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Thick-film type limited current hydrogen sensor and preparation method thereof

A limiting current and sensor technology, applied in the direction of instruments, scientific instruments, material analysis by electromagnetic means, etc., can solve problems such as affecting promotion and application, unstable sealing of reference electrodes, etc., to avoid dimensional changes and blockages, improve work performance, ease of use

Inactive Publication Date: 2010-01-13
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[Zheng Minhui, Chen Xiang, Acta Metall Sinica, 30(1994) B238.] used SrCeO 3 type proton conductor as the electrolyte, Ca / CaH 2 do Reference electrode, obtained a hydrogen sensor that can work continuously for 60 hours, but due to Ca / CaH 2 The existence of instability and sealing problems of the reference electrode affects its promotion and application

Method used

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  • Thick-film type limited current hydrogen sensor and preparation method thereof
  • Thick-film type limited current hydrogen sensor and preparation method thereof
  • Thick-film type limited current hydrogen sensor and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Press Sr 1.18 Ce 0.45 Zr 0.45 Y 0.10 o 3-δ and SrCe 0.95 T m 0.05 o 3-δ Weigh the corresponding reagents according to the stoichiometric ratio, and mix the raw materials, ZrO 2 Balls and absolute ethanol were mixed according to the mass ratio of 1:2:0.5, then put into a polytetrafluoroethylene ball mill jar, milled for 10 hours, and the ground slurry was naturally dried and then put into a resistance furnace. Pre-burn at ℃ for 10 hours, and then set aside after cooling down to room temperature.

[0027] SrCe 0.95 T m 0.05 o 3-δ Preparation of slurry. SrCe pre-fired at 1300°C 0.95 T m 0.05 o 3-δ The powder was mixed with terpineol containing 6%wt ethyl cellulose at a ratio of 45:55, added an appropriate amount of absolute ethanol and ball-milled on a ball mill for 3 hours, and then put into a sealed jar for later use.

[0028] Weigh about 1g of proton conductor Sr pre-fired at 1300°C 1.18 Ce 0.45 Zr 0.45 Y 0.10 o 3-δ Powder, pressed into a circle at 1...

Embodiment 2

[0032] Press Sr 1.18 Ce 0.45 Zr 0.45 Y 0.10 o 3-δ and SrCe 0.95 T m 0.05 o 3-δ Weigh the corresponding reagents according to the stoichiometric ratio, and mix the raw materials, ZrO 2 Balls and absolute ethanol were mixed according to the mass ratio of 1:2:0.5, then put into a polytetrafluoroethylene ball mill jar, milled for 10 hours, and the ground slurry was naturally dried and then put into a resistance furnace. Pre-burn at ℃ for 10 hours, and then set aside after cooling down to room temperature.

[0033] Sr 1.18 Ce 0.45 Zr 0.45 Y 0.10 o 3-δ Preparation of slurry. Precalcined Sr at 1300°C 1.18 Ce 0.45 Zr 0.45 Y 0.10 o 3-δ After the powder was mixed with terpineol containing 6%wt ethyl cellulose at a ratio of 45:55, an appropriate amount of absolute ethanol was added and ball milled on a ball mill for 3 hours, and then put into a sealed jar for later use.

[0034] Weigh about 1g of mixed conductor SrCe pre-fired at 1300°C 0.95 T m 0.05 o 3-δ Powder, p...

Embodiment 3

[0038] With the above-mentioned proton conductor BaCe 0.90 Y 0.10 o 3-δ The sheet is used as the substrate, and the surface is coated with mixed conductor SrCe by screen printing technology. 0.95 T m 0.05 o 3-δ The uniform film was dried in a vacuum oven at 105°C for 5 minutes to evaporate the solvent. Then apply a new layer of film and re-dry, and repeat this process. After repeating 10 times, take out the substrate and sinter at 1550°C for 6h. Polish both sides of the wafer clean, coat with silver paste, and bake at 800°C for 1h. A limiting current hydrogen sensor with a dense diffusion barrier layer was prepared.

[0039] The performance test of the hydrogen sensor at 750°C shows that at a voltage of 0.8V, the hydrogen concentration has a linear relationship with the limiting current (see Figure 7 ).

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Abstract

The invention relates to a thick-film type limited current hydrogen sensor and a preparation method thereof, belonging to the technical field of electrochemical gas sensors. The sensor consists of dense proton conductor slices and dense proton / electron mixed thick conductor films or dense proton / electron mixed conductor slices and dense thick conductor films. The composition of the proton conductor slices is AB(1-x)RxO(3-delta)(x is more than or equal to 0 and less than or euqal to 0.3), wherein A is Ca, Sr or Ba; B is one or more of Ce, Zr, Nb and Ti; and R is one or more of Sc, Y, La, Pr, Nd, Dy, Ho, Er, Lu, Gd and In. The composition of the proton / electron mixed conductor slices is AB(1-x)R'xO(3-delta) (x is more than or equal to 0 and less than or euqal to 0.3), wherein A is Ca, Sr or Ba; B is one or more of Ce, Zr, Nb and Ti; and R' is one or more of Sm, Eu, Tb, Yb, Tm, Mn and Ti. The preparation method of the sensor comprises the following steps: preparing two kinds of conductor powder; preparing the dense proton conductors and the dense proton / electron mixed conductor slices; preparing thick films by a screen print technology; and assembling the sensor. The sensor is suitable for the detection of hydrogen in gas.

Description

technical field [0001] The invention belongs to the technical field of electrochemical gas sensors, and in particular relates to a thick film limiting current type hydrogen sensor and a preparation method thereof. Background technique [0002] During aluminum smelting and casting, the melt reacts with water in the atmosphere to absorb hydrogen. When solidified, the dissolved hydrogen will be precipitated and cause many pores, seriously affecting the performance of the material, so it must be dehydrogenated below a certain level. In order to control the dehydrogenation process, it is required to quickly and accurately measure the hydrogen content in molten aluminum. [0003] Electrochemical sensors have the advantages of strong selectivity, fast response, and continuous online measurement. The electrochemical sensors currently used for hydrogen determination can be divided into concentration cell type and limiting current type. [0004] Iwahara et al. used SrCeO 3 , BaCeO...

Claims

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Application Information

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IPC IPC(8): G01N27/407
Inventor 周会珠王岭戴磊李跃华朱靖赵艳琴李帅
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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