CN102235992B - Gas sensor and preparation method thereof - Google Patents
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Abstract
The invention provides a gas sensor, successively comprising an insulating layer, a reference gas layer and a sensing layer from bottom to top. The gas sensor is characterized by that: the insulating layer contains alumina and glass powder, the reference gas layer contains yttrium-stabilized zirconia, alumina and glass powder, and the sensing layer contains zirconia, alumina and glass powder. Theinvention also provides a preparation method for the gas sensor, comprising the steps of superposing the insulating layer, the reference gas layer and the sensing layer from bottom to top successively for compacting and sintering. The gas sensor provided by the invention has high bonding force of each layer, so that the gas sensor has good sealing performance.
Description
Technical field
The present invention relates to a kind of gas sensor and preparation method thereof.
Background technology
Along with The development in society and economy, the pollution of atmospheric environment is more and more serious, and controlling various discharge of harmful gases becomes a social subject under discussion gradually, and wherein industrial gaseous waste and vehicle exhaust are the emphasis that people pay close attention to, and N in the monitoring emission gases
xO/C
xH and O
2Content be that people study one of maximum problem.The at present common element that is used for the monitoring emission gases mainly is automotive oxygen sensor.Gas situation after automotive oxygen sensor is used for burning feeds back to control unit of engine in real time, engine electric-controlled spraying system is then accurately controlled air-fuel ratio according to the signal that lambda sensor provides, thereby adjust the air-fuel ratio (A/F, air and quality of gasoline ratio) of combination gas near theoretical value.
For example, a kind of preparation method of plate type oxygen sensor chip is disclosed among the CN101042366A, earlier prepare sensor chip, intermediate (being the reference gas-bearing formation) and heating plate by The tape casting, wherein the base material of sensor chip, intermediate and heating plate all adopts YSZ, and insulation course adopts aluminium oxide; Before lamination hot pressing, be coated with the ceramic powder of YSZ or salic 80-99% at the perfecting of intermediate.This method can to a certain degree improve the adhesion between sensor chip, intermediate, the heating plate at the coated on both sides ceramic powder of intermediate, but each lamination adhesion does not still reach requirement, makes that the sealing of chip oxygen sensor is relatively poor.
Summary of the invention
The invention solves and heterogeneously in the preparation process that exists in the prior art make that in conjunction with difficulty each lamination adhesion of gas sensor is weak, the technical matters of sealing difference.
The invention provides a kind of gas sensor, comprise insulation course, reference gas-bearing formation and sensing layer from bottom to up successively, wherein said insulation course contains aluminium oxide and glass dust, described reference gas-bearing formation contains YSZ, aluminium oxide and glass dust, and described sensing layer contains yttrium stable zirconium oxide, aluminium oxide and glass dust.
The present invention also provides a kind of preparation method of gas sensor, comprises that sintering obtains described gas sensor with the stack compacting successively from bottom to up of insulation course, reference gas-bearing formation and sensing layer.
Gas sensor provided by the invention, composition by suitable adjusting insulation course, reference gas-bearing formation and sensing layer, in reference gas-bearing formation and sensing layer, add aluminium oxide, and in three laminations, all add glass dust, thereby improve the heterogeneous combination degree of reference gas substrate, insulation course and sensing layer, improve the adhesion between insulation course, reference gas-bearing formation and the sensing layer, thereby guarantee that gas sensor has better seal.From the test result of table 1 as can be seen, before and after the gas sensor test provided by the invention the air pressure pressure change less than 0.05MPa, anti-pulling intensity reach 1.7MPa and more than.
Embodiment
The invention provides a kind of gas sensor, comprise insulation course, reference gas-bearing formation and sensing layer from bottom to up successively, it is characterized in that, described insulation course contains aluminium oxide and glass dust, described reference gas-bearing formation contains yttrium stable zirconium oxide, aluminium oxide and glass dust, and described sensing layer contains yttrium stable zirconium oxide, aluminium oxide and glass dust.
The present inventor finds by a large amount of experiments: contain aluminium oxide in the reference gas-bearing formation, can improve the adhesion of reference gas-bearing formation and insulation course; Similarly, also contain aluminium oxide in the sensing layer, the assurance sensing layer is combined with the part homogeneity of reference gas-bearing formation, thereby improves adhesion; In addition, all contain glass dust in insulation course of the present invention, reference gas-bearing formation and the sensing layer, make on the one hand the material part homogeneity of insulation course, reference gas-bearing formation and sensing layer; Glass dust can be used for strengthen the combination degree of aluminium oxide and YSZ on the other hand, specifically comprises in (1) insulation course in the aluminium oxide and reference gas-bearing formation in YSZ and aluminium oxide in YSZ, (2) reference gas-bearing formation, (3) reference gas-bearing formation among the YSZ and sensing layer in aluminium oxide, (4) reference gas-bearing formation the combination between the aluminium oxide and YSZ in YSZ in the aluminium oxide and sensing layer and (5) sensing layer.Therefore, the insulation course of gas sensor of the present invention, reference gas-bearing formation and sensing layer have higher adhesion, thereby make gas sensor have better seal, prolong the serviceable life of gas sensor of the present invention.
In addition, the present inventor also finds, contains glass dust in the sensing layer and also has following advantage: (a) glass dust can suppress too growing up of zirconia crystal grain in the sensing layer, makes the electrical property of YSZ more stable; (b) glass dust can reduce the intercrystalline grain boundary resistance of zirconia, especially reduces the boundary resistance value between zirconia and the electrode, thereby reduces voltage loss, strengthens voltage signal.
The content of aluminium oxide is 92-98wt% in the described insulation course, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 85-95wt% in the described reference gas-bearing formation, and the content of aluminium oxide is 2-8wt%, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 80-95wt% in the described sensing layer, and the content of aluminium oxide is 2-15wt%, and the content of glass dust is 2-8wt%.
All contain glass dust in insulation course of the present invention, reference gas-bearing formation and the sensing layer, described glass dust is to well known to a person skilled in the art the class material with glassy phase that is formed by multiple inorganic oxide pre-burning.Under the preferable case, contain 5-40wt% monox, 30-60wt% boron oxide, 10-35wt% bismuth oxide, 2-10wt% Lithia, 5-20wt% strontium oxide strontia, 2-20wt% massicot, 5-25wt% aluminium oxide and 2-8wt% zirconia in the glass dust that the present invention adopts.
In the described glass dust, monox, boron oxide and bismuth oxide are the glass principal phase, are conducive to interpenetrating of zirconia and alumina layer, thereby strengthen the combination degree of aluminium oxide and YSZ; Lithia and strontium oxide strontia can improve the glass high-temperature conductivity; Massicot is used for expansion vitrification point, the chemical stability of reinforcing glass body; Intensity when aluminium oxide is used for improving the glass dust sintering also helps crystallization in addition; Zirconia helps crystallization, the intensity of reinforcing glass phase and thermal shock resistance, and effectively reduce the thermal expansivity of glassy phase.
As a kind of preferred implementation of the present invention, can also contain the adjustment body of 2-10wt% in the described glass dust, described adjustment body is selected from nickel oxide, scandium oxide or europium oxide.Described glass dust is adjusted body, can form the mixed transition phase with boundary electrode by YSZ in sensing layer, reduces boundary resistance and sensor internal resistance.
Among the present invention, be provided with well heater in the described gas sensor insulation course, make sensing layer reach working temperature for sensing layer is heated.Described insulation course below is provided with the well heater substrate.Two surfaces up and down of sensing layer are respectively equipped with induction electrode, and respectively as test electrode and contrast electrode, it is poor to be used for test sensing layer both sides gas concentration.
Described well heater substrate is zirconia curtain coating substrate, preferably adopts 5% mole of YSZ curtain coating substrate.Described YSZ curtain coating substrate can be purchased or make by oneself, and wherein self-control method prepares the method for ceramic substrate for the known The tape casting of those skilled in the art.
Among the present invention, the thickness of described insulation course is 30-60 μ m, and the reference thickness of gas is 300-600 μ m, and the thickness of dielectric substrate is 300-500 μ m.Under the preferable case, the thickness of insulation course is 40-50 μ m, and the reference thickness of gas is 400-600 μ m, the thickness 400-500 μ m of dielectric substrate.
The present invention also provides the preparation method of described gas sensor, comprises that sintering obtains described gas sensor with the stack compacting successively from bottom to up of insulation course, reference gas-bearing formation and sensing layer.
Wherein, prepare the method for printing screen that the method for insulation course can adopt those skilled in the art to use always, specifically may further comprise the steps: on the well heater substrate, print insulation course slurry, electrode slurry, insulation course slurry successively, oven dry can obtain being attached to the on-chip insulation course of well heater, is designated as first lamella.Among the present invention, described insulation course slurry is the potpourri that contains insulation course powder material and insulation course organic carrier, and wherein insulation course powder material contains aluminium oxide and glass dust.
Contain organic solvent and organic resin in the described insulation course organic carrier.Various components all adopt the various components that those skilled in the art use always in the described insulation course organic carrier, for example organic solvent is selected one or more in dibutyl phthalate and/or the cyclohexanone terpinol for use, and organic resin adopts ethyl cellulose and/or polyvinyl butyral.Insulation course powder material with 100 weight portions is benchmark, and the consumption of organic solvent is the 10-35 weight portion, and the consumption of organic resin is the 5-15 weight portion.
The method for preparing the reference gas-bearing formation is conventionally known to one of skill in the art, for example directly adopts dry-pressing or the mode of the reference gas-bearing formation slurry of filming, and drying and moulding can obtain reference gas-bearing formation of the present invention then, is designated as second lamella.Among the present invention, described reference gas-bearing formation slurry is the potpourri that contains reference gas-bearing formation powder material and reference gas-bearing formation organic carrier, and wherein reference gas-bearing formation powder material contains yttrium stable zirconium oxide, aluminium oxide and glass dust.Described reference gas-bearing formation organic carrier is the organic ink system for the preparation of the YSZ cast sheet common to those skilled in the art, does not give unnecessary details herein.Reference gas-bearing formation powder material with 100 weight portions is benchmark, and the consumption of reference gas-bearing formation organic carrier is the 20-60 weight portion.
Prepare described sensing layer method, generally speaking, comprising: first curtain coating sensing layer slurry obtains the sensing layer substrate, distinguishes electrode coated slurry by silk-screen printing technique in sensing layer substrate upper and lower surface then, oven dry at last can obtain described sensing layer, is designated as the 3rd lamella.Among the present invention, described sensing layer slurry is the potpourri that contains sensing layer powder material and sensing layer organic carrier, and wherein sensing layer powder material contains yttrium stable zirconium oxide, aluminium oxide and glass dust.Described sensing layer organic carrier is the organic ink system for the preparation of the YSZ cast sheet common to those skilled in the art, does not give unnecessary details herein.Sensing layer powder material with 100 weight portions is benchmark, and the consumption of sensing layer organic carrier is the 20-60 weight portion.
Among the present invention, the content of aluminium oxide is 92-98wt% in the described insulation course powder material, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 85-95wt% in the described reference gas-bearing formation powder material, and the content of aluminium oxide is 2-8wt%, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 80-95wt% in the described sensing layer powder material, and the content of aluminium oxide is 2-15wt%, and the content of glass dust is 2-8wt%.
Among the preparation method among the present invention, the electrode slurry that the electrode slurry that adopts is used always for those skilled in the art is as pure palladium, gold, platinum slurry or palladium, gold, platinum alloy slurry.Can also contain in terpinol, olein, the castor oil one or more in the described electrode slurry.
Among the present invention, combination degree when burning altogether for improving insulation course, reference gas-bearing formation and sensing layer, thereby improve sealing and the thermal shock resistance of gas sensor, under the preferable case, adopt identical organic carrier system in the insulation course organic carrier that adopts respectively when preparing described insulation course, reference gas-bearing formation, sensing layer, reference gas-bearing formation organic carrier and the sensing layer organic carrier.
According to preparation method provided by the invention, first lamella, second lamella and the 3rd lamella of above-mentioned preparation are superposeed successively by from bottom to up order, keep the insulation course of first lamella up, can obtain gas sensor of the present invention by compacting, sintering then.The condition of compacting comprises: pressure is 30-250MPa, and the time is 10s-30min; The condition of sintering comprises: temperature is 1300-1650 ℃, and the time is 0.5-4 hour.
Below in conjunction with embodiment gas sensor of the present invention and preparation method thereof is described further.The raw material that adopts in embodiment and the Comparative Examples all is available commercially.
Embodiment 1
(1) raw material preparation:
Glass dust is formed: 20wt% monox, 40wt% boron oxide, 15wt% bismuth oxide, 5wt% Lithia, 5wt% strontium oxide strontia, 2wt% massicot, 5wt% aluminium oxide, 2wt% zirconia, 2wt% nickel oxide, 2wt% scandium oxide, 2wt% europium oxide.
The insulation course slurry: 96 weight portion aluminium oxide, 4 weight portion glass dust, organic carrier be totally 40 weight portions: wherein cyclohexanone terpinol 30 weight portions, ethyl cellulose 10 weight portions.
Reference gas-bearing formation slurry: 90 weight portion yttrium stable zirconium oxides, 5 weight portion aluminium oxide, 5 weight portion glass dust, organic carrier 40 weight portions.
Sensing layer slurry: 92 weight portion yttrium stable zirconium oxides, 5 weight portion aluminium oxide, 3 weight portion glass dust, organic carrier 40 weight portions.
(2) be coated with insulating layer coating slurry, platinum electrode and insulation course slurry successively on a surface of zirconia cast sheet, drying obtains being attached to the on-chip insulation course of well heater, is designated as first lamella.
(3) dry-pressing reference gas-bearing formation slurry, drying and moulding obtains the reference gas-bearing formation, is designated as second lamella.
(4) curtain coating sensing layer slurry, preparation sensing layer substrate; At sensing layer substrate two sides serigraphy platinum electrode, obtain sensing layer after the drying, be designated as the 3rd lamella.
The insulation course of (5) first lamellas up, according to from bottom to up order first lamella, second lamella and the 3rd lamella are superposeed successively, under 50 ℃ with the 110MPa system of defeating 20 minutes, 1350 ℃ of sintering 3h then, obtain the gas sensor of present embodiment, be designated as A1.
Embodiment 2
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), the insulation course slurry: 92 weight portion aluminium oxide, 8 weight portion glass dust, organic carrier be totally 40 weight portions: wherein cyclohexanone terpinol 25 weight portions, ethyl cellulose 15 weight portions;
Reference gas-bearing formation slurry: 90 weight portion yttrium stable zirconium oxides, 4 weight portion aluminium oxide, 6 weight portion glass dust, organic carrier 40 weight portions.
Sensing layer slurry: 92 weight portion yttrium stable zirconium oxides, 4 weight portion aluminium oxide, 4 weight portion glass dust, organic carrier 40 weight portions.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as A2.
Embodiment 3
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), in the insulation course slurry: the insulation course slurry: 98 weight portion aluminium oxide, 2 weight portion glass dust, organic carrier be totally 40 weight portions: wherein cyclohexanone terpinol 20 weight portions, ethyl cellulose 20 weight portions;
Reference gas-bearing formation slurry: 90 weight portion yttrium stable zirconium oxides, 8 weight portion aluminium oxide, 2 weight portion glass dust, organic carrier 40 weight portions.
Sensing layer slurry: 85 weight portion yttrium stable zirconium oxides, 10 weight portion aluminium oxide, 5 weight portion glass dust, organic carrier 40 weight portions.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as A3.
Embodiment 4
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), glass dust is formed: 25wt% monox, 40wt% boron oxide, 15wt% bismuth oxide, 5wt% Lithia, 5wt% strontium oxide strontia, 3wt% massicot, 5wt% aluminium oxide, 2wt% zirconia.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as A4.
Embodiment 5
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), glass dust is formed: 25wt% monox, 25wt% boron oxide, 15wt% bismuth oxide, 5wt% Lithia, 10wt% strontium oxide strontia, 5wt% massicot, 10wt% aluminium oxide, 5wt% zirconia.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as A5.
Comparative Examples 1
Adopt 101042366A embodiment 1 disclosed method to prepare the gas sensor of this Comparative Examples, be designated as D1.
Comparative Examples 2
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), the insulation course slurry: 100 weight portion aluminium oxide, organic carrier be totally 40 weight portions: wherein cyclohexanone terpinol 30 weight portions, ethyl cellulose 10 weight portions.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as D2.
Comparative Examples 3
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), reference gas-bearing formation slurry: 90 weight portion yttrium stable zirconium oxides, 10 weight portion aluminium oxide, organic carrier 40 weight portions.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as D3.
Comparative Examples 4
Adopt the method identical with embodiment 1 to prepare the gas sensor of present embodiment, difference is:
In the step (1), sensing layer slurry: 100 weight portion yttrium stable zirconium oxides, organic carrier 40 weight portions.
By above-mentioned steps, obtain the gas sensor of present embodiment, be designated as D4.
Performance test:
1, performing leak test:
Gas sensor A1-A5 and D1-D4 are poured P (0)=1MPa gas, the gaseous tension P (3min) behind employing air-leakage detector XT070050 (the brilliant electronic instrument in Tianjin, Shenzhen company limited) the test duration 3min in gas sensor A1-A5 and the D1-D4.Test result is as shown in table 1.
2, adhesion test:
Employing patches pulling capacity tester 16 (Shanghai turns round and look at and steps on Industrial Co., Ltd.) gas sensor A1-A5 and D1-D4 is applied initial pull strength L (0)=1MPa, increase 0.1MPa every 10s, when occurring obviously peeling off to the gas sensor structures of samples, record anti-pulling intensity L (t) at this moment, test result is as shown in table 1.
Table 1
| Sample | P(0)/MPa | P(3min)/MPa | L(0)/MPa | L(t)/MPa |
| A1 | 1 | 0.9998 | 1 | 2.3 |
| A2 | 1 | 0.9995 | 1 | 1.9 |
| A3 | 1 | 0.9925 | 1 | 1.7 |
| A4 | 1 | 0.9756 | 1 | 1.8 |
| A5 | 1 | 0.9520 | 1 | 1.7 |
| D1 | 1 | 0.6255 | 1 | 1.1 |
| D2 | 1 | 0.7055 | 1 | 1.2 |
| D3 | 1 | 0.8174 | 1 | 1.3 |
| D4 | 1 | 0.4257 | 1 | 1.3 |
From the test result of last table 2 as can be seen, gas pressure intensity changes less than 0.05MPa before and after the gas sensor test of the present invention, is starkly lower than the Comparative Examples test result, illustrates that the gas sensor that provides of the present invention has better seal; And the anti-pulling intensity of gas sensor of the present invention reach 1.7MPa and more than, illustrate between each layer of gas sensor of the present invention to have adhesion preferably.
Claims (8)
1. gas sensor, comprise insulation course, reference gas-bearing formation and sensing layer from bottom to up successively, it is characterized in that, described insulation course contains aluminium oxide and glass dust, described reference gas-bearing formation contains yttrium stable zirconium oxide, aluminium oxide and glass dust, and described sensing layer contains yttrium stable zirconium oxide, aluminium oxide and glass dust;
Contain 5-40wt% monox, 30-60wt% boron oxide, 10-35wt% bismuth oxide, 2-10wt% Lithia, 5-20wt% strontium oxide strontia, 2-20wt% massicot, 5-25wt% aluminium oxide and 2-8wt% zirconia in the described glass dust;
The glass dust that also contains 2-10wt% in the described glass dust is adjusted body, and described glass dust is adjusted body and is selected from nickel oxide, scandium oxide or europium oxide.
2. gas sensor according to claim 1 is characterized in that, the content of aluminium oxide is 92-98wt% in the described insulation course, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 85-95wt% in the described reference gas-bearing formation, and the content of aluminium oxide is 2-8wt%, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 80-95wt% in the described sensing layer, and the content of aluminium oxide is 2-15wt%, and the content of glass dust is 2-8wt%.
3. gas sensor according to claim 1 and 2 is characterized in that, is provided with well heater in the insulation course, and the insulation course below is provided with the well heater substrate, and two surfaces up and down of sensing layer are respectively equipped with test electrode and contrast electrode.
4. gas sensor according to claim 1 is characterized in that, the thickness of insulation course is 30-60 μ m, and the reference thickness of gas is 300-600 μ m, and the thickness of sensing layer is 300-500 μ m.
5. the preparation method of the described gas sensor of claim 1 comprises that sintering obtains described gas sensor with the stack compacting successively from bottom to up of insulation course, reference gas-bearing formation and sensing layer.
6. method according to claim 5 is characterized in that, the method for preparing insulation course is included in and is coated with insulating layer coating slurry, electrode slurry, insulation course slurry on the well heater substrate successively, and oven dry can obtain described insulation course at the well heater substrate surface; Described insulation course slurry is the potpourri that contains insulation course powder material and insulation course organic carrier, and described insulation course powder material contains aluminium oxide and glass dust;
The method for preparing the reference gas-bearing formation comprises dry-pressing or the reference gas-bearing formation slurry of filming, and moulding obtains described reference gas-bearing formation; Described reference gas-bearing formation slurry is the potpourri that contains reference gas-bearing formation powder material and reference gas-bearing formation organic carrier, and described reference gas-bearing formation powder material contains yttrium stable zirconium oxide, aluminium oxide and glass dust;
The method for preparing described sensing layer comprises that first curtain coating sensing layer slurry obtains the sensing layer substrate, and at the upper and lower surface of the sensing layer substrate slurry that prints electrode respectively, oven dry can obtain described sensing layer then; Described sensing layer slurry is the potpourri that contains sensing layer powder material and sensing layer organic carrier, and sensing layer powder material contains yttrium stable zirconium oxide, aluminium oxide and glass dust.
7. method according to claim 6 is characterized in that, the content of aluminium oxide is 92-98wt% in the described insulation course powder material, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 85-95wt% in the described reference gas-bearing formation powder material, and the content of aluminium oxide is 2-8wt%, and the content of glass dust is 2-8wt%; The content of yttrium stable zirconium oxide is 80-95wt% in the described sensing layer powder material, and the content of aluminium oxide is 2-15wt%, and the content of glass dust is 2-8wt%.
8. method according to claim 5 is characterized in that, the condition of described compacting comprises: pressure is 30-250MPa, and the time is 10s-30min; The condition of sintering comprises: temperature is 1300-1650 ℃, and the time is 0.5-4 hour.
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| CN102910903B (en) * | 2012-11-08 | 2015-03-25 | 中国科学院上海硅酸盐研究所 | Low-temperature cofiring method of zirconia-based sensor |
| CN106882921B (en) * | 2015-12-16 | 2019-09-06 | 辽宁省轻工科学研究院有限公司 | A kind of seal, sealing materials and preparation method thereof of resistance to 750 DEG C of high temperature |
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| US7211180B2 (en) * | 2003-02-10 | 2007-05-01 | Robert Bosch Corporation | Contamination-resistant gas sensor element |
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