CN111060560B - Ru-WO3 nano material and preparation method and application thereof - Google Patents
Ru-WO3 nano material and preparation method and application thereof Download PDFInfo
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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Abstract
The invention relates to the technical field of gas sensor sensitive materials, and particularly discloses a Ru-WO3 nano material and a preparation method and application thereof. The Ru-WO 3 The nanometer material is prepared by uniformly loading Ru nanometer particles on WO 3 The length of the obtained flaky crystal on the surface of the nanoparticle is 150-160nm, the width of the obtained flaky crystal is 150-160nm, and the thickness of the obtained flaky crystal is 25-30 nm. Ru-WO of the invention 3 The nano material has higher specific surface area and catalytic activity, and WO is modified by Ru 3 The specific flaky crystal structure obtained by the nano particles has the excellent characteristics of high response speed, high response value and high sensitivity to xylene gas.
Description
Technical Field
The invention relates to the technical field of gas sensor sensitive materials, in particular to a Ru-WO3 nano material and a preparation method and application thereof.
Background
In recent decades, with the rapid development of economy and industrialization, the emission of organic volatile compounds such as benzene, toluene, xylene, formaldehyde, acetone has attracted much attention. Xylene, a toxic gaseous pollutant, is widely used and released in the industrial production field, including as a chemical intermediate in the synthesis of polyesters, paints, rubbers and solvents in the leather industry, and also in gasoline, cigarettes, smoke, building and decorative materials, etc. The emission of xylene gas can cause air pollution and harm to human health, and long term exposure to 14ppm xylene and short term inhalation of as low as 50ppm xylene can damage the respiratory system, central nervous system, liver, kidneys, eyes and skin of a human. Therefore, it is also crucial to effectively detect the content of xylene gas in the environment.
Among various gas sensors, the metal oxide semiconductor type gas sensor is one of the most widely used gas sensors at present because of its advantages of high sensitivity, good selectivity, fast response recovery, low cost, convenient carrying and the like. The metal oxide semiconductor gas sensor can directly adsorb gas to be detected by using a sensitive material, so that characteristics such as electrical properties of the material and the like are changed, and the concentration of the gas to be detected is detected by detecting the change of output signals of a peripheral circuit to a sensitive element. However, the preparation method of the metal oxide semiconductor sensitive material in the gas sensor is complex, the utilization rate of noble metal is low, the preparation cost is high, the sensitivity to detection gas is low, and the like, and the application field of the metal oxide semiconductor type gas sensor is limited.
Disclosure of Invention
Aiming at the problems of complex preparation method, low utilization rate of noble metal, high preparation cost and low sensitivity to detection gas of the sensitive material on the existing gas sensor, the invention provides Ru-WO 3 A nano material and a preparation method and application thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
Ru-WO 3 The nanometer material is prepared by uniformly loading Ru nanometer particles on WO 3 The length of the obtained flaky crystal on the surface of the nanoparticle is 150-160nm, the width of the obtained flaky crystal is 150-160nm, and the thickness of the obtained flaky crystal is 25-30 nm.
Compared with the prior art, the Ru-WO provided by the invention 3 The nano material has higher specific surface area and catalytic activity, and WO is modified by Ru 3 The nano particles can be prepared into flaky crystals with specific structure, p-xylene gasThe body has the excellent characteristics of high response speed, high response value and high sensitivity.
The invention also provides the Ru-WO 3 The preparation method of the nano material at least comprises the following steps:
a. the sheet WO is prepared by a hydrothermal method 3 Nanoparticles;
b. subjecting the sheet WO 3 Dissolving nanoparticles in ethylene glycol, adding RuCl 3 Uniformly mixing, heating and reacting at 140 ℃ and 160 ℃ for 3-6h, collecting the precipitate, and drying to obtain Ru-WO 3 And (3) nano materials.
Compared with the prior art, the Ru-WO provided by the invention 3 Preparation method of nano material by mixing sheet-like WO 3 Dissolving nanoparticles in ethylene glycol, adding RuCl 3 WO reactive at a specific temperature to form Ru-supported 3 The flaky crystal has a uniform structure, Ru is uniformly modified on the surface of the flaky crystal structure, the flaky crystal has high gas catalytic activity, the response sensitivity to dimethylbenzene can reach below 100ppm, and the preparation method is simple, low in cost, high in preparation efficiency and capable of realizing mass production.
Wherein the ethylene glycol can reduce RuCl 3 Ru in (1) 3+ Forming a metal simple substance and enabling the formed Ru metal simple substance to be rapidly combined to the flaky WO 3 On the nano-particles, the reduction rate is high, so that Ru-WO is prepared 3 The loss rate of Ru in the process of the nano material is below 30 percent, and Ru-WO is effectively increased 3 The load rate of Ru in the nano material is increased, and Ru-WO is increased 3 The activity of the nano material reduces the preparation cost.
Preferably, the hydrothermal method in step a is used for preparing the flaky WO 3 The specific process of the nano particles is as follows: hydrochloric acid was added dropwise to Na 2 WO 4 Evenly mixing the solution, adding oxalic acid, reacting for 3-6h at 85-95 ℃, and sintering the precipitate obtained by the reaction for 2-3h at 480-520 ℃ to obtain the flaky WO 3 And (3) nanoparticle powder.
Wherein, the precipitate obtained by the reaction is dried for 12 to 24 hours at the temperature of between 60 and 80 ℃ and then sintered.
Preferred aboveFlaky WO prepared by hydrothermal method 3 Nanoparticles by addition of hydrochloric acid dropwise to Na 2 WO 4 In solution, hydrochloric acid can make Na 2 WO 4 Formation of WO 3 And in the form of dropwise addition to Na 2 WO 4 Adding hydrochloric acid to the solution to ensure the formation of WO 3 The WO formed can be further ensured by forming a nano-sized crystal structure having a small and uniform particle diameter and then adding a specific amount of oxalic acid 3 The crystal is a flaky structure with uniform size and high specific surface area, and ensures the subsequent Ru-WO formation 3 The crystalline structure and size uniformity of the nanomaterial.
Preferably, the concentration of the hydrochloric acid is 10-12mol/L, and the Na is 2 WO 4 The concentration of the solution is 50-55 mg/ml; the hydrochloric acid and Na 2 WO 4 The volume ratio of the solution is 0.8-1.2: 1.
Preferably, the dropping speed of the hydrochloric acid is 0.05-0.5 ml/s.
The preferable dropping speed of the hydrochloric acid further ensures the formed flaky WO 3 Uniformity of morphology of the nanoparticle structure.
Preferably, the adding amount of the oxalic acid is Na 2 WO 4 1-1.5 times of the mass.
Preferably, WO flakes are present in step b per ml of said glycol 3 The addition amount of the nano particles is 80-120 mg.
Preferably, said RuCl is step b 3 In the amount of WO flakes 3 8-12% of the mass of the nano particles.
Preferably, the drying process in step b is drying the reaction precipitate at 60-80 ℃ for 12-24 h.
The present invention provides the Ru-WO 3 Application of nano material in detecting volatile gas.
Preferably, the volatile gas is xylene.
The present invention provides a method for producing a compound using the Ru-WO 3 The gas sensor with nano material as sensitive material includes a sensitive element, the Ru-WO 3 The nano material is coated on the sensitive element, and the coating thickness is 20-40 μm.
Compared with the prior art, the gas sensor of the invention is characterized in that the Ru-WO is coated on the sensitive element 3 The nanometer material can quickly and accurately detect the volatile harmful gases such as dimethylbenzene, acetone, ethanol and the like in the air, particularly the detection limit of the dimethylbenzene in the air can be as low as below 100ppm, the reaction is sensitive, the detection accuracy is high, and the gas sensor has the advantages of simple structure, convenience in manufacturing, small volume and convenience in carrying, and can detect the content of the harmful volatile gases in multiple occasions.
The gas sensor also comprises a base and a protective cover; the sensitive element is fixed above the base, and the protective cover is arranged above the sensitive element. Wherein the base is a six-pin tube seat; the sensitive element is formed by taking Ni-Cr alloy with the resistance value of 35-40 omega as a heating wire to penetrate through Al with a ring-shaped Au electrode 2 O 3 Ceramic tubes, said Ru-WO 3 Coating Al with nano material 2 O 3 The surface of the ceramic tube;
the Ru-WO 3 The method for coating the nano material on the surface of the sensitive element comprises the following steps: Ru-WO 3 The nanometer material is put into a mortar and ground for 20 to 30 minutes, then water is dripped into the mortar and the grinding is continued for 20 to 30 minutes, wherein the Ru-WO 3 The mass ratio of the nano material to the water is 5:1-3, and viscous slurry is obtained; and (3) coating the obtained sticky slurry on the surface of a sensitive element, and drying for 1-3h at the temperature of 60-80 ℃.
Drawings
FIG. 1 shows Ru-WO obtained in example 1 of the present invention 3 Scanning electron microscope images of the nano materials;
FIG. 2 shows Ru-WO obtained in example 1 of the present invention 3 X-ray diffraction patterns of nanomaterials
FIG. 3 is a schematic view showing the structure of a gas sensor in example 1 of the present invention; the device comprises a base, a protective cover 1, a sensitive element 2, a sensitive element 3 and a base;
fig. 4 is a graph showing the detection of response values of the gas sensor in example 1 of the present invention to a plurality of volatile gases.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Ru-WO 3 The nanometer material is prepared by uniformly loading Ru nanometer particles on WO 3 The length of the obtained flaky crystal on the surface of the nanoparticle is 150-160nm, the width of the obtained flaky crystal is 150-160nm, and the thickness of the obtained flaky crystal is 25-30 nm.
The Ru-WO 3 The preparation method of the nano material comprises the following steps:
a. preparing flaky WO by adopting a hydrothermal method 3 The specific process of the nano particles is as follows: 10mol/L hydrochloric acid is added dropwise to 50mg/ml Na according to the dropping speed of 0.05ml/s 2 WO 4 In solution, the hydrochloric acid and Na 2 WO 4 The volume ratio of the solution is 0.8:1, oxalic acid is added after the solution is uniformly mixed, the mixture is stirred for 3 hours in an oil bath at 85 ℃, then the mixed solution is centrifugally precipitated, the obtained precipitate is dried for 12 hours at 60 ℃, the dried precipitate is sintered for 2 hours in a muffle furnace at 480 ℃, and green flaky WO is obtained 3 And (3) nanoparticle powder.
b. The obtained sheet-like WO 3 Dissolving the nanoparticle powder in ethylene glycol, and obtaining flaky WO in each milliliter of ethylene glycol 3 Adding 80mg of nano particle powder, dissolving completely, adding sheet WO 3 RuCl with nanoparticle powder mass of 8% 3 Uniformly mixing, heating and reacting at 140 ℃ for 3h, centrifuging the mixed solution, washing and separating to obtain precipitate, drying the precipitate at 60 ℃ for 12h, drying and grinding to obtain Ru-WO 3 And (3) nano materials.
For the Ru-WO obtained in example 1 3 The nano material is observed by a scanning electron microscope, the observation result is shown in figure 1, and the obtained Ru-WO 3 The crystal structure of the nano material is a uniform sheet structure, the length of the nano material is 150-160nm, the width of the nano material is 150-160nm, and the thickness of the nano material is 25-30 nm;
for the sheet-like WO obtained in example 1 3 Nanoparticle powder and Ru-WO 3 The crystal structure of the nanometer material is subjected to X-ray diffraction analysis, the obtained X-ray diffraction pattern is shown in figure 2, and compared with a standard pattern (JCPDS:87-2393), the sheet WO 3 Nanoparticle powder and Ru-WO 3 WO appears in X-ray diffraction patterns of the nano-materials 3 Characteristic peaks, indicating the resulting flaky WO 3 Nanoparticle powder and Ru-WO 3 The nano material does contain WO 3 And (4) crystals.
Using the obtained Ru-WO 3 The gas sensor using nano material as sensitive material, as shown in fig. 3, includes a base 3, a sensitive element 2 and a protective cover 1; the sensing element 2 is fixed above the base 3, and the surface of the sensing element is coated with the Ru-WO 3 A nanomaterial; the protective cover 1 is arranged above the sensitive element 2; the Ru-WO 3 The thickness of the coating of the nano material is 20 mu m; wherein, the base 3 is a six-pin tube seat; the sensing element 2 is formed by passing Ni-Cr alloy with a resistance value of 35 omega as a heating wire through Al with a ring-shaped Au electrode 2 O 3 Obtained by ceramic tube, Ru-WO 3 Coating Al with nano material 2 O 3 The surface of the ceramic tube;
Ru-WO 3 the method for coating the nano material on the surface of the sensitive element 2 comprises the following steps: Ru-WO 3 The nano material is put into a mortar and ground for 20 minutes, then water is dripped into the mortar and the grinding is continued for 20 minutes, wherein the Ru-WO 3 The mass ratio of the nano material to the water is 5:1, so that viscous slurry is obtained; the obtained viscous paste was coated on the surface of the sensor 2 and then dried at 60 ℃ for 1 hour.
The response sensitivity of the gas sensor obtained in this embodiment to eight gases, i.e., ethanol, methanol, acetone, benzene, toluene, xylene, ammonia gas and nitrogen dioxide, is detected, and the detection result is shown in fig. 4, when the temperature is 280 ℃ and the gas concentration is 100ppm, the response value of the gas sensor to xylene reaches 73, the response value to ethanol reaches 33, and the response value to acetone reaches 37.
Example 2
Ru-WO 3 The nanometer material is prepared by uniformly loading Ru nanometer particles on WO 3 The length of the obtained flaky crystal on the surface of the nanoparticle is 150-158nm, the width of the obtained flaky crystal is 150-160nm, and the thickness of the obtained flaky crystal is 25-28 nm.
The Ru-WO 3 The preparation method of the nano material comprises the following steps:
a. the sheet WO is prepared by a hydrothermal method 3 The specific process of the nano particles is as follows: 11mol/L hydrochloric acid is added dropwise to 52mg/ml Na according to the dropping speed of 0.05ml/s 2 WO 4 In solution, the hydrochloric acid and Na 2 WO 4 The volume ratio of the solution is 1:1, oxalic acid is added after the solution is uniformly mixed, the mixture is stirred for 4 hours in an oil bath at the temperature of 90 ℃, then the mixed solution is centrifugally precipitated, the obtained precipitate is dried for 18 hours at the temperature of 70 ℃, the dried precipitate is sintered for 2.5 hours in a muffle furnace at the temperature of 500 ℃, and green flaky WO is obtained 3 And (3) nanoparticle powder.
b. The obtained sheet-like WO 3 Dissolving nanoparticle powder in ethylene glycol, and obtaining flaky WO in each milliliter of ethylene glycol 3 Adding 100mg of nano particle powder, dissolving completely, adding sheet WO 3 RuCl with 10% of nano particle powder mass 3 Uniformly mixing, heating and reacting for 4h at 150 ℃, centrifuging the mixed solution, washing and separating to obtain a precipitate, drying the precipitate for 18h at 60 ℃, drying and grinding to obtain Ru-WO 3 And (3) nano materials.
For the Ru-WO obtained in example 2 3 The nano material is observed by a scanning electron microscope to obtain Ru-WO 3 The crystal structure of the nano material is a uniform sheet structure, the length of the nano material is 150-158nm, the width of the nano material is 150-160nm, and the thickness of the nano material is 25-28 nm;
for the sheet-like WO obtained in example 2 3 Nanoparticle powder and Ru-WO 3 Subjecting the crystal structure of the nanomaterial to X-ray diffraction analysis, wherein the WO is in the form of flakes 3 Nanoparticle powder and Ru-WO 3 WO appears in X-ray diffraction patterns of the nano-materials 3 Characteristic peaks, indicating the resulting flaky WO 3 Nanoparticle powder and Ru-WO 3 The nano material does contain WO 3 And (4) crystals.
Ru-WO obtained in this example 3 The structure of the gas sensor using nano material as sensitive material is the same as that of the gas sensor in the embodiment 1, wherein Ru-WO 3 The nanomaterial was coated to a thickness of 30 μm in the same manner as in example 1.
The sensitivity of the gas sensor obtained in this example to the response of xylene was measured, and at a temperature of 280 ℃ and a xylene gas concentration of 100ppm, the response of the gas sensor to xylene reached 75, the response to ethanol reached 37, and the response to acetone reached 43.
Example 3
Ru-WO 3 The nanometer material is prepared by uniformly loading Ru nanometer particles on WO 3 The length of the obtained flaky crystal on the surface of the nanoparticle is 154-160nm, the width of the obtained flaky crystal is 152-160nm, and the thickness of the obtained flaky crystal is 25-30 nm.
The Ru-WO 3 The preparation method of the nano material comprises the following steps:
a. the sheet WO is prepared by a hydrothermal method 3 The specific process of the nano particles is as follows: dropwise adding 12mol/L hydrochloric acid to 55mg/ml Na at a dropwise adding speed of 0.1ml/s 2 WO 4 In solution, the hydrochloric acid and Na 2 WO 4 The volume ratio of the solution is 1.2:1, oxalic acid is added after the solution is uniformly mixed, the mixture is stirred for 6 hours in an oil bath at the temperature of 95 ℃, then the mixed solution is centrifugally precipitated, the obtained precipitate is dried for 24 hours at the temperature of 80 ℃, the dried precipitate is sintered for 3 hours in a muffle furnace at the temperature of 520 ℃, and green flaky WO is obtained 3 And (3) nanoparticle powder.
b. The obtained sheet-like WO 3 Dissolving the nanoparticle powder in ethylene glycol, and obtaining flaky WO in each milliliter of ethylene glycol 3 The addition amount of the nanoparticle powder was 120mg, and after sufficient dissolution, the flaky WO was added 3 RuCl with nanoparticle powder mass of 12% 3 Uniformly mixing, heating and reacting for 6h at 160 ℃, centrifuging the mixed solution, washing and separating to obtain a precipitate, drying the precipitate for 24h at 80 ℃, and grinding after drying to obtain Ru-WO 3 And (3) nano materials.
For the Ru-WO obtained in example 3 3 The nano material is observed by a scanning electron microscope to obtain Ru-WO 3 The crystal structure of the nano material is a uniform sheet structure, the length of the nano material is 154-160nm, the width of the nano material is 152-160nm, and the thickness of the nano material is 25-30 nm;
for the sheet-like WO obtained in example 3 3 Nanoparticle powder and Ru-WO 3 Subjecting the crystal structure of the nanomaterial to X-ray diffraction analysis, wherein the WO is in the form of flakes 3 Nanoparticle powder and Ru-WO 3 WO appears in X-ray diffraction patterns of the nano-materials 3 Characteristic peaks, indicating the resulting flaky WO 3 Nanoparticle powder and Ru-WO 3 The nano material does contain WO 3 And (4) crystals.
Ru-WO obtained in this example 3 The structure of the gas sensor using nano material as sensitive material is the same as that of the gas sensor in the embodiment 1, wherein Ru-WO 3 The nanomaterial was coated to a thickness of 40 μm in the same manner as in example 1.
The response sensitivity of the gas sensor obtained in the present example to xylene was measured, and at a temperature of 280 ℃ and a xylene gas concentration of 100ppm, the response value of the gas sensor to xylene reached 80, the response value to ethanol reached 32, and the response value to acetone reached 40.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. Ru-WO 3 The application of the nano material in detecting volatile gas, wherein the volatile gas is dimethylbenzene, and the application is characterized in that: the Ru nano particles are uniformly loaded on WO 3 The length of the flaky crystal is 150-160nm, the width of the flaky crystal is 150-160nm, and the thickness of the flaky crystal is 25-30 nm;
the Ru-WO 3 The nano material is prepared by the following method:
a. the sheet WO is prepared by a hydrothermal method 3 Nanoparticle: hydrochloric acid was added dropwise to Na 2 WO 4 Evenly mixing the solution, adding oxalic acid, reacting at 85-95 ℃ for 3-6h, and sintering the precipitate obtained by the reaction at 480-520 ℃ for 2-3h to obtain flaky WO 3 A nanoparticle powder;
b. mixing the sheet-shaped WO 3 Dissolving nanoparticles in ethylene glycol, adding RuCl 3 Uniformly mixing, heating and reacting at 140 ℃ and 160 ℃ for 3-6h, collecting the precipitate, and drying to obtain Ru-WO 3 And (3) nano materials.
2. Ru-WO according to claim 1 3 The application of the nano material in detecting volatile gas is characterized in that: the concentration of the hydrochloric acid is 10-12mol/L, and the Na is 2 WO 4 The concentration of the solution is 50-55 mg/mL; the hydrochloric acid is mixed with Na 2 WO 4 The volume ratio of the solution is 0.8-1.2: 1.
3. Ru-WO according to claim 1 3 The application of the nano material in detecting volatile gas is characterized in that: the dropping speed of the hydrochloric acid is 0.05-0.5 mL/s.
4. Ru-WO according to claim 1 3 The application of the nano material in detecting volatile gas is characterized in that: the addition amount of the oxalic acid is Na 2 WO 4 1-1.5 times of the mass.
5. Ru-WO according to claim 1 3 The application of the nano material in detecting volatile gas is characterized in that: WO flaked per ml of said glycol in step b 3 The addition amount of the nano particles is 80-120 mg; and/or
Said RuCl in step b 3 In an amount of WO in the form of flakes 3 8-12% of the mass of the nano particles.
6. Use of the Ru-WO as defined in claim 1 3 The gas sensor with the nano material as the sensitive material is characterized in that: comprising a sensor element, said Ru-WO 3 The nano material is coated on the sensitive element, and the coating thickness is 20-40 μm.
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| CN112593248B (en) * | 2020-12-15 | 2021-09-03 | 苏州大学张家港工业技术研究院 | Ruthenium and iron co-doped tungsten oxide and preparation method and application thereof |
| CN113030196B (en) * | 2021-02-25 | 2022-09-30 | 微纳感知(合肥)技术有限公司 | WO (WO) 3 Preparation method of gas-sensitive material, prepared gas-sensitive material and application thereof |
| CN113173602B (en) * | 2021-04-14 | 2023-10-13 | 扬州大学 | Preparation method of n-nonanal volatile gas sensitive material |
| CN114709428B (en) * | 2022-02-16 | 2024-04-19 | 江苏科技大学 | Defect tungsten oxide/ruthenium nanoparticle composite catalyst and preparation method and application thereof |
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