CN104535117B - Compound sensor and preparation method thereof - Google Patents
Compound sensor and preparation method thereof Download PDFInfo
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- CN104535117B CN104535117B CN201510045184.8A CN201510045184A CN104535117B CN 104535117 B CN104535117 B CN 104535117B CN 201510045184 A CN201510045184 A CN 201510045184A CN 104535117 B CN104535117 B CN 104535117B
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Abstract
The invention relates to a compound sensor and a preparation method thereof. The compound sensor comprises a Gd2Zr2O7 transparent ceramic base body and a compound layer, wherein the compound layer coats the Gd2Zr2O7 transparent ceramic base body and comprises Gd2Zr2O7 and Pt. The compound sensor provided by the invention has great practical value in radiation intensity detection and an environment gas.
Description
Technical field
The invention discloses a kind of compound sensor technology of preparing, belong to radiant intensity detection and the detection of environmental gas
Field.
Background technology
Need radiant intensity etc. to be detected in addition it is also necessary to detect to the gas in environment in some radiation environments,
The concentration of oxygen in irradiation intensity and gas can be detected if there are a kind of portable sensor simultaneously, sensing can be substantially reduced
The volume of device.It is therefore contemplated that being capable of the compound sensor that radiant intensity and environmental gas detect will have pole
Big practical value.
The general sensor using conductive material preparation with environmental gas detecting function, but, general conductive material
If metal and alloy-based semiconductor equalizing are opaque material, transparent conductive material refers to: (1) to visible ray (λ=380～
Light transmission 780nm) is high；(2) electric (ion) conductance is high.Exactly it is seen that the mean transmissivity tavg > 80% of light, electric
Resistance rate is 10-3ω·cm.The transparent band gap width meaning that material big (eg > 3ev) and free electron is few；On the other hand,
Opaque more than the high material of electrical conductivity and often free electron.The material that only can simultaneously meet both conditions is only possible to use
To prepare nesa coating.But if this problem can be avoided using the material of diversion, realizing diversion
The light of required specific band can be passed through simultaneously.
At present, also there is no the report with regard to above-mentioned compound sensor in prior art, more do not comprise nesa coating
Compound sensor.
Content of the invention
It is contemplated that overcome the functional limitation of existing sensor, the invention provides one kind is capable of radiant intensity
And the compound sensor of environmental gas detection and preparation method thereof.
The invention provides a kind of compound sensor, described compound sensor includes gd2zr2o7Crystalline ceramics matrix and
It is coated on gd2zr2o7On crystalline ceramics matrix and form include gd2zr2o7Composite bed with pt.
It is preferred that gd2zr2o7The thickness of crystalline ceramics matrix is 0.5 2mm.
It is preferred that gd in composite bed2zr2o7Mass ratio with pt is (90 99): (1 10), and the thickness of composite bed is
0.01—0.06mm.
It is preferred that gd2zr2o7Doped with rare earth element, rare earth element include tb, pr, ce, nd, tm, sm, eu, tb, dy,
At least one in ho, yb.
Also, present invention also offers a kind of preparation method of above-mentioned compound sensor, comprising:
1) prepare gd2zr2o7Ceramic powder；
2) first adopt step 1) gd for preparing2zr2o7Ceramic powder prepares biscuit of ceramics, then by biscuit of ceramics successively warp
Biscuiting and sintering, obtain gd2zr2o7Crystalline ceramics matrix；
3) by step 1) gd for preparing2zr2o7Ceramic powder and pt are scattered in organic solvent, are answered after uniformly mixing
Close layer slurry；
4) by step 3) the composite bed slurry prepared is coated on step 2) gd for preparing2zr2o7Crystalline ceramics matrix, and warp
It is dried, sinters, obtain described compound sensor.
It is preferred that gd2zr2o7Ceramic powder is doped with rare earth element.
It is preferred that step 2) in, biscuiting temperature is 800-1000 DEG C, and the time is 1-3 hour；Sintering temperature be 1750 DEG C-
1950 DEG C, the time is 2-15 hour.
It is preferred that step 3) in, than for 1:0.2 2, organic solvent includes Oleum Pini for the weight of described pt and organic solvent
Alcohol, ethyl cellulose or pvb, dibutyl phthalate, weight is than for terpineol: ethyl cellulose or pvb: phthalic acid
Dibutyl ester=1:0.03-0.2:0.03-0.2.
It is preferred that step 4) in, 75 95 DEG C of baking temperature, drying time is 12 24 hours；Sintering temperature 1350
DEG C 1600 DEG C, temperature retention time 14 hours.
Beneficial effects of the present invention:
By the technical scheme in the application, the detection function of sensor is expanded further, and type is enriched further.This
The compound sensor of bright preparation, in terms of gas detecting, has a certain degree of performance boost with respect to existing sensor.Additionally,
Gd in compound sensor in the application2zr2o7Doped with rare earth element, thus the detection function of radiant intensity can be provided simultaneously with.
Compound sensor in the application detects in radiant intensity and environmental gas will produce great practical value.
Brief description
The photo of the compound sensor that Fig. 1 is prepared for the present invention；
The x-ray of the compound sensor that Fig. 2 is prepared for the present invention excites lower luminescent spectrum.
Specific embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment it should be appreciated that accompanying drawing and following embodiment
It is merely to illustrate the present invention, and the unrestricted present invention.
The invention discloses a kind of compound sensor technology of preparing, it is mainly used in radiating by force in the severe rugged environment have radiation
Degree detection and the detection of environmental gas.Comprising: the technology of preparing of transparent ion conductive material, electrode fabrication, it is combined
Sensor technology of preparing.
Methods described includes:
A () prepares rear-earth-doped gd2zr2o7 ceramic powder using wet chemical method；
B ceramic powder prepared by step (a) is prepared biscuit of ceramics by ()；
C biscuit of ceramics biscuiting in atmosphere that step (b) is prepared by ()；
Biscuit of ceramics after d biscuiting that step (c) is obtained by () is sintered；
E the dispersion of the mixture of gd2zr2o7 ceramic powder and pt is prepared slurry by () in organic solvent, described pt with have
The weight of machine solvent is than for 1:0.2～2；
F () covers the mixture paste that step (e) obtains on gd2zr2o7 ceramic matrix surface；
G oxygen sensor chip prepared by step (f) is dried by ()；
H dried oxygen sensor chip is sintered by ().
Described rear-earth-doped gd2zr2o7Pottery, described rare earth doping elements include tb, pr, ce, nd, tm, sm, eu,
tb、dy、ho、yb；The biscuiting temperature of pottery is 900 DEG C, 2 hours；The sintering temperature of pottery is 1750 DEG C～1950 DEG C, 2～15
Hour.
Described gd2zr2o7The metallization material of ceramic base oxygen sensor is pt.
In step (e), organic solvent selects the mixing of terpineol, ethyl cellulose or pvb, dibutyl phthalate
Thing, weight is than for terpineol: ethyl cellulose or pvb: dibutyl phthalate=1:0.03～0.2:0.03～0.2.
In step (e), described pt and with the weight of organic solvent than for 1:0.2～2.
In step (f), described covering method includes silk screen printing or spraying, coating, dipping.
The described drying of step (g) is 75～95 DEG C of baking temperature, and drying time is 12～24 hours.
It is sintered to 1350 DEG C～1600 DEG C of sintering temperature, temperature retention time 1～4 hour described in step (h).
Compound sensor has response firstly the need of to irradiation intensity, and usual rare earth doping transparent material can realize this mesh
, but most transparent material does not have ionic conductivity.This problem can be avoided using the material of diversion,
Realizing while diversion is sub-, passing through the light of required specific band.The application that this patent comprises needs conductive (from
Son) while, the light of required specific band can be passed through.This patent proposes using rear-earth-doped gd2zr2o7Pottery.?
gd2zr2o7Ceramic matrix surface-coated electrode material, can be prepared into gas sensor.Including the detection to oxygen.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this
Some nonessential improvement that bright the above is made and adjustment belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only one of OK range example, and that is, those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Tb:gd2zr2o7The preparation of electrically conducting transparent ceramic base compound sensor
(1) the deionized water zrocl for 0.4mol/l for the compound concentration respectively first2Solution and concentration are 0.2mol/l's
Gadolinium trinitrate solution, concentration are the tb (no of 0.002mol/l3)3Solution.Measure the zrocl preparing2Solution, gd (no3)3Solution,
tb(no3)3Solution, and adjust ph value to 7 with ammonia, be sufficiently stirred for half an hour and under the conditions of 100 DEG C heating 24h obtain white
Precipitation；
(2) by white precipitate elder generation deionized water cyclic washing sucking filtration, till no cl- in the white precipitate, finally
With absolute ethanol washing 2 times and sucking filtration, this purpose is the reunion reducing between powder body；
(3) white precipitate after washing is calcined 2h at 1000 DEG C, obtain tb:gd2zr2o7Ceramic powder；
(4) by the tb:gd obtaining2zr2o7Ceramic powder obtains through dry-pressing (pressure 20mpa), isostatic pressed (200mpa) molding
To gd2zr2o7 biscuit of ceramics；
(5) by the tb:gd obtaining2zr2o7Biscuit of ceramics through biscuiting (900 DEG C of -2h of temperature), to remove wherein in molding
During introduce organic impurities；
(6) will be through biscuiting tb:gd2zr2o7Biscuit of ceramics, is sintered burning in vacuum drying oven (vacuum: < 10-3pa)
1830 DEG C of -10h of junction temperature；
(7) by tb:gd2zr2o7Ceramic powder and pt mixture dispersion prepare slurry in organic solvent, described pt and
With the weight of organic solvent than for 1:0.2～2；
(8) mixture paste that step (7) obtains is covered in tb:gd2zr2o7Ceramic matrix surface；
(9) oxygen sensor chip prepared by step (8) is dried；75～95 DEG C of baking temperature, drying time is 12～24
Hour；
(10) dried oxygen sensor chip is sintered.Metallization is sintered to 1350 DEG C～1600 DEG C of sintering temperature, protects
Warm 1～4 hour time；
The tb:gd obtaining2zr2o7Crystalline ceramics base compound sensor is as shown in Figure 1；
X-ray excite under luminescent spectrum as shown in Figure 2；
Fig. 1 is surface-coated gd2zr2o7With the gd after pt electrode2zr2o7Crystalline ceramics compound sensor chip；
Fig. 2 is the tb:gd being excited with x-ray2zr2o7The emission spectra of crystalline ceramics.
Claims (9)
1. a kind of compound sensor is it is characterised in that described compound sensor includes gd2zr2o7Crystalline ceramics matrix and painting
It is overlying on gd2zr2o7On crystalline ceramics matrix and form include gd2zr2o7Composite bed with pt.
2. compound sensor according to claim 1 is it is characterised in that gd2zr2o7The thickness of crystalline ceramics matrix is
0.5—2mm.
3. compound sensor according to claim 1 and 2 is it is characterised in that gd in composite bed2zr2o7Mass ratio with pt
For (90 99): (1 10), the thickness of composite bed is 0.01 0.06 mm.
4. compound sensor according to claim 1 and 2 is it is characterised in that gd2zr2o7Doped with rare earth element, rare earth
Element includes at least one in tb, pr, ce, nd, tm, sm, eu, tb, dy, ho, yb.
5. in a kind of claim 1-4 arbitrary described compound sensor preparation method it is characterised in that include:
1) prepare gd2zr2o7Ceramic powder；
2) first adopt the gd of step 1) preparation2zr2o7Ceramic powder prepares biscuit of ceramics, then by biscuit of ceramics successively through biscuiting,
And sintering, obtain gd2zr2o7Crystalline ceramics matrix；
3) gd prepared by step 1)2zr2o7Ceramic powder and pt are scattered in organic solvent, obtain composite bed after uniformly mixing
Slurry；
4) composite bed slurry prepared by step 3) is coated on step 2) gd for preparing2zr2o7Crystalline ceramics matrix, and drying,
Sintering, obtains described compound sensor.
6. preparation method according to claim 5 is it is characterised in that gd2zr2o7Ceramic powder is doped with rare earth element.
7. the preparation method according to claim 5 or 6 is it is characterised in that step 2) in, biscuiting temperature is 800-1000
DEG C, the time is 1-3 hour；Sintering temperature is 1750 DEG C -1950 DEG C, and the time is 2-15 hour.
8. the preparation method according to claim 5 or 6 is it is characterised in that in step 3), the weight of described pt and organic solvent
Amount ratio is 1:0.2 2, and organic solvent includes terpineol, ethyl cellulose or pvb, dibutyl phthalate, and weight ratio is
Terpineol: ethyl cellulose or pvb: dibutyl phthalate=1:0.03-0.2:0.03-0.2.
9. the preparation method according to claim 5 or 6 is it is characterised in that in step 4), and 75 95 DEG C of baking temperature is done
The dry time is 12 24 hours；1350 DEG C 1600 DEG C of sintering temperature, temperature retention time 14 hours.
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| CN201510045184.8A CN104535117B (en) | 2015-01-29 | 2015-01-29 | Compound sensor and preparation method thereof |
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|---|---|---|---|
| CN201510045184.8A CN104535117B (en) | 2015-01-29 | 2015-01-29 | Compound sensor and preparation method thereof |
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| CN104535117B true CN104535117B (en) | 2017-01-18 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5686347A (en) * | 1979-12-14 | 1981-07-14 | Matsushita Electric Ind Co Ltd | Sensor for oxygen gas |
| CN1289439C (en) * | 2004-08-04 | 2006-12-13 | 中国科学院上海硅酸盐研究所 | Lanthanum hafnate base transparent ceramics and its preparing method |
| CN101465172A (en) * | 2008-12-31 | 2009-06-24 | 中国科学院上海硅酸盐研究所 | Transparent conductive film with compound structure and preparation method thereof |
| CN103755390A (en) * | 2014-01-20 | 2014-04-30 | 中国科学院上海硅酸盐研究所 | Method for improving metallization intensity of zirconia ceramics of oxygen sensor |
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