CN101694477B - Experimental device of gas-sensitive temperature property test of carbon nano tube sensor and method - Google Patents
Experimental device of gas-sensitive temperature property test of carbon nano tube sensor and method Download PDFInfo
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Abstract
An experimental device of gas-sensitive temperature property test of a carbon nano tube sensor and a method belong to the technical field of property test of the carbon nano tube sensor. The device mainly includes a cylinder, a vacuum pump, an alternating current contactor, a digital display regulator, an electric stove, a thermal resistor, an impedance analyzer and the like. By using the device, the method conducts the gas-sensitive temperature property test of the carbon nano tube on different detection gases at different temperatures. The device and the method can measure the gas-sensitive temperature property of the carbon nano tube sensor under different defected gases, find out the optimal working temperature of the carbon nano tube sensor under defected gases, have high accuracy and sensitivity of measurement, convenient operation and easy promotion and application, and the method is simple. The device and the method can be widely applied to the analysis and application of the gas-sensitive temperature property of carbon nano tube sensors for scientific research, teaching and study institutions.
Description
Technical field
The invention belongs to carbon nano tube sensor characteristic test technical field, be specifically related to a kind of experimental provision and method of gas-sensitive temperature property test of carbon nano tube sensor.
Background technology
Make miniature gas-sensitive sensor with CNT, have advantages such as response is fast, highly sensitive, working temperature is low, size is little, some scholars are applied to sensor field especially for gas detection with CNT in recent years, have obtained considerable progress.Gas sensor is to utilize the gas sensing layer surface generation absorption of gas molecule to be measured and sensor or chemical reaction to cause that electric charge shifts, and then causes sensor electricity characteristic to change detected gas.Absorption takes place in detected gas and CNT or chemical reaction must could be realized at a certain temperature, and promptly temperature is to influence the principal element that gas sensor detects performance.Therefore, study the temperature characterisitic and the temperature variant relation of gas sensing property of CNT, thereby find out the optimum working temperature of carbon nano tube sensor detected gas, make its gas sensing property reach best, the accuracy that improves detected gas.
Existing gas-sensitive temperature property test of carbon nano tube sensor device; Like interim " the multi-walled carbon nano-tubes air-sensitive Study on Properties " literary composition of " vacuum science with technology " 2003 9, October the 23rd volume the 5th; The experimental provision that uses is made up of the airtight glass container of 250ml, 500ml quartz glass tube, four point probe tester and thermopair, has tested the N of CNT in circulation
2And O
2In temperature characterisitic, the major defect of this device is: lack the adjustment part, can not control temperature in real time, thereby test accuracy is low, can not test CNT temperature characterisitic in a vacuum simultaneously.Interim " based on the gas sensing property research of the sensor of multiple-wall carbon nanotube " literary composition of volume the 1st in " sensing technology journal " March in 2005 the 18th and for example to toluene; The experimental provision that adopts is made up of sealed gas chamber, gas admittance valve, air outlet valve, syringe and electrochemical analyser; This device only can be tested the gas sensing property of CNT, can not test its temperature characterisitic.
Summary of the invention
The objective of the invention is weak point to existing gas-sensitive temperature property test of carbon nano tube sensor device; A kind of experimental provision and method of gas-sensitive temperature property test of carbon nano tube sensor are provided, have simple in structure, easy to operate, can analysis temperature characteristic to characteristics such as the influence of air-sensitive performance, accuracy height.
Principle of the present invention: the temperature characterisitic in apparatus of the present invention is analyzed by accurate electric impedance analyzer, and test speed is fast, and precision is high; Utilize the sealing property of vacuum pump, vacuum meter and tensimeter test experiment device and the air pressure situation in the monitoring sealed gas chamber; Electric furnace, A.C. contactor, digital display adjusting apparatus and thermal resistance have constituted the temperature control loop joint; Thermal resistance is used to monitor real time temperature; The digital display adjusting apparatus is used for being provided with temperature value and scope, the break-make and the heat time heating time of the open and close controlling electric furnace through A.C. contactor, realizes the real-time control to temperature; Electric furnace is placed on the sealed gas chamber bottom, links to each other with the A.C. contactor of outside through binding post, and digital display adjusting apparatus one end is connected with A.C. contactor, and the other end connects thermal resistance, and thermal resistance places in the protection tube that is embedded in the sealed gas chamber side.
The technical scheme that realizes the object of the invention is: a kind of experimental provision of gas-sensitive temperature property test of carbon nano tube sensor mainly comprises cylinder body, vacuum pump, A.C. contactor, digital display adjusting apparatus, electric furnace, thermal resistance, electric impedance analyzer etc.Cylinder body is the cylindrical shape of bottom surface sealing; Material is a stainless steel, and its wall thickness is that 4-6mm, internal diameter are 80-100mm, the high 80-100mm of being, at the top of cylinder body installing circular head; Circular head is connected with cylinder body through the screw rod nut through O-ring seals; Make cylinder interior become a seal cavity, in order to bear inside and outside air pressure and the corrosivity of tested gas in the experimentation, cylinder body is placed on the ground through A-frame.Vacuum pump is communicated with a side of cylinder body, and on the wireway between vacuum meter needle-valve and the tensimeter needle-valve, also is equiped with the air inlet needle-valve through wireway and through ball valve, vacuum meter and vacuum meter needle-valve, tensimeter and tensimeter needle-valve.Vacuum pump and ball valve are extracted tested gas out after experiment finishes in order to vacuumize in the cylinder body with sealing before testing.The air inlet needle-valve is in order to feed tested gas in the cylinder body after vacuumizing.Vacuum meter and vacuum meter needle-valve are in order to the vacuum tightness after quilt vacuumizes in the monitoring cylinder body and the sealing property of check cylinder body.Tensimeter and tensimeter needle-valve feed the air pressure in the detected gas rear-bank rotor housing in order to monitoring.Weld a support in the bottom of cylinder interior; Placement one electric furnace below support; The power of electric furnace is 500W or 1000W; Through being embedded in cylinder base and being connected with A.C. contactor with the binding post of cylinder body insulation, A.C. contactor is connected with power supply with the digital display adjusting apparatus respectively through lead electric furnace through lead, and power supply is the 220V alternating current.Placement refractory brick on support; End on refractory brick is placed carbon nano tube sensor; The protection tube of dress thermal resistance in the other end on refractory brick is glued with; Carbon nano tube sensor is connected with electric impedance analyzer through the top that is embedded in side of cylinder block and with the binding post of cylinder body insulation through lead, and electric impedance analyzer passes through lead and is connected with power supply, and power supply is the 220V alternating current; Thermal resistance in the protection tube is connected with the digital display adjusting apparatus through the bottom that is embedded in side of cylinder block and with the binding post of cylinder body insulation through lead, in order to the real-time working temperature of controlling carbon nanotube sensor.
A kind of experimental technique of gas-sensitive temperature property test of carbon nano tube sensor utilizes this experimental provision, and under different detected gas, the concrete steps of gas-sensitive temperature property test of carrying out carbon nano tube sensor are following:
(1) experiment is prepared
Earlier carbon nano tube sensor is placed on the refractory brick in the cylinder body, through lead carbon nano tube sensor is linked to each other with electric impedance analyzer through binding post, electric impedance analyzer is connected with the 220V AC power through lead.Through lead electric furnace is connected with A.C. contactor through binding post, A.C. contactor is connected with the 220V AC power through lead again.Thermal resistance in the protection tube is connected with the digital display adjusting apparatus through binding post through binding post through lead then, the digital display adjusting apparatus is connected with A.C. contactor through lead.Through the screw rod nut cylinder body is sealed through O-ring seals with circular head at last.
(2) vacuumize
After the completion of (1) step; Closing presure indicator valve and air inlet needle-valve are opened vacuum meter needle-valve and ball valve, and the open vacuum pump vacuumizes cylinder body; Vacuumize and close ball valve and vacuum pump after finishing; Leave standstill the registration of observing vacuum meter in 12 hours again, check its sealing property qualified after, note the initial resistivity value of the carbon nano tube sensor of digital display adjusting apparatus temperature displayed value and electric impedance analyzer demonstration this moment;
(3) the gas-sensitive temperature property analysis of carbon nano tube sensor under detected gas
(2) step was opened the air inlet needle-valve after accomplishing again, fed detected gas via draft tube through the air inlet needle-valve; When the air pressure after feeding detected gas equals an atmospheric pressure; Close the vacuum meter needle-valve, open the tensimeter needle-valve simultaneously, reach the experiment air pressure that is provided with in advance up to air pressure; The different temperatures value that is provided with through the digital display adjusting apparatus then; Measure carbon nano tube sensor under the detected gas, the resistance value under the temperature is set through electric impedance analyzer in difference; Make the gas-sensitive temperature property curve then, and find out the optimum working temperature of carbon nano tube sensor detected gas; After experiment finishes, open ball valve, the open vacuum pump; Detected gas is evacuated to outdoor processing, when the cylinder body internal gas pressure is pumped down to when equaling an atmospheric pressure closing presure indicator valve; Open the vacuum meter needle-valve simultaneously, after the tested gas in the cylinder body is pumped, close ball valve and vacuum pump.
After the present invention adopts technique scheme, mainly contain following effect:
(1) apparatus of the present invention have increased the air pressure control section, i.e. vacuum pump, vacuum meter and tensimeter had both strengthened the sealing property of cylinder body, can under different air pressure, measure the gas sensing property of carbon nano tube sensor again, had improved accuracy of test.
(2) apparatus of the present invention have increased the real-time control section of temperature, i.e. A.C. contactor and digital display adjusting apparatus can be measured the gas sensing property of carbon nano tube sensor under different temperatures, further improved accuracy of test.
(3) utilize apparatus of the present invention can measure the gas-sensitive temperature property of carbon nano tube sensor under different detected gas; Be the influence of temperature characterisitic to air-sensitive performance; Thereby find out the optimum working temperature of carbon nano tube sensor detected gas; This can improve the accuracy of detected gas, can improve the sensitivity of carbon nano tube sensor again.
(4) the inventive method is to utilize apparatus of the present invention, and to the gas-sensitive temperature property of different detected gas, method is simple, and is easy to operate, is easy to apply under different temperatures for the measurement carbon nano tube sensor.
The present invention can be widely used in scientific research, teaching, institute analysis and the application to the carbon nano tube sensor gas-sensitive temperature property.
Description of drawings
Fig. 1 is the synoptic diagram of apparatus of the present invention;
Fig. 2 is that carbon nano tube sensor is at SF
6Gas-sensitive temperature property curve map under the discharge decomposition components gas.
Among the figure: 1. circular head; 2.O shape O-ring seal; 3. screw rod nut; 4. cylinder body; 5. tensimeter; 6. tensimeter needle-valve; 7. vacuum meter; 8. vacuum meter needle-valve; 9. ball valve; 10. vacuum pump; 11. air inlet needle-valve; 12. carbon nano tube sensor; 13. refractory brick; 14. A-frame; 15. binding post; 16. A.C. contactor; 17. digital display adjusting apparatus; 18. electric furnace; 19. support; 20. protection tube; 21. thermal resistance; 22. electric impedance analyzer; 23. power supply.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
As shown in Figure 1, a kind of experimental provision of gas-sensitive temperature property test of carbon nano tube sensor mainly comprises cylinder body 4, vacuum pump 10, A.C. contactor 16, digital display adjusting apparatus 17, electric furnace 18, thermal resistance 21, electric impedance analyzer 22 etc.Cylinder body 4 is the cylindrical shape of bottom surface sealing, and material is a stainless steel, and its wall thickness is 6mm; Internal diameter is 100mm, and height is 100mm, at the top of cylinder body 4 installing circular head 1; Circular head 1 is connected with cylinder body 4 through screw rod nut 3 through O-ring seals 2; Make cylinder body 4 inside become a seal cavity, in order to bear inside and outside air pressure and the corrosivity of tested gas in the experimentation, cylinder body 4 is placed on the ground through A-frame 14.Vacuum pump 10 is communicated with a side of cylinder body, and on the wireway between vacuum meter needle-valve 8 and the tensimeter needle-valve 6, also is equiped with air inlet needle-valve 11 through wireway and through ball valve 9, vacuum meter 7 and vacuum meter needle-valve 8, tensimeter 5 and tensimeter needle-valve 6.Vacuum pump 10 vacuumizes in order to test in the preceding cylinder body 4 with sealing with ball valve 9, after experiment finishes, tested gas is extracted out.Air inlet needle-valve 11 is in order to feed tested gas in the cylinder body 4 after vacuumizing.Vacuum meter 7 is interior by the sealing property of vacuum tightness after vacuumizing and check cylinder body 4 in order to monitoring cylinder body 4 with vacuum meter needle-valve 8.Tensimeter 5 feeds the air pressure in the detected gas rear-bank rotor housing 4 with tensimeter needle-valve 6 in order to monitoring.Weld a support 19 in cylinder body 4 inner bottoms; Placement one electric furnace 18 below support 19; The power of electric furnace 18 is 1000W; Through being embedded in cylinder body 4 bottoms and being connected with A.C. contactor 16 with the binding post 15 of cylinder body 4 insulation, A.C. contactor 16 is connected with power supply 23 with digital display adjusting apparatus 17 respectively through lead electric furnace 18 through lead, and power supply 23 is the 220V alternating current.Placement refractory brick 13 on support 19; End on refractory brick 13 is placed carbon nano tube sensor 12; The protection tube 20 of dress thermal resistance 21 in the other end on refractory brick 13 is glued with; Carbon nano tube sensor 12 is connected with electric impedance analyzer 22 through the top that is embedded in side of cylinder block and with the binding post 15 of cylinder body insulation through lead, and electric impedance analyzer 22 passes through lead and is connected with power supply 23, and power supply 23 is the 220V alternating current; Thermal resistance 21 in the protection tube 20 is connected with digital display adjusting apparatus 17 through the bottom that is embedded in cylinder body 4 sides and with the binding post 15 of cylinder body insulation through lead, in order to the real-time working temperature of controlling carbon nanotube sensor.
Embodiment 2
As shown in Figure 1, a kind of experimental provision of gas-sensitive temperature property test of carbon nano tube sensor, with embodiment 1, wherein: the wall thickness of cylinder body 4 is that 4mm, internal diameter are 80mm, the high 80mm of being, the power of electric furnace 18 is 500W.
Embodiment 3
As shown in Figure 1, a kind of experimental provision of gas-sensitive temperature property test of carbon nano tube sensor, with embodiment 1, wherein: the wall thickness of cylinder body 4 is that 5mm, internal diameter are 90mm, the high 90mm of being.
Embodiment 4
A kind of concrete steps of experimental technique of gas-sensitive temperature property test of carbon nano tube sensor are following:
(1) experiment is prepared
Earlier carbon nano tube sensor 12 is placed on the refractory brick 13 in the cylinder body 4, through lead carbon nano tube sensor 12 is linked to each other with electric impedance analyzer 22 through binding post 15, electric impedance analyzer 22 is connected with 220V AC power 23 through lead.Through lead electric furnace 18 is connected with A.C. contactor 16 through binding post 15, A.C. contactor 16 is connected with 220V AC power 23 through lead again.Thermal resistance in the protection tube 20 21 is connected with digital display adjusting apparatus 17 through binding post 15 through binding post 15 through lead then, digital display adjusting apparatus 17 is connected with A.C. contactor 16 through lead.Through screw rod nut 3 cylinder body 4 is sealed through O-ring seals 2 with circular head 1 at last.
(2) vacuumize
After the completion of (1) step; Closing presure indicator valve 6 and air inlet needle-valve 11 are opened vacuum meter needle-valve 8 and ball valve 9, and 10 pairs of cylinder bodies 4 of open vacuum pump vacuumize; Vacuumize and close ball valve 9 and vacuum pump 10 after finishing; Leave standstill the registration of observing vacuum meter 7 in 12 hours again, check its sealing property qualified after, note 25 ℃ of digital display adjusting apparatus 17 temperature displayed values and the initial resistivity value of the carbon nano tube sensor of electric impedance analyzer 22 demonstrations this moment;
(3) the gas-sensitive temperature property analysis of carbon nano tube sensor under tested gas
(2) step was opened air inlet needle-valve 11 after accomplishing again, fed SF to be detected via draft tube through air inlet needle-valve 11
6Discharge decomposition components gas when cylinder body 4 internal gas pressures equal an atmospheric pressure, is closed vacuum meter needle-valve 8, opens tensimeter needle-valve 6 simultaneously, up to feeding SF to be detected
6Discharge decomposition components gas reaches till the experiment air pressure 0.2MPa that is provided with in advance; Through digital display adjusting apparatus 17 temperature is separately positioned on 25 ℃, 45 ℃, 65 ℃, 85 ℃, 105 ℃ and 125 ℃ then, measures carbon nano tube sensor 12 through electric impedance analyzer 22 and be provided with under the temperature (promptly 25 ℃, 45 ℃, 65 ℃, 85 ℃, 105 ℃ and 125 ℃) at SF in difference respectively
6Resistance value under the discharge decomposition components gas is made curve, and is as shown in Figure 2, and finds out carbon nano tube sensor and detect SF
6The optimum working temperature of discharge decomposition components gas is 85 ℃; After experiment finishes, open ball valve 9, open vacuum pump 10 is evacuated to outdoor processing with detected gas, and when cylinder body 4 internal gas pressures are pumped down to when equaling an atmospheric pressure, closing presure indicator valve 6 is opened vacuum meter needle-valve 8 simultaneously, SF to be detected in cylinder body
6After being pumped, discharge decomposition components gas closes ball valve 9 and vacuum pump 10.
As shown in Figure 2, utilize apparatus of the present invention at SF
6Tested the gas-sensitive temperature property of carbon nano tube sensor under the discharge decomposition components gas; I, II, III, IV, V and VI among the figure, respectively when temperature is 25 ℃, 125 ℃, 45 ℃, 105 ℃, 65 ℃ and 85 ℃: the resistance relative changing value of carbon nano tube sensor is curve over time.Know from Fig. 2: when curve VI is 85 ℃ in temperature; The resistance relative changing value of carbon nano tube sensor has reached 8% in 4 minutes; Its changing value is greater than curve I, II, III, IV and the V changing value in the identical time, promptly carbon nano tube sensor in the time of 85 ℃ to SF to be detected
6The gas sensing property of discharge decomposition components gas reaches best; Thereby valid certificates apparatus of the present invention can realize test fully to the carbon nano tube sensor gas-sensitive temperature property; Find out the optimum working temperature of carbon nano tube sensor detected gas, improved the accuracy of detected gas.
Claims (2)
1. the experimental provision of a gas-sensitive temperature property test of carbon nano tube sensor; Mainly comprise cylinder body (4), vacuum pump (10), electric impedance analyzer (22); It is characterized in that said device also comprises A.C. contactor (16), digital display adjusting apparatus (17), electric furnace (18), thermal resistance (21), cylinder body (4) is the cylindrical shape of bottom surface sealing, and its wall thickness is 4-6mm; Internal diameter is 80-100mm; Height is 80-100mm, and at the top of cylinder body (4) installing circular head (1), circular head (1) is connected with cylinder body (4) through screw rod nut (3) through o shape O-ring seal (2); Cylinder body (4) is placed on the ground through A-frame (14); Vacuum pump (10) is communicated with a side of cylinder body through wireway and through ball valve (9), vacuum meter (7) and vacuum meter needle-valve (8), tensimeter (5) and tensimeter needle-valve (6), and on the wireway between vacuum meter needle-valve (8) and the tensimeter needle-valve (6); Also be equiped with air inlet needle-valve (11); A support (19) is welded in bottom in that cylinder body (4) is inner, placement one electric furnace (18) below support (19), and the power of electric furnace (18) is 500W or 1000W; Electric furnace (18) through lead through being embedded in cylinder body (4) bottom and being connected with A.C. contactor (16) with the binding post (15) of cylinder body (4) insulation; A.C. contactor (16) is connected with 220V AC power (23) with digital display adjusting apparatus (17) respectively through lead, placement refractory brick (13) on support (19), and the end on refractory brick (13) is placed carbon nano tube sensor (12); The protection tube (20) of dress thermal resistance (21) in the other end on refractory brick (13) is glued with; Carbon nano tube sensor (12) is connected with electric impedance analyzer (22) through the top that is embedded in side of cylinder block and with the binding post (15) of cylinder body insulation through lead, and electric impedance analyzer (22) is connected with 220V AC power (23) through lead, and the interior thermal resistance (21) of protection tube is connected with digital display adjusting apparatus (17) through the bottom that is embedded in cylinder body (4) side and with binding post (15) that cylinder body (4) insulate through lead.
2. the experimental technique of a gas-sensitive temperature property test of carbon nano tube sensor utilizes the described experimental provision of claim 1, and the gas-sensitive temperature property of carbon nano tube sensor is tested, and it is characterized in that the concrete steps of said method are following:
(1) experiment is prepared
Earlier carbon nano tube sensor (12) is placed on the refractory brick (13) in the cylinder body (4); Passing through lead again links to each other through binding post (15) carbon nano tube sensor (12) with electric impedance analyzer (22); Electric impedance analyzer (22) is connected with 220V AC power (23) through lead; Through lead electric furnace (18) is connected with A.C. contactor (16) through binding post (15) again; A.C. contactor (16) is connected with 220V AC power (23) through lead; Thermal resistance (21) in the protection tube (20) is connected with digital display adjusting apparatus (17) through binding post (15) through binding post (15) through lead then, digital display adjusting apparatus (17) is connected with A.C. contactor (16) through lead, uses circular head (1) cylinder body (4) to be sealed through screw rod nut (3) through o shape O-ring seal (2) at last;
(2) vacuumize
After the completion of (1) step; Closing presure indicator valve (6) and air inlet needle-valve (11) are opened vacuum meter needle-valve (8) and ball valve (9), and open vacuum pump (10) vacuumizes cylinder body (4); Vacuumize and close ball valve (9) and vacuum pump (10) after finishing; Leave standstill the registration of observing vacuum meter 7 in 12 hours again, check its sealing property qualified after, note the initial resistivity value of the carbon nano tube sensor of digital display adjusting apparatus (17) temperature displayed value and electric impedance analyzer (22) demonstration this moment;
(3) the gas-sensitive temperature property analysis of carbon nano tube sensor under detected gas
(2) step was opened air inlet needle-valve (11) after accomplishing again, fed detected gas via draft tube through air inlet needle-valve (11); When the air pressure after feeding detected gas equals an atmospheric pressure, close vacuum meter needle-valve (8), open tensimeter needle-valve (6) simultaneously; Reach in advance the experiment air pressure that is provided with up to air pressure, the different temperatures value that is provided with through digital display adjusting apparatus (17) is then measured carbon nano tube sensor under the detected gas, in difference the resistance value under the temperature is set through electric impedance analyzer (22); Make the gas-sensitive temperature property curve then, and find out the optimum working temperature of carbon nano tube sensor detected gas, after experiment finishes; Open ball valve (9), open vacuum pump (10) is evacuated to outdoor processing with detected gas; When cylinder body (4) internal gas pressure is pumped down to when equaling an atmospheric pressure; Closing presure indicator valve (6) is opened vacuum meter needle-valve (8) simultaneously, after the tested gas of cylinder body (4) is pumped, closes ball valve (9) and vacuum pump (10).
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| CN102072784B (en) * | 2011-02-16 | 2012-11-28 | 西安交通大学 | Carbon nanotube film ionizing gas temperature sensor and temperature measuring method thereof |
| CN102323303B (en) * | 2011-08-26 | 2012-11-28 | 重庆大学 | Experimental apparatus and method for testing gas-sensitive temperature characteristic of carbon nanotube sensor |
| CN103176146B (en) * | 2011-12-20 | 2015-04-29 | 中国科学院合肥物质科学研究院 | Hall and air-sensitive measuring device |
| CN102645642B (en) * | 2012-05-21 | 2014-02-12 | 哈尔滨工业大学 | Temperature property testing device of amorphous metal fibers |
| CN103048358B (en) * | 2012-12-24 | 2014-11-05 | 东北师范大学 | Test system of semiconductor micro-nano monocrystal gas sensor |
| CN103293199B (en) * | 2013-05-21 | 2015-06-10 | 重庆大学 | Experiment device and method for testing air-sensitive property of titanium dioxide nanotube sensor |
| CN104535859B (en) * | 2014-12-19 | 2017-09-01 | 桂林电子科技大学 | The method for testing CNT temperature characterisitic |
| CN105973967B (en) * | 2016-07-15 | 2018-06-15 | 中国科学院福建物质结构研究所 | A kind of controllable more device field-effect transistor sealing test devices of atmosphere |
| CN106645956A (en) * | 2016-10-11 | 2017-05-10 | 吉林大学 | New gas-sensitive material testing system |
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