CN101625335A - Thick-film type limited current hydrogen sensor and preparation method thereof - Google Patents
Thick-film type limited current hydrogen sensor and preparation method thereof Download PDFInfo
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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
The invention belongs to the electrochemical gas sensor technical field, be specifically related to a kind of thick film limit-current type hydrogen gas sensor and preparation method thereof.
Background technology
When aluminium melting and casting, the water in melt and the atmosphere reacts and inhales hydrogen.When solidifying, the hydrogen of dissolving can be separated out and be caused many pores, has a strong impact on the performance of material, and therefore necessary dehydrogenation is to certain level.For the control certain embodiments, require to measure quickly and accurately hydrogen richness in the aluminium liquid.
It is strong that electrochemical sensor has selectivity, and response is quick, and can realize the advantage of online METHOD FOR CONTINUOUS DETERMINATION.The electrochemical sensor that is used for hydrogen mensuration at present can be divided into concentration cell type and limit-current type.
Human SrCeO such as Iwahara
3, BaCeO
3And CaZrO
3The matrix proton conduction is as solid electrolyte, prepared concentration cell type hydrogen gas sensor with hydrogen or hydrated salt as contrast electrode, obtained highly stable electromotive force [Yajima N, Iwahara H, Fukatsu N, et al., Journal of Japan Institute of Light Metal, 42 (1992) 263].Zheng Minhui etc. [Zheng Minhui, Chen Xiang, Acta Metallurgica Sinica, 30 (1994) B238.] use SrCeO
3The type proton conductor is an electrolyte, Ca/CaH
2Do
Contrast electrode, but 60 hours hydrogen gas sensor of continuous working obtained, but because Ca/CaH
2The existence of contrast electrode instability and sealing problem influences its promotion and application.People such as Yajima are with the CaZr of perovskite structure
0.9In
0.1O
3Being solid electrolyte, is that contrast electrode has constituted hydrogen gas sensor with 1% hydrogen, and experimental result and Telegas method meet [K.Ktahira well in aluminum melt, H.Matsumoto, H.Iwahara, Sensors and Actuators B, 73 (2001) 130], and realized commercialization.People such as the Fray of univ cambridge uk have developed on this basis with CaZr
0.9In
0.1O
3Be solid electrolyte, Zr/ZrH
xHydrogen sensor [D P Lapham and D J Fray, Ionics, 8 (2002) 391] for contrast electrode.High, the favorable reproducibility of the stability of sensor.
Because the logarithmic relationship that is divided into of the signal of concentration cell type hydrogen gas sensor and hydrogen, therefore in whole mensuration, signal changes less, inadequately sensitivity.And that the limit-current type hydrogen sensor has is highly sensitive, do not need contrast electrode, preparation is simple, be easy to microminiaturization.At present, the limit-current type hydrogen sensor has been developed aperture diffused sensor [Noboru Taniguchi, Tomohiro Kuroha, Chiharu Nishimura.Solid State Ionics, 176 (2005) 2979].
The present invention adopts fine and close electronics/proton mixed conducting material to prepare a kind of thick-film type limited current hydrogen sensor as diffusion barrier layer.This sensor can be measured density of hydrogen in the aluminum melt, also can be used for detection and production control to density of hydrogen in the gas.
Summary of the invention
The object of the present invention is to provide a kind of new thick-film type limited current hydrogen sensor and preparation method thereof.
Technical scheme of the present invention and technical characterictic are:
The present invention is a kind of preparation method of thick-film type limited current hydrogen sensor.It is characterized in that this thick-film type limited current type hydrogen gas sensor is made up of the proton conductor of densification and fine and close proton/electron mixed conductor, its percentage by weight is: proton conductor 98～99.9%, proton/electron mixed conductor 2～0.1%, or proton/electron mixed conductor 98～99.9%, proton conductor 2～0.1%.This thick-film type limited current hydrogen sensor preparation may further comprise the steps: the preparation of proton conductor and proton/electron mixing conductor powder; The preparation of the proton/electron mixed conductor sheet of fine and close proton conductor or densification; The assembling of adopting screen printing technique to prepare corresponding thick film and sensor.
Proton conductor has perovskite structure as electrolyte, and the chemical composition of proton conductor is AB
1-xR
xO
3-δ, wherein A is Ca, Sr or Ba; B is one or more among Ce, Zr, Nb, the Ti; R is one or more among Sc, Y, La, Pr, Nd, Dy, Ho, Er, Lu, Gd, the In, and x is a molal quantity, x span: 0≤x≤0.3.
As the proton/electron mixed conductor of diffusion barrier, have the hydrogen function, the chemical composition of proton/electron mixed conductor is AB
1-xR '
xO
3-δ, wherein A is Ca, Sr or Ba; B is one or more among Ce, Zr, Nb, the Ti; R ' is one or more among Sm, Eu, Tb, Yb, Tm, Mn, the Ti, and x is a molal quantity, x span: 0≤x≤0.3.
The preparation of proton conductor powder: the proton conductor powder adopts the solid state reaction preparation.Carry out raw material by the chemical composition of proton conductor and take by weighing the acquisition batch, with batch and zirconium oxide abrasive body ball, absolute ethyl alcohol is put into the teflon ball grinder after in 1: 2: 0.5 ratio mixing of mass ratio, obtain slurry behind the wet ball grinding 10h, slurry dried naturally treat to put into the resistance kiln roasting after the ethanol volatilization, calcination atmosphere is an air atmosphere, sintering temperature is 1000～1300 ℃, cooling is cooled to normal temperature behind the roasting 10h, after roasting, add cementing agent PVB (polyvinyl butyral) 1% (percentage by weight in the powder, add), it is pressed preceding method wet ball grinding 10h once more, go out mill and dry back acquisition proton conductor powder.
The preparation of proton/electron mixing conductor powder: proton/electron mixed conductor adopts the solid state reaction preparation.Chemical composition by proton/electron mixed conductor takes by weighing raw material acquisition batch, with batch and zirconium oxide abrasive body ball, absolute ethyl alcohol is put into the teflon ball grinder after in 1: 2: 0.5 ratio mixing of mass ratio, obtain slurry behind the ball milling 10h, slurry dried naturally treat to put into the resistance kiln roasting after the ethanol volatilization, calcination atmosphere is an air atmosphere, sintering temperature is respectively at 1000-1300 ℃, cooling is cooled to normal temperature behind the roasting 10h, after roasting, add cementing agent PVB (polyvinyl butyral) 1% (percentage by weight in the powder, add), it is pressed preceding method wet ball grinding 10h once more, go out mill and dry back acquisition proton/electron mixing conductor powder.
The preparation of the proton/electron mixed conductor sheet of fine and close proton conductor or densification: proton conductor powder or proton/electron mixing conductor powder are put in the punching block, under 5MPa pressure, tentatively be compressed to the disk of diameter 15mm, further pressurization is closely knit with 300MPa pressure with sheet parison body to adopt the cold isostatic pressure machine then, obtains the proton conductor closely knit base substrate of sheet type or proton/closely knit base substrate of electron mixed conductor sheet shape.At 1550 ℃ of sintering 10h, the intensification of sintering process and rate of temperature fall are 1～3 ℃/min with the sheet shape base substrate of pressurization after closely knit.
The preparation of thick-film type sensor: adopt screen printing technique on fine and close proton conductor piece, to prepare proton/electron mixed conductor film, or on fine and close proton/electron mixed conductor sheet, prepare proton conducting membranes, film thickness is 5-30 μ m, in 1550 ℃ of sintering 10h, the intensification of sintering process and rate of temperature fall are 1～3 ℃/min then.Silver slurry is coated on two planes of the sheet shape sintered body behind the sintering, it is made behind 800 ℃ of roasting 1h have the rete limit-current type hydrogen sensor that dense diffusion barrier hinders layer again.
The principle of work of sensor: have dense diffusion barrier and hinder the thick-film type limited current sensor of layer to be composited, draw two contact conductors that are connected with external power at the outside surface of compound interface and solid electrolyte respectively by solid electrolyte (sheet or thick film) and one deck electronics/hydrogen ion mixed conductor hydrogen permeation membrane (sheet or thick film) that hydrogen ion conducts.Utilize external power that hydrogen is at the interface extracted out, and hydrogen diffuse into the interface by diffusion barrier layer under the promotion of concentration difference.When the rate of propagation of hydrogen by barrier layer became the speed limit link of whole hydrogen migration process, pump hydrogen electric current is the value of reaching the limit of just.Obviously, the size of limiting current is directly relevant with the hydrogen concentration in the environment, and this is has the survey hydrogen principle of work that dense diffusion barrier hinders the thick-film type limited current hydrogen sensor of layer.
The invention has the advantages that: sensor the two poles of the earth are in the identical atmosphere, thereby can make chip or other shape; This new limit-current type hydrogen sensor has been avoided problems such as change of pinhole type size sensor and obstruction, can improve the serviceability of sensor, and make preparation technology simple, easy to use.
Description of drawings
Fig. 1 proton conductor Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δSEM photo 1550 ℃ of sintering 10h rear surfaces
Fig. 2 hydrogen gas sensor Ag|Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δ| SrCe
0.95Tm
0.05O
3-δFilm | the synoptic diagram of Ag
Fig. 3 is at 800 ℃ of sensors A g|Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δ| SrCe
0.95Tm
0.05O
3-δFilm | the electric current-current potential characteristic curve diagram of Ag in variable concentrations hydrogen
Fig. 4 is at 800 ℃ of 0.8V polarizing voltage lower sensor Ag|Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δ| SrCe
0.95Tm
0.05O
3-δFilm | the electric current of Ag and the graph of relation of density of hydrogen
Fig. 5 hydrogen gas sensor Ag|Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δFilm | SrCe
0.95Tm
0.05O
3-δ| the synoptic diagram of Ag
Fig. 6 is at 800 ℃ of 0.8V polarizing voltage lower sensor Ag|Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δFilm | SrCe
0.95Tm
0.05O
3-δ| the electric current of Ag and the graph of relation of density of hydrogen
Fig. 7 is at 750 ℃ of 0.8V polarizing voltage lower sensor Ag|BaCe
0.90Y
0.10O
3-δ| SrCe
0.95Tm
0.05O
3-δFilm | the graph of relation of Ag electric current and density of hydrogen
Embodiment
Embodiment 1
Press Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δAnd SrCe
0.95Tm
0.05O
3-δStoichiometric proportion weighing reagent corresponding is with raw material, ZrO
2Ball, absolute ethyl alcohol are put into the teflon ball grinder after in 1: 2: 0.5 ratio mixing of mass ratio, and ball milling 10h puts into resistance furnace after the slurry that mill is good dries naturally, and air atmosphere is in 1300 ℃ of pre-burning 10h, reduce to normal temperature after, standby.
SrCe
0.95Tm
0.05O
3-δThe preparation of slurry.SrCe with 1300 ℃ of pre-burnings
0.95Tm
0.05O
3-δPowder adds an amount of absolute ethyl alcohol ball milling 3h on bowl mill with after the terpinol that contains the 6%wt ethyl cellulose mixes according to 45: 55 ratio, and the wide-necked bottle of putting into sealing then is standby.
Take by weighing about 1g the proton conductor Sr of 1300 ℃ of pre-burnings
1.18Ce
0.45Zr
0.45Y
0.10O
3-δPowder is pressed into circle in 15MPa, and the disk diameter is about 15mm.Take out circular piece, become closely knit circular piece in cold isostatic pressure machine 300MPa oil pressure, in 1550 ℃ of sintering 10h.The SEM photo of material surface as shown in Figure 1.
With above-mentioned proton conductor sheet is matrix, adopts screen printing technique to form mixed conductor SrCe relatively uniformly on its surface
0.95Tm
0.05O
3-δFilm was put in it in 105 ℃ the vacuum drying chamber dry 5 minutes, made solvent evaporates.Be coated with the new film of last layer afterwards again, dry again, so repeatedly, treat to take out substrate after the repetition 5 times, in 1550 ℃ of sintering 6h.Clean the polishing of the two sides of disk, coat the silver slurry, 800 ℃ of roasting 1h.The dense diffusion barrier that makes hinders layer limit-current type hydrogen sensor structure as shown in Figure 2.
Electric current-current potential characteristic curve under 800 ℃ of hydrogen sensor different hydro concentration is seen Fig. 3.As seen from the figure, hydrogen sensor is under probe temperature, and hydrogen concentration has significantly limiting current platform during less than 7936ppm.Limiting current and voltage that limiting current initially occurs increase with the increase of hydrogen concentration.Under 0.8V voltage, hydrogen concentration and limiting current have the linear relationship (see figure 4).
Press Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δAnd SrCe
0.95Tm
0.05O
3-δStoichiometric proportion weighing reagent corresponding is with raw material, ZrO
2Ball, absolute ethyl alcohol are put into the teflon ball grinder after in 1: 2: 0.5 ratio mixing of mass ratio, and ball milling 10h puts into resistance furnace after the slurry that mill is good dries naturally, and air atmosphere is in 1300 ℃ of pre-burning 10h, reduce to normal temperature after, standby.
Sr
1.18Ce
0.45Zr
0.45Y
0.10O
3-δThe preparation of slurry.Sr with 1300 ℃ of pre-burnings
1.18Ce
0.45Zr
0.45Y
0.10O
3-δPowder is with after the terpinol that contains the 6%wt ethyl cellulose mixes according to 45: 55 ratio, and adding an amount of absolute ethyl alcohol ball milling 3h on bowl mill, to put into the wide-necked bottle of sealing then standby.
Take by weighing the mixed conductor SrCe of 1300 ℃ of pre-burnings about 1g
0.95Tm
0.05O
3-δPowder is pressed into circle in 15MPa, and the disk diameter is about 15mm.Take out circular piece, become closely knit circular piece,, obtain fine and close mixed conductor sheet in 1550 ℃ of sintering 10h in cold isostatic pressure machine 300MPa oil pressure.
With above-mentioned mixed conductor sheet is matrix, adopts screen printing technique evenly to coat proton conductor Sr on its surface
1.18Ce
0.45Zr
0.45Y
0.10O
3-δFilm was put in it in 105 ℃ the vacuum drying chamber dry 5 minutes, made solvent evaporates.Be coated with the new film of last layer afterwards again, dry again, so repeatedly, treat to take out substrate after the repetition 10 times, in 1550 ℃ of sintering 6h.Clean the polishing of the two sides of disk, coat the silver slurry, 800 ℃ of roasting 1h obtain the thick film sensor (see figure 5).
Show that 800 ℃ of hydrogen sensor performance tests under the 0.8V polarizing voltage, hydrogen concentration and limiting current have the linear relationship (see figure 6).
With above-mentioned proton conductor BaCe
0.90Y
0.10O
3-δSheet is a matrix, adopts screen printing technique to be coated with mixed conductor SrCe on its surface
0.95Tm
0.05O
3-δUniform films, it was put in 105 ℃ the vacuum drying chamber dry 5 minutes, make solvent evaporates.Be coated with the new film of last layer afterwards again, dry again, so repeatedly, treat to take out substrate after the repetition 10 times, in 1550 ℃ of sintering 6h.Clean the polishing of the two sides of disk, coat the silver slurry, 800 ℃ of roasting 1h.Make dense diffusion barrier and hinder a layer limit-current type hydrogen sensor.
Show that 750 ℃ of hydrogen sensor performance tests under 0.8V voltage, hydrogen concentration and limiting current have the linear relationship (see figure 7).
Claims (7)
1, a kind of thick-film type limited current hydrogen sensor and preparation method thereof, it is characterized in that this thick-film type limited current hydrogen sensor is made up of the proton conductor of densification and fine and close proton/electron mixed conductor, its percentage by weight is: proton conductor 98～99.9%, proton/electron mixed conductor 2～0.1%, or proton/electron mixed conductor 98～99.9%, proton conductor 2～0.1%.This thick-film type limited current hydrogen sensor preparation may further comprise the steps: the preparation of proton conductor and proton/electron mixing conductor powder; The preparation of the proton/electron mixed conductor sheet of fine and close proton conductor and densification; The assembling of adopting screen printing technique on sheet, to prepare corresponding thick film and sensor.
2, thick-film type limited current hydrogen sensor as claimed in claim 1 and preparation method thereof, the chemical composition that it is characterized in that proton conductor is AB
1-xR
xO
3-δ, wherein A is Ca, Sr or Ba; B is one or more among Ce, Zr, Nb, the Ti; R is one or more among Sc, Y, La, Pr, Nd, Dy, Ho, Er, Lu, Gd, the In, and x is a molal quantity, its span: 0≤x≤0.3.
3, thick-film type limited current hydrogen sensor as claimed in claim 1 and preparation method thereof, the chemical composition that it is characterized in that proton/electron mixed conductor is AB
1-xR '
xO
3-δ, wherein A is Ca, Sr or Ba; B is one or more among Ce, Zr, Nb, the Ti; R ' is one or more among Sm, Eu, Tb, Yb, Tm, Mn, the Ti, and x is a molal quantity, its span: 0≤x≤0.3.
4, thick-film type limited current hydrogen sensor as claimed in claim 1 and preparation method thereof, the preparation that it is characterized in that the proton conductor powder are to adopt the solid state reaction preparation.Carry out raw material by the chemical composition of proton conductor and take by weighing the acquisition batch, with batch and zirconium oxide abrasive body ball, absolute ethyl alcohol is put into the teflon ball grinder after in 1: 2: 0.5 ratio mixing of mass ratio, obtain slurry behind the wet ball grinding 10h, slurry dried naturally treat to put into the resistance kiln roasting after the ethanol volatilization, calcination atmosphere is an air atmosphere, sintering temperature is 1000～1300 ℃, cooling is cooled to normal temperature behind the roasting 10h, after roasting, add cementing agent PVB (polyvinyl butyral) 1% (percentage by weight in the powder, add), it is pressed preceding method wet ball grinding 10h once more, dry the back and obtain the proton conductor powder.
5, thick-film type limited current hydrogen sensor as claimed in claim 1 and preparation method thereof, the preparation that it is characterized in that proton/electron mixing conductor powder are to adopt the solid state reaction preparation.Chemical composition by proton/electron mixed conductor takes by weighing raw material acquisition batch, with batch and zirconium oxide abrasive body ball, absolute ethyl alcohol is put into the teflon ball grinder after in 1: 2: 0.5 ratio mixing of mass ratio, obtain slurry behind the ball milling 10h, slurry dried naturally treat to put into the resistance kiln roasting after the ethanol volatilization, calcination atmosphere is an air atmosphere, sintering temperature is respectively at 1000-1300 ℃, cooling is cooled to normal temperature behind the roasting 10h, after roasting, add cementing agent PVB (polyvinyl butyral) 1% (percentage by weight in the powder, add), it is pressed preceding method wet ball grinding 10h once more, dry the back and obtain proton/electron mixing conductor powder.
6, thick-film type limited current hydrogen sensor as claimed in claim 1 and preparation method thereof, the preparation that it is characterized in that proton conductor or proton/electron mixed conductor sheet is that proton conductor powder or proton/electron mixing conductor powder are put in the punching block, under 5MPa pressure, tentatively be compressed to the disk of diameter 15mm, further pressurization is closely knit at 300MPa pressure with sheet parison body to adopt the cold isostatic pressure machine then, obtains the proton conductor closely knit base substrate of sheet type or proton/closely knit base substrate of electron mixed conductor sheet type.At 1550 ℃ of sintering 10h, the intensification of sintering process and rate of temperature fall are 1～3 ℃/min with the sheet shape base substrate of pressurization after closely knit.
7, thick-film type limited current hydrogen sensor as claimed in claim 1 and preparation method thereof, it is characterized in that the thick-film type transducer production method is to adopt the screen printing technique coating method, promptly adopt screen printing technique on fine and close proton conductor piece, to prepare proton/electron mixed conductor film, or on fine and close proton/electron mixed conductor sheet, prepare proton conducting membranes, film thickness is 5-30 μ m, in 1550 ℃ of sintering 10h, the intensification of sintering process and rate of temperature fall are 1～3 ℃/min then.The silver slurry is coated on two planes of the sheet shape sintered body behind the sintering, again it is made the thick-film type limited current hydrogen sensor behind 800 ℃ of roasting 1h.
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| CN112986315A (en) * | 2021-02-27 | 2021-06-18 | 深圳市博盛科电子有限公司 | Method for detecting chemical gas in environment with temperature change |
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| WO2015158272A1 (en) * | 2014-04-17 | 2015-10-22 | 武汉大学 | Method for manufacturing hydrogen gas sensor by using noble metal doped titanium dioxide nano-powder |
| CN104291813A (en) * | 2014-09-22 | 2015-01-21 | 华中科技大学 | Method for preparing and forming solid electrolyte tube for hydrogen detection |
| CN104291813B (en) * | 2014-09-22 | 2016-06-22 | 华中科技大学 | A kind of preparation surveying hydrogen solid electrolyte tube and manufacturing process |
| CN108344081A (en) * | 2017-01-24 | 2018-07-31 | 青岛海尔空调器有限总公司 | A kind of air-conditioning and safety detection method |
| CN108344081B (en) * | 2017-01-24 | 2021-01-29 | 青岛海尔空调器有限总公司 | Air conditioner and safety detection method |
| CN106872548A (en) * | 2017-03-01 | 2017-06-20 | 福州大学 | A kind of current mode NOx sensor pyrochlore solid electrolyte material and preparation method thereof |
| CN110746187A (en) * | 2019-10-24 | 2020-02-04 | 东北大学 | Potassium niobate based high-temperature proton conductor material and preparation method thereof |
| CN110746187B (en) * | 2019-10-24 | 2021-11-05 | 东北大学 | Potassium niobate based high-temperature proton conductor material and preparation method thereof |
| CN112986315A (en) * | 2021-02-27 | 2021-06-18 | 深圳市博盛科电子有限公司 | Method for detecting chemical gas in environment with temperature change |
| CN115932013A (en) * | 2023-03-10 | 2023-04-07 | 华北理工大学 | Sensor with cobalt tungstate prepared by molten salt method as sensitive electrode and manufacturing method thereof |
| CN115950940A (en) * | 2023-03-10 | 2023-04-11 | 华北理工大学 | SO with strontium titanate as sensitive electrode 2 Sensor and preparation method and application thereof |
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Application publication date: 20100113 |