CN105203601A - Hydrogen gas sensitive material, preparation method thereof and preparation method of hydrogen gas sensitive device - Google Patents

Hydrogen gas sensitive material, preparation method thereof and preparation method of hydrogen gas sensitive device Download PDF

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Publication number
CN105203601A
CN105203601A CN201510732765.9A CN201510732765A CN105203601A CN 105203601 A CN105203601 A CN 105203601A CN 201510732765 A CN201510732765 A CN 201510732765A CN 105203601 A CN105203601 A CN 105203601A
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hydrogen gas
powder
nano
sno
coralliform
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林志东
洪玉元
孟柱
付萍
王学华
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Wuhan Institute of Technology
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Wuhan Institute of Technology
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Abstract

The invention relates to a hydrogen gas sensitive material, a preparation method thereof and a preparation method of a hydrogen gas sensitive device. The hydrogen gas sensitive device comprises components as follows: I), a substrate, namely SnO2 based nano-powder; II), Rh2O3, wherein the admixing amount of Rh2O3 accounts for 0.1%-5% of the substrate, namely the SnO2 based nano-powder by mass. The preparation method of the hydrogen gas sensitive material comprises steps as follows: glucose is added to an aqueous solution of SnCl4*5H2O and mixed uniformly, a mixed solution is obtained and transferred to a hydrothermal reaction kettle for reaction, then a reaction product is subjected to centrifugal separation, washed, dried and sintered, and the substrate, namely coralliform SnO2 based nano-powder is obtained; 2), a soluble Rh compound containing ethanol solution is added to the coralliform SnO2 nano-powder, fine grinding is performed until ethanol is completely volatilized, a hydrogen gas sensitive blank is obtained, and the hydrogen gas sensitive material is obtained after the hydrogen gas sensitive blank is subjected to follow-up annealing. The hydrogen gas sensitive material has the advantages of high sensitivity to hydrogen, good selectivity and short response time and meets the requirement of the hydrogen gas sensitive device.

Description

The preparation method of hydrogen gas material and preparation and hydrogen gas device
Technical field
The invention belongs to Metal Oxide Semiconductor Gas Sensing Element Technology field, relate to the preparation method of a kind of hydrogen gas material and preparation and hydrogen gas device.
Background technology
Hydrogen, as the lightest gas, has combustibility and very easily burns, and hydrogen energy source is as a kind of important secondary energy simultaneously, uses in a large number in life He in industry.Because hydrogen colorless and odorless, be not easy to be humanly perceptible, in factory work and life, reach explosible limit concentration and meet naked light once there is hydrogen gas leakage and concentration and will explode; If suck a large amount of hydrogen in life, because hydrogen is relatively light, can to surrounding diffusion, Human Lung is steeped oneself-meeting swell, and compressing heart causes expiratory dyspnea, heavy then cause suffocating.In addition hydrogen storage is got up more difficult, need install hydrogen alarm and monitoring device, in case hydrogen gas leakage.
Current most of gas alarm uses semiconductor gas sensor, wherein again based on metal-oxide semiconductor (MOS), as SnO 2, ZnO, WO 3, TiO 2deng being main matrix material, in home market, gas sensor 95% is traditional heater-type structure, because the thermal capacitance of heater-type gas sensor is large, reduces the impact of ambiance on heating-up temperature, ensure that the stability of material structure.The most key technology of gas-sensitive sensor device research field is the exploitation of gas sensitive.A lot of metal oxide semiconductor material is all lower to hydrogen sensitivity, but to other gases such as ethanol, there is higher sensitivity, occur in other words monitoring mistake so be not easy to monitor hydrogen when detecting, therefore prepare a kind ofly to hydrogen, there is high sensitivity, gas sensor that selectivity is strong has great practical significance.
Summary of the invention
Technical matters to be solved by this invention is for above shortcomings in prior art, provide a kind of highly sensitive, can the gas sensitive and preparation method thereof of effective monitoring hydrogen.
For solving the problems of the technologies described above, technical scheme provided by the invention is:
There is provided a kind of hydrogen gas material, it includes:
I) matrix SnO 2nano-powder;
II) Rh 2o 3, its incorporation is matrix SnO 2the 0.1-5% of nano-powder amount of substance.
By such scheme, described SnO 2nano-powder is coralliform SnO 2nano-powder, particle diameter is 5-100nm.
The present invention also provides the preparation method of above-mentioned hydrogen gas material, and it comprises the following steps:
1) SnCl is got 45H 2o is configured to the aqueous solution that concentration is 0.1-1mol/L, then adds glucose wherein, wherein glucose and SnCl 45H 2the mol ratio of O is 0.5-4:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 120-250 DEG C, hydro-thermal reaction 6-36 hour, after reaction terminates by reaction product centrifuging and wash, after drying in 400-550 DEG C of sintering 0.5-4 hour, obtain matrix coralliform SnO 2nano-powder;
2) to step 1) gained coralliform SnO 2nano-powder adds solubility containing the ethanolic solution of Rh compound, makes solubility contain gained Rh after Rh compound oxidation 2o 3quality account for matrix coralliform SnO 2the 0.1-5% of nano-powder quality, then carries out fine gtinding until ethanol volatilizees completely, obtains hydrogen gas blank, and hydrogen gas blank obtains hydrogen gas material through subsequent anneal process.
By such scheme, step 2) described solubility is RhCl containing Rh compound 33H 2o, (NH 4) 3rhCl 6h 2o, [Rh (PPh 3) 3] Cl 2, [Rh (C 2h 4) 2] Cl 2or Rh (CH 2cOO) 3.
The technical scheme that the preparation method of hydrogen gas device of the present invention adopts comprises the following steps:
1) SnCl is got 45H 2o is configured to the aqueous solution that concentration is 0.1-1mol/L, then adds glucose wherein, wherein glucose and SnCl 45H 2the mol ratio of O is 0.5-4:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 120-250 DEG C, hydro-thermal reaction 6-36 hour, after reaction terminates by reaction product centrifuging and wash, after drying in 400-550 DEG C of sintering 0.5-4 hour, obtain matrix coralliform SnO 2nano-powder;
2) to step 1) gained coralliform SnO 2nano-powder adds solubility containing the ethanolic solution of Rh compound, makes solubility contain gained Rh after Rh compound oxidation 2o 3quality account for matrix coralliform SnO 2the 0.1-5% of nano-powder quality, then fine gtinding is carried out until ethanol volatilizees completely, obtain hydrogen gas blank, by hydrogen gas blank with appropriate absolute ethyl alcohol furnishing pasty state, then its even application is surperficial at electrode tube, through 400-550 DEG C of annealing in process 0.5-4 hour after naturally drying in the shade, i.e. the core of obtained hydrogen gas device: gas sensing electrode pipe, finally according to heater-type structure traditional handicraft, gas sensing electrode pipe is welded, voltage ageing, encapsulation, obtained hydrogen gas device.
Beneficial effect of the present invention is: hydrogen gas material provided by the invention is highly sensitive to hydrogen, and sensing range is wide, and Monitoring lower-cut is low to moderate 10ppm, selectivity is good simultaneously, effectively can avoid the interference of the organic gass such as ethanol, the response time is short, meets the requirement of high-performance hydrogen gas device.
The key technical indexes of the hydrogen gas device obtained by hydrogen gas material of the present invention is as follows:
1) units test scope: 10-50000ppm (gas volume fraction: 1ppm=1 × 10 -6);
2) device operating temperature: 150-350 DEG C;
3) detection sensitivity: 50-2000;
4) the device reaction time: be less than 20s;
5) device release time: be less than 20s.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with embodiment, the present invention is described in further detail, but embodiment can not be construed as limiting the invention.
Embodiment 1
Prepare hydrogen gas device, step is as follows:
1) SnCl of 1.75g is taken 45H 2o is configured to the aqueous solution of 0.1mol/L, then adds 3.60g glucose wherein, glucose and SnCl 45H 2the mol ratio of O is 4:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, progressively be warming up to 180 DEG C, hydro-thermal reaction 12 hours, by reaction product centrifuging, suction filtration, repeatedly wash afterwards (with AgNO with deionized water and ethanol successively after reaction terminates 3solution detects without remaining Cl -), 80 DEG C of low temperature dryings, finally sinter 1 hour in 450 DEG C, obtain matrix coralliform tetragonal structure SnO 2nano-powder;
2) 0.5g matrix coralliform obtained above tetragonal structure SnO is taken 2nano-powder and 4mLRhCl 3ethanolic solution (concentration is 0.005mol/L) carry out fine gtinding until ethanol volatilizees completely, obtain hydrogen gas blank (radium chloride subsequent anneal oxidation after gained Rh 2o 3quality account for matrix coralliform SnO 21% of nano-powder quality);
Get the hydrogen gas blank of appropriate preparation, carry out X-ray diffractometer (XRD) and isothermal nitrogen adsorption-desorption (BET) test to it, result shows that this material particle size is 9.5nm, and specific surface area is 75.197m 2/ g, has minimum particle diameter and larger specific surface area, contributes to very much the air-sensitive performance promoting material.
3) by the appropriate absolute ethyl alcohol furnishing pasty state of above-mentioned hydrogen gas blank, then its even application is surperficial at aluminium oxide ceramics electrode tube, naturally through 450 DEG C of annealing in process 1 hour after drying in the shade, the i.e. core of obtained hydrogen gas device: gas sensing electrode pipe, finally according to heater-type structure traditional handicraft, gas sensing electrode pipe is welded, voltage ageing, encapsulation, obtained hydrogen gas device.
The Testing system of gas-sensor built WS-30A instrument that the hydrogen gas device of preparation adopts Zhengzhou Wei Sheng Electronic Technology Co., Ltd to produce is carried out air-sensitive performance test, method of testing is static volumetric method, record: when working temperature is 300 DEG C, 400 are reached to the sensitivity of 500ppm hydrogen steam, response time and release time are respectively 5s and 15s, show extraordinary sensitivity to hydrogen steam.
Embodiment 2
Prepare hydrogen gas device, step is as follows:
1) SnCl of 1.75g is taken 45H 2o is configured to the aqueous solution of 0.1mol/L, then adds 1.81g glucose wherein, glucose and SnCl 45H 2the mol ratio of O is 2:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, progressively be warming up to 200 DEG C, hydro-thermal reaction 24 hours, by reaction product centrifuging, suction filtration, repeatedly wash afterwards (with AgNO with deionized water and ethanol successively after reaction terminates 3solution detects without remaining Cl -), 80 DEG C of low temperature dryings, finally sinter 1 hour in 450 DEG C, obtain matrix coralliform tetragonal structure SnO 2nano-powder;
2) 0.5g matrix coralliform obtained above tetragonal structure SnO is taken 2nano-powder and 0.4mLRhCl 3ethanolic solution (concentration is 0.005mol/L) carry out fine gtinding until ethanol volatilizees completely, obtain hydrogen gas blank (radium chloride subsequent anneal oxidation after gained Rh 2o 3quality account for matrix coralliform SnO 20.1% of nano-powder quality);
Adopt the method identical with embodiment 1 to test hydrogen gas blank prepared by the present embodiment, recording its particle diameter is 10.5nm, and specific surface area is 72.59m 2/ g.
3) with above-mentioned hydrogen gas blank for raw material, the method similar to embodiment 1 is adopted to obtain hydrogen gas device, record: when working temperature is 250 DEG C, 200 are reached to the sensitivity of 1000ppm hydrogen steam, response time and release time are respectively 4s and 16s, show extraordinary sensitivity to hydrogen steam.
Embodiment 3
Prepare hydrogen gas device, step is as follows:
1) SnCl of 175.3g is taken 45H 2o is configured to the aqueous solution of 1mol/L, then adds 180.0g glucose wherein, glucose and SnCl 45H 2the mol ratio of O is 2:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, progressively be warming up to 200 DEG C, hydro-thermal reaction 6 hours, by reaction product centrifuging, suction filtration, repeatedly wash afterwards (with AgNO with deionized water and ethanol successively after reaction terminates 3solution detects without remaining Cl -), 80 DEG C of low temperature dryings, finally sinter 1 hour in 450 DEG C, obtain matrix coralliform tetragonal structure SnO 2nano-powder;
2) 50g matrix coralliform obtained above tetragonal structure SnO is taken 2nano-powder and 200mLRhCl 3ethanolic solution (concentration is 0.01mol/L) carry out fine gtinding until ethanol volatilizees completely, obtain hydrogen gas blank (radium chloride subsequent anneal oxidation after gained Rh 2o 3quality account for matrix coralliform SnO 21% of nano-powder quality);
Adopt the method identical with embodiment 1 to test hydrogen gas blank prepared by the present embodiment, recording its particle diameter is 9.8nm, and specific surface area is 75.351m 2/ g.
3) with above-mentioned hydrogen gas blank for raw material, the method similar to embodiment 1 is adopted to obtain hydrogen gas device, record: when working temperature is 300 DEG C, 420 are reached to the sensitivity of 1000ppm hydrogen steam, response time and release time are respectively 7s and 14s, show extraordinary sensitivity to hydrogen steam.
Embodiment 4
Prepare hydrogen gas device, step is as follows:
1) SnCl of 350g is taken 45H 2o is configured to the aqueous solution of 1mol/L, then adds 90g glucose wherein, glucose and SnCl 45H 2the mol ratio of O is 0.5:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 200 DEG C, hydro-thermal reaction 12 hours, by reaction product centrifuging, suction filtration, repeatedly wash afterwards (with AgNO with deionized water and ethanol successively after reaction terminates 3solution detects without remaining Cl -), 80 DEG C of low temperature dryings, finally sinter 1 hour in 450 DEG C, obtain matrix coralliform tetragonal structure SnO 2nano-powder;
2) 100g matrix coralliform obtained above tetragonal structure SnO is taken 2nano-powder and 80mLRh (PPh 3) 3the ethanolic solution (concentration is 0.01mol/L) of Cl carries out fine gtinding until ethanol volatilizees completely, obtains hydrogen gas blank (the rear gained Rh of radium chloride subsequent anneal oxidation 2o 3quality account for matrix coralliform SnO 20.2% of nano-powder quality);
3) with above-mentioned hydrogen gas blank for raw material, the method similar to embodiment 1 is adopted to obtain hydrogen gas device, record: when working temperature is 300 DEG C, 120 are reached to the sensitivity of 100ppm hydrogen steam, response time and release time are respectively 7s and 19s, show extraordinary sensitivity to hydrogen steam.
Embodiment 5
Prepare hydrogen gas device, step is as follows:
1) SnCl of 350g is taken 45H 2o is configured to the aqueous solution of 1mol/L, then adds 180g glucose wherein, glucose and SnCl 45H 2the mol ratio of O is 1:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 200 DEG C, hydro-thermal reaction 12 hours, by reaction product centrifuging, suction filtration, repeatedly wash afterwards (with AgNO with deionized water and ethanol successively after reaction terminates 3solution detects without remaining Cl -), 80 DEG C of low temperature dryings, finally sinter 1 hour in 450 DEG C, obtain matrix coralliform tetragonal structure SnO 2nano-powder;
2) 10g matrix coralliform obtained above tetragonal structure SnO is taken 2nano-powder and 40mLRh (CH 2cOO) 3ethanolic solution (concentration is 0.01mol/L) carry out fine gtinding until ethanol volatilizees completely, obtain hydrogen gas blank (radium chloride subsequent anneal oxidation after gained Rh 2o 3quality account for matrix coralliform SnO 21% of nano-powder quality);
3) with above-mentioned hydrogen gas blank for raw material, the method similar to embodiment 1 is adopted to obtain hydrogen gas device, record: when working temperature is 300 DEG C, 600 are reached to the sensitivity of 2000ppm hydrogen steam, response time and release time are respectively 23s and 36s, show extraordinary sensitivity to hydrogen steam.
Embodiment 6
Prepare hydrogen gas device, step is as follows:
1) SnCl of 350g is taken 45H 2o is configured to the aqueous solution of 1mol/L, then adds 180g glucose wherein, glucose and SnCl 45H 2the mol ratio of O is 1:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 200 DEG C, hydro-thermal reaction 12 hours, by reaction product centrifuging, suction filtration, repeatedly wash afterwards (with AgNO with deionized water and ethanol successively after reaction terminates 3solution detects without remaining Cl -), 80 DEG C of low temperature dryings, finally sinter 1 hour in 450 DEG C, obtain matrix coralliform tetragonal structure SnO 2nano-powder;
2) 10g matrix coralliform obtained above tetragonal structure SnO is taken 2nano-powder and 80mL (NH 4) 3rhCl 6h 2the ethanolic solution (concentration is 0.01mol/L) of O carries out fine gtinding until ethanol volatilizees completely, obtains hydrogen gas blank (the rear gained Rh of radium chloride subsequent anneal oxidation 2o 3quality account for matrix coralliform SnO 22% of nano-powder quality);
3) with above-mentioned hydrogen gas blank for raw material, the method similar to embodiment 1 is adopted to obtain hydrogen gas device, record: when working temperature is 300 DEG C, 50 are reached to the sensitivity of 10ppm hydrogen steam, response time and release time are respectively 20s and 30s, show extraordinary sensitivity to hydrogen steam.
Each raw material cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can realize the present invention; Embodiment is not enumerated at this.Bound value, the interval value of technological parameter of the present invention (as temperature, time etc.) can realize the present invention, do not enumerate embodiment at this.

Claims (5)

1. a hydrogen gas material, is characterized in that including:
I) matrix SnO 2nano-powder;
II) Rh 2o 3, its incorporation is matrix SnO 2the 0.1-5% of nano-powder quality.
2. hydrogen gas material according to claim 1, is characterized in that described SnO 2nano-powder is coralliform SnO 2nano-powder, particle diameter is 5-100nm.
3. a preparation method for the hydrogen gas material described in claim 1 or 2, is characterized in that comprising the following steps:
1) SnCl is got 45H 2o is configured to the aqueous solution that concentration is 0.1-1mol/L, then adds glucose wherein, wherein glucose and SnCl 45H 2the mol ratio of O is 0.5-4:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 120-250 DEG C, hydro-thermal reaction 6-36 hour, after reaction terminates by reaction product centrifuging and wash, after drying in 400-550 DEG C of sintering 0.5-4 hour, obtain matrix coralliform SnO 2nano-powder;
2) to step 1) gained coralliform SnO 2nano-powder adds solubility containing the ethanolic solution of Rh compound, makes solubility contain gained Rh after Rh compound oxidation 2o 3quality account for matrix coralliform SnO 2the 0.1-5% of nano-powder quality, then carries out fine gtinding until ethanol volatilizees completely, obtains hydrogen gas blank, and hydrogen gas blank obtains hydrogen gas material through subsequent anneal process.
4. the preparation method of hydrogen gas material according to claim 3, is characterized in that step 2) described solubility containing Rh compound be RhCl 33H 2o, (NH 4) 3rhCl 6h 2o, [Rh (PPh 3) 3] Cl 2, [Rh (C 2h 4) 2] Cl 2or Rh (CH 2cOO) 3.
5. a preparation method for hydrogen gas device, is characterized in that, comprises the following steps:
1) SnCl is got 45H 2o is configured to the aqueous solution that concentration is 0.1-1mol/L, then adds glucose wherein, wherein glucose and SnCl 45H 2the mol ratio of O is 0.5-4:1, make it mix under agitation and obtain mixed solution, again mixed solution is transferred in hydrothermal reaction kettle, be warming up to 120-250 DEG C, hydro-thermal reaction 6-36 hour, after reaction terminates by reaction product centrifuging and wash, after drying in 400-550 DEG C of sintering 0.5-4 hour, obtain matrix coralliform SnO 2nano-powder;
2) to step 1) gained coralliform SnO 2nano-powder adds solubility containing the ethanolic solution of Rh compound, makes solubility contain gained Rh after Rh compound oxidation 2o 3quality account for matrix coralliform SnO 2the 0.1-5% of nano-powder quality, then fine gtinding is carried out until ethanol volatilizees completely, obtain hydrogen gas blank, by hydrogen gas blank with appropriate absolute ethyl alcohol furnishing pasty state, then its even application is surperficial at electrode tube, through 400-550 DEG C of annealing in process 0.5-4 hour after naturally drying in the shade, i.e. the core of obtained hydrogen gas device: gas sensing electrode pipe, finally according to heater-type structure traditional handicraft, gas sensing electrode pipe is welded, voltage ageing, encapsulation, obtained hydrogen gas device.
CN201510732765.9A 2015-10-31 2015-10-31 Hydrogen gas sensitive material, preparation method thereof and preparation method of hydrogen gas sensitive device Pending CN105203601A (en)

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CN105606652A (en) * 2016-01-15 2016-05-25 武汉工程大学 Selective ethanol gas-sensitive material, selective ethanol gas-sensitive element and preparation method of selective ethanol gas-sensitive material
CN105819498A (en) * 2016-03-17 2016-08-03 武汉大学 Nano SnO2 hollow microsphere, preparation method and applications thereof
CN107870635A (en) * 2017-11-06 2018-04-03 龚土婷 Hydrogen using workshop safety hydrogen control device
CN110092412A (en) * 2019-05-09 2019-08-06 上海纳米技术及应用国家工程研究中心有限公司 Preparation method for gas sensor CuO-Ag modification stannic oxide nano material and products thereof and application
CN110274934A (en) * 2018-03-14 2019-09-24 全球能源互联网研究院有限公司 A kind of gas sensitive and preparation method thereof
CN110346421A (en) * 2019-06-27 2019-10-18 重庆大学 A kind of gas sensitive and its preparation method and application

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CN105606652A (en) * 2016-01-15 2016-05-25 武汉工程大学 Selective ethanol gas-sensitive material, selective ethanol gas-sensitive element and preparation method of selective ethanol gas-sensitive material
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CN110092412A (en) * 2019-05-09 2019-08-06 上海纳米技术及应用国家工程研究中心有限公司 Preparation method for gas sensor CuO-Ag modification stannic oxide nano material and products thereof and application
CN110092412B (en) * 2019-05-09 2021-12-03 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of CuO-Ag modified tin oxide nano material for gas sensor, product and application thereof
CN110346421A (en) * 2019-06-27 2019-10-18 重庆大学 A kind of gas sensitive and its preparation method and application

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RJ01 Rejection of invention patent application after publication

Application publication date: 20151230

RJ01 Rejection of invention patent application after publication