CN103323498A - Resistance type relative humidity sensor based on graphene carbon nanotube composite material - Google Patents
Resistance type relative humidity sensor based on graphene carbon nanotube composite material Download PDFInfo
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- CN103323498A CN103323498A CN2013102898630A CN201310289863A CN103323498A CN 103323498 A CN103323498 A CN 103323498A CN 2013102898630 A CN2013102898630 A CN 2013102898630A CN 201310289863 A CN201310289863 A CN 201310289863A CN 103323498 A CN103323498 A CN 103323498A
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Abstract
The invention discloses a resistance type relative humidity sensor based on a graphene carbon nanotube composite material. The resistance type relative humidity sensor based on the graphene carbon nanotube composite material comprises a substrate and a sensitive layer positioned on the substrate, wherein a pair of electrodes are printed on the sensitive layer and are connected to an ohmmeter through electrode leads; the sensitive layer is made of the graphene carbon nanotube composite material; the graphene carbon nanotube composite material is directly deposited on the substrate by using a chemical vapor deposition method. The resistance type relative humidity sensor based on the graphene carbon nanotube composite material is simple and reliable in structure, low in cost and easy to produce in batches. The relative humidity sensor is convenient to carry, and the indexes in the aspects of reaction time, consistency, precision and the like are higher than those of the humidity sensor produced by using the traditional mode. By adoption of the chemical vapor deposition method, the direction preparation of the graphene carbon nanotube composite material is realized and a preparation process is simplified; a prepared graphene carbon nanotube has controllable appearance and excellent optical and electrical properties, so that the application of the graphene carbon nanotube composite material is greatly facilitated.
Description
Technical field
The present invention relates to a kind of resistance-type relative humidity sensor, be specifically related to a kind of resistance-type relative humidity sensor based on the Graphene carbon nano tube compound material.
Background technology
The various fields of humidity sensor in productive life plays an important role, and the humidity-sensitive element of humidity sensor mainly contains resistance-type, condenser type two large classes at present.Wherein the characteristics of hygristor are to cover the film that one deck is made with wet sensory material at substrate, and when airborne water vapor adsorption was on humidity-sensitive film, resistivity and the resistance value of element all changed, and utilized this characteristic can measure humidity.The kind of hygristor is a lot, such as the special hygristor of burning, silicon hygristor, ceramic hygristor etc.Above-mentioned hygristor production efficiency is lower, and traditional mode of production is difficult to improve the quality of element, thereby affects applying of moisture sensor.Graphene and carbon nano-tube are the carbon nanomaterial of typical sp2 hydridization, and have special physical property.Graphene is the bi-dimensional cellular shape structure by the tightly packed one-tenth of monolayer carbon atom, is the basic structural unit that consists of other dimension material with carbon elements.Graphene has the ballistic transport characteristic of the ballistic transport characteristic of very high carrier concentration, mobility and submicron-scale.Diversified shape and the structure of carbon nano-tube make it have many potential using values.Along with going deep into of nano materials research, the application prospect of Graphene and carbon nano tube compound material also constantly shows.Yet existing technology of preparing needs it is shifted after need to dividing one-step growth or growth to finish to Graphene and carbon nano-tube, thereby has greatly limited the application of Graphene and carbon nano tube compound material.
Summary of the invention
The objective of the invention is for overcoming above-mentioned the deficiencies in the prior art, a kind of resistance-type relative humidity sensor based on the Graphene carbon nano tube compound material is provided.The present invention is simple and reliable for structure, cost is low, be easy to the realization batch production, and this relative humidity sensor is easy to carry and the index at aspects such as reaction time, consistance, degree of accuracy all is higher than the humidity sensor that traditional approach is produced.Adopt chemical vapour deposition technique, realized the direct preparation of Graphene carbon nano tube compound material, simplified preparation technology, the pattern of the Graphene carbon nano-tube for preparing simultaneously is controlled and have excellent optics and electrology characteristic, and the application of the Graphene carbon nano tube compound material that greatly promotes.
For achieving the above object, the present invention adopts following technical proposals:
A kind of resistance-type relative humidity sensor based on the Graphene carbon nano tube compound material comprises substrate and is positioned at sensitive layer on the substrate that be printed with pair of electrodes on the described sensitive layer, this a pair of electrode all is connected to ohmmeter by contact conductor; Described sensitive layer is the Graphene carbon nano tube compound material, and described Graphene carbon nano tube compound material passes through the chemical vapour deposition technique Direct precipitation on substrate.
Described substrate is unpolished piezoid.
The preparation method of above-mentioned resistance-type relative humidity sensor, concrete steps are as follows:
1) catalytic metal paillon foil and substrate are put into reacting furnace, in 800～1200 ℃ of scopes to catalytic metal paillon foil and substrate surface annealing in process, in reacting furnace, pass into carbon-source gas, by chemical vapour deposition technique so that substrate surface direct growth graphene nano pipe compound substance;
2) have on the substrate of Graphene carbon nano tube compound material at surface deposition, print electrode I and electrode II, and electrode I and electrode II be connected to ohmmeter.
The concrete grammar of described step 1) is:
11) the catalytic metal paillon foil is placed the constant temperature of reacting furnace regional, substrate places the territory, stove tail region of reacting furnace;
12) air pressure in the reacting furnace is evacuated to end vacuum state 1.33 * 10
-4～3.99 * 10
-4Pa keeps vacuum state after 15～40 minutes, and the air pressure in the quartz ampoule is risen to 0.133～0.399Pa, injects hydrogen, and its flow control is at 50～100mL/min.; After reacting furnace reaches design temperature, constant temperature 20～60 minutes, annealing;
13) in the reacting furnace that vacuumizes, pass into carbon-source gas, by chemical vapour deposition technique so that substrate surface direct growth graphene nano pipe compound substance;
14) after growth is finished, be cooled to room temperature, take out the long substrate that the Graphene carbon nano tube compound material is arranged.
Described catalytic metal paillon foil is Copper Foil or nickel foil, and described substrate is unpolished piezoid.
Described carbon-source gas is methane, and its flow control is at 50～300mL/min..
The growth time of described Graphene carbon nano tube compound material is controlled at 30～180 minutes.
Described reacting furnace comprises tubular furnace and the quartz ampoule supporting with it, one side of described quartz ampoule is connected with the carbon-source gas flowmeter with hydrogen flowmeter respectively by vacuum meter, and hydrogen flowmeter is connected with the carbon-source gas flowmeter with hydrogen and is connected with the carbon-source gas gas cylinder; Opposite side is connected with vacuum pump by valve.
The invention has the beneficial effects as follows, substrate adopts unpolished piezoid, and sensitive layer adopts the Graphene carbon nano tube compound material, and the technological process of whole humidity sensor is simple and reliable, cost is low, be easy to realize batch production.The present invention is directly grown in substrate surface by chemical vapour deposition technique with one step of Graphene carbon nano tube compound material, save unnecessary transfer link, the Graphene carbon nano tube compound material of preparation has excellent electricity and optical property thus, thus the application of the Graphene carbon nano tube compound material that greatly promotes.The structure of Graphene carbon nano tube compound material uniqueness is to compare traditional humidity sensor based on the resistance-type relative humidity sensor of Graphene carbon nano tube compound material more microminiaturized, and the index at aspects such as reaction time, consistance, degree of accuracy all is higher than the humidity sensor that traditional approach is produced.
Description of drawings
Fig. 1 is the reacting furnace structural representation that the present invention prepares the Graphene carbon nano tube compound material;
Fig. 2 is the process flow diagram that the present invention prepares the Graphene carbon nano tube compound material;
Fig. 3 is the scanning electron microscope image that the present invention prepares the Graphene carbon nano tube compound material;
Fig. 4 is the Raman spectrogram that the present invention prepares the Graphene carbon nano tube compound material.
Fig. 5 is the high-resolution-ration transmission electric-lens image that the present invention prepares the Graphene carbon nano tube compound material;
Fig. 6 is the visible transmission collection of illustrative plates that the present invention prepares the Graphene carbon nano tube compound material;
Fig. 7 is that the invention process is based on the schematic diagram of the resistance-type relative humidity sensor of Graphene carbon nano tube compound material;
Fig. 8 is resistance and the relative humidity graph of a relation that resistance-type relative humidity sensor provided by the invention is measured;
11. hydrogen flowmeters wherein, 12. carbon-source gas flowmeters, 13. quartz ampoules, 14. tubular furnace, 15. vacuum meters, 16. nickel foils, 17. unpolished piezoid, 18. valves, 61. substrates, 62. sensitive layers, 63. electrode I, 64. electrode II, 65. ohmmeters, 66, contact conductor I, 67. contact conductor II.
Embodiment
The present invention will be further elaborated below in conjunction with drawings and Examples, should be noted that following explanation only is in order to explain the present invention, its content not to be limited.
As shown in Figure 7, the present invention includes substrate 61 and be positioned at sensitive layer 62 on the substrate 61, be printed with pair of electrodes on the sensitive layer 62, i.e. electrode I63 and electrode II64, electrode I63 and electrode II64 are connected to ohmmeter 65 by contact conductor I66 and contact conductor II67 respectively; Sensitive layer 62 is the Graphene carbon nano tube compound material.
The Graphene carbon nano tube compound material passes through the chemical vapour deposition technique Direct precipitation on substrate, to utilize reacting furnace shown in Figure 1 to realize, it comprises hydrogen flowmeter 11, carbon-source gas flowmeter 12, quartz ampoule 13, tubular furnace 14, vacuum meter 15, nickel foil 16, unpolished piezoid 17, the chemical gas-phase deposition system that valve 18 forms, quartz ampoule 13 places tubular furnace 14, the vacuum meter 15 that passes through of quartz ampoule 13 is connected with the carbon-source gas flowmeter with hydrogen flowmeter 11 respectively and is connected, hydrogen flowmeter 11 links to each other with the carbon-source gas gas cylinder with hydrogen respectively with carbon-source gas flowmeter 12, and the opposite side of quartz ampoule 13 links to each other with vacuum pump by valve 18.
Fig. 2 shows the process flow diagram of preparation Graphene carbon nano tube compound material, by chemical vapour deposition technique, directly prepares the Graphene carbon nano tube compound material in unpolished piezoid previous step, comprises following preparation process:
1. get 6 * 8cm
2Nickel foil 16 place the constant temperature zone of quartz ampoule 13;
2. get unpolished piezoid 17 and place territory, quartz ampoule 13 stove tail region;
3. open vacuum pump the air pressure of quartz ampoule 13 is evacuated to end vacuum state 3.99 * 10
-4Pa;
4. keep vacuum state 3.99 * 10
-4After Pa15 minute, the air pressure of quartz ampoule 13 is raised to 0.399Pa;
5. hydrogen flowmeter 11 is set as 50mL/min., and hydrogen is injected vacuum chamber;
6. after tubular furnace 14 reached 1100 degrees centigrade of design temperatures, constant temperature was annealed in 20 minutes;
7. carbon-source gas flowmeter 12 is set as 150mL/min., and methane is injected vacuum chamber, stops to grow in 60 minutes;
8. close carbon-source gas flowmeter 12 and the temperature of tubular furnace 14 is down to room temperature fast;
9. close hydrogen flowmeter 13 and vacuum pump;
10. open valve 18, with air quartz ampoule 13 air pressure are filled to an atmospheric pressure state;
11. open quartz ampoule 13 vacuum interfaces, take out the quartz substrate that has deposited the Graphene carbon nano tube compound material.
With reference to the accompanying drawings 7, prepare after the piezoid of deposition Graphene carbon nano tube compound material, further finish following technique, can make the resistance-type relative humidity sensor based on the Graphene carbon nano tube compound material;
12. the electrode preparation, on the piezoid 61 of the Graphene carbon nano tube compound material that deposits the direct preparation of chemical meteorology deposition method, print electrode I63 and electrode II64, electrode I63 and electrode II64 are silver electrode;
13. Au wire bonding welds electrode I63 and electrode II64 respectively with contact conductor I66 and contact conductor II67;
14. contact conductor I66 and contact conductor II67 all are connected with ohmmeter;
15. detect.
Fig. 3 is the scanning electron microscope image of the Graphene carbon nano tube compound material of embodiment of the invention preparation, and as can be seen from this figure: (1) large-area carbon nano-tube has deposited to the Graphene surface; (2) length of the carbon nano-tube of preparation is about 1.5 microns.
Fig. 4 is the Raman spectrogram of the Graphene carbon nano tube compound material of embodiment of the invention preparation, and as can be seen from this figure: there be characteristic peak G peak and the 2D peak of Graphene in (1); (2) there is the characteristic peak G ' peak of carbon nano-tube, further specifies the present embodiment and successfully prepare the Graphene carbon nano tube compound material.
Fig. 5 is the high-resolution-ration transmission electric-lens image of the Graphene carbon nano tube compound material of embodiment of the invention preparation, has confirmed more fully the successful preparation of Graphene carbon nano tube compound material from this figure.
Fig. 6 is the visible transmission collection of illustrative plates that the present invention prepares the Graphene carbon nano tube compound material, and as can be seen from this figure: this compound substance has good transmitance, not because the appearance of carbon nano-tube makes transmitted spectrum occur significantly absorbing.
Fig. 8 is resistance and the relative humidity graph of a relation that resistance-type relative humidity sensor provided by the invention is measured, and as can be seen from this figure: the humidity sensor of the present invention's preparation has higher sensitivity.
Although above-mentionedly by reference to the accompanying drawings the specific embodiment of the present invention is described; but be not limiting the scope of the invention; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (8)
1. resistance-type relative humidity sensor based on the Graphene carbon nano tube compound material, it is characterized in that, comprise substrate and be positioned at sensitive layer on the substrate, be printed with pair of electrodes on the described sensitive layer, this a pair of electrode all is connected to ohmmeter by contact conductor; Described sensitive layer is the Graphene carbon nano tube compound material, and described Graphene carbon nano tube compound material passes through the chemical vapour deposition technique Direct precipitation on substrate.
2. resistance-type relative humidity sensor according to claim 1 is characterized in that, described substrate is unpolished piezoid.
3. the preparation method of claim 1 or 2 described resistance-type relative humidity sensors is characterized in that, concrete steps are as follows:
1) catalytic metal paillon foil and substrate are put into reacting furnace, in 800～1200 ℃ of scopes to catalytic metal paillon foil and substrate surface annealing in process, in reacting furnace, pass into carbon-source gas, by chemical vapour deposition technique so that substrate surface direct growth graphene nano pipe compound substance;
2) have on the substrate of Graphene carbon nano tube compound material at surface deposition, print electrode I and electrode II, and electrode I and electrode II be connected to ohmmeter.
4. preparation method according to claim 3 is characterized in that, the concrete grammar of described step 1) is:
11) the catalytic metal paillon foil is placed the constant temperature of reacting furnace regional, substrate places the territory, stove tail region of reacting furnace;
12) air pressure in the reacting furnace is evacuated to end vacuum state 1.33 * 10
-4～3.99 * 10
-4Pa keeps vacuum state after 15～40 minutes, and the air pressure in the quartz ampoule is risen to 0.133～0.399Pa, injects hydrogen, and its flow control is at 50～100mL/min.; After reacting furnace reaches design temperature, constant temperature 20～60 minutes, annealing;
13) in the reacting furnace that vacuumizes, pass into carbon-source gas, by chemical vapour deposition technique so that substrate surface direct growth graphene nano pipe compound substance;
14) after growth is finished, be cooled to room temperature, take out the long substrate that the Graphene carbon nano tube compound material is arranged.
5. preparation method according to claim 4 is characterized in that, described catalytic metal paillon foil is Copper Foil or nickel foil, and described substrate is unpolished piezoid.
6. preparation method according to claim 4 is characterized in that, described carbon-source gas is methane, and its flow control is at 50～300mL/min..
7. preparation method according to claim 4 is characterized in that, the growth time of described Graphene carbon nano tube compound material is controlled at 30～180 minutes.
8. preparation method according to claim 4, it is characterized in that, described reacting furnace comprises tubular furnace and the quartz ampoule supporting with it, one side of described quartz ampoule is connected with the carbon-source gas flowmeter with hydrogen flowmeter respectively by vacuum meter, and hydrogen flowmeter is connected with the carbon-source gas flowmeter with hydrogen and is connected with the carbon-source gas gas cylinder; Opposite side is connected with vacuum pump by valve.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569079A (en) * | 2015-01-29 | 2015-04-29 | 重庆墨希科技有限公司 | Graphene nano wall resistance-type humidity sensor and preparation method thereof |
| CN104569078A (en) * | 2015-01-29 | 2015-04-29 | 重庆墨希科技有限公司 | Flexible graphene nano wall resistance-type humidity sensor and preparation method thereof |
| CN105784788A (en) * | 2016-05-09 | 2016-07-20 | 吉林大学 | Paper-based flexible humidity sensitive element and preparation method thereof |
| CN106814110A (en) * | 2017-01-05 | 2017-06-09 | 华中科技大学 | A kind of stretchable semiconductor resistance-type flexible gas sensor and preparation method thereof |
| CN107655781A (en) * | 2017-09-05 | 2018-02-02 | 吉林大学 | A kind of QCM type humidity sensors based on acidifying oxide/carbon nanometer tube and preparation method thereof |
| CN108593717A (en) * | 2018-04-26 | 2018-09-28 | 京东方科技集团股份有限公司 | A kind of humidity sensor and preparation method thereof, electronic equipment |
| CN109111122A (en) * | 2017-06-23 | 2019-01-01 | 北京大学 | A kind of preparation method of graphene-carbon nano tube compound glass |
| CN109827925A (en) * | 2019-03-14 | 2019-05-31 | 中国农业大学 | On-line continuous pesticide droplet deposition characteristics detection device and method |
| CN113203774A (en) * | 2021-04-28 | 2021-08-03 | 北京梦之墨科技有限公司 | Liquid sensor, manufacturing method thereof and liquid sensing system |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569079A (en) * | 2015-01-29 | 2015-04-29 | 重庆墨希科技有限公司 | Graphene nano wall resistance-type humidity sensor and preparation method thereof |
| CN104569078A (en) * | 2015-01-29 | 2015-04-29 | 重庆墨希科技有限公司 | Flexible graphene nano wall resistance-type humidity sensor and preparation method thereof |
| CN105784788A (en) * | 2016-05-09 | 2016-07-20 | 吉林大学 | Paper-based flexible humidity sensitive element and preparation method thereof |
| CN105784788B (en) * | 2016-05-09 | 2019-01-11 | 吉林大学 | A kind of paper base flexibility dew cell and preparation method thereof |
| CN106814110A (en) * | 2017-01-05 | 2017-06-09 | 华中科技大学 | A kind of stretchable semiconductor resistance-type flexible gas sensor and preparation method thereof |
| CN109111122A (en) * | 2017-06-23 | 2019-01-01 | 北京大学 | A kind of preparation method of graphene-carbon nano tube compound glass |
| CN109111122B (en) * | 2017-06-23 | 2020-08-28 | 北京大学 | Preparation method of graphene-carbon nanotube composite glass |
| CN107655781A (en) * | 2017-09-05 | 2018-02-02 | 吉林大学 | A kind of QCM type humidity sensors based on acidifying oxide/carbon nanometer tube and preparation method thereof |
| CN108593717A (en) * | 2018-04-26 | 2018-09-28 | 京东方科技集团股份有限公司 | A kind of humidity sensor and preparation method thereof, electronic equipment |
| CN109827925A (en) * | 2019-03-14 | 2019-05-31 | 中国农业大学 | On-line continuous pesticide droplet deposition characteristics detection device and method |
| CN109827925B (en) * | 2019-03-14 | 2023-01-13 | 中国农业大学 | Online continuous pesticide droplet deposition characteristic detection device and method |
| CN113203774A (en) * | 2021-04-28 | 2021-08-03 | 北京梦之墨科技有限公司 | Liquid sensor, manufacturing method thereof and liquid sensing system |
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