CN114264699A - Preparation method of graphene electrode of gas sensor - Google Patents
Preparation method of graphene electrode of gas sensor Download PDFInfo
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- CN114264699A CN114264699A CN202111503974.8A CN202111503974A CN114264699A CN 114264699 A CN114264699 A CN 114264699A CN 202111503974 A CN202111503974 A CN 202111503974A CN 114264699 A CN114264699 A CN 114264699A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 24
- 239000000758 substrate Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 9
- 239000007789 gas Substances 0.000 description 17
- 239000006185 dispersion Substances 0.000 description 8
- 239000007921 spray Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007590 electrostatic spraying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The invention relates to the field of graphene, and discloses a preparation method of a graphene electrode of a gas sensor. The invention aims to solve the problem that the sensitivity is affected when the existing graphene sensor is prepared, and particularly provides a preparation method of a graphene electrode of a gas sensor.
Description
Technical Field
The invention relates to the field of graphene, in particular to a preparation method of a graphene electrode of a gas sensor.
Background
A gas sensor is a transducer that converts a certain gas volume fraction into a corresponding electrical signal. The probe conditions the gas sample through the gas sensor, typically including filtering out impurities and interfering gases, drying or refrigerating the instrument display. The sensitivity of a gas sensor depends on the ratio of the variation of the sensor output to the variation of the measured input, mainly on the technology used in the sensor structure, and is closely related to the relationship of the sensor electrodes. Most gas sensors are designed on the principles of biochemistry, electrochemistry, physics, and optics. The first consideration is to select a sensitive technique that is sufficiently sensitive to detect the percentage of the valve limit or minimum explosion limit of the target gas.
Graphene is a new material with sp hybridized connected carbon atoms tightly packed into a single-layer two-dimensional honeycomb lattice structure. The material has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The specific surface area of the graphene is larger than that of a conventional sensor material, and the specific surface area which is not available in a large number of conventional sensors can be provided, so that the sensitivity of the sensor can be greatly improved.
Although graphene has an excellent effect in the application of sensors, due to the particularity of graphene, the sensitivity of the preparation method and process is affected, mainly because: firstly, due to the reasons of small specific surface of graphene and the like, agglomeration phenomenon is easy to occur, so that the dispersion performance of graphene is poor, a dispersing agent is required to be added during dispersion, and then the dispersing agent is removed, but the dispersing agent is not easy to remove, so that the performance exertion of the graphene is influenced; secondly, when the sensor is prepared, a solvent containing graphene is dripped on an electrode, and the dripping characteristic easily causes the unevenness of a dripped graphene film, thereby influencing the sensitivity of the sensor electrode.
Disclosure of Invention
The invention aims to solve the problem that the sensitivity is affected when the existing graphene sensor is prepared, and provides a preparation method of a graphene electrode of a gas sensor, which can be used for preparing a graphene film with better uniformity.
The basic technical scheme of the invention is as follows: the preparation method of the graphene electrode of the gas sensor comprises an electrode dropping step, wherein reduced graphene oxide drops are dropped on the surface of the electrode, the reduced graphene oxide drops are wrapped by bubbles during dropping, and the bubbles are broken when contacting with the electrode substrate and are dropped on the electrode substrate.
During manufacturing, graphene ink is required to be manufactured firstly, then the graphene ink is coated on the surface of an electrode, and the gas sensor electrode is obtained after drying; in the invention, the preparation process of the graphene ink can be the same as the preparation process of the existing graphene ink, for example, the process shown in the preparation method of the graphene composite ink for the gas sensor disclosed in the invention patent of Chinese patent application No. 201811619987X; the invention is characterized in that when the reduced graphene oxide ink (namely the graphene composite ink) is coated on an electrode, the reduced graphene oxide ink adopts a dropping mode, however, due to the surface tension of the drop and the change of air flow, the dropping mode is easy to form satellite drops, and the phenomenon of uneven reduced graphene oxide film on the surface of the electrode can be caused by the formation of the satellite drops; therefore, the reduced graphene oxide ink is wrapped by the bubbles, even satellite droplets are formed in the bubbles in the falling process of the wrapped droplets, and the droplets in the bubbles are fused in the falling process even if the satellite droplets exist in the bubbles in the falling process of the bubbles, so that the reduced graphene oxide layer after dropping is more uniform and has higher sensitivity.
Further, the electrode dropping step also comprises a drop preparation step before, wherein reduced graphene oxide powder prepared in advance is dispersed into an organic solvent and uniformly dispersed in an ultrasonic grinding mode to prepare the reduced graphene oxide drops. Due to the fact that the dispersion of graphene is poor, graphene molecules and an organic solvent are fully fused in an ultrasonic grinding mode, so that the addition of a dispersing agent can be reduced or avoided, the uniformity of graphene components of the prepared reduced graphene oxide liquid drops is improved after the dispersion uniformity of graphene is improved, the uniformity of the reduced graphene oxide film after liquid dropping is improved, and the sensitivity is improved.
Further, in the electrode dropping step, an electrostatic dropping method is adopted for dropping. The electrostatic dropping method is characterized in that the electrode substrate and the liquid drops have different charges, and during dropping, the reduced graphene oxide liquid drops are more uniformly contacted with the electrode substrate due to the attraction effect of the charges, so that the uniformity is better, and the sensitivity is better.
Further, the diameter of the bubbles is 2mm or less. The smaller the bubble, the higher the uniformity.
Further, the diameter of the bubbles is 1mm or less. The surfactant for generating fine bubbles disclosed in the chinese invention patent application No. 201010293327.4 discloses bubbles having a high stability, and the bubbles having a diameter of 1mm or less, and the stability of the bubbles in the Ross-Miles test, which is expressed by the height of the bubbles immediately after the test liquid is discharged to 5 minutes after the test, is 35mm or less, and the bubbles required in the present invention can be realized.
Further, the diameter of the reduced graphene oxide liquid drop is in the micron order.
Further, the bubbles are from a liquid containing a surfactant, and the surfactant raw material includes methanol and ethylene glycol.
Further, the bubble generation process is to dissolve the bubble raw material in bubble water and blow the dissolved bubble raw material under pressure by a slit type.
Further, the reduced graphene oxide powder in the step of preparing the droplets is nano-scale powder.
Further, the organic solvent in the dropping step includes one or more of ethanol, acetone, tetrahydrofuran, and N, N-dimethylformamide.
Drawings
Fig. 1 is a schematic diagram of a concentric double-layer showerhead used in a method for preparing a graphene electrode of a gas sensor according to the present invention.
Detailed Description
The following is further detailed by way of specific embodiments:
the first embodiment is as follows: the preparation method of the graphene electrode of the gas sensor comprises the following steps:
step one to step three refer to application number 201210390063.3, named as steps a to c in the invention patent of a gas sensor based on reduced graphene oxide and a preparation method thereof;
the method comprises the following steps: preparation of graphene oxide dispersion liquid
Placing the nano-scale graphite oxide in water, and carrying out ultrasonic treatment for 3 hours at 40-100 kHz to form a single-sheet dispersed suspension; the graphite oxide is prepared by a Hummers method, a Brodie method or a Staudenmai method; the concentration of the graphene oxide dispersion liquid is 0.5-3 mg/mL;
step two: preparation of reduced graphene oxide/polyaniline hybrid material
Adding aniline hydrochloric acid solution into the graphene oxide dispersion liquid obtained in the step one, wherein the mass ratio of aniline hydrochloric acid solution to graphene oxide dispersion liquid is 1:5, the molar concentration of the prepared aniline hydrochloric acid solution is 0.5-2M, performing magnetic stirring for 24 hours under the oil bath condition of 60-90 ℃, performing suction filtration, and washing for 2-3 times to obtain solid powder;
step three, preparation of reduced graphene oxide
B, placing the reduced graphene oxide/polyaniline hybrid material obtained in the step b in an ammonia water solution with the molar concentration of 0.5-2M, magnetically stirring for 1-12 h, performing suction filtration, washing with water until the filtrate is neutral, washing with an organic solvent until the filtrate is colorless, washing with ethanol for 2-3 times, and performing vacuum drying at 60 ℃ for 12-24 h to obtain solid powder;
step four, droplet preparation step
Dispersing the reduced graphene oxide powder prepared in the step three into an N, N-dimethyl acetamide or N-methyl pyrrolidone organic solvent, uniformly dispersing in an ultrasonic grinding mode, and using an ultrasonic ball mill or an ultrasonic grinding machine, wherein the ultrasonic ball mill is sold by Shanghai Kun right biological science and technology limited company, is of a model PZ-150L, is made of a titanium alloy material, and is rotated into a storage container under the grinding conditions of the grinding rotation speed of 1500-3500 r/min, the ultrasonic power of 150-850 KW and the grinding time of 12-20h, and then the reduced graphene oxide powder is dispersed by ultrasonic to prepare reduced graphene oxide liquid drops;
step five, preparing bubble liquid
Prepared by mixing 0.02% aqueous solution of methanol, ethylene glycol, polyalcohol, ethylenediamine and trimethylenediamine according to the method of surfactant for generating micro-bubbles disclosed in the Chinese invention patent with the application number of 201010293327.4;
step six, electrode dropping step
Dropping reduced graphene oxide droplets onto the surface of the electrode, adopting an electrostatic dropping method, adopting an electrostatic spraying machine of American Gurueli type w100 as electrostatic spraying equipment, enabling an electrostatic spray gun to carry negative charges under the discharge of an electrode needle, and connecting an electrode substrate with a grounding wire to carry positive charges; the spray head of the electrostatic spray gun is a concentric double-layer spray head, as shown in fig. 1, and comprises an inner spray cavity 2 and an outer spray cavity 1, wherein the inner spray cavity 2 is used for dripping reduced graphene oxide liquid drops, and the outer spray cavity 1 is used for forming bubbles; during the dropping liquid, spout chamber 1 and bubble aqueous solution intercommunication outward, spout chamber 2 and reduced graphene oxide liquid drop intercommunication in, the in-process of pressurization spraying, the bubble wraps up reduced graphene oxide liquid drop to fall to the electrode substrate, when the bubble contacts with the electrode substrate, the bubble breaks, reduced graphene oxide liquid drop drips to the electrode substrate, makes after the drying.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that variations and modifications can be made by those skilled in the art without departing from the structure of the present invention. These should also be construed as the scope of the present invention, and they should not be construed as affecting the effectiveness of the practice of the present invention or the applicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (10)
1. The preparation method of the graphene electrode of the gas sensor is characterized by comprising the following steps: the method comprises an electrode dropping step, wherein reduced graphene oxide drops are dropped onto the surface of an electrode, the reduced graphene oxide drops are wrapped by bubbles during dropping, and the bubbles are broken when contacting with an electrode substrate, so that the reduced graphene oxide drops are dropped onto the electrode substrate.
2. The method for preparing a graphene electrode for a gas sensor according to claim 1, wherein: the method is characterized in that a liquid drop preparation step is further included before the electrode liquid dropping step, prepared reduced graphene oxide powder is dispersed into an organic solvent in advance, and the reduced graphene oxide powder is uniformly dispersed in an ultrasonic grinding mode to prepare the reduced graphene oxide liquid drops.
3. The method for preparing a graphene electrode for a gas sensor according to claim 2, wherein: in the electrode dropping step, an electrostatic dropping method is adopted during dropping.
4. The method for preparing a graphene electrode for a gas sensor according to claim 3, wherein: the diameter of the air bubbles is less than 2 mm.
5. The method for preparing the graphene electrode for the gas sensor according to claim 4, wherein: the diameter of the air bubbles is less than 1 mm.
6. The method for preparing the graphene electrode for the gas sensor according to claim 5, wherein: the diameter of the reduced graphene oxide liquid drop is micron-sized.
7. The method for preparing a graphene electrode for a gas sensor according to claim 6, wherein: the bubbles are from liquid containing surfactant, and the surfactant comprises methanol and ethylene glycol.
8. The method for preparing a graphene electrode for a gas sensor according to claim 7, wherein: the bubble generation process is to dissolve a bubble raw material in bubble water and blow the bubble raw material by slit pressurization.
9. The method for preparing a graphene electrode for a gas sensor according to claim 8, wherein: in the step of preparing the liquid drop, the reduced graphene oxide powder is nano-scale powder.
10. The method for preparing a graphene electrode for a gas sensor according to claim 9, wherein: the organic solvent in the dripping step comprises one or more of ethanol, acetone, tetrahydrofuran and N, N-dimethylformamide.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928646A (en) * | 2004-12-28 | 2010-12-29 | 三洋化成工业株式会社 | Surfactant for fine-bubble formation |
| CN102879431A (en) * | 2012-10-15 | 2013-01-16 | 苏州大学 | Gas sensor based on reduced graphene oxide and preparation method thereof |
| CN103934133A (en) * | 2014-04-25 | 2014-07-23 | 京东方科技集团股份有限公司 | Spray head and spraying method |
| WO2015102401A1 (en) * | 2013-12-31 | 2015-07-09 | 엘지디스플레이 주식회사 | Synthesis method for solution-processable graphene |
| CN109243671A (en) * | 2018-11-29 | 2019-01-18 | 圣盟（廊坊）新材料研究院有限公司 | A kind of preparation method of graphene composite conductive slurry |
| CN111791623A (en) * | 2020-07-21 | 2020-10-20 | 艾感科技(广东)有限公司 | Method and device for preparing gas sensor array by inkjet printing |
| CN112618517A (en) * | 2020-12-14 | 2021-04-09 | 浙江大学 | Preparation method of P/H microspheres wrapped with hydrophobic solid powder |
| CN213666810U (en) * | 2020-11-04 | 2021-07-13 | 河北工业大学 | Double-pipeline water dropper |
-
2021
- 2021-12-10 CN CN202111503974.8A patent/CN114264699A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928646A (en) * | 2004-12-28 | 2010-12-29 | 三洋化成工业株式会社 | Surfactant for fine-bubble formation |
| CN102879431A (en) * | 2012-10-15 | 2013-01-16 | 苏州大学 | Gas sensor based on reduced graphene oxide and preparation method thereof |
| WO2015102401A1 (en) * | 2013-12-31 | 2015-07-09 | 엘지디스플레이 주식회사 | Synthesis method for solution-processable graphene |
| CN103934133A (en) * | 2014-04-25 | 2014-07-23 | 京东方科技集团股份有限公司 | Spray head and spraying method |
| CN109243671A (en) * | 2018-11-29 | 2019-01-18 | 圣盟（廊坊）新材料研究院有限公司 | A kind of preparation method of graphene composite conductive slurry |
| CN111791623A (en) * | 2020-07-21 | 2020-10-20 | 艾感科技(广东)有限公司 | Method and device for preparing gas sensor array by inkjet printing |
| CN213666810U (en) * | 2020-11-04 | 2021-07-13 | 河北工业大学 | Double-pipeline water dropper |
| CN112618517A (en) * | 2020-12-14 | 2021-04-09 | 浙江大学 | Preparation method of P/H microspheres wrapped with hydrophobic solid powder |
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