CN109580726B - Method for preparing gas sensor by directly growing ZnO nanowire on electrode - Google Patents
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Abstract
The invention discloses a method for preparing a gas sensor by directly growing ZnO nanowires on an electrode, which comprises the following steps: weighing 0.4-0.6g of Zn precursor, dissolving the Zn precursor in 50mL of deionized water to form a Zn precursor solution, and continuously stirring; dropwise adding 1.4-1.6mL of ammonia water into the Zn precursor solution, continuously stirring for 6-10min, and then placing the solution into a high-pressure reaction kettle, wherein the solution is at a height of 1/2-2/3 of the high-pressure reaction kettle; immersing the electrode plate into the solution of the high-pressure reaction kettle, screwing and sealing the cover of the reaction kettle to carry out hydrothermal reaction at the hydrothermal temperature of 70-80 ℃ for 20-30h, then finishing the reaction, drying, and roasting the electrode plate at the temperature of 100-500 ℃ to obtain the gas sensor. The ZnO nanowire gas-sensitive material disclosed by the invention is uniform in morphology and large in specific surface area, so that the problem of non-uniformity in the process of coating the material on an electrode is avoided, and the problem of falling off of the gas-sensitive material on the electrode is also avoided.
Description
Technical Field
The invention relates to the technical field of chemical sensors, in particular to a method for preparing a gas sensitive element by directly growing ZnO nanowires on an electrode.
Background
The gas sensor, which is an important branch of the sensor field, is mainly used for detecting the type and concentration of a gas in an environment, and generally, the gas sensor converts the concentration information of the gas into an electrical signal, and obtains the condition of the gas to be detected in the environment according to the strength of the electrical signal.
The zinc oxide gas sensitive material is one of three gas sensitive materials in the world, and not only has higher gas sensitive performance, but also has rich raw material reserves and simple preparation. ZnO is an important semiconductor metal oxide, and is one of the hot spots for research on gas-sensitive materials due to its stable physicochemical properties and sensitivity to combustible gases.
Zinc oxide, commonly known as zinc white, is a wide band gap N-type semiconductor metal oxide with a band gap of 3.37eV and an exciton binding energy of 60 meV. Has three crystal structures of wurtzite type, sphalerite type and salt rock type. The zinc oxide nano material has good chemical stability, thermal stability, easy doping and certain catalytic property, and is widely applied to the fields of gas sensors, lithium batteries, ultracapacitors, photocatalysis, sewage treatment and the like in a plurality of semiconductor metal oxides. The gas-sensitive material has unique effects in monitoring atmospheric pollution and detecting leakage of toxic, harmful, flammable and explosive gases.
The existing preparation of gas-sensitive elements generally prepares gas-sensitive materials first, and coats or paints the gas-sensitive materials on electrodes, and the method has the following defects: 1) the surface is uneven in the coating or smearing process (the gas-sensitive performance is influenced by the uniformity of the gas-sensitive material on the surface of the electrode, and the more uniform the gas-sensitive material is, the better the gas-sensitive performance is); 2) the firmness of the gas-sensitive material on the electrode can cause flaws, so that the gas-sensitive material falls off.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing a gas sensor by directly growing ZnO nanowires on an electrode; the ZnO nanowire gas-sensitive material directly grown on the electrode obtained by the invention has uniform appearance and large specific surface area, and avoids the problem of non-uniformity in the process of coating the electrode with the material and the problem of falling off of the gas-sensitive material on the electrode.
In order to solve the technical problems, the invention adopts the following technical scheme: the method comprises the steps of weighing a certain amount of Zn precursor, adding a certain amount of water as a solvent, then dropwise adding a certain amount of ammonia water, and directly immersing an electrode plate into a solution by adjusting the proportion of the precursor, the ammonia water amount and other conditions to prepare the ZnO gas-sensitive nanowire material for direct growth.
The invention relates to a method for preparing a gas sensor by directly growing ZnO nanowires on an electrode, which comprises the following steps:
1) weighing 0.4-0.6g of Zn precursor, dissolving the Zn precursor in 50mL of deionized water to form a Zn precursor solution, and continuously stirring;
2) dropwise adding 1.4-1.6mL of ammonia water into the Zn precursor solution, continuously stirring for 6-10min, and then placing the solution into a high-pressure reaction kettle, wherein the solution is at a height of 1/2-2/3 of the high-pressure reaction kettle;
3) immersing the electrode plate into the solution of the high-pressure reaction kettle, screwing and sealing the cover of the reaction kettle to carry out hydrothermal reaction at the hydrothermal temperature of 70-80 ℃ for 20-30h, then finishing the reaction, naturally cooling, taking out the electrode plate, cleaning, then putting into a constant-temperature drying oven at 40-70 ℃, drying, then putting the electrode plate into a tubular furnace, and roasting at the temperature of 100-500 ℃ to obtain the gas-sensitive element with the ZnO nanowire directly grown on the electrode plate.
As a further improvement of the technical scheme, in the step 1), the Zn precursor is Zn (NO)3)2·6H2And O. If other zinc salts are used, a stable linear structure cannot be formed.
Preferably, in step 1), the mass of the Zn precursor is 0.5 g. According to certain preferred embodiments of the present invention, in step 1), the stirring is magnetic stirring for 1 to 2 hours.
As a further improvement of the technical scheme, in the step 2), the amount of the ammonia water is 1.5 mL; the amount of the precursor is proportional to the amount of ammonia water, and if the proportion is changed, the shape of ZnO is changed, and a stable linear structure cannot be formed.
As a further improvement of the technical scheme, in the step 3), the hydrothermal temperature is 72-77 ℃; more preferably, in step 3), the hydrothermal temperature is 75 ℃; temperature is an important condition affecting morphology, outside this range, a stable linear structure cannot be formed.
Preferably, in the step 3), the hydrothermal time is 20-25 h; more preferably, in step 3), the hydrothermal time is 20 h; time is also an important condition affecting morphology, and stable linear structures cannot be formed outside this range.
Preferably, in step 3), the washing is performed by using deionized water and absolute ethyl alcohol respectively.
Preferably, in the step 3), the constant-temperature drying temperature is 50-65 ℃; more preferably, in the step 3), the constant temperature drying temperature is 60 ℃; the drying temperature is too high, the water solution in the ZnO growing on the surface is evaporated too fast, and holes are easily formed on the surface, so that the gas-sensitive performance of the material is influenced.
Preferably, in the step 3), the roasting temperature is 200-400 ℃; more preferably, the temperature of the calcination is 350 ℃.
Any range recited herein is intended to include the endpoints and any number between the endpoints and any subrange subsumed therein or defined therein.
The starting materials of the present invention are commercially available, unless otherwise specified, and the equipment used in the present invention may be any equipment conventionally used in the art or may be any equipment known in the art.
Compared with the prior art, the invention has the following beneficial effects:
the ZnO nanowire gas-sensitive material directly grown on the electrode obtained by the invention has uniform appearance and large specific surface area, and avoids the problem of non-uniformity in the process of coating the electrode with the material and the problem of falling off of the gas-sensitive material on the electrode.
Drawings
The following detailed description of embodiments of the invention is provided in connection with the accompanying drawings
FIG. 1 is an XRD spectrum of a gas sensitive material of a directly grown ZnO nanowire prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a gas sensitive material with directly grown ZnO nanowires in example 1 of the present invention.
Fig. 3 is a working temperature-sensitivity curve of the direct growth of ZnO nanowires in example 1 of the present invention.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
The invention relates to a method for preparing a gas sensor by directly growing ZnO nanowires on an electrode, which comprises the following steps: in summary, a certain amount of Zn precursor is weighed, a certain amount of water is added as a solvent, a certain amount of ammonia water is dripped, and the electrode plate is directly immersed into the solution to prepare the ZnO gas-sensitive nanowire material for direct growth by adjusting the conditions of the precursor proportion, the ammonia water amount and the like.
The invention relates to a method for preparing a gas sensor by directly growing ZnO nanowires on an electrode, which comprises the following steps:
1) weighing 0.4-0.6g of Zn precursor, dissolving the Zn precursor in 50mL of deionized water to form a Zn precursor solution, and continuously stirring;
2) dropwise adding 1.4-1.6mL of ammonia water into the Zn precursor solution, continuously stirring for 6-10min, and then placing the solution into a high-pressure reaction kettle, wherein the solution is at a height of 1/2-2/3 of the high-pressure reaction kettle;
3) immersing the electrode plate into the solution of the high-pressure reaction kettle, screwing and sealing the cover of the reaction kettle to carry out hydrothermal reaction at the hydrothermal temperature of 70-80 ℃ for 20-30h, then finishing the reaction, naturally cooling, taking out the electrode plate, cleaning, then putting into a constant-temperature drying oven at 40-70 ℃ for heating for 8-15 h, then putting the electrode plate into a tubular furnace, and roasting at the temperature of 100-500 ℃ to obtain the gas-sensitive element with the ZnO nanowire directly grown on the electrode plate.
According to certain embodiments of the invention, in step 1), the Zn precursor is Zn (NO)3)2·6H2And O. If other zinc salts are used, a stable linear structure cannot be formed.
According to certain preferred embodiments of the present invention, in step 1), the mass of the Zn precursor is 0.5 g. According to certain preferred embodiments of the present invention, in step 1), the stirring is magnetic stirring for 1 to 2 hours.
According to certain preferred embodiments of the present invention, in step 2), the amount of the aqueous ammonia is 1.5 mL; the amount of the precursor is proportional to the amount of ammonia water, and if the proportion is changed, the shape of ZnO is changed, and a stable linear structure cannot be formed.
According to certain preferred embodiments of the present invention, in step 3), the hydrothermal temperature is 72-77 ℃; more preferably, in step 3), the hydrothermal temperature is 75 ℃; temperature is an important condition affecting morphology, outside this range, a stable linear structure cannot be formed.
According to certain preferred embodiments of the present invention, in step 3), the hydrothermal time is 20 to 25 hours; more preferably, in step 3), the hydrothermal time is 20 h; time is also an important condition affecting morphology, and stable linear structures cannot be formed outside this range.
According to certain preferred embodiments of the present invention, in step 3), the washing is performed using deionized water and absolute ethanol, respectively.
According to certain preferred embodiments of the present invention, in the step 3), the temperature of the constant temperature drying is 50-65 ℃; more preferably, in the step 3), the constant temperature drying temperature is 60 ℃; the drying temperature is too high, the water solution in the ZnO growing on the surface is evaporated too fast, and holes are easily formed on the surface, so that the gas-sensitive performance of the material is influenced.
According to certain preferred embodiments of the present invention, in step 3), the temperature of the roasting is 200-; more preferably, the temperature of the calcination is 350 ℃.
Example 1
A method for preparing a gas sensor by directly growing ZnO nanowires on an electrode comprises the following steps:
1) weigh 0.5g Zn (NO)3)2·6H2Dissolving the zinc nitrate into 50mL of deionized water to form a zinc nitrate solution, and continuously magnetically stirring for 1 h;
2) dropwise adding 1.5mL of ammonia water into the zinc nitrate solution, continuously stirring for 10min, and then loading the solution into a high-pressure reaction kettle with the volume of 50mL, wherein the reaction solution is up to the two-thirds height of the reaction kettle;
3) immersing 3 electrode plates into the reaction liquid of a high-pressure reaction kettle, screwing and sealing a reaction kettle cover to carry out hydrothermal reaction at the temperature of 75 ℃, finishing the reaction after 20h, naturally cooling, taking out the electrode plates, washing with deionized water and absolute ethyl alcohol, putting into a constant-temperature drying oven at the temperature of 60 ℃ for heating for 8-15 h, putting into a tubular furnace, and roasting at the temperature of 350 ℃ for 1h to obtain the gas-sensitive nanomaterial of the directly-grown ZnO nanowire.
FIG. 1 is an XRD spectrum of a gas sensitive material of a directly grown ZnO nanowire prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a gas sensitive material with directly grown ZnO nanowires in example 1 of the present invention.
Example 2
Except Zn (NO) in step 1)3)2·6H2The same conditions as in example 1 were used except that the amount of O was changed to 0.6 g.
Example 3
The conditions were the same as in example 1 except that the magnetic stirring time in step 1) was controlled to 2 hours.
Example 4
The same conditions as in example 1 were used except that the amount of the aqueous ammonia solution added dropwise in step 2) was controlled to 1.6 mL.
Example 5
The same conditions as in example 1 were applied except that the height of the reaction solution to the reaction vessel in step 2) was controlled to be one half.
Example 6
The same conditions as in example 1 were used except that the hydrothermal temperature in step 3) was controlled to 80 ℃.
Example 7
The reaction conditions were the same as in example 1 except that the reaction time in step 3) was controlled to 30 hours.
Example 8
The same conditions as in example 1 were used except that the drying temperature was controlled to 50 ℃ at the constant temperature in step 3).
Example 9
The same conditions as in example 1 were used except that the baking temperature in the tubular furnace in step 3) was controlled to 200 ℃.
Through detection: the technical effects equivalent to those of example 1 can be obtained in all of examples 2 to 9. Wherein, the generation of metal oxide ZnO peak can be seen from the corresponding XRD pattern, which indicates the applicability of the method.
Comparative example 1
Except step 1) Zn (NO)3)2·6H2The conditions were the same as in example 1 except that the mass of O was changed to 1 g.
Comparative example 2
The same conditions as in example 1 were used except that the hydrothermal temperature in step 3) was controlled to 100 ℃.
Through detection: the final ZnO morphologies obtained in comparative examples 1 and 2 were difficult to control to uniform, regular linear structures, and irregular shapes such as rods or blocks were formed.
Comparative example 3
The same conditions as in example 1 were applied except that the reaction solution in step 2) was poured into the autoclave and the level was controlled to be at the overflow.
Comparative example 4
The conditions were the same as in example 1 except that the hydrothermal time in step 3) was controlled to 40 hours.
Through detection: the directly grown ZnO airtight materials obtained in the comparative examples 3 and 4 are thick, small in specific surface and poor in gas sensitivity.
Comparative example 5
Example 1 was repeated with the only difference that: in step 1), ZnCl is used as the Zn precursor2In place of Zn (NO)3)2·6H2O, as a result: the ZnO morphology cannot form a uniform and regular linear structure.
Comparative example 6
Example 1 was repeated with the only difference that: in the step 1), ZnSO is used for the Zn precursor4In place of Zn (NO)3)2·6H2O, with the result that the ZnO morphology does not form a uniform, regular linear structure.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.
Claims (13)
1. A method for preparing a gas sensor by directly growing ZnO nanowires on an electrode is characterized by comprising the following specific steps:
1) weighing 0.4-0.6g of Zn precursor, dissolving the Zn precursor in 50mL of deionized water to form a Zn precursor solution, and continuously stirring;
2) dropwise adding 1.4-1.6mL of ammonia water into the Zn precursor solution, continuously stirring for 6-10min, and then placing the solution into a high-pressure reaction kettle, wherein the solution is at a height of 1/2-2/3 of the high-pressure reaction kettle;
3) immersing the electrode plate into a high-pressure reaction kettle solution, screwing and sealing a reaction kettle cover to carry out hydrothermal reaction, wherein the hydrothermal temperature is 70-80 ℃, the reaction is finished after 20-30h, taking out the electrode plate after natural cooling, putting the electrode plate into a constant-temperature drying oven at 40-70 ℃ for heating for 8-15 h after cleaning, then putting the electrode plate into a tubular furnace, and roasting at the temperature of 100-500 ℃ to obtain a gas-sensitive element for directly growing ZnO nanowires on the electrode plate;
in the step 1), the Zn precursor is Zn (NO)3)2·6H2O。
2. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 1), the mass of the Zn precursor is 0.5 g.
3. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 1), the stirring is magnetic stirring for 1-2 h.
4. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 2), the amount of the ammonia water is 1.5 mL.
5. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 3), the hydrothermal temperature is 72-77 ℃.
6. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 5, wherein the method comprises the following steps: in the step 3), the hydrothermal temperature is 75 ℃.
7. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 3), the hydrothermal time is 20-25 h.
8. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 7, wherein the method comprises the following steps: in the step 3), the hydrothermal time is 20 h.
9. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 3), the cleaning is respectively carried out by using deionized water and absolute ethyl alcohol.
10. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 3), the constant-temperature drying temperature is 50-65 ℃.
11. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 10, wherein the method comprises the following steps: in the step 3), the constant-temperature drying temperature is 60 ℃.
12. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 1, wherein the method comprises the following steps: in the step 3), the roasting temperature is 200-400 ℃.
13. The method for preparing the gas sensor by directly growing the ZnO nanowire on the electrode according to claim 12, wherein the method comprises the following steps: the roasting temperature is 350 ℃.
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| CN102398918A (en) * | 2011-11-17 | 2012-04-04 | 东南大学 | Method for in-situ growth of nano zinc oxide on surface of electrode substrate material |
| CN107991350A (en) * | 2017-11-17 | 2018-05-04 | 济南大学 | The preparation of bar-shaped ZnO/ZIF-8 a kind of and its low temperature H2Sensitlzing effect |
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| CN104316566B (en) * | 2014-10-11 | 2017-06-13 | 武汉工程大学 | A kind of gas sensitive and its preparation and application |
| CN106970117B (en) * | 2017-03-27 | 2019-11-12 | 东北大学 | A kind of NO based on electrode surface growth in situ nano-ZnO2Sensor |
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| CN102398918A (en) * | 2011-11-17 | 2012-04-04 | 东南大学 | Method for in-situ growth of nano zinc oxide on surface of electrode substrate material |
| CN107991350A (en) * | 2017-11-17 | 2018-05-04 | 济南大学 | The preparation of bar-shaped ZnO/ZIF-8 a kind of and its low temperature H2Sensitlzing effect |
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| Direct hydrothermal growth of ZnO nanosheets on electrode for ethanol sensing;Dianxing Ju et al.;《Sensors and Actuators B》;20140429;444–451 * |
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