CN-121990611-A - Micro-flower WO3 nano material and preparation method and application thereof

Abstract

The invention provides a micro-flower WO 3 nano material, a preparation method and application thereof, and relates to the technical field of gas-sensitive materials, wherein the preparation method of the micro-flower WO 3 nano material comprises the following steps of dissolving WCl 6 in absolute ethyl alcohol, stirring in a water bath, then placing washed and dried luffa sponge LO in a precursor solution, standing at room temperature, taking out the impregnated LO, drying in an oven, and finally calcining the dried LO in a muffle furnace to obtain the micro-flower WO 3 nano material.

Inventors

• WANG YUE
• WEN JUNSHENG
• FU JIAXING
• TIAN WENYUE
• GUO XINWEI
• LI JIAPENG
• DU JINCHENG
• HUANG XIN
• WANG CHUNJIE

Assignees

• 渤海大学

Dates

Publication Date

20260508

Application Date

20260211

Priority Date

20260126

Claims (10)

1. 1. The preparation method of the micro-flower WO 3 nanometer material is characterized by comprising the following steps: Step S1, dissolving WCl 6 in absolute ethyl alcohol, and stirring to form a precursor solution; S2, immersing the washed and dried vegetable sponge into the precursor solution, and standing to enable the vegetable sponge to fully adsorb the precursor solution; step S3, taking out the immersed luffa pulp and drying; And S4, placing the dried vegetable sponge into a muffle furnace for calcination to obtain the WO 3 nanometer material with the micro-pattern structure.
2. 2. The method for preparing the micro-flower WO 3 nano-material according to claim 1, wherein in step S1, 1.2gWCl 6 is dissolved in 30ml of absolute ethanol, the stirring is performed under the water bath condition, the temperature is 50-60 ℃, and the stirring time is 30-60 minutes.
3. 3. The method for preparing the micro-flower WO 3 nanometer material according to claim 1, wherein the amount of the vegetable sponge used in the step S2 is 1g, and the standing is performed at room temperature for 12-24 hours.
4. 4. The method for preparing a micro-flower WO 3 nanomaterial according to claim 1, wherein the drying in step S3 is performed in an oven at 60 ℃ for 12-24 hours.
5. 5. The method for preparing a micro-flower WO 3 nanomaterial according to claim 1, wherein the calcining temperature in step S4 is 600-1000 ℃ for 2 hours at a temperature rising rate of 5 ℃ per minute.
6. 6. The method for preparing a micro-flower WO 3 nanomaterial according to claim 1, wherein the temperature of calcination in step S4 is preferably 1000 ℃.
7. 7. A micropattern WO 3 nanomaterial, characterised in that it is prepared by a method according to any one of claims 1 to 6.
8. 8. Use of the micropattern WO 3 nanomaterial according to claim 7 as a gas sensitive semiconductor material.
9. 9. The application of the micro-flower WO 3 nanometer material according to claim 8, which is characterized in that the specific application method is that: Grinding the micro-pattern WO 3 nano material to obtain micro-pattern WO 3 nano material powder; Mixing the micro-flower WO 3 nano-material powder with deionized water and ethanol to form viscous pasty slurry; Uniformly coating the thick paste slurry on the surface of a metal electrode on an alumina ceramic tube; fixing the coated alumina ceramic tube on a base, and installing a heating resistance wire therein to form a gas sensor, wherein the resistance wire is connected to a heating end in the center of the base, so as to complete the assembly of the triethylamine gas sensor; and (3) placing the assembled triethylamine gas sensor on an aging table for aging treatment to finish the preparation of the triethylamine gas sensor.
10. 10. The application of the micro-flower WO 3 nano-material according to claim 9, wherein the specific application method is: Grinding the micro-flower WO 3 nano-material with the mass percentage of 33-35% in a mortar to obtain micro-flower WO 3 nano-material powder; Mixing the micro-flower WO 3 nano material powder with 55-58% of deionized water and 9-12% of ethanol by mass percent to form viscous pasty slurry; Uniformly coating the thick paste on the surface of a metal electrode on an alumina ceramic tube by using a screen printing technology, and repeating the coating operation for 5-7 times; uniformly coating the thick paste slurry around the metal electrode by using a brushing method, and brushing 1-3 layers; Fixing the coated alumina ceramic tube on a six-foot base, and installing a heating resistance wire therein to form a gas sensor, wherein the resistance wire is connected with a heating end in the center of the base, so as to complete the assembly of the triethylamine gas sensor; Placing the assembled triethylamine gas sensor on an aging table, and performing aging treatment for 24 hours at the temperature of 100-200 ℃ to finish the preparation of the triethylamine gas sensor; Wherein, the stable resistance value of the triethylamine gas sensor in the triethylamine atmosphere is Rg, the stable resistance value in the air is Ra, and the response performance is characterized by the ratio of Ra/Rg.

Description

Micro-flower WO3 nano material and preparation method and application thereof Technical Field The invention relates to the technical field of gas-sensitive materials, in particular to a micro-pattern WO 3 nano-material, a preparation method and application thereof. Background Gas sensing is an indispensable core technology in many fields and plays a vital role in environmental monitoring, industrial production flow management and the like. The existing gas-sensitive materials have the problems of poor perception, poor selectivity, low response value and the like in the aspect of serving as a gas sensor, and particularly triethylamine is used as a typical volatile organic compound, and the core physical and chemical properties of the triethylamine comprise flammability, high toxicity and pungent smell. Since triethylamine contains an active amino functional group, triethylamine is endowed with the capability of participating in various chemical reactions. Based on this characteristic, triethylamine is often used as a reaction intermediate or catalyst in the field of organic synthesis, and exhibits a non-negligible effect in both of these fields. But because of its flammability and high toxicity, it presents a non-negligible threat to human health and production safety. Related studies have shown that if a human body is exposed to a high concentration of triethylamine for a long period of time or a short period of time, organic injuries such as headache, pulmonary edema, gastroenteritis and the like may be induced, and more serious injuries may cause death. The concentration of triethylamine in air must not exceed 10 ppm according to the standard established by NIOSH. At present, various methods for detecting triethylamine exist in a chromatographic method, an electrochemical analysis method and the like, but the problems of large equipment volume, high instrument acquisition cost and the like of the methods generally exist, so that the method is difficult to realize wide popularization and application in the market, and the oxide semiconductor gas sensor receives wide attention due to the characteristics of simplicity and convenience in operation, high sensitivity, good stability, quick response and recovery. However, the conventional semiconductor metal oxide gas-sensitive material (such as SnO 2, znO, etc.) has the problems of poor selectivity, low response value, etc. for detecting triethylamine. Therefore, the novel sensitive material with high sensitivity, high selectivity and excellent stability for triethylamine and the simple preparation method are developed, and the novel sensitive material has important significance for realizing efficient, accurate and portable monitoring of the triethylamine. Disclosure of Invention The invention provides a micro-flower WO 3 nano material, a preparation method and application thereof, and aims to solve the problems of poor detection selectivity and low response value of the conventional triethylamine. In a first aspect, the invention provides a preparation method of a micro-flower WO 3 nano-material, which comprises the following steps: Step S1, dissolving WCl 6 in absolute ethyl alcohol, and stirring to form a precursor solution; S2, immersing the washed and dried vegetable sponge into the precursor solution, and standing to enable the vegetable sponge to fully adsorb the precursor solution; step S3, taking out the immersed luffa pulp and drying; And S4, placing the dried vegetable sponge into a muffle furnace for calcination to obtain the WO 3 nanometer material with the micro-pattern structure. Further, 1.2gWCl 6 is dissolved in 30ml of absolute ethanol in step S1, the stirring is performed under water bath conditions, the temperature is 50-60 ℃, and the stirring time is 30-60 minutes. Further, the vegetable sponge is used in the amount of 1g in the step S2, and the standing is carried out at room temperature for 12-24 hours. Further, the drying in step S3 is performed in an oven at a temperature of 60 ℃ for a time of 12-24 hours. Further, the calcination temperature in the step S4 is 600-1000 ℃, the time is 2 hours, and the temperature rising rate is 5 ℃ per minute. Further, the temperature of the calcination in step S4 is preferably 1000 ℃. In a second aspect, the invention provides a micro-flower WO 3 nanomaterial prepared by the preparation method. In a second aspect, the invention also provides application of the micro-flower WO 3 nano-material as a gas-sensitive semiconductor material, which is used for detecting triethylamine gas. Further, the specific application method is as follows: Grinding the micro-pattern WO 3 nano material to obtain micro-pattern WO 3 nano material powder; Mixing the micro-flower WO 3 nano-material powder with deionized water and ethanol to form viscous pasty slurry; Uniformly coating the thick paste slurry on the surface of a metal electrode on an alumina ceramic tube; fixing the coated alumina ceramic tube on a base, and insta