method who detects the gas sensor array of phoenix aromatic white spirit, and size of the present invention is little, and cost is low, reproducible, energy long-term stable operation, and the impact of the γ-ray emission that coexists is little, high to the resolution performance of mixed gas.
A kind of preparation method who detects the gas sensor array of phoenix aromatic white spirit who realizes the object of the invention, comprises step:
(1) with vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, alkyd resin evaporation on different quartz substrates;
(2) the good quartz substrate of evaporation is welded on circuit board.
In described step (1), the vacuum tightness of vacuum coating equipment is 1 * 10
-6-1 * 10
-5mbar.
In described step (1), four kinds of thin polymer film evaporation thickness are 50 μ m-100 μ m.
In described step (1), evaporation temperature is 80-120 ℃.
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, energy long-term stable operation, and the impact of the γ-ray emission that coexists 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 does not need the loaded down with trivial details pretreatment process of sample when detecting phoenix aromatic white spirit, can directly carry out, and fast response time, accuracy is high.
Embodiment
For better explanation the present invention, below the technical scheme in the embodiment of the present invention is clearly and completely described.
The characteristic volatile ingredient of analyzing in phoenix aromatic white spirit (take Xifeng as example) by GC-MS in laboratory is water, ethanol, ethyl acetate, ethyl hexanoate.In structural formula according to sodium polyacrylate, have carboxyl, easily and between hydrone form more intense hydrogen bond action, so sodium polyacrylate is soluble in water, it has good compatibility to water; Oxygen atom according to the hydrogen atom on silicon methyl in poly-trimethyl silicane-1-propine structure easily and in ethanol molecule forms stronger hydrogen bond action, judges that it is soluble in ethanol, and it has good compatibility to ethanol; Very approaching according to the solubility parameters (δ=8.9) of polystyrene and the solubility parameters (δ=9.1) of ethyl acetate, and the degree of their polarity and formation hydrogen bond about equally, so polystyrene is soluble in ethyl acetate, ethyl acetate p-poly-phenyl ethene has good compatibility; According to containing electrophilic group (COOH) in Structure Detemination of Alkyd Resins, in ethyl hexanoate, contain electron donating group (OCOCH
3), the intermolecular hydrogen bond action in addition of alkyd resin and ethyl hexanoate, judges that alkyd resin is soluble in ethyl hexanoate in addition, alkyd resin has good compatibility to ethyl hexanoate.Following table is characterization compound in Xifeng and the fluoropolymer resin structural formula of compatibility sensitivity thereof:
Therefore four kinds of polymkeric substance in the present invention respectively in corresponding and phoenix aromatic white spirit principal ingredient water, ethanol, ethyl acetate, ethyl hexanoate etc. have good compatibility.When the mixed gas in detecting sample white wine passes through this gas sensor array, polymer film can be to there being higher responsiveness, by piezoelectric system, obtain the electric signal collection of illustrative plates of comprehensive response, obtain reflecting the characteristic spectrum storehouse of this sample, by contrasting with the standard diagram of phoenix aromatic white spirit, to reach detecting the qualitative analysis of sample white wine.
Embodiment 1:
1, test sodium polyacrylate used and buy in Aladdin reagent company limited, 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 purity is 99.8%; Alkyd resin is bought in Aladdin reagent company limited, and molecular weight is 2,000,000; Ethyl hexanoate is bought in Aladdin reagent company limited, and purity is 99%.
2, on UNIVEX-300 type vacuum coating equipment, by sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, alkyd resin evaporation, at diameter, be that 8mm thickness is that on the circular quartz substrate of 0.8mm, its concrete steps are as follows respectively:
(1) select 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) 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) pass through F
1and F
5display screen is switched to the interface of bleeding, starts to bleed, after starting to bleed, forbid power-off;
(5) on thickness setting instrument, setting evaporation thickness is 50 μ m; In the baffle controls interface of main screen, change control mode into auto;
(6) when vacuum tightness reaches 1 * 10
-6during mbar, start 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 (inner side) heated by electrodes No. 1.Regulate electric current to vacuum the temperature inside the box to rise to 80 ℃, by view window, observe heating boat situation.Press the open button of film-thickness monitoring and open baffle plate, start evaporation.When thickness reaches 50 μ m, the automatic closing baffle plate of film-thickness monitoring, to external, cuts off electric current by the control mode switch of hot evaporation power-supply controller of electric.This layer material evaporation completes;
(8) evaporation continues to vacuumize about 10 minutes after completing, and stops bleeding after waiting plating material completely cooling again;
(9) while closing vacuum pump, be switched to the interface of bleeding, press switch after molecular pump first start stall, now on molecular pump power source controller, show the load of molecular pump.After load pilot lamp extinguishes, main screen is switched to inflation interface, press inflation button and start inflation.Now need to open the reduction valve of High Purity Nitrogen, back pressure forbids surpassing an atmospheric pressure.After having exitted, open bell jar, 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, alkyd resin respectively evaporation at diameter, be that 8mm thickness is on the circular quartz substrate of 0.8mm.
3, on the contact angle instrument that the model of buying in Beijing Orient De Fei Instrument Ltd. is OCA20, measure 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 polystyrene is better; The contact angle of ethyl hexanoate and alkyd resin film is 23 °, shows that the compatibility of ethyl hexanoate and alkyd resin is better.
4, four kinds of polymer film piezoids of preparation in step 2 are welded in respectively on circuit board, make gas sensor, be finally arranged in a row in the plastics box that is fixed on long * wide * height=40 * 1.5 * 12mm, made gas sensor array.
Embodiment 2:
1, agents useful for same and polymkeric substance are in the same manner as in Example 1.
2, on UNIVEX-300 type vacuum coating equipment, be 12mm respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, alkyd resin evaporation at diameter, on the circular quartz substrate that thickness is 0.8mm, its concrete steps are as follows:
(1) select suitable substrate frame, place quartz substrate and alkyd resin;
(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) pass through F
1and F
5display screen is switched to the interface of bleeding, starts to bleed, after starting to bleed, forbid power-off;
(5) on thickness setting instrument, setting evaporation thickness is 80 μ m; In the baffle controls interface of main screen
Change control mode into auto;
(6) when vacuum tightness reaches 0.5 * 10
-5during mbar, start 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 (inner side) heated by electrodes No. 1.Regulate electric current to vacuum the temperature inside the box to rise to 100 ℃, by view window, observe heating boat situation.Press the open button of film-thickness monitoring and open baffle plate, start evaporation.When thickness reaches 80 μ m, the automatic closing baffle plate of film-thickness monitoring, to external, cuts off electric current by the control mode switch of hot evaporation power-supply controller of electric.This layer material evaporation completes;
(8) evaporation continues to vacuumize about 10 minutes after completing, and stops bleeding after waiting plating material completely cooling again;
(9) while closing vacuum pump, be switched to the interface of bleeding, press switch after molecular pump first start stall, now on molecular pump power source controller, show the load of molecular pump.After load pilot lamp extinguishes, main screen is switched to inflation interface, press inflation button and start inflation.Now need to open the reduction valve of High Purity Nitrogen, back pressure forbids surpassing an atmospheric pressure.After having exitted, open bell jar, take out sample and plating material, evaporation process completes, orderly close-down High Purity Nitrogen, primary power, recirculated cooling water and pressurized air;
(10) by sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene philosophy evaporation, at diameter, be in like manner, 12mm, on the circular quartz substrate that thickness is 0.8mm.
3, the contact angle of measuring every kind of reagent and its corresponding thin polymer film on the contact angle instrument that the model of buying in Beijing Orient De Fei Instrument Ltd. is OCA20 is identical in measurement result and embodiment 1.
4, four kinds of polymer film piezoids of preparation in step 2 are welded in respectively on circuit board, make gas sensor, be finally arranged in a row in the plastics box that is fixed on long * wide * height=55 * 1.5 * 15mm, just made gas sensor array.
Embodiment 3:
1, agents useful for same and polymkeric substance are in the same manner as in Example 1.
2, on UNIVEX-300 type vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, alkyd resin evaporation at grow * wide=10 * 10mm, on the square quartz substrate that thickness is 0.8mm, its concrete steps are as follows:
(1) select suitable substrate frame, place quartz substrate and alkyd resin;
(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) pass through F
1and F
5display screen is switched to the interface of bleeding, starts to bleed, after starting to bleed, forbid power-off;
(5) on thickness setting instrument, setting evaporation thickness is 100 μ m; Baffle controls interface at main screen
Middlely change control mode into auto;
(6) when vacuum tightness reaches 1 * 10
-5during mbar, start 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 (inner side) heated by electrodes No. 1.Regulate electric current to vacuum the temperature inside the box to rise to 120 ℃, by view window, observe heating boat situation.Press the open button of film-thickness monitoring and open baffle plate, start evaporation.When thickness reaches 100 μ m, the automatic closing baffle plate of film-thickness monitoring, to external, cuts off electric current by the control mode switch of hot evaporation power-supply controller of electric.This layer material evaporation completes;
(8) evaporation continues to vacuumize about 10 minutes after completing, and stops bleeding after waiting plating material completely cooling again;
(9) while closing vacuum pump, be switched to the interface of bleeding, press switch after molecular pump first start stall, now on molecular pump power source controller, show the load of molecular pump.After load pilot lamp extinguishes, main screen is switched to inflation interface, press inflation button and start inflation.Now need to open the reduction valve of High Purity Nitrogen, back pressure forbids surpassing an atmospheric pressure.After having exitted, open bell jar, 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, polystyrene philosophy evaporation at grow * wide=10 * 10mm, on the square quartz substrate that thickness is 0.8mm.
3, the contact angle of measuring every kind of reagent and its corresponding thin polymer film on the contact angle instrument that the model of buying in Beijing Orient De Fei Instrument Ltd. is OCA20 is identical in measurement result and embodiment 1.
4, four kinds of polymer film piezoids of preparation in step 2 are welded in respectively on circuit board, make gas sensor, be finally arranged in a row in the plastics box that is fixed on long * wide * height=50 * 1.5 * 12mm, just made gas sensor array.
The gas sensor array of making by the method, in conjunction with piezoelectric system, can be made into electric nasus system, while detecting sample, gas sensor array is placed in to the bottleneck of sample white wine, bottleneck is opened, when smells of wine pass through the injection port of gas sensor box, polymer film on gas sensor array is by the feature volatile ingredient of this wine of absorption, make its mass penalty, this phenomenon obtains the electric signal spectrogram of comprehensive response by piezoelectric system, obtain reflecting the feature spectrogram of sample white wine, this spectrogram contrasts with the standard spectrogram as identification phoenix aromatic white spirit, to reach the qualitative analysis of the sample white wine to being detected.
The present invention is by analyzing the physicochemical property of the feature volatile matter of phoenix aromatic white spirit, study and screen the thin polymer film coating material of suitable compatibility sensitivity, study and gather the feature intelligent of phoenix aromatic white spirit and smell news collection of illustrative plates, by collection of illustrative plates, compare, 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, energy long-term stable operation, the gas that coexists is little on the impact of its generation, high to the resolution performance of mixed gas.And the electric nasus system that it is made in conjunction with piezoelectric system does not need the loaded down with trivial details pretreatment process of sample when detecting phoenix aromatic white spirit, can directly carry out, fast response time, accuracy is high.
The above; be only the present invention's embodiment preferably, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in 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 phoenix aromatic white spirit, is characterized in that, comprises step:
(1) with vacuum coating equipment respectively by sodium polyacrylate, poly-trimethyl silicane-1-propine, polystyrene, alkyd resin evaporation on different quartz substrates;
(2) the good quartz substrate of evaporation is welded on circuit board.
2. the preparation method of the gas sensor array of detection phoenix aromatic white spirit according to claim 1, is characterized in that, in described step (1), the vacuum tightness of vacuum coating equipment is 1 * 10
-6-1 * 10
-5mbar.
3. the preparation method of the gas sensor array of detection phoenix aromatic white spirit according to claim 1, is characterized in that, in described step (1), the evaporation thickness of four kinds of thin polymer films is 50 μ m-100 μ m.
4. the preparation method of the gas sensor array of detection phoenix aromatic white spirit according to claim 1, is characterized in that, in described step (1), evaporation temperature is 80-120 ℃.
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