CN102636527A - Inlaid plate-shaped oxygen sensor and preparation method thereof - Google Patents
Inlaid plate-shaped oxygen sensor and preparation method thereof Download PDFInfo
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- CN102636527A CN102636527A CN2012101193712A CN201210119371A CN102636527A CN 102636527 A CN102636527 A CN 102636527A CN 2012101193712 A CN2012101193712 A CN 2012101193712A CN 201210119371 A CN201210119371 A CN 201210119371A CN 102636527 A CN102636527 A CN 102636527A
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Abstract
The invention relates to the technical field of a zirconium dioxide oxygen sensor for an automobile electric injection engine, in particular to an inlaid plate-shaped oxygen sensor and a preparation method thereof. The inlaid plate-shaped oxygen sensor comprises a ceramic heater, a zirconia sensitive element, a glass glaze sealing layer, a heating circuit, a reference gas channel, an alumina base body and a groove, wherein the zirconia sensitive element is arranged in the ceramic heater; the ceramic heater is connected with the zirconia sensitive element through the glass glaze sealing layer; the ceramic heater consists of the alumina base body and the groove; the groove is arranged on the upper surface of the alumina base body, and the heating circuit is arranged on the lower surface; and the reference gas channel is arranged between the zirconia sensitive element and the groove. The inlaid plate-shaped oxygen sensor provided by the invention improves the high-temperature insulation performance of the product, has fast response to electric signal, reduces the energy consumption and production cost, has long service life and is easy to popularize.
Description
Technical field
The present invention relates to the technical field of a kind of automotive electric injection engine, especially a kind of inserted tabular lambda sensor and preparation method thereof with zirconia oxygen.
Background technology
Phase automobile industry development is swift and violent, and exhaust emission standard constantly improves, and the requirement of oxygen sensor in use for car is also improved constantly.At present domestic what generally adopt is the tubular type zirconia oxygen, uses tubulose zirconium dioxide sensing probe, the middle aluminium oxide ceramics heating core of introducing; Type of heating is an indirect heating, and product size is big, complex structure; Response speed is slow, is difficult to satisfy the exhaust emissions requirement of present increasingly stringent.Begin to use in batches the tabular lambda sensor of integral type in the world, but owing to adopted high temperature or middle temperature burning technology system altogether, ubiquity complex process, the low shortcoming of dielectric voltage withstand when material cost height, the easy blowby of heater circuit, work.
Summary of the invention
Existing zirconia oxygen product size is big in order to overcome, complex structure, response speed is slow and material cost is high deficiency, the invention provides a kind of inserted tabular lambda sensor and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is: a kind of inserted tabular lambda sensor; Comprise ceramic heater, zirconia sensitive element, glass glaze sealant, heating circuit, reference gas passage, alumina substrate and groove; Be provided with the zirconia sensitive element in the ceramic heater; Ceramic heater is connected through the glass glaze sealant with the zirconia sensitive element, and ceramic heater is made up of alumina substrate and groove, and the alumina substrate upper surface is provided with groove; Lower surface is provided with the heating circuit, is provided with reference gas passage between zirconia sensitive element and the groove.
According to another embodiment of the invention, comprise that further zirconia sensitive element one side is provided with interior electrode, opposite side is provided with external electrode, and the external electrode surface is covered with porous protective layer.
According to another embodiment of the invention, comprise that further heating circuit front portion is covered with one deck glass glaze insulation course, two heatings of formation circuit pins are exposed at the rear portion.
The present invention solves the another kind of technical scheme that its technical matters adopts: a kind of inserted tabular lambda sensor preparation method, and its preparation method may further comprise the steps:
One. ceramic heater is a matrix with 95 aluminium oxide ceramics of densified sintering product, offers groove in the alumina base surface;
Two. the alumina substrate lower surface at the band groove adopts thick film silk-screen printing technique printing heating circuit; Anterior printed glass glaze insulation course at the heating circuit; Two heatings of formation circuit pins are exposed at the rear portion; And then sintering in 1200 ℃ the air, combining closely with stove cooling back heating circuit, glass glaze insulation course and alumina substrate is integrally formed;
Three. the zirconia sensitive element is that 5 moles of yttrium stable zirconium oxides with densified sintering product are that matrix is processed the strip thin slice; Sheet thickness is 0.4mm-0.6mm; Electrode and external electrode in the upper and lower surfaces of thin slice prints respectively, simultaneously, the porous protective layer of electrode surface printing outside; And then sintering in 1200 ℃ the air, combining closely with electrode, external electrode, porous protective layer and zirconia matrix in the stove cooling back is integrally formed;
Four. the zirconia sensitive element is embedded in the groove of ceramic heater; Seam crossing filling glass glaze sealant; Sintering in 1200 ℃ air; Combining closely through the glass glaze sealant with stove cooling rear oxidation zirconium sensitive element and ceramic heater is integrally formed, and finally forms inserted tabular lambda sensor.
According to another embodiment of the invention; Further comprise between the groove of said reference gas passage by zirconia sensitive element and ceramic heater and forming; Reference gas passage and atmosphere, this reference air flue width is 0.8mm-1.0 mm, highly is 0.4mm-0.5mm.
According to another embodiment of the invention; The printing slurry that further comprises said heating circuit is made up of Metal Palladium powder, metal platinum powder, frit and the mixing of organic solution material; Wherein the granularity of Metal Palladium powder, platinum powder and frit is the 1.5-2.5 micron, and the weight ratio of palladium powder, platinum powder and frit is: the palladium powder is 80-85; Platinum powder is 3; Frit is 12-17.
According to another embodiment of the invention; The printing slurry that further comprises said interior electrode and external electrode is made up of metal platinum powder, spherical graphite powder, frit and the mixing of organic solution material; Wherein the granularity of metal platinum powder, spherical graphite powder and frit is the 1.5-2.5 micron, and the weight ratio of metal platinum powder, spherical graphite powder and frit is: the metal platinum powder is 75-80; The spherical graphite powder is 10, and frit is 10-15.
According to another embodiment of the invention; The printing slurry that further comprises said porous protective layer is made up of 5 moles of yttrium stable zirconium oxide powder, spherical graphite powder, frit and the mixing of organic solution material; Wherein the granularity of zirconia powder is the 0.3-0.4 micron; The granularity of spherical graphite powder and frit is the 1.5-2.5 micron, and the weight proportion of zirconia powder, spherical graphite powder and frit is: zirconia powder is 78-82; The spherical graphite powder is 5; Frit is 13-17.
According to another embodiment of the invention; Comprise that further frit, the frit in the porous protective layer printing slurry, the frit in the interior electrode printing slurry and the frit in the external electrode printing slurry in said glass glaze insulation course, glass glaze sealant, the heating circuit printing slurry constitute by the glass powdered frit; This glass powdered frit be a kind of unleaded in warm glass powdered frit; Its granularity is the 1.5-2.5 micron, and each weight ratio of constituents is: aluminium oxide is 29; Zirconia is 27; Monox is 32; Lithia is 4; Bismuth oxide is 5; Zinc paste is 3.
The invention has the beneficial effects as follows that this inserted tabular lambda sensor has improved the high temperature insulation characteristic of product, electric response speed is fast, has reduced energy consumption and production cost, has prolonged the serviceable life of product, is easy to use promote.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is a structural representation of the present invention;
Fig. 2 is a front elevation of the present invention;
Fig. 3 is a rear view of the present invention;
Fig. 4 is an alumina substrate groove structure synoptic diagram of the present invention;
Fig. 5 is the responsive meta structure synoptic diagram of zirconia of the present invention;
Fig. 6 is well heater of the present invention and sensitive element mosaic texture synoptic diagram.
1. ceramic heaters among the figure, 2. zirconia sensitive element, 3. glass glaze sealant, 4. heating circuit, 5. reference gas passage, 6. porous protective layer, 7. in electrode, 8. external electrode, 9. glass glaze insulation course, 10. heating circuit pin, 11. alumina substrates, 12. grooves.
Embodiment
Like Fig. 1 is structural representation of the present invention; A kind of inserted tabular lambda sensor and preparation method thereof comprises ceramic heater 1, zirconia sensitive element 2, glass glaze sealant 3, heating circuit 4, reference gas passage 5, alumina substrate 11 and groove 12, is provided with zirconia sensitive element 2 in the ceramic heater 1; Ceramic heater 1 is connected through glass glaze sealant 3 with zirconia sensitive element 2; Ceramic heater 1 is made up of alumina substrate 11 and groove 12, and alumina substrate 11 upper surfaces are provided with groove 12, and lower surface is provided with heating circuit 4; Be provided with reference gas passage 5 between zirconia sensitive element 2 and the groove 12; Reduced the energy consumption of sensor, technology is simple, low cost of manufacture.
Like Fig. 2 is front elevation of the present invention, and zirconia sensitive element 2 one sides are provided with interior electrode 7, and opposite side is provided with external electrode 8, and external electrode 8 surfaces are covered with porous protective layer 6, have accelerated electric response speed.
Like Fig. 3 is rear view of the present invention, and heating circuit 4 front portions are covered with one deck glass glaze insulation course 9, and two heatings of formation circuit pins 10 are exposed at the rear portion, have improved high temperature insulation characteristic greatly.
A kind of inserted tabular lambda sensor preparation method, its preparation method may further comprise the steps:
One. ceramic heater 1 is a matrix with 95 aluminium oxide ceramics of densified sintering product, offers groove 12 on alumina substrate 11 surfaces, and is as shown in Figure 4;
Two. alumina substrate 11 lower surfaces at band groove 12 adopt thick film silk-screen printing technique printing heating circuit 4; Anterior printed glass glaze insulation course 9 at heating circuit 4; Two heatings of formation circuit pins 10 are exposed at the rear portion; And then sintering in 1200 ℃ the air, combining closely with stove cooling back heating circuit 4, glass glaze insulation course 9 and alumina substrate 11 is integrally formed, as shown in Figure 2;
Three. zirconia sensitive element 2 is that 5 moles of yttrium stable zirconium oxides with densified sintering product are that matrix is processed the strip thin slice, and sheet thickness is 0.4mm-0.6mm, electrode 7 and external electrode 8 in the upper and lower surfaces of thin slice prints respectively; Simultaneously, at external electrode 8 surface printing porous protective layers 6, and then sintering in 1200 ℃ the air; Electrode 7, external electrode 8, porous protective layer 6 and zirconia matrix are combined closely and are integrally formed in cooling off afterwards with stove; As shown in Figure 5, be the responsive first matrix of zirconia owing to adopted 5 moles of yttrium partially stabilized zirconias of oxidation, be embedded in high-intensity 95 aluminium oxide ceramics matrix surfaces; Extruding force and impulsive force that later stage encapsulation and product produce when using are mainly born by 95 alumina substrates; The responsive unit of the relatively low zirconia of intensity is stressed little, so improved the requirement of strength of product, adapts to bad working environment in the engine; Because heater circuit is to be attached on the 95 good aluminium oxide ceramics matrixes of high temperature insulation characteristic; Greatly improved the high temperature insulation characteristic of product, there is not heating current blowby phenomenon in 850 ℃ of following dielectric voltage withstands of heating circuit greater than 1000V;
Four. zirconia sensitive element 2 is embedded in the groove of ceramic heater 1 seam crossing filling glass glaze sealant 3, sintering in 1200 ℃ air; Combine closely through glass glaze sealant 3 with ceramic heater 1 with stove cooling rear oxidation zirconium sensitive element 2 and to be integrally formed; The inserted tabular lambda sensor of final formation, as shown in Figure 6, adopt inserted platy structure; Ceramic heater and the responsive unit of oxygen are formed an integral body through glass glaze sealant high temperature bonding; Become real direct heating arrangement, the power of calandria is 6～9 watts under direct current 12V voltage, is about half of conventional tubular lambda sensor heating power.
Form between the groove 12 of said reference gas passage 5 by zirconia sensitive element 2 and ceramic heater 1, reference gas passage 5 and atmosphere, these reference gas passage 5 width are 0.8mm-1.0 mm, highly are 0.4mm-0.5mm.
The printing slurry of said heating circuit 4 is mixed by Metal Palladium powder, metal platinum powder, frit and organic solution material and forms; Wherein the granularity of Metal Palladium powder, platinum powder and frit is the 1.5-2.5 micron, and the weight ratio of palladium powder, platinum powder and frit is: the palladium powder is 80-85; Platinum powder is 3; Frit is 12-17.
The printing slurry of electrode 7 and external electrode 8 is made up of metal platinum powder, spherical graphite powder, frit and the mixing of organic solution material in said; Wherein the granularity of metal platinum powder, spherical graphite powder and frit is the 1.5-2.5 micron, and the weight ratio of metal platinum powder, spherical graphite powder and frit is: the metal platinum powder is 75-80; The spherical graphite powder is 10, and frit is 10-15.Because internal and external electrode all is employed in and has added the spherical glass powder in the preparation raw material platinum powder and regulate adhesion and formation microcellular structure with dag; Dag uses as pore former, the platinum electrode of porous both catalytic activity is high, can guarantee penetrating smoothly of oxonium ion under the high temperature again; Heater circuit directly calorifies the responsive unit of zirconia through alumina substrate simultaneously; Heating has been shortened and has been arrived the stand-by period that lambda sensor heats up and activates after the engine start rapidly, has accelerated response speed.
The printing slurry of said porous protective layer 6 is mixed by 5 moles of yttrium stable zirconium oxide powder, spherical graphite powder, frit and organic solution material and forms; Wherein the granularity of zirconia powder is the 0.3-0.4 micron; The granularity of spherical graphite powder and frit is the 1.5-2.5 micron, and the weight proportion of zirconia powder, spherical graphite powder and frit is: zirconia powder is 78-82; The spherical graphite powder is 5; Frit is 13-17.
Frit in said glass glaze insulation course 9, glass glaze sealant 3, the heating circuit 4 printing slurries, the frit in the porous protective layer 6 printing slurries, the frit in the interior electrode 7 printing slurries and the frit in the external electrode 8 printing slurries constitute by the glass powdered frit; This glass powdered frit be a kind of unleaded in warm glass powdered frit; Its granularity is the 1.5-2.5 micron, and each weight ratio of constituents is: aluminium oxide is 29; Zirconia is 27; Monox is 32; Lithia is 4; Bismuth oxide is 5; Zinc paste is 3.
This inserted tabular lambda sensor has improved the high temperature insulation characteristic of product, and electric response speed is fast, has reduced energy consumption and production cost, has prolonged the serviceable life of product, is easy to use promote.
Embodiment:
One. preparation glass powdered frit: by weight aluminium oxide: each material of the accurate weighing of the ratio of zirconia: monox: Lithia: bismuth oxide: zinc paste=29:27:32:4:5:3; Add 50% water; With the zirconium oxide balls is that mill is situated between; With agitating ball mill ball milling 2 hours, carry out force drying after the taking-up.Dried material powder places in the corundum crucible and 1400 ℃ of following high-temperature fusion; The glass metal of fusion is processed bigger oarse-grained glass dust after through shrend; Oarse-grained glass dust is levigate through stirring mill again, and the granularity of the dried glass powdered frit of ball milling is the 1.5-2.5 micron;
Two. preparation organic solution: the organic solution material is transparent viscous solution; Form by terpinol, polyvinyl butyral PVB and castor oil; According to the weight proportion terpinol: polyvinyl butyral PVB: castor oil is that the ratio of 79:15:6 is deployed into the thickness clear solution, and its viscosity is 5000-6000mPa.s down for 23 ℃;
Three. preparation printing slurry: the printing wet end furnish is: the solid powder summation is 68-72, and organic solution is 32-28, in its ratio weighing material, stirs the back and forms thickness material group, and is rolling evenly through three rolling mills again.Slurry is in the time of 23 ℃ uniformly, and its viscosity is at 7-10 ten thousand mPa.s.The printing slurry can add an amount of terpinol and do thinning agent adjustment viscosity before printing, so that serigraphy.
Four. on alumina substrate 11 and 5 moles of zirconia thin slices, print each functional layer respectively respectively; Each functional layer thickness is controlled by following: 15 microns in heating circuit; 50 microns of glass glaze insulation courses, 15 microns of internal and external electrodes, 70 microns of zirconia porous protective layers; Each layer allows the thickness deviation of 10%-15%, is completed for printing air dry under each functional layer room temperature of back.
Five. dry back ceramic heater 1 is put into the box circuit of rapid temperature rise and drop respectively with zirconia sensitive element 2 and is carried out sintering, and sintering temperature is 1200 ℃, is incubated 30 minutes, and with the stove cooling, sintering post-heater room temperature resistance is between 7 Ω-8 Ω.
Six. the ceramic heater 1 behind the sintering carries out the assembly unit sealing-in with zirconia sensitive element 2; With manual groove 12 seam crossings that evenly are coated on the alumina substrate 11 of ceramic heat 1 of glass glaze insulation paste; Accurately put into zirconia sensitive element 2, alignment compresses air dry under the room temperature of back.
Seven. dried assembly is put into the box circuit of rapid temperature rise and drop and is carried out sintering; Sintering temperature is 1200 ℃; Be incubated 30 minutes; The complete fusion of glass glaze insulation paste this moment, the filling groove seam crossing forms glass glaze sealant 3, and combining closely through glass glaze sealant 3 with ceramic heater 1 with stove cooling rear oxidation zirconium sensitive element 2 is integrally formed.
Claims (9)
1. inserted tabular lambda sensor; Comprise ceramic heater (1), zirconia sensitive element (2), glass glaze sealant (3), heating circuit (4), reference gas passage (5), alumina substrate (11) and groove (12); Be provided with zirconia sensitive element (2) in the ceramic heater (1); Ceramic heater (1) is connected through glass glaze sealant (3) with zirconia sensitive element (2); It is characterized in that ceramic heater (1) is made up of alumina substrate (11) and groove (12), alumina substrate (11) upper surface is provided with groove (12); Lower surface is provided with heating circuit (4), is provided with reference gas passage (5) between zirconia sensitive element (2) and the groove (12).
2. inserted tabular lambda sensor according to claim 1 is characterized in that, zirconia sensitive element (2) one sides are provided with interior electrode (7), and opposite side is provided with external electrode (8), and external electrode (8) surface is covered with porous protective layer (6).
3. inserted tabular lambda sensor according to claim 1 is characterized in that, heating circuit (4) front portion is covered with one deck glass glaze insulation course (9), and two heatings of formation circuit pins (10) are exposed at the rear portion.
4. inserted tabular lambda sensor preparation method is characterized in that its preparation method may further comprise the steps:
One. ceramic heater (1) is a matrix with 95 aluminium oxide ceramics of densified sintering product, offers groove (12) on alumina substrate (11) surface;
Two. alumina substrate (11) lower surface at band groove (12) adopts thick film silk-screen printing technique printing heating circuit (4); Anterior printed glass glaze insulation course (9) at heating circuit (4); Two heatings of formation circuit pins (10) are exposed at the rear portion; And then sintering in 1200 ℃ the air, combining closely with stove cooling back heating circuit (4), glass glaze insulation course (9) and alumina substrate (11) is integrally formed;
Three. zirconia sensitive element (2) is that 5 moles of yttrium stable zirconium oxides with densified sintering product are that matrix is processed the strip thin slice; Sheet thickness is 0.4mm-0.6mm; Upper and lower surfaces at thin slice prints interior electrode (7) and external electrode (8) respectively; Simultaneously; At external electrode (8) surface printing porous protective layer (6), and then sintering in 1200 ℃ the air, combining closely with electrode (7), external electrode (8), porous protective layer (6) and zirconia matrix (11) in the stove cooling back is integrally formed;
Four. zirconia sensitive element (2) is embedded in the groove (12) of ceramic heater (1); Seam crossing filling glass glaze sealant (3); Sintering in 1200 ℃ air; Combining closely through glass glaze sealant (3) with stove cooling rear oxidation zirconium sensitive element (2) and ceramic heater (1) is integrally formed, and finally forms inserted tabular lambda sensor.
5. inserted tabular lambda sensor preparation method according to claim 4; It is characterized in that; Form between the groove of said reference gas passage (5) by zirconia sensitive element (2) and ceramic heater (1); Reference gas passage (5) and atmosphere, this reference gas passage (7) width is 0.8mm-1.0 mm, highly is 0.4mm-0.5mm.
6. inserted tabular lambda sensor preparation method according to claim 4; It is characterized in that; The printing slurry of said heating circuit (4) is mixed by Metal Palladium powder, metal platinum powder, frit and organic solution material and forms; Wherein the granularity of Metal Palladium powder, platinum powder and frit is the 1.5-2.5 micron, and the weight ratio of palladium powder, platinum powder and frit is: the palladium powder is 80-85; Platinum powder is 3; Frit is 12-17.
7. inserted tabular lambda sensor preparation method according to claim 4; It is characterized in that; The printing slurry of electrode (7) and external electrode (8) is made up of metal platinum powder, spherical graphite powder, frit and the mixing of organic solution material in said; Wherein the granularity of metal platinum powder, spherical graphite powder and frit is the 1.5-2.5 micron, and the weight ratio of metal platinum powder, spherical graphite powder and frit is: the metal platinum powder is 75-80; The spherical graphite powder is 10, and frit is 10-15.
8. inserted tabular lambda sensor preparation method according to claim 4; It is characterized in that; The printing slurry of said porous protective layer (6) is mixed by 5 moles of yttrium stable zirconium oxide powder, spherical graphite powder, frit and organic solution material and forms; Wherein the granularity of zirconia powder is the 0.3-0.4 micron, and the granularity of spherical graphite powder and frit is the 1.5-2.5 micron, and the weight proportion of zirconia powder, spherical graphite powder and frit is: zirconia powder is 78-82; The spherical graphite powder is 5; Frit is 13-17.
9. inserted tabular lambda sensor preparation method according to claim 4; It is characterized in that; Frit in said glass glaze insulation course (9), glass glaze sealant (3), heating circuit (4) the printing slurry, the frit in porous protective layer (6) the printing slurry, the frit in interior electrode (7) the printing slurry and the frit in external electrode (8) the printing slurry constitute by the glass powdered frit; This glass powdered frit be a kind of unleaded in warm glass powdered frit; Its granularity is the 1.5-2.5 micron, and each weight ratio of constituents is: aluminium oxide is 29; Zirconia is 27; Monox is 32; Lithia is 4; Bismuth oxide is 5; Zinc paste is 3.
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| CN104198564A (en) * | 2014-09-24 | 2014-12-10 | 云南云天化股份有限公司 | Oxygen sensor protection layer and preparation method thereof |
| CN107796860A (en) * | 2016-08-29 | 2018-03-13 | 南京瀚雅健康科技有限公司 | A kind of current type solid electrolyte oxygen analyte sensors |
| CN111491403A (en) * | 2020-04-21 | 2020-08-04 | 苏州好特斯模具有限公司 | Material for manufacturing thick film heater |
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Application publication date: 20120815 |