KR20220115158A - Hydrogen sulfide gas sensor containing aluminum-doped tin oxide nanomaterials - Google Patents

Abstract

The present invention relates to a metal oxide-based sensor doped for detecting hydrogen sulfide gas, and a manufacturing method thereof. Tin oxide nanomaterial is doped with aluminum to increase a specific surface area due to an effect of a nano-size to detect hydrogen sulfide gas at high sensitivity. Moreover, according to the present invention, the tin oxide nanomaterial doped with aluminum is applied to a gas sensor to have an excellent hydrogen oxide gas detection property in various humidity environments.

Description

Hydrogen sulfide gas sensor containing aluminum-doped tin oxide nanomaterials

The present invention relates to a hydrogen sulfide gas sensor including a tin oxide nanomaterial doped with aluminum, a manufacturing method thereof, and a hydrogen sulfide gas detection method using the gas sensor.

Gas sensors have been used in a wide range of fields such as chemistry, pharmaceuticals, environment, and medicine, and are expected to be studied more in the future. A technology that detects harmful substances and pollutants in the air in real time is indispensable to maintain a good living and working environment. In particular, hydrogen sulfide (H ₂ S) generated by bisulfide and sulfide ions in the industrial process of manufacturing sulfur or sulfuric acid, which is widely used in the industry, and manufacturing dyes and cosmetics is exposed to high concentrations when exposed to high concentrations. It can cause very serious symptoms such as damage to the mucous membrane and unconsciousness or permanent brain damage, apoptosis, and vasodilatation. There is an increasing need for a sensor that detects

Meanwhile, materials having a band-gap of 3.0-4.8 eV among metal oxides (ZnO, SnO ₂ , WO ₃ , TiO ₂ , etc.) may have semiconductor properties. When an external gas (NO _x , CO, H ₂ , HC, SO _x , etc.) is adsorbed on the surface of the metal oxide having semiconductor characteristics, the resistance of the metal oxide is changed through the oxidation/reduction process. As the change range of the resistance increases, the sensing characteristic (Sensitivity) of the sensor including the metal oxide is improved.

In order to improve these properties, the surface area of the metal oxide can be increased or a metal nanomaterial can be attached to the surface to detect harmful gases, but there are problems in reproducibility, stability, sensing performance and detection limit improvement.

Korean Patent Publication No. 10-2014-0104784 Korean Patent Publication No. 10-2016-0136811 Korean Patent Publication No. 10-2017-0114192 Korean Patent Publication No. 10-2017-0123850 Korean Patent Publication No. 10-2018-0096050 Korean Patent Registration No. 10-2051757

It is an object of the present invention to solve the problems of the prior art, and to provide a gas sensor having excellent hydrogen sulfide gas detection ability even in various humidity environments using aluminum-doped tin oxide nanomaterials.

Another object of the present invention is to provide a composition for detecting hydrogen sulfide gas comprising a tin oxide nanomaterial doped with aluminum.

Another object of the present invention is to provide a method for manufacturing a hydrogen sulfide gas sensor including a tin oxide nanomaterial doped with aluminum.

Another object of the present invention is to provide a method for detecting hydrogen sulfide gas using a hydrogen sulfide gas sensor including a tin oxide nanomaterial doped with aluminum.

In order to achieve the above object,

The present invention provides a hydrogen sulfide gas sensor comprising a tin oxide nanomaterial doped with aluminum.

In addition, the present invention provides a composition for detecting hydrogen sulfide gas comprising a tin oxide nanomaterial doped with aluminum.

Also, the present invention

disposing an electrode on a substrate; and

Depositing a tin oxide nanomaterial doped with aluminum on the electrode to form a sensing layer; provides a method of manufacturing a hydrogen sulfide gas sensor, including a.

In addition, the present invention

A step of reacting a sample suspected of containing hydrogen sulfide by contacting the hydrogen sulfide gas sensor of claim 1; and

It provides a method for detecting hydrogen sulfide gas, comprising the step of measuring one or more indicators selected from the group consisting of a fluorescence signal, absorption, and optical change of the reacted reactant.

The aluminum-doped tin oxide nanomaterial of the present invention is doped with aluminum, and the specific surface area is increased due to the effect of the nanosize, so that it is possible to detect hydrogen sulfide gas with high sensitivity.

In addition, the gas sensor of the present invention is excellent in the ability to detect hydrogen sulfide gas even in a variety of humidity environments using such aluminum-doped tin oxide nanomaterials.

1 is an SEM image of a nanomaterial according to an embodiment of the present invention.
2 is a TEM image of a nanomaterial according to an embodiment of the present invention.
3 is an XRD analysis result of a nanomaterial according to an embodiment of the present invention.
4 is TEM mapping data of a nanomaterial according to an embodiment of the present invention.
5 is an XPS analysis result of a nanomaterial according to an embodiment of the present invention.
6 is a BET analysis result of a nanomaterial according to an embodiment of the present invention.
7 is a UPS analysis result of a nanomaterial according to an embodiment of the present invention.
8 is an evaluation result of hydrogen sulfide gas sensing characteristics of the gas sensor according to an embodiment of the present invention.
9 is data on the sensitivity and the sensitivity of the gas sensor according to an embodiment of the present invention.
10 is a selective detection graph of a gas sensor according to an embodiment of the present invention.

Hereinafter, the present invention will be described in detail. In describing the present invention, detailed descriptions of related known configurations or functions may be omitted.

The terms or words used in the present specification and claims are not limited and interpreted in a conventional or dictionary meaning, but should be interpreted as meanings and concepts consistent with the technical matters of the present invention.

The embodiments described in this specification and the configurations shown in the drawings are preferred embodiments of the present invention, and do not represent all of the technical spirit of the present invention, so various equivalents and modifications that can be substituted for them at the time of the present application are provided. there may be

The present invention provides a hydrogen sulfide gas sensor comprising a tin oxide nanomaterial doped with aluminum.

The hydrogen sulfide gas sensor

Board;

an electrode disposed on the substrate; and

and a sensing layer including a tin oxide nanomaterial doped with aluminum formed on the electrode.

The hydrogen sulfide gas sensor may be manufactured by forming an electrode and a sensing layer on a substrate, or may be manufactured by disposing an electrode on a substrate and then forming a sensing layer on the electrode, and after forming a sensing layer on the substrate, sensing It can also be formed by disposing an electrode on the layer.

The substrate may be a ceramic substrate, an alumina (Al ₂ O ₃ ) substrate, a silicon (Si) substrate on which an insulating layer is deposited, a silicon oxide (SiO ₂ ) substrate, or the like.

The aluminum-doped tin oxide nanomaterial may have a size of 3 to 30 nm.

When the size of the nanomaterial is less than 3 nm, problems such as a drop in dispersion due to aggregation may occur, and when the size of the nanomaterial exceeds 30 nm, problems such as a decrease in surface area may occur. Accordingly, the sensing characteristic of the gas sensor may be deteriorated.

The sensing layer may have a shape selected from the group consisting of a line pattern, a lattice shape, a curved shape, a cylindrical shape, a square pillar shape, an inverted cone shape, a rectangular parallelepiped shape, a top shape, a cup shape, and a U shape on the electrode.

The sensing layer is chemical vapor deposition (CVD), atomic layer deposition, sputtering, laser ablation, plasma deposition, thermochemical vapor deposition, and spray coating on the electrode group consisting of It can be formed by deposition by a method selected from.

As the electrode, platinum (Pt), gold (Au), silver (Ag), nickel (Ni), copper (Cu), titanium (Ti), or the like may be used alone or as a composite layer.

The electrode may be disposed on the substrate with a first electrode and a second electrode spaced apart from each other, and a portion where the first electrode and the second electrode are spaced apart from each other to expose the sensing layer is substantially a sensing region in the hydrogen sulfide sensor. area).

In addition, the present invention provides a composition for detecting hydrogen sulfide gas comprising a tin oxide nanomaterial doped with aluminum.

The composition may constitute a hydrogen sulfide gas detection kit by further including a detection material or detection device of the reactant.

Also, the present invention

disposing an electrode on a substrate; and

Depositing a tin oxide nanomaterial doped with aluminum on the electrode to form a sensing layer; provides a method of manufacturing a hydrogen sulfide gas sensor, including a.

In the manufacturing method,

The aluminum-doped tin oxide nanomaterial is

(a) preparing a solution by mixing tin chloride pentahydrate (SnCl ₄ -5H ₂ O, Tin chloride pentahydrate), aluminum nitrate (Al(NO ₃ ) ₃ , aluminum nitrate) and a solvent;

(b) adding ammonia to the solution of step (a);

(c) hydrothermal synthesis of the solution of step (b);

(d) filtering the solution of step (c) and drying the solution to prepare a powder;

(e) first calcining the powder of step (d); and

(f) secondary calcination of the material of step (e); may be prepared by a method comprising.

In this case, the solvent may include water, ethanol, or a mixture thereof.

The ammonia is preferably added until the pH of the solution becomes 5.

The hydrothermal synthesis may be performed at a temperature of 150 to 250° C., a pressure of 250 to 1,200 atm, and a time of 10 to 48 hours.

The first and second calcinations may be performed at 300 to 800° C. for 1 to 8 hours, respectively.

The first and second calcinations may be performed in a box furnace.

The substrate may be a ceramic substrate, an alumina (Al ₂ O ₃ ) substrate, a silicon (Si) substrate on which an insulating layer is deposited, a silicon oxide (SiO ₂ ) substrate, or the like.

The aluminum-doped tin oxide nanomaterial may have a size of 3 to 30 nm.

The sensing layer may be manufactured in a shape selected from the group consisting of a line pattern, a grid shape, a curved shape, a cylindrical shape, a square pillar shape, an inverted cone shape, a rectangular parallelepiped shape, a top shape, a cup shape, and a U shape on the electrode. have.

The sensing layer is chemical vapor deposition (CVD), atomic layer deposition, sputtering, laser ablation, plasma deposition, thermochemical vapor deposition, and spray coating on the electrode group consisting of It can be formed by deposition by a method selected from.

The electrode may be disposed on a substrate with a first electrode and a second electrode spaced apart from each other.

In addition, the present invention

A step of reacting a sample suspected of containing hydrogen sulfide by contacting the hydrogen sulfide gas sensor of claim 1; and

It provides a method for detecting hydrogen sulfide gas, comprising the step of measuring one or more indicators selected from the group consisting of a fluorescence signal, absorption, and optical change of the reacted reactant.

In the detection method,

The indicator may be generated by a dimer obtained through hydrogen sulfide bonding of aluminum-doped tin oxide nanomaterials in the presence of hydrogen sulfide in the sample.

Hereinafter, the present invention will be described in more detail through examples. These examples are only for illustrating the present invention in more detail, and it is obvious to those skilled in the art that the scope of the present invention is not limited by these examples according to the gist of the present invention. .

Example 1 Synthesis of tin oxide nanomaterials (pristine SnO ₂ )

4.2072 g of SnCl ₄ -5H ₂ O was added to 80 ml of DI water and mixed at room temperature using a stirrer.

Ammonia was added to this solution under magnetic stirring until the pH reached 5. After transferring the solution to an autoclave, hydrothermal synthesis was performed in an oven at 160° C. for 12 hours. After filtering the powder using a filter, drying was performed at 120° C. for 12 hours.

Thereafter, the nanomaterial was prepared by calcining in a box furnace at 600°C for 2 hours, and then calcining in a tube furnace at 600°C for 2 hours.

Example 2 Synthesis of aluminum-doped tin oxide nanomaterials (SnO ₂ -Al (1:0.16))

4.2072 g of SnCl ₄ -5H ₂ O was added to 80 ml of DI water and mixed at room temperature using a stirrer. And Al(NO ₃ ) ₃ A tin oxide nanomaterial doped with aluminum was prepared in the same manner as in Example 1, except that a solution was prepared by adding 2.11 mol.

Example 3 Synthesis of aluminum-doped tin oxide nanomaterials (SnO ₂ -Al (1:0.33))

4.2072 g of SnCl ₄ -5H ₂ O was added to 80 ml of DI water and mixed at room temperature using a stirrer. And aluminum-doped tin oxide nanomaterials were prepared in the same manner as in Example 1, except that 4.22 mol of Al(NO ₃ ) ₃ was added to prepare a solution.

Example 4 Hydrogen sulfide gas sensor (pristine SnO ₂ )

Au interdigitated electrodes were deposited on the Al ₂ O ₃ substrate by DC sputtering. The electrode was deposited at 80 mA for 12 minutes, and the final thickness was 300 nm.

A hydrogen sulfide gas sensor was prepared by spray-coating the nanomaterial prepared according to Example 1 on the electrode.

Example 5 Hydrogen sulfide gas sensor (SnO ₂ -Al (1:0.16))

A hydrogen sulfide gas sensor was manufactured in the same manner as in Example 4 except that the aluminum-doped tin oxide nanomaterial prepared according to Example 2 was used instead of the nanomaterial prepared according to Example 1.

Example 6 Hydrogen sulfide gas sensor (SnO ₂ -Al (1:0.33))

A hydrogen sulfide gas sensor was manufactured in the same manner as in Example 4, except that the aluminum-doped tin oxide nanomaterial prepared according to Example 3 was used instead of the nanomaterial prepared according to Example 1.

Experimental Example 1 Material analysis (check material shape)

The shapes of the nanomaterials synthesized in Examples 1 to 3 were confirmed using Scanning Electron Microscopy (SEM, JEOL-7800F, JEOL Ltd) and a transmission electron microscope (TEM, Talos F200X, FEI).

Referring to FIG. 1, first, (1a) of FIG. 1 is a nanomaterial synthesized from Example 1 (pristine SnO ₂ ), and (1b) of FIG. 1 is a nanomaterial synthesized from Example 2 (SnO ₂ -Al (1) :0.16)), (1c) of FIG. 1 shows an SEM image of the nanomaterial (SnO ₂ -Al (1:0.33)) synthesized from Example 3.

All of the nanomaterials synthesized in Examples 1 to 3 were confirmed to form very homogeneous nanoparticles, and it was confirmed that aggregation occurred due to the nanosize effect.

TEM analysis was performed to confirm a more detailed shape. Referring to FIG. 2 , first, (2a) of FIG. 2 is a nanomaterial synthesized from Example 1 (pristine SnO ₂ ), and (2b) of FIG. 2 is an Example The nanomaterial synthesized from 2 (SnO ₂ -Al (1:0.16)), (2c) of FIG. 2 shows a TEM image of the nanomaterial synthesized from Example 3 (SnO ₂ -Al (1:0.33)) .

It was confirmed that all of the nanomaterials synthesized in Examples 1 to 3 had a very small nanosize of 5 to 20 nm, and it was confirmed that the size of the nanoparticles decreased as doping progressed.

Experimental Example 2 Material analysis (chemical composition confirmation)

Chemicals of nanomaterials synthesized from Examples 2 and 3 using Energy dispersive X-ray spectroscope (EDS, Talos F200X, FEI) and high angle annular dark field scanning transmission electron microscope (HAADF-STEM) belonging to TEM analysis equipment The composition was confirmed.

Referring to Figure 4, first (ae) of Figure 4 is a nanomaterial synthesized from Example 2 (SnO ₂ -Al (1:0.16)), Figure 4 (fj) is a nanomaterial synthesized from Example 3 ( The TEM mapping result of SnO ₂ -Al (1:0.33)) is shown.

All of the nanomaterials synthesized from Examples 2 and 3 were confirmed to have Sn, O, and Al elements, and the Al composition was 2.82 at% of the nanomaterial synthesized from Example 2 (SnO ₂ -Al (1:0.16)), respectively. The nanomaterial synthesized from Example 3 (SnO ₂ -Al (1:0.33)) was confirmed to be 3,89 at%.

Experimental Example 3 Material analysis (chemical states check)

Chemical states of the nanomaterials synthesized in Examples 1 to 3 were confirmed using X-ray photo-electron spectroscopy (XPS, Thermo Fisher Scientific Co.).

Referring to FIG. 5, first, FIG. 5a shows the results of XPS surveys of nanomaterials synthesized from Examples 1 to 3. All of the nanomaterials synthesized from Examples 1 to 3 had Sn and O elements, and the nanomaterials synthesized from Examples 2 and 3 (SnO ₂ -Al (1:0.16), SnO ₂ -Al (1:0.33)) Al elements were additionally observed.

Figure 5b shows the chemical state of the Al 2p region of the nanomaterial synthesized from Examples 1 to 3; In the nanomaterial synthesized from Example 1 (pristine SnO ₂ ), it was confirmed that there was no Al-related pick, and in the nanomaterial synthesized from Example 2 (SnO ₂ -Al (1:0.16)) 73.8 eV, from Example 3 In the synthesized nanomaterial (SnO ₂ -Al (1:0.33)), a broader Al-related peak of 73.8 to 74 eV was confirmed. This is considered to be because Al ₂ O ₃ was generated as the Al doping amount increased as the Al concentration increased, as in the XRD result.

Figure 5c shows the O1s region of the nanomaterial synthesized from Examples 1 to 3. The nanomaterial synthesized from Example 1 (pristine SnO ₂ ) was observed to pick at 530 eV, and when doping proceeded, a pick was observed at 529.6 eV. It is considered that this shape appears because, when doping proceeds, defects are created in the lattice and many oxygen species are formed on the surface of the material.

Experimental Example 4 Material analysis (confirmation of crystal structure)

The crystal structures of the nanomaterials synthesized from Examples 1 to 3 were confirmed using X-ray diffraction (XRD, SmartLab, Rigaku) with Cu Kα radiation (λ=1.5418 Å).

Referring to FIG. 3 , first, in FIG. 3 ( 3a ), all of the nanomaterials synthesized in Examples 1 to 3 were JCPDS card No. When compared to 41-1445, it was confirmed that all SnO ₂ had a crystal structure. In addition, as doping progressed, the tendency of the pick to widen was confirmed. It was confirmed that the aluminum element penetrated into the tin oxide crystal structure and there was a possibility of doping.

In addition, it was confirmed that there is a very fine aluminum oxide pick in (3b) and (3c) of FIG. As the concentration of Al increased, it was found that Al ₂ O ₃ in which Al and O were combined was observed very finely.

Experimental Example 5 Material analysis (check the band structure)

The band structure of the nanomaterial synthesized in Examples 1 to 3 was confirmed by confirming the work function using ultraviolet photoelectron spectroscopy (UPS, Thermo Fisher Scientific Co.).

Referring to FIG. 7 , the work function of the nanomaterial synthesized from Example 1 (pristine SnO ₂ ) is 4.3, the nanomaterial synthesized from Example 2 (SnO ₂ -Al (1:0.16)) is 4.6, Example 3 The nanomaterial synthesized from (SnO ₂ -Al (1:0.33)) showed 4.9. It is determined that Al penetrates into the SnO ₂ lattice and has different work functions.

Experimental Example 6 Material analysis (specific surface area confirmation)

By using Brunauer-Emmett-Teller analysis (BET, TriStar II 3020, Micrometrics Instrument Corporation), the degree of adsorption of the nanomaterials synthesized from Examples 1 to 3 to H ₂ S gas was confirmed to determine the specific surface area.

Referring to FIG. 6 , the specific surface area of the nanomaterial synthesized from Example 1 (pristine SnO ₂ ) is 22.082, the nanomaterial synthesized from Example 2 (SnO ₂ -Al (1:0.16)) is 28.439, Example The nanomaterial synthesized from 3 (SnO ₂ -Al (1:0.33)) showed 78.087. As confirmed by SEM and TEM, it is determined that the specific surface area increases due to the nanosize effect as the size of nanoparticles decreases as doping progresses. In addition, as doping proceeds through XRD and XPS, crystal defects are generated, and it is judged that the reactivity with H ₂ S gas is improved.

Experimental Example 7 Gas sensing characteristic evaluation

The gas sensors manufactured according to Examples 4 to 6 were placed in a chamber equipped with a ceramic heater, and gas sensing characteristics were measured using a self-manufactured gas sensing system. The target toxic gas and argon (Air) gas were mixed using MFCs (mass flow controllers). The total flow rate was set to 500 sccm, and the resistance in the air state was expressed as Ra and the target toxic gas was expressed as Rg, and the resistance was measured using a Keithley 2450. Response was determined as R = Ra/Rg (reducing gas). The response time was set as 90% of the final resistance value reached by flowing the target toxic gas.

The hydrogen sulfide (H ₂ S) gas sensing characteristic evaluation results of the gas sensors manufactured according to Examples 4 to 6 are shown in FIG. 8 . The results of the sensitivity and the reaction rate of the gas sensor to hydrogen sulfide (H ₂ S) gas are shown in FIG. 9 and Table 1 below. A selective detection graph for 10 ppm of other gases (C ₂ H ₅ OH, NH ₃ , C ₇ H ₈ ) containing hydrogen sulfide of the gas sensor prepared according to Example 6 is shown in FIG. 10 .

H ₂ S gas concentration (ppm) Example 4 (Pristine SnO ₂ ) Example 5 (SnO ₂ -Al(1:0.16)) Example 6 (SnO ₂ -Al(1:0.33)) Sensitivity ((Ra/Rg) Response speed (s) Sensitivity ((Ra/Rg) Response speed (s) Sensitivity ((Ra/Rg) Response speed (s) 20 7.13 9 14.18 238 17.38 35 10 3.69 7 7.21 247 8.76 53 6 2.48 8 5.31 230 6.72 117 2 2.00 28 2.42 152 2.71 162

Referring to FIG. 8 , all of the gas sensors manufactured according to Examples 4 to 6 showed n-type behavior with respect to hydrogen sulfide gas 20, 10, 6, and 2 ppm. In addition, the gas sensor (SnO ₂ -Al(1:0.33)) prepared according to Example 6 showed better sensitivity at all hydrogen sulfide gas concentrations.

9 and Table 1, the gas sensors prepared according to Examples 5 and 6 (SnO ₂ -Al (1:0.16), SnO ₂ -Al (1:0.33)) were prepared according to the gas prepared according to Example 4 All of the H ₂ S gas sensitivity was higher than that of the sensor (pristine SnO ₂ ).

However, the gas sensor prepared according to Example 4 (pristine SnO ₂ ) was prepared according to Examples 5 and 6 (SnO ₂ -Al (1:0.16), SnO ₂ -Al (1:0.33)) to the It was found that the response rate was faster than This is because the response ends relatively quickly due to the low sensitivity, so the response speed appears to be fast.

In addition, the gas sensor prepared according to Example 6 (SnO ₂ -Al (1:0.33)) showed a faster response rate than the gas sensor prepared according to Example 5 (SnO ₂ -Al (1:0.16)). confirmed that.

Referring to FIG. 10, first, the gas sensor (SnO ₂ -Al (1:0.33)) prepared according to Example 6 in FIGS. 10 (a) and (b) is hydrogen sulfide (H ₂ S) for each gas. Sensitivity of 8.76, C ₂ H ₅ OH 2.42, NH ₃ 2.41, and C ₇ H ₈ 1.14 was shown. Therefore, it was confirmed that the gas sensor (SnO ₂ -Al (1:0.33)) prepared according to Example 6 had excellent sensitivity to hydrogen sulfide (H ₂ S) gas compared to other gases.

Referring to FIGS. 10 (c) and (d) regarding the humidity effect test of the sensor, hydrogen sulfide at 0RH% of relative humidity of the gas sensor (SnO ₂ -Al (1:0.33)) prepared according to Example 6 ( The sensitivity of H ₂ S) gas was 8.76, but when the relative humidity was increased to 30RH%, the sensitivity was 1.53. This is considered to be because more water molecules are adsorbed to the gas adsorption site, making it difficult to adsorb hydrogen sulfide (H ₂ S) gas.

Claims (9)

A hydrogen sulfide gas sensor comprising aluminum-doped tin oxide nanomaterials.
According to claim 1,
Board;
an electrode disposed on the substrate; and
A hydrogen sulfide gas sensor comprising a; a sensing layer comprising a tin oxide nanomaterial doped with aluminum formed on the electrode.
A composition for detecting hydrogen sulfide gas comprising a tin oxide nanomaterial doped with aluminum.
disposing an electrode on a substrate; and
Forming a sensing layer by depositing a tin oxide nanomaterial doped with aluminum on the electrode; comprising, a method of manufacturing a hydrogen sulfide gas sensor.
5. The method of claim 4,
The aluminum-doped tin oxide nanomaterial is
(a) preparing a solution by mixing tin chloride pentahydrate (SnCl ₄ -5H ₂ O, Tin chloride pentahydrate), aluminum nitrate (Al(NO ₃ ) ₃ , aluminum nitrate) and a solvent;
(b) adding ammonia to the solution of step (a);
(c) hydrothermal synthesis of the solution of step (b);
(d) filtering the solution of step (c) and drying the solution to prepare a powder;
(e) first calcining the powder of step (d); and
(f) secondary calcination of the material of step (e);
6. The method of claim 5,
The hydrothermal synthesis is a method of manufacturing a hydrogen sulfide gas sensor, characterized in that the temperature is 150 to 250 ℃, the pressure is 250 to 1,200 atm, and is performed for 10 to 48 hours.
6. The method of claim 5,
The first and second calcinations are each performed at 300 to 800° C. for 1 to 8 hours.
A step of reacting a sample suspected of containing hydrogen sulfide by contacting the hydrogen sulfide gas sensor of claim 1; and
A method for detecting hydrogen sulfide gas, comprising measuring one or more indicators selected from the group consisting of a fluorescence signal, absorption, and optical change of the reacted reactant.
9. The method of claim 8,
The indicator is a method for detecting hydrogen sulfide gas, characterized in that when hydrogen sulfide is present in the sample, the aluminum-doped tin oxide nanomaterial is generated by a dimer obtained through hydrogen sulfide bonding.

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