CN109709161B - Gold/palladium alloy particle modified tin oxide composite material and preparation method and application thereof - Google Patents
Gold/palladium alloy particle modified tin oxide composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a tin oxide composite material modified by gold/palladium alloy particles, and a preparation method and application thereof. The invention has good gas sensitivity, can be used as a sensing layer of a resistance type metal oxide gas sensor to realize ultrahigh selectivity detection of dimethyl disulfide gas, does not need expensive detection equipment, and has low detection cost, simple operation, rapidness and high efficiency.
Description
Technical Field
The invention relates to a gas-sensitive sensing material, in particular to a gold/palladium alloy particle modified tin oxide composite material and a preparation method and application thereof.
Background
Dimethyl disulfide is a typical volatile sulfur-containing toxic substance widely found in sewage treatment, oil refining processes and wood pulp industry. Has great harm to human and animals, and even at low concentration, can cause great damage to human respiratory and nervous systems after long-term contact. Therefore, there is an urgent need to develop some detection techniques to monitor such toxic gases in real time. Currently, several techniques have emerged, such as gas chromatography/mass spectrometry detection, biosensing detection, electrochemical detection and optical detection. These techniques suffer from a number of disadvantages including high cost, high power consumption, complex equipment and testing procedures, and relatively time consuming. Therefore, a method for detecting dimethyldisulfide in real time, which is low in cost and simple in operation, is urgently needed to be developed.
The resistance type metal oxide gas sensor has the advantages of small volume, low cost, high sensitivity, high response and recovery speed, simple operation and the like, and is popular among researchers. However, in the prior art, the resistance type metal oxide gas sensor has poor selectivity, and a resistance type metal oxide gas sensor capable of detecting dimethyl disulfide gas with high selectivity is not available.
Disclosure of Invention
The invention provides a gold/palladium alloy particle modified tin oxide composite material, a preparation method and application thereof, aiming at solving the technical problems that equipment for detecting dimethyl disulfide gas in the prior art is expensive, the operation process is complex, the detection time is long, the on-site and real-time detection cannot be carried out, and the existing resistance type metal oxide gas sensor cannot carry out high-selectivity detection on the dimethyl disulfide gas.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the gold/palladium alloy particle modified tin oxide composite material comprises the following steps:
and step A, adding the tin tetrachloride pentahydrate into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 10-30 min, adding the 35-40 wt% hydrochloric acid solution, placing the mixture at 150-200 ℃ for closed reaction for 5-24 h, and performing solid-liquid separation and washing to obtain the tin oxide hollow sphere.
And B, dispersing tin oxide into the ethanol/toluene mixed solution to enable the concentration of tin oxide particles in the mixed solution to be 0.1-3 mg/mL, stirring for 10-30 min, then sequentially adding ammonia water and 3-aminopropyltriethoxysilane, stirring for 10-48 h at the temperature of 20-100 ℃, and then carrying out solid-liquid separation and washing to obtain the amino-modified tin oxide particles.
C, dispersing the tin oxide particles modified by the amino groups into deionized water, controlling the concentration of the tin oxide particles to be 0.5-2.5 mg/mL, then adding a mixed solution of potassium chloropalladate and chloroauric acid, stirring for 2-12 hours at the temperature of 25-60 ℃, and then carrying out centrifugal separation to obtain tin oxide particles modified by both chloropalladate radicals and chloroauric acid radicals; dispersing the ion-modified tin oxide particles into deionized water, adding sodium borohydride, reacting for 2-10 h at 25-60 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 0.5-10 h at 50-400 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
The gold/palladium alloy particle modified tin oxide composite material is prepared by the preparation method of the gold/palladium alloy particle modified tin oxide composite material.
The tin oxide composite material modified by the gold/palladium alloy particles is used as a sensing material in a gas sensing device.
According to the technical scheme provided by the invention, the preparation method of the tin oxide composite material modified by the gold/palladium alloy particles comprises the steps of firstly modifying the surfaces of tin oxide particles by using 3-aminopropyltriethoxysilane, loading the gold/palladium alloy particles on the surfaces of the tin oxide particles by using an in-situ reduction method, and finally carrying out a mild annealing process. The tin oxide composite material modified by the gold/palladium alloy particles can be used as a sensing material in a gas sensing device and is used for carrying out super-selective detection on dimethyl disulfide gas. The invention has good gas sensitivity, can be used as a gas-sensitive sensing layer to realize real-time monitoring of dimethyl disulfide gas, has low use cost, does not need expensive detection equipment, and has simple operation, rapidness and high efficiency.
Drawings
FIG. 1 is a scanning electron microscope photograph, a transmission electron microscope photograph, a high resolution transmission electron microscope photograph, an X-ray electron energy spectrum scanning chart and an X-ray electron energy spectrum scanning chart of the tin oxide composite material modified by the gold/palladium alloy particles prepared in step c1 in example 1 of the present invention.
Fig. 2 is a schematic diagram of a gas-sensitive performance test result obtained by detecting dimethyl disulfide gas with the tin oxide composite modified by the gold/palladium alloy particles prepared in step c1 in example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
Details not described in the present invention are well known to those skilled in the art.
The invention relates to a gold/palladium alloy particle modified tin oxide composite material, a preparation method and application thereof, wherein the preferred specific implementation modes are as follows:
the preparation method comprises the following steps:
the preparation method of the gold/palladium alloy particle modified tin oxide composite material is characterized by comprising the following steps:
step A, adding tin tetrachloride pentahydrate and ethanol into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 10-30 min, adding 35-40 wt% of hydrochloric acid solution, placing at 150-200 ℃ for closed reaction for 5-24 h, and performing solid-liquid separation and washing to obtain a tin oxide hollow sphere;
b, dispersing tin oxide into the ethanol/toluene mixed solution to enable the concentration of tin oxide particles in the mixed solution to be 0.1-3 mg/mL, stirring for 10-30 min, then sequentially adding ammonia water and 3-aminopropyltriethoxysilane, stirring for 10-48 h at the temperature of 20-100 ℃, and then carrying out solid-liquid separation and washing to obtain amino-modified tin oxide particles;
c, dispersing the tin oxide particles modified by the amino groups into deionized water, controlling the concentration of the tin oxide particles to be 0.5-2.5 mg/mL, then adding a mixed solution of potassium chloropalladate and chloroauric acid, stirring for 2-12 hours at the temperature of 25-60 ℃, and then carrying out centrifugal separation to obtain tin oxide particles modified by both chloropalladate radicals and chloroauric acid radicals; dispersing the ion-modified tin oxide particles into deionized water, adding sodium borohydride, reacting for 2-10 h at 25-60 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 0.5-10 h at 50-400 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
In the step B, the volume ratio of ethanol to toluene in the ethanol/toluene mixed solution is 1: 0.2-20; the amount of the ammonia water is 5-25 times of the total mass of the tin oxide particles; the amount of the 3-aminopropyltriethoxysilane used is 5-30 times of the total mass of the tin oxide particles.
In the step C, the using amount of the potassium chloropalladate is 0.001-0.1 time of the total mass of the amino-modified tin oxide particles; the dosage of the chloroauric acid is 0.001-0.1 time of the total mass of the amino-modified tin oxide particles; the mass of the sodium borohydride is 0.01-0.5 times of the total mass of the amino-modified tin oxide particles.
The tin oxide composite material modified by the gold/palladium alloy particles is prepared by adopting the preparation method of the tin oxide composite material modified by the gold/palladium alloy nanoparticles.
The tin oxide composite material modified by the gold/palladium alloy particles is used as a sensing material in a gas sensing device.
The sensing material in the gas sensing device is used for detecting dimethyl disulfide.
Compared with the prior art, the tin oxide composite material modified by the gold/palladium alloy particles provided by the invention has at least the following beneficial effects:
(1) the tin oxide composite material modified by the gold/palladium alloy particles provided by the invention has a shell size of 180-250 nm, has a hollow structure, and has the gold/palladium alloy particles with the size of about 2-5 nm distributed on the surfaces of tin oxide particles. The tin oxide composite material modified by the gold/palladium alloy particles not only has excellent catalytic action generated by the gold/palladium alloy particles, but also has larger specific surface area, and is beneficial to gas diffusion, so that the gas-sensitive performance of the tin oxide composite material is greatly improved.
(2) The tin oxide composite material modified by the gold/palladium alloy particles can be used as a sensing material or a gas sensitive element of a resistance type metal oxide gas sensor, has excellent sensing performance on dimethyl disulfide gas, and can realize ultrahigh selectivity detection on the dimethyl disulfide gas. By detecting different concentrations of dimethyldisulfide gas: when the concentration of the carbon disulfide gas to be detected is as low as 5ppm, the tin oxide composite material modified by the gold/palladium alloy particles provided by the invention can still effectively detect the carbon disulfide gas, and the detection repeatability is very good. Through the same concentration detection of 10 different gases, the tin oxide composite material modified by the gold/palladium alloy particles provided by the invention has higher response to dimethyl disulfide gas only and has almost no response to other gases.
(3) The tin oxide composite material modified by the gold/palladium alloy particles can be coated on a gas-sensitive test electrode for performing super-selective detection on dimethyl disulfide gas, so that the tin oxide composite material modified by the gold/palladium alloy particles for performing dimethyl disulfide gas detection has the advantages of low use cost, no need of expensive detection equipment, simplicity in operation, rapidness, high efficiency and the like, and the tin oxide composite material modified by the gold/palladium alloy particles provided by the invention can be easily and widely prepared into a resistance type metal oxide gas sensor for performing specific detection on the dimethyl disulfide gas.
(4) The preparation method of the gold/palladium alloy particle modified tin oxide composite material provided by the invention is simple, rapid and efficient.
In conclusion, the embodiment of the invention has good gas-sensitive selection characteristic, can be used as a sensing layer of a resistance type metal oxide gas sensor to realize ultrahigh selectivity detection of dimethyl disulfide gas, does not need expensive detection equipment, and has the advantages of low detection cost, simple operation, rapidness and high efficiency.
In order to more clearly show the technical scheme and the technical effects provided by the present invention, the following detailed description is provided for the gold/palladium alloy particle modified tin oxide composite material provided by the embodiment of the present invention, and the preparation method and the application thereof.
Example 1
A preparation method of a gold/palladium alloy particle modified tin oxide composite material can comprise the following steps:
step a1, adding tin tetrachloride pentahydrate into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 30min, adding 35-40 wt% of hydrochloric acid solution, placing at 200 ℃ for closed reaction for 10h, and performing solid-liquid separation and washing to obtain the tin oxide hollow sphere.
And b1, dispersing 0.2g of tin oxide into 100mL of ethanol/toluene mixed solution (the volume ratio of ethanol to toluene is 1:2.5), magnetically stirring for 30min, then sequentially adding 3mL of ammonia water and 3mL of 3-aminopropyltriethoxysilane, stirring for 48h at 80 ℃, and then carrying out solid-liquid separation and washing to obtain the amino-modified tin oxide particles.
Step c1, dispersing 50mg of the amino-modified tin oxide particles into 50mL of deionized water, adding a mixed solution of 10mL of 0.5mg/mL potassium chloropalladate aqueous solution and 10mL of 0.5mg/mL chloroauric acid aqueous solution, stirring at 30 ℃ for 12h, and performing centrifugal separation to obtain the common modified tin oxide particles of chloropalladate and chloroauric acid; dispersing the ion-modified tin oxide particles into 40mL of deionized water, adding 3mL of sodium borohydride aqueous solution with the concentration of 0.1mg/mL, reacting for 5h at 25 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 1h at 250 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
Specifically, the following morphology and performance tests are performed on the gold/palladium alloy particle modified tin oxide composite material provided in embodiment 1 of the present invention:
(1) the tin oxide composite material modified with gold/palladium alloy particles prepared in example 1 of the present invention was observed by using a Scanning Electron Microscope (SEM), a Transmission Electron Microscope (TEM), a high-resolution transmission electron microscope (HR-TEM), and an X-ray electron energy spectrum, respectively, to obtain a scanning electron micrograph (SEM image), a transmission electron micrograph (TEM image), a high-resolution transmission electron microscope (HR-TEM), and an X-ray electron energy spectrum scanning and scanning image as shown in fig. 1. Wherein, FIG. 1a is an SEM image of the tin oxide composite material modified by the Au/Pd alloy particles obtained in step c1 of example 1, FIG. 1b is a TEM image of the Au/Pd alloy particle-modified tin oxide composite material obtained in step c1 of example 1, FIG. 1c is a TEM image of a tin oxide composite material modified with gold/palladium alloy particles obtained in step c1 of example 1, FIG. 1d is an HRTEM image of the Au/Pd alloy particle-modified Sn oxide composite material obtained in step c1 of example 1, FIG. 1f is a scanning line diagram of the X-ray electron energy spectrum of the tin oxide composite material modified by the Au/Pd alloy particles obtained in step c1 in example 1, FIG. 1g is a scanning X-ray electron spectrum of the tin oxide composite material modified by the Au/Pd alloy particles obtained in step c1 in example 1. As can be seen from fig. 1: the tin oxide composite material modified by the gold/palladium alloy particles prepared in step c1 in the embodiment 1 of the invention has a hollow structure, and the gold/palladium alloy particles have a size of 2-5 nm and are uniformly distributed on the surfaces of the tin oxide particles.
(2) A static gas-sensitive test system is adopted to perform a gas-sensitive performance test on the tin oxide composite material modified by the gold/palladium alloy particles prepared in the step c1 in the embodiment 1 of the invention by using dimethyl disulfide gas, so as to obtain a gas-sensitive performance test result schematic diagram shown in fig. 2. Fig. 2a is an optimum operating temperature test chart for detecting dimethyl disulfide gas of the tin oxide composite material modified by gold/palladium alloy particles prepared in step c1 in example 1 of the present invention, fig. 2b is a repeatability test chart for detecting dimethyl disulfide gas of the tin oxide composite material modified by gold/palladium alloy particles prepared in step e1 in example 1 of the present invention, fig. 2c is a diagram for selectively gas-sensitive testing 10 different gases of the tin oxide composite material modified by gold/palladium alloy particles prepared in step c1 in example 1 of the present invention in a static gas-sensitive testing system, and fig. 2d is a diagram for performing gradient performance test of dimethyl disulfide gas of the tin oxide composite material modified by gold/palladium alloy particles prepared in step c1 in example 1 of the present invention. As can be seen from fig. 2: the tin oxide composite material modified by the gold/palladium alloy particles prepared in step c1 in example 1 of the invention has the optimum operation temperature of 135 ℃ for the gas sensitive test of dimethyl disulfide gas, and has excellent repeatability and super selectivity to the dimethyl disulfide gas. Meanwhile, the method has a lower detection limit which can reach 5 ppm.
Example 2
A preparation method of a gold/palladium alloy particle modified tin oxide composite material can comprise the following steps:
step a2, adding tin tetrachloride pentahydrate into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 20min, adding 35-40 wt% of hydrochloric acid solution, placing at 180 ℃ for sealed reaction for 10h, and performing solid-liquid separation and washing to obtain the tin oxide hollow sphere.
And b2, dispersing 0.3g of tin oxide into 100mL of ethanol/toluene mixed solution (the volume ratio of ethanol to toluene is 1:3), magnetically stirring for 30min, then sequentially adding 2mL of ammonia water and 3mL of 3-aminopropyltriethoxysilane, stirring for 24h at 80 ℃, and then carrying out solid-liquid separation and washing to obtain the amino-modified tin oxide particles.
Step c2, dispersing 50mg of the amino-modified tin oxide particles into 50mL of deionized water, adding a mixed solution of 10mL of 0.4mg/mL potassium chloropalladate aqueous solution and 10mL of 0.6mg/mL chloroauric acid aqueous solution, stirring at 30 ℃ for 12 hours, and performing centrifugal separation to obtain the tin oxide particles jointly modified by chloropalladate ions and chloroauric acid radicals; dispersing the ion-modified tin oxide particles into 50mL of deionized water, adding 4mL of sodium borohydride aqueous solution with the concentration of 0.1mg/mL, reacting for 5h at 25 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 1h at 200 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
Example 3
A preparation method of a gold/palladium alloy particle modified tin oxide composite material can comprise the following steps:
step a3, adding tin tetrachloride pentahydrate into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 30min, adding 35-40 wt% of hydrochloric acid solution, placing at 180 ℃ for closed reaction for 12h, and performing solid-liquid separation and washing to obtain the tin oxide hollow spheres.
And b3, dispersing 0.4g of tin oxide into 100mL of ethanol/toluene mixed solution (the volume ratio of ethanol to toluene is 1:4), magnetically stirring for 30min, then sequentially adding 4mL of ammonia water and 2mL of 3-aminopropyltriethoxysilane, stirring for 48h at 80 ℃, and then carrying out solid-liquid separation and washing to obtain the amino-modified tin oxide particles.
Step c3, dispersing 40mg of the amino-modified tin oxide particles into 50mL of deionized water, adding a mixed solution of 10mL of 0.2mg/mL potassium chloropalladate aqueous solution and 10mL of 0.4mg/mL chloroauric acid aqueous solution, stirring at 30 ℃ for 12h, and performing centrifugal separation to obtain the common modified tin oxide particles of chloropalladate and chloroauric acid; dispersing the ion-modified tin oxide particles into 40mL of deionized water, adding 3mL of sodium borohydride aqueous solution with the concentration of 0.1mg/mL, reacting for 5h at 25 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 1.5h at 220 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
Example 4
A preparation method of a gold/palladium alloy particle modified tin oxide composite material can comprise the following steps:
step a4, adding tin tetrachloride pentahydrate into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 30min, adding 35-40 wt% of hydrochloric acid solution, placing at 200 ℃ for closed reaction for 10h, and performing solid-liquid separation and washing to obtain the tin oxide hollow sphere.
And b4, dispersing 0.5g of tin oxide into 100mL of ethanol/toluene mixed solution (the volume ratio of ethanol to toluene is 1:2), magnetically stirring for 30min, then sequentially adding 4mL of ammonia water and 5mL of 3-aminopropyltriethoxysilane, stirring for 48h at 80 ℃, and then carrying out solid-liquid separation and washing to obtain the amino-modified tin oxide particles.
Step c4, dispersing 50mg of the amino-modified tin oxide particles into 50mL of deionized water, adding a mixed solution of 10mL of 0.3mg/mL potassium chloropalladate aqueous solution and 10mL of 0.6mg/mL chloroauric acid aqueous solution, stirring at 30 ℃ for 12 hours, and performing centrifugal separation to obtain the tin oxide particles jointly modified by chloropalladate ions and chloroauric acid radicals; dispersing the ion-modified tin oxide particles into 40mL of deionized water, adding 5mL of sodium borohydride aqueous solution with the concentration of 0.1mg/mL, reacting for 5h at 25 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 1.5h at 200 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (5)
1. A preparation method of a gold/palladium alloy particle modified tin oxide composite material is characterized by comprising the following steps:
step A, adding tin tetrachloride pentahydrate and ethanol into an ethanol aqueous solution according to the weight ratio of 35-40 wt% of hydrochloric acid solution to 0.5-2: 50-150: 1, stirring for 10-30 min, adding 35-40 wt% of hydrochloric acid solution, placing at 150-200 ℃ for closed reaction for 5-24 h, and performing solid-liquid separation and washing to obtain a tin oxide hollow sphere;
b, dispersing tin oxide into the ethanol/toluene mixed solution to enable the concentration of tin oxide particles in the mixed solution to be 0.1-3 mg/mL, stirring for 10-30 min, then sequentially adding ammonia water and 3-aminopropyltriethoxysilane, stirring for 10-48 h at the temperature of 20-100 ℃, and then carrying out solid-liquid separation and washing to obtain amino-modified tin oxide particles;
c, dispersing the tin oxide particles modified by the amino groups into deionized water, controlling the concentration of the tin oxide particles to be 0.5-2.5 mg/mL, then adding a mixed solution of potassium chloropalladate and chloroauric acid, stirring for 2-12 hours at the temperature of 25-60 ℃, and then carrying out centrifugal separation to obtain tin oxide particles modified by both chloropalladate radicals and chloroauric acid radicals; dispersing the ion-modified tin oxide particles into deionized water, adding sodium borohydride, reacting for 2-10 h at 25-60 ℃, performing solid-liquid separation and washing, drying at 60 ℃, and calcining for 0.5-10 h at 50-400 ℃ to finally obtain the gold/palladium alloy-modified tin oxide composite particles.
2. The method for preparing the gold/palladium alloy particle-modified tin oxide composite material according to claim 1, wherein in the step B, the volume ratio of ethanol to toluene in the ethanol/toluene mixed solution is 1: 0.2-20; the amount of the ammonia water is 5-25 times of the total mass of the tin oxide particles; the amount of the 3-aminopropyltriethoxysilane used is 5-30 times of the total mass of the tin oxide particles.
3. The method for preparing a gold/palladium alloy particle-modified tin oxide composite material according to claim 1, wherein in step C, the amount of potassium chloropalladate is 0.001 to 0.1 times the total mass of the amino-modified tin oxide particles; the dosage of the chloroauric acid is 0.001-0.1 time of the total mass of the amino-modified tin oxide particles; the mass of the sodium borohydride is 0.01-0.5 times of the total mass of the amino-modified tin oxide particles.
4. A gold/palladium alloy particle-modified tin oxide composite material, characterized by being prepared by the method for preparing a gold/palladium alloy particle-modified tin oxide composite material according to any one of claims 1 to 3.
5. The application of the tin oxide composite material modified by the gold/palladium alloy particles is characterized in that the tin oxide composite material modified by the gold/palladium alloy particles in the claim 4 is used as a sensing material in a gas sensing device; the sensing material in the gas sensing device is used for detecting dimethyl disulfide.
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| CN110988047B (en) * | 2019-11-05 | 2021-04-06 | 华中科技大学 | Palladium monoatomic doped indium oxide composite material and preparation and application thereof |
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| 有机硫恶臭气体的优化分离技术研究;高超;《中国优秀硕士学位论文全文库 工程科技I辑》;20160315;B027-270 * |
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