CN106348752A - Method for co-sintering oxygen sensor ceramic matrix, electrode and electrode protective layer - Google Patents
Method for co-sintering oxygen sensor ceramic matrix, electrode and electrode protective layer Download PDFInfo
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- CN106348752A CN106348752A CN201610778511.5A CN201610778511A CN106348752A CN 106348752 A CN106348752 A CN 106348752A CN 201610778511 A CN201610778511 A CN 201610778511A CN 106348752 A CN106348752 A CN 106348752A
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Abstract
The invention relates to a sintering process of oxygen sensor-zirconium oxide pipe, in particular to a method for co-sintering an oxygen sensor ceramic matrix, an electrode and an electrode protective layer. The method for co-sintering the oxygen sensor ceramic matrix, the electrode and the electrode protective layer comprises the following technological processes: 1, forming the ceramic matrix through injection molding and degreasing; 2, manufacturing the platinum electrode; 3, dip-coating the protective layer; 4, co-sintering, wherein the used protective layer slurry is subjected to ball milling and contains pore-forming components, so that the protective layer has high sintering activity and certain pore-forming property; in addition, the protective layer and the matrix contain the same material components, and the protective layer and the matrix can be firmly sintered together during high-temperature co-sintering according to the similar compatibility principle, so that the problem that the protective layer is liable to fall off or peel off is completely solved, the production technological process is simplified and the cost is reduced.
Description
Technical field
The present invention relates to a kind of sintering process of oxygen sensor tubular zirconium-oxide, more particularly, to tubular zirconium-oxide ceramic matrix
Method with platinum electrode and electrode protecting layer co-sintering.
Technical background
Oxygen sensor is widely used in Engine Injection Mass and adjusts and Exhaust Emission Control, reduces oil consumption and control dirt to reach
The purpose of dye gas discharge.And the core component realizing oxygen sensor function is its internal tubular zirconium-oxide (or zirconium oxide piece).
The production technology of generally tubular zirconium-oxide is the making that ceramic matrix is separately repeatedly sintered with platinum electrode and electrode protecting layer
Technique, and such sintering process to be easily caused electrode adhesion poor, protective layer peels off, going out the problems such as product poor electrical performance
Existing；Increased energy consumption increases the production cycle again simultaneously.
Content of the invention
For solving the above problems, the present invention provides one kind relatively easy quick, and product electrical property is all relative with mechanical performance
The method of the co-sintering of preferable tubular zirconium-oxide ceramic matrix and electrode and electrode protecting layer.
For achieving the above object, the present invention mainly employs the following technical solutions and is solved: a kind of oxygen sensor ceramic base
Body and the method for electrode and electrode protecting layer co-sintering, including following technical process: 1, injection moulding ceramic matrix defat: will
It is mixed with ceramic feeding injection moulding on precise injection molding machine of binding agent；Injection molding base substrate alumina powder is buried
Enter and in mullite sagger, carry out defat；Will be clean to ceramic matrix outer surface and bore cleaning after defat is complete；2nd, make platinum electrode:
By platinum slurry brushing shown in ceramic matrix surfaces externally and internally, brushing shape as accompanying drawing 1, Fig. 2；Painting is brushed electrode ceramic matrix
Dry and casket burns to 800～1000 DEG C；Survey internal and external electrode resistance≤10 ω afterwards；3rd, dipping protective layer: electrode will be made
In ceramic matrix immersion protective layer slurry, keep 2～5 seconds, take out, be placed in baking oven carrying out 150 DEG C of drying.4th, co-sintering:
The zirconium pipe of good for dipping protective layer is placed in mullite sagger, in high temperature furnace, casket burns to 1400～1600 DEG C, and stove is cooled to 300
～500 DEG C of taking-ups.
Wherein ceramic matrix be on precise injection molding machine molding it is ensured that size accurately consistent.Used by defat
Alumina powder is the inert alumina powder that 200～800 mesh have siphon；Degreasing process is warming up to 800 with 40～60h～
1000 DEG C and be incubated 2～5h and carry out, after the completion of defat, cool to 200～300 DEG C of taking-ups with the furnace.The solid phase of platinum slurry used
Content is 40%～60%；Zirconium pipe external electrode curved surface screen printing machine is printed to network structure (see figure 1), interior electrode point gum machine
Scribble one and enclose and draw contact conductor inside ceramic matrix, in requirement, electrode encloses and external electrode along inner tubal wall coats one simultaneously
Just corresponding to (see figure 2) along the circle that outer tube wall coats, two electrode pin pad printer are printed；Make electrode process also include by
The ceramic matrix that painting brushes electrode is dried with 150～200 DEG C of insulation 30min in an oven, afterwards painting is made electrode
Matrix is neatly put in mullite sagger and is put into together in box-type high-temperature furnace and rises to 800～1200 DEG C simultaneously with 8～20 DEG C/min
Insulation 1～2h, cools to 400～500 DEG C of taking-up air coolings with the furnace, the resistance of last test electrode it is desirable to internal and external electrode resistance not
More than 10 ω.Protective layer slurry used is one or more ceramic powders therein such as spinelle, aluminium oxide and organic or inorganic
Ball milling 10～the 24h in comprehensive planetary ball mill such as binding agent and diluent, pore creating material makes, and has thinner granularity
With certain sintering activity.In addition the sintering process of co-sintering process is: with 6～12h rise to 1000～1200 DEG C of insulations 0.8～
1.2h, then 1400～1600 DEG C of insulation 2～3h of 2～5h intensification, cool to 400～500 DEG C of taking-up air coolings with the furnace.
The main advantage of the present invention is: 1, ceramic matrix is to be obtained by precise injection and degreasing process, matrix chi
Very little accurate, low production cost.2nd, the making of electrode is carried out before the non-porcelain of matrix, such electrode particle and ceramic matrix
The space on surface is mutually inlayed, and electrode adhesion is higher；Non- porcelain pottery has certain absorbency simultaneously, is easy to printing behaviour
Make.3rd, external electrode uses surface mesh silk-screen technology, and the grid electrode of printing has not only saved electrode cost, Er Qieyou
Considerably increase the length of base electrode tail gas three phase boundary so that zirconium pipe electrical property is more excellent.4th, protective layer used
Slurry is through ball milling processing, contains pore-creating composition again, therefore has good sintering activity and certain pore-creating character；In addition protect
Sheath and matrix contain identical material composition, and according to similar compatibility principle, when high temperature co-firing is tied, protective layer can be with matrix
Being sintered together securely, thus thoroughly solving the problems, such as that protective layer easily peels or flakes off, and simplifying production technology mistake
Journey, reduces cost.
Brief description
Fig. 1 is the latticed external electrode schematic diagram of brushing of the present invention.
Fig. 2 is the interior electrode schematic diagram of brushing of the present invention.
Fig. 3 is the schematic diagram and office after ceramic matrix of the present invention and platinum electrode and electrode protecting layer co-sintering
Portion's enlarged drawing.
Fig. 4 is the process flow diagram of the present invention
In Fig. 13: 1 be ceramic matrix 2 be external electrode 3 be interior electrode 4 be electrode protecting layer
Specific implementation method
1 accompanying drawing 4 is described in detail to the specific implementation method of the present invention below in conjunction with the accompanying drawings.
Embodiment 1
A kind of oxygen sensor ceramic matrix includes following technical process with the method for electrode and electrode protecting layer co-sintering: 1, injects
Forming ceramic matrix: the ceramic feeding being mixed with binding agent is injected into the ceramic matrix shown in Fig. 1 on precise injection molding machine
Shape；2nd, defat: injection molding base substrate is had the inert alumina powder embedment mullite sagger of siphon with 200 mesh
In, and put into and in draft glue discharging furnace, carry out defat, degreasing process is warming up to 800 DEG C with 40h and is incubated 2h and carries out, after the completion of defat, with
Stove is cooled to 300 DEG C of taking-ups, and will be clean to ceramic matrix outer surface and bore cleaning；3rd, brushing platinum electrode: by solid concentration
Platinum slurry brushing for 40% is printed and is reticulated knot in ceramic matrix surfaces externally and internally, wherein external electrode curved surface screen printing machine
Structure (see figure 1), interior electrode point gum machine is scribbled one inside ceramic matrix and is enclosed and draw contact conductor, simultaneously electrode edge in requirement
The circle that inner tubal wall coats encloses just corresponding (see figure 2) with external electrode along outer tube wall coats one, and two electrode pin pad printer print
Brush.Dried applying the ceramic matrix brushing electrode with 150 DEG C of insulation 30min in an oven, afterwards painting is made electrode
Matrix is neatly put in mullite sagger.4th, pre-burning electrode: put into box height together with saggar by applying the matrix making electrode
Rise to 800 DEG C with 8 DEG C/min in warm stove and be incubated 1h, cool to 400 DEG C of taking-up air coolings with the furnace.5th, survey electrode resistance: test is pre-
The resistance of burned electrode is it is desirable to interior external resistance is less than 10 ω；6th, dipping protective layer: the ceramic matrix making electrode is soaked
Enter in protective layer slurry, keep 2 seconds, take out, be placed in baking oven carrying out 150 DEG C of drying.Protective layer slurry used be spinelle,
One or more ceramic powders therein such as aluminium oxide and organic or inorganic binding agent and diluent etc. are in comprehensive planet ball
In grinding machine, ball milling 10h makes.7th, co-sintering: the zirconium pipe of good for dipping protective layer is placed in mullite sagger, and puts into together
Carry out the co-sintering of ceramic matrix, electrode and protective layer, sintering process rises to 1000 DEG C of insulation 0.8h with 6h in high temperature sintering furnace,
2h heats up 1400 DEG C and is incubated 2h again, cools to 300 DEG C of taking-up air coolings with the furnace.
Embodiment 2
A kind of oxygen sensor ceramic matrix includes following technical process with the method for electrode and electrode protecting layer co-sintering: 1, injects
Forming ceramic matrix: the ceramic feeding being mixed with binding agent is injected into the ceramic matrix shown in Fig. 1 on precise injection molding machine
Shape；2nd, defat: injection molding base substrate is had the inert alumina powder embedment mullite sagger of siphon with 500 mesh
In, and put into and in draft glue discharging furnace, carry out defat, degreasing process is warming up to 900 DEG C with 50h and is incubated 3h and carries out, after the completion of defat, with
Stove is cooled to 400 DEG C of taking-ups, and will be clean to ceramic matrix outer surface and bore cleaning；3rd, brushing platinum electrode: by solid concentration
Platinum slurry brushing for 50% is printed and is reticulated knot in ceramic matrix surfaces externally and internally, wherein external electrode curved surface screen printing machine
Structure (see figure 1), interior electrode point gum machine is scribbled one inside ceramic matrix and is enclosed and draw contact conductor, simultaneously electrode edge in requirement
The circle that inner tubal wall coats encloses just corresponding (see figure 2) with external electrode along outer tube wall coats one, and two electrode pin pad printer print
Brush.Dried applying the ceramic matrix brushing electrode with 180 DEG C of insulation 30min in an oven, afterwards painting is made electrode
Matrix is neatly put in mullite sagger.4th, pre-burning electrode: put into box height together with saggar by applying the matrix making electrode
Rise to 1000 DEG C with 15 DEG C/min in warm stove and be incubated 1h, cool to 450 DEG C of taking-up air coolings with the furnace.5th, survey electrode resistance: test
The resistance of pre- burned electrode is it is desirable to interior external resistance is less than 10 ω；6th, dipping protective layer: the ceramic matrix of electrode will be made
In immersion protective layer slurry, keep 3 seconds, take out, be placed in baking oven carrying out 150 DEG C of drying.Protective layer slurry used is that point is brilliant
Stone, aluminium oxide one or two ceramic powders therein and organic or inorganic binding agent and diluent are in comprehensive planetary ball mill
In machine, ball milling 15h makes.7th, co-sintering: the zirconium pipe of good for dipping protective layer is placed in mullite sagger, and puts height together into
Carry out the co-sintering of ceramic matrix, electrode and protective layer, sintering process rises to 1100 DEG C of insulation 1h with 9h, then 4h in warm sintering furnace
Heat up 1550 DEG C of insulation 2.5h, cools to 400 DEG C of taking-up air coolings with the furnace.
Embodiment 3
A kind of oxygen sensor ceramic matrix includes following technical process with the method for electrode and electrode protecting layer co-sintering: 1, injects
Forming ceramic matrix: the ceramic feeding being mixed with binding agent is injected into the ceramic matrix shown in Fig. 1 on precise injection molding machine
Shape；2nd, defat: injection molding base substrate is had the inert alumina powder embedment mullite sagger of siphon with 800 mesh
In, and put into and in draft glue discharging furnace, carry out defat, degreasing process is warming up to 1000 DEG C with 60h and is incubated 5h and carries out, after the completion of defat, with
Stove is cooled to 500 DEG C of taking-ups, and will be clean to ceramic matrix outer surface and bore cleaning；3rd, brushing platinum electrode: by solid concentration
Platinum slurry brushing for 60% is printed and is reticulated knot in ceramic matrix surfaces externally and internally, wherein external electrode curved surface screen printing machine
Structure (see figure 1), interior electrode point gum machine is scribbled one inside ceramic matrix and is enclosed and draw contact conductor, simultaneously electrode edge in requirement
The circle that inner tubal wall coats encloses just corresponding (see figure 2) with external electrode along outer tube wall coats one, and two electrode pin pad printer print
Brush.Dried applying the ceramic matrix brushing electrode with 200 DEG C of insulation 30min in an oven, afterwards painting is made electrode
Matrix is neatly put in mullite sagger.4th, pre-burning electrode: put into box height together with saggar by applying the matrix making electrode
Rise to 1200 DEG C with 20 DEG C/min in warm stove and be incubated 2h, cool to 500 DEG C of taking-up air coolings with the furnace.5th, survey electrode resistance: test
The resistance of pre- burned electrode is it is desirable to interior external resistance is less than 10 ω；6th, dipping protective layer: the ceramic matrix of electrode will be made
In immersion protective layer slurry, keep 5 seconds, take out, be placed in baking oven carrying out 150 DEG C of drying.Protective layer slurry used is that point is brilliant
One or more ceramic powders therein such as stone, aluminium oxide and organic or inorganic binding agent and diluent etc. are in comprehensive planet
In ball mill, ball milling 24h makes.7th, co-sintering: the zirconium pipe of good for dipping protective layer is placed in mullite sagger, and puts together
Enter to carry out the co-sintering of ceramic matrix, electrode and protective layer in high temperature sintering furnace, sintering process rises to 1200 DEG C of insulations with 12h
1h, then 1600 DEG C of insulation 3h of 5h intensification, cool to 500 DEG C of taking-up air coolings with the furnace.
3 embodiments are hardness according to forming ceramic matrix and electrode general character carries out different pieces of information distribution, serve phase
The more excellent effect to its characteristic, the invention discloses a kind of ceramic matrix of oxygen sensor sensing element tubular zirconium-oxide and platinum electrode
And the method for electrode protecting layer co-sintering.Platinum electrode and ceramic matrix and protective layer and ceramic base can be made by the method
Body first mutually inlays parcel in the state of un-sintered, then make at high temperature again its interpenetrate fusion make ceramic matrix with
The bond strength of electrode and protective layer is more firm, solves electrode and protective layer holds caducous problem；Especially, the present invention
It is mentioned to the latticed curved surface silk-screen technology of zirconium pipe external electrode, this technology has not only saved precious metal material, and increased
The length of the three phase boundary of electrode, substantially increases chemical property and the response performance of zirconium pipe；Injection technique ensure that simultaneously
The accuracy of ceramic matrix size；Furthermore protective layer slurry is after ball milling, there is more preferable matrix affinity, rheological characteristic, sintering
Activity and pore-forming systematicness.
Various sintering process provided in the present invention and various parameters can set with raw materials for production, production environment, machine
The difference of standby, production capacity and management method and change, various techniques therefore provided by the present invention and parameter only have ginseng
The property examined, is not meant to that it is limitation of the present invention condition.
Claims (8)
1. a kind of oxygen sensor ceramic matrix and the method for electrode and electrode protecting layer co-sintering are it is characterised in that include following
Technical process: (1) injection moulding ceramic matrix defat: the ceramic feeding being mixed with binding agent is noted on precise injection molding machine
Penetrate molding；By injection molding base substrate with carrying out defat in alumina powder embedment mullite sagger, by ceramic base after defat is complete
External surface and bore cleaning are clean；
(2) make platinum electrode: by platinum slurry brushing in ceramic matrix surfaces externally and internally；Painting is brushed electrode ceramic matrix dry
And casket burns to 800～1000 DEG C；Survey internal and external electrode resistance≤10 ω afterwards；
(3) dipping protective layer: the ceramic matrix making electrode is immersed in protective layer slurry, keeps 2～5 seconds, take out, juxtaposition
Carry out 150 DEG C of drying in baking oven；
(4) co-sintering: the zirconium pipe of good for dipping protective layer is placed in mullite sagger, in high temperature furnace casket burn to 1400～
1600 DEG C, stove is cooled to 300～500 DEG C of taking-ups.
2. the method for a kind of oxygen sensor ceramic matrix according to claim 1 and electrode and electrode protecting layer co-sintering its
It is characterised by, defat is warming up to 800～1000 DEG C with 40～60h and is incubated 2～5h and carries out, and the alumina powder used by defat is
200～800 mesh have the inert alumina powder of siphon.
3. the method for a kind of oxygen sensor ceramic matrix according to claim 1 and electrode and electrode protecting layer co-sintering its
It is characterised by, in step (2), the solid concentration of platinum slurry used is 40%～60%.
4. the method for a kind of oxygen sensor ceramic matrix according to claim 1 and electrode and electrode protecting layer co-sintering,
It is characterized in that, zirconium pipe external electrode curved surface screen printing machine is printed to network structure.
5. the method for a kind of oxygen sensor ceramic matrix according to claim 1 and electrode and electrode protecting layer co-sintering,
It is characterized in that, in zirconium pipe, electrode point gum machine is scribbled one inside ceramic matrix and is enclosed and draw contact conductor, requires interior simultaneously
The circle that electrode is coated along outer tube wall along the circle that inner tubal wall coats with external electrode is just corresponding.
6. a liang electrode pin pad printer is printed；
A kind of oxygen sensor ceramic matrix according to claim 1 and the method for electrode and electrode protecting layer co-sintering, its
It is characterised by, the process making electrode includes being incubated applying the ceramic matrix brushing electrode with 150～200 DEG C in an oven
30min is dried, and neatly puts into applying the matrix making electrode in mullite sagger and puts into box-type high-temperature furnace together afterwards
In rise to 800～1200 DEG C with 8～20 DEG C/min and be incubated 1～2h, cool to 400～500 DEG C of taking-up air coolings with the furnace.
7. the method for a kind of oxygen sensor ceramic matrix according to claim 1 and electrode and electrode protecting layer co-sintering its
Be characterised by, protective layer slurry used by step (3) be spinelle, aluminium oxide one or two ceramic powders therein with organic or
Inorganic binder and diluent, pore creating material ball milling 10～24h in comprehensive planetary ball mill make, and have thinner granule
Degree and certain sintering activity.
8. a kind of ceramic matrix of oxygen sensor sensing element according to claim 1 is burnt altogether with electrode and electrode protecting layer
The method of knot it is characterized in that, also include before step (4) rising to 1000～1200 DEG C of insulation 0.8～1.2h with 6～12h, then
In step (4), 1400～1600 DEG C of insulation 2～3h are warming up to 2～5h.
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| CN201610778511.5A CN106348752A (en) | 2016-08-31 | 2016-08-31 | Method for co-sintering oxygen sensor ceramic matrix, electrode and electrode protective layer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111505084A (en) * | 2019-01-31 | 2020-08-07 | 苏州工业园区传世汽车电子有限公司 | Sensing element and preparation method thereof |
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