CN103776888B - A kind of oxygen sensor used in vehicle based on insulated by oxide slurry and manufacture method thereof - Google Patents
A kind of oxygen sensor used in vehicle based on insulated by oxide slurry and manufacture method thereof Download PDFInfo
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Abstract
The invention discloses a kind of oxygen sensor used in vehicle based on insulated by oxide slurry, wherein, first insulating barrier, the second insulating barrier and the 3rd insulating barrier are made up of insulation paste, insulation paste includes the material of following weight portion: the inorganic particle being made up of oxide 46 parts, organic carrier 24 parts, auxiliary agent 13 parts.Each layer matrix of this oxygen sensor used in vehicle, especially insulating barrier all use oxide to make, the sinter bonded degree that each base layer has had, and this sensor has preferable sensitivity, simultaneously, it is not necessary to the toxic solvent such as butanone, dimethylbenzene, it is to avoid because human body is worked the mischief by noxious substance.
Description
Technical field
The present invention relates to sensor, particularly relate to a kind of oxygen sensor used in vehicle based on insulated by oxide slurry and
Its manufacture method.
Background technology
Recently as the development of automobile market, it has been a kind of trend that automobile enters every household, but vapour
At the beginning of tail gas has become one of main source of atmospheric pollution, especially 2013, many days of Beijing area experience
Fog thick weather, PM2.5 exceeds standard three times more than, makes the quality of the life of the people suffer the biggest threat,
Fog weather can cause rhinitis, bronchitis, is in this environment for a long time and also can induce pulmonary carcinoma.2013 1
Month 1 day, China started state four discharge standard the most comprehensively and controls the vehicle exhaust pollution to air, and car
It is the sensing element that waste gas is detected by only one with oxygen sensor.The system of existing chip oxygen sensor
The standby butanone that mainly uses, dimethylbenzene system curtain coating obtains cast sheet and uses transition zone to control the insulation of sensor
Property, use foreign body to fill and obtain air duct, having residue in sintering process exists, and affects sensor
Sensitivity, meanwhile, in sensor production process use organic solvent majority be that butanone, dimethylbenzene etc. have
Poison solvent, easily pollutes environment, and works the mischief health.
Summary of the invention
The technical problem to be solved in the present invention is, for the deficiencies in the prior art, it is provided that a kind of based on oxidation
The oxygen sensor used in vehicle of thing insulation paste and manufacture method thereof, each layer matrix of this oxygen sensor used in vehicle, especially
It is that insulating barrier all uses elite oxide to make, the sinter bonded degree that each base layer has had, and this sensing
Utensil has preferable sensitivity, improves product quality.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that.
A kind of oxygen sensor used in vehicle based on insulated by oxide slurry, it includes what stacking from top to bottom was arranged
Sensitive layer matrix, air duct layer, air duct supporter and zone of heating matrix, described sensitive layer matrix
Upper surface is printed with outer working electrode and porous protective layer successively, in the lower surface of this sensitive layer matrix is printed with
Working electrode, on described air duct layer, corresponding described interior working electrode offers air duct, described heating
The upper surface of layer matrix is printed with the first insulating barrier successively, adds thermode and the second insulating barrier, described zone of heating
The lower surface of matrix is printed with the 3rd insulating barrier and heating conductive pin, described outer working electrode and interior work successively
Make electrode to draw hole by conduction and be electrically connected with, described in add thermode and heating conductive pin to draw hole by conduction electric
Property connect, wherein, described first insulating barrier, the second insulating barrier and the 3rd insulating barrier are made up of insulation paste,
Described insulation paste includes the material of following weight portion: the inorganic particle 4-6 part being made up of oxide, has airborne
Body 2-4 part, auxiliary agent 1-3 part.
Preferably, described insulation paste includes the material of following weight portion: inorganic particle 5 parts, organic carrier 3
Part, auxiliary agent 2 parts, wherein, described inorganic particle includes the material of following weight portion: aluminium oxide 20 parts, oxygen
Changing zirconium 1 part, wherein aluminium oxide is the aluminium oxide of α phase low-temperature sintered alumina 6 parts and γ phase particle diameter ＜ 15nm
The mixture of 14 parts；Described organic carrier is the mixed liquor after water bath processing, and this organic carrier includes following heavy
The material of amount part: terpineol 25 parts, ethyl cellulose 1 part；Described auxiliary agent includes the material of following weight portion:
Dispersant 6 parts, binding agent 3 parts, levelling agent 3 parts, thixotropic agent 1 part.
Preferably, the thickness of described sensitive layer matrix is: 0.5-0.7mm, and the thickness of described air duct layer is
0.3-0.4mm, the thickness of described air duct supporter is 0.2-0.3mm, the thickness of described zone of heating matrix
For 0.5-0.7mm.
Preferably, described in add the thickness of thermode be 10-15 μm, described outer working electrode and interior working electrode
Thickness is 10-15 μm, and the thickness of described first insulating barrier, the second insulating barrier and the 3rd insulating barrier is
30-35 μm, porous protective layer thickness is 70-80 μm.
A kind of oxygen sensor used in vehicle manufacture method based on insulated by oxide slurry, it comprises the steps: step
Rapid S1, prepares insulation paste, and described insulation paste includes the material of following weight portion: inorganic particle 4-6 part,
Organic carrier 2-4 part, auxiliary agent 1-3 part, inorganic particle, organic carrier and auxiliary agent are mixed, and uses planet
Obtaining insulation paste after ball mill ball milling, when its physical property is temperature 25 DEG C, viscosity is 100 ± 20Pa s, attached
Put forth effort as 12N/mm2, resistivity is 3.1x 1012Ω·cm；Step S2, utilizes blanking die, by sensitivity
Layer matrix, air duct layer, air duct supporter and zone of heating matrix press preset thickness cut-parts respectively, then
Stamping-out hole, location and conduction draw hole, afterwards to air duct layer stamping-out air duct respectively；Step S3, utilizes
Screen printing apparatus, the upper surface at zone of heating matrix prints the first insulating barrier successively, adds thermode and second
Insulating barrier, the lower surface at zone of heating matrix prints the 3rd insulating barrier and heating conductive pin successively, in sensitivity
The upper surface of layer matrix prints outer working electrode and porous protective layer successively, and the lower surface at sensitive layer matrix prints
Working electrode in brush；Step S4, by sensitive layer matrix, air duct layer, air duct supporter and heating
Layer matrix stacks gradually, and utilizes temperature isostatic pressing machine under vacuum with preset pressure lamination, uses stamping-out afterwards
Grinding tool stamping-out becomes pre-set dimension, obtains sensor green compact；Step S5, sensor green compact covers porous and holds burning
Pressing plate, sinters with sintering furnace.
Preferably, in described step S1, described insulation paste includes the material of following weight portion: inorganic particle
5 parts, organic carrier 3 parts, auxiliary agent 2 parts, wherein, described inorganic particle includes the material of following weight portion:
Aluminium oxide 20 parts, zirconium oxide 1 part, wherein aluminium oxide is α phase low-temperature sintered alumina 6 parts and γ phase particle diameter
The mixture of the aluminium oxide of ＜ 15nm 14 parts；Described organic carrier is the mixed liquor after water bath processing, and this has
Airborne body includes the material of following weight portion: terpineol 25 parts, ethyl cellulose 1 part；Described auxiliary agent includes
The material of following weight portion: dispersant 6 parts, binding agent 3 parts, levelling agent 3 parts, thixotropic agent 1 part；Should
In step, it is first temperature 80 DEG C in water-bath, under the conditions of time 8h or magnetic agitation 3h, prepares terpineol
With the mixed solution of ethyl cellulose, add inorganic particle and dispersant afterwards, utilize planetary ball mill to turn
Speed is 250r/min ball milling 12 hours, is sequentially added into binding agent, levelling agent, thixotropic agent afterwards, with rotating speed is
250r/min ball milling 24 hours, obtains insulation paste, and when its physical property is temperature 25 DEG C, viscosity is 100
± 20Pa s, adhesive force is 12N/mm2, resistivity is 3.1 x 1012Ω·cm。
Preferably, in described step S2, first with vacuum packing machine, each zirconium oxide curtain coating green compact upper,
Lower both sides add corrosion resistant plate, and recycling pellosil carries out vacuum coater, and utilization temperature isostatic pressing machine with pressure is
8-15MPa, temperature be 70 DEG C under the conditions of pressurize 10 minutes, more respectively to sensitive layer matrix, air duct layer,
Air duct supporter and zone of heating matrix carry out cut-parts.
Preferably, in described step S2, the thickness of described sensitive layer matrix is: 0.5-0.7mm, described sky
The thickness of gas channel layer is 0.3-0.4mm, and the thickness of described air duct supporter is 0.2-0.3mm, described
The thickness of zone of heating matrix is 0.5-0.7mm.
Preferably, in described step S3, described in add the thickness of thermode be 10-15 μm, described outer working electrode
It is 10-15 μm, described first insulating barrier, the second insulating barrier and the 3rd insulation with the thickness of interior working electrode
The thickness of layer is 30-35 μm, and protective layer thickness is 70-80 μm；In described step S4, described sensitivity
After layer matrix, air duct layer, air duct supporter and zone of heating matrix stack gradually, use stainless steel clamp
Plate is with 0.4-0.6Mpa pressure precompressed, and recycling pellosil carries out vacuum coater, and temperature isostatic pressing machine parameter is arranged
For pressure 8-15Mpa, temperature 70 C, the dwell time is 8-15min, becomes sensing with blanking die stamping-out afterwards
Device green compact, a length of 60mm of these sensor green compact, width is 5mm.
Preferably, in described step S5, described porous hold burning pressing plate be thickness be the porous oxygen of 0.5-0.8mm
Changing aluminum load bearing board, described sintering furnace is Si-Mo rod sintering furnace, sinters 2 hours with temperature for 1450-1550 DEG C.
In oxygen sensor used in vehicle based on insulated by oxide slurry disclosed by the invention, the first insulating barrier, second
Insulating barrier and the 3rd insulating barrier are made up of insulation paste, and insulation paste includes the material of following weight portion: by oxygen
Inorganic particle 4-6 part that compound is constituted, organic carrier 2-4 part, auxiliary agent 1-3 part.This oxygen sensor used in vehicle
Each layer matrix, especially insulating barrier all use oxide to make, the sinter bonded degree that each base layer has had,
And this sensor has preferable sensitivity, simultaneously, it is not necessary to the toxic solvent such as butanone, dimethylbenzene, it is to avoid
Because human body is worked the mischief by noxious substance.
Accompanying drawing explanation
Fig. 1 is the exploded view of oxygen sensor used in vehicle.
Detailed description of the invention
With embodiment, the present invention is described in more detail below in conjunction with the accompanying drawings.
The invention discloses a kind of oxygen sensor used in vehicle based on insulated by oxide slurry, as it is shown in figure 1, its
Include the sensitive layer matrix 3 of the setting of stacking from top to bottom, air duct layer 5, air duct supporter 6 and
Zone of heating matrix 9, the upper surface of sensitive layer matrix 3 is printed with outer working electrode 2 and porous protective layer 1 successively,
The lower surface of this sensitive layer matrix 3 is printed with interior working electrode 4, corresponding interior working electrode on air duct layer 5
4 offer air duct, and the upper surface of zone of heating matrix 9 is printed with the first insulating barrier 12 successively, adds thermoelectricity
Pole 8 and the second insulating barrier 7, the lower surface of zone of heating matrix 9 is printed with the 3rd insulating barrier 10 and heating successively
Conductive pin 11, outer working electrode 2 draws hole with interior working electrode 4 by conduction and is electrically connected with, adds thermode
8 draw hole with heating conductive pin 11 by conduction is electrically connected with, wherein,
Sensitive layer matrix 3, air duct layer 5, air duct supporter 6 and zone of heating matrix 9 are starched by curtain coating
Material is made, and casting slurry includes the material of following weight portion: Zirconium powder 5-7 part, organic solvent 3-5 part,
Auxiliary agent 0.5-1.5 part；
First insulating barrier the 12, second insulating barrier 7 and the 3rd insulating barrier 10 are made up of insulation paste, insulation paste
Material including following weight portion: the inorganic particle 4-6 part being made up of oxide, organic carrier 2-4 part, helps
Agent 1-3 part；
Porous protective layer 1 is made up of protective paste, and protective paste includes the material of following weight portion: oxide
3-5 part, pore creating material 1-3 part, organic carrier 1-3 part, auxiliary agent 0.5-1.5 part.
Each layer matrix of above-mentioned oxygen sensor used in vehicle all uses zirconia material to make, in sintering process, and each base
The sinter bonded degree that body layer has had, especially air duct layer, it is not necessary in air duct fill carbon dust,
The Organic substances such as starch, it is to avoid affect the sensitivity of sensor because residue is present in air duct.Above-mentioned knot
While structure can ensure that air duct size, reduce different to air duct cavity when processed sensor green compact
The filling of thing, it is to avoid foreign body burns the residual of excess after sintering, extends the service life of sensor.This is automobile-used
The manufacture method of oxygen sensor comprises the steps:
Step S1, prepares casting slurry, and casting slurry includes the material of following weight portion: Zirconium powder 5-7
Part, organic solvent 3-5 part, auxiliary agent 0.5-1.5 part, utilize planetary ball mill ball milling casting slurry, use afterwards
Casting machine is cast, formed zirconium oxide curtain coating green compact, with zirconium oxide curtain coating green compact make sensitive layer matrix 3,
Air duct layer 5, air duct supporter 6 and zone of heating matrix 9；
Preparing insulation paste, insulation paste includes the material of following weight portion: inorganic particle 4-6 part, has airborne
Body 2-4 part, auxiliary agent 1-3 part, inorganic particle, organic carrier and auxiliary agent are mixed, and uses planetary ball mill
Obtaining insulation paste after ball milling, when its physical property is temperature 25 DEG C, viscosity is 100 ± 20Pa s, and adhesive force is
12N/mm2, resistivity is 3.1 x 1012Ω·cm；
Preparing protective paste, protective paste includes the material of following weight portion: oxide 3-5 part, pore creating material
1-3 part, organic carrier 1-3 part, auxiliary agent 0.5-1.5 part, by oxide, pore creating material, organic carrier 1-3 part
Mixing with auxiliary agent, and obtain protective paste after planetary ball mill ball milling, this protective paste is 25 in temperature
DEG C time viscosity be 300 ± 50Pa s, adhesive force is 12N/mm2；
Step S2, utilizes blanking die, by sensitive layer matrix 3, air duct layer 5, air duct supporter
6 and zone of heating matrix 9 respectively by preset thickness cut-parts, then stamping-out hole, location and conduction draw hole respectively, the most right
Air duct layer 5 stamping-out air duct；
Step S3, utilizes screen printing apparatus, and the upper surface at zone of heating matrix 9 prints the first insulation successively
Layer 12, add thermode 8 and the second insulating barrier 7, it is exhausted that the lower surface at zone of heating matrix 9 prints the 3rd successively
Edge layer 10 and heating conductive pin 11, the upper surface at sensitive layer matrix 3 prints outer working electrode 2 He successively
Porous protective layer 1, working electrode 4 in the lower surface of sensitive layer matrix 3 prints；
Step S4, by sensitive layer matrix 3, air duct layer 5, air duct supporter 6 and zone of heating matrix
9 stack gradually, and utilize temperature isostatic pressing machine under vacuum with preset pressure lamination pressing, grind with stamping-out afterwards
Tool stamping-out becomes pre-set dimension, obtains sensor green compact；
Step S5, sensor green compact covers porous and holds burning pressing plate, sinter with sintering furnace.
In order to the concrete technical scheme of the present invention is better described, the present invention is about above-mentioned casting slurry, insulation
Slurry and protective paste proposition below embodiment:
Embodiment 1:
In the present embodiment, casting slurry includes the material of following weight portion: Zirconium powder 6 parts, You Jirong
Agent 4 parts, auxiliary agent 1 part, particle diameter ＜ 1 μm of Zirconium powder, wherein,
Organic solvent includes the material of following weight portion: analytical pure acetic acid fat and/or 7 parts of acetic acid the third fat, point
Analysis straight alcohol and/or isobutanol 3 parts, the organic solvent in the present invention, have employed avirulent acetic acid fat and/
Or acetic acid the third fat and ethanol and/or isobutanol, its compared to existing technology in use butanone, dimethylbenzene etc. poisonous
For the mode of solvent, it is to avoid the pollution to environment and the harm to health；
Auxiliary agent includes the material of following weight portion: dispersant 1 part, binding agent 7 parts, plasticizer 1 part.
Wherein, curtain coating auxiliary agent is that imported from America PVB makees binding agent, and its vitrification point is 62-72 DEG C, has
The strongest caking property, can reduce green sheet isostatic pressed overlapping pressure and laminate the time, dividing with triethanolamine
Powder, Shou Nuo company of the U.S. provides model to be that S2075 reagent makees plasticizer.
Embodiment 2:
In the present embodiment, insulation paste includes the material of following weight portion: inorganic particle 5 parts, organic carrier 3
Part, auxiliary agent 2 parts, wherein,
Inorganic particle includes the material of following weight portion: aluminium oxide 20 parts, zirconium oxide 1 part, wherein aluminium oxide
Mixture for α phase low-temperature sintered alumina 6 parts He the aluminium oxide 14 parts of γ phase particle diameter ＜ 15nm；
Organic carrier is the mixed liquor after water bath processing, and this organic carrier includes the material of following weight portion: pine
Oleyl alcohol 25 parts, ethyl cellulose 1 part；
Auxiliary agent includes the material of following weight portion: dispersant 6 parts, binding agent 3 parts, levelling agent 3 parts, touches
Become agent 1 part.
Embodiment 3:
In the present embodiment, protective paste includes the material of following weight portion: oxide 4 parts, pore creating material 2 parts,
Organic carrier 2 parts, auxiliary agent 1 part, wherein,
Oxide includes the mixing of one or more of following weight portion material: aluminium oxide 20 parts, zirconium oxide 1
Part, magnesium oxide 1 part, silicon oxide 1 part；
Pore creating material be particle size range be the nano-carbon powder of 0.1 μm-1 μm；
Organic carrier includes the material of following weight portion: terpineol 58 parts, ethyl cellulose 25 parts, ethanol 2
Part；
Auxiliary agent includes the material of following weight portion: binding agent 6 parts, dispersant 3 parts, plasticizer 3 parts, stream
Flat agent 1 part.
About the manufacture method of this oxygen sensor used in vehicle based on insulated by oxide slurry, the present invention proposes as follows
Embodiment:
Embodiment 4:
In the present embodiment, in step S1, casting slurry includes the material of following weight portion: Zirconium powder 6
Part, organic solvent 4 parts, auxiliary agent 1 part, particle diameter ＜ 1 μm of Zirconium powder, wherein,
Organic solvent includes the material of following weight portion: analytical pure acetic acid fat and/or 7 parts of acetic acid the third fat, point
Analysis straight alcohol and/or isobutanol 3 parts；
Auxiliary agent includes the material of following weight portion: dispersant 1 part, binding agent 7 parts, plasticizer 1 part；
In this step, first Zirconium powder, organic solvent and dispersant are mixed by above-mentioned weight,
Utilize planetary ball mill with rotating speed for 250r/min ball milling 15 hours, add binding agent and plasticizer afterwards, with
Rotating speed is 250r/min ball milling 12 hours, by casting slurry froth in vacuum after ball milling, utilizes casting machine to flow
Prolong, obtain zirconium oxide curtain coating green compact.
Embodiment 5:
In the present embodiment, in step S1, insulation paste includes the material of following weight portion: inorganic particle 5 parts,
Organic carrier 3 parts, auxiliary agent 2 parts, wherein,
Inorganic particle includes the material of following weight portion: aluminium oxide 20 parts, zirconium oxide 1 part, wherein aluminium oxide
Mixture for α phase low-temperature sintered alumina 6 parts He the aluminium oxide 14 parts of γ phase particle diameter ＜ 15nm；
Organic carrier is the mixed liquor after water bath processing, and this organic carrier includes the material of following weight portion: pine
Oleyl alcohol 25 parts, ethyl cellulose 1 part；
Auxiliary agent includes the material of following weight portion: dispersant 6 parts, binding agent 3 parts, levelling agent 3 parts, touches
Become agent 1 part；
In this step, under the conditions of water-bath is temperature 80 DEG C, first prepare the mixing of terpineol and ethyl cellulose
Solution, adds inorganic particle and dispersant afterwards, utilizes planetary ball mill with rotating speed for 250r/min ball milling 12
Hour, add binding agent, levelling agent, thixotropic agent afterwards, with rotating speed for 250r/min ball milling 24 hours,
To insulation paste, when its physical property is temperature 25 DEG C, viscosity is 100 ± 20Pa s, and adhesive force is 12N/mm2,
Resistivity is 3.1 x 1012Ω·cm。
Embodiment 6
In the present embodiment, in step S1, protective paste includes the material of following weight portion: oxide 4 parts,
Pore creating material 2 parts, organic carrier 2 parts, auxiliary agent 1 part, wherein,
Oxide includes the mixing of one or more of following weight portion material: aluminium oxide 20 parts, zirconium oxide 1
Part, magnesium oxide 1 part, silicon oxide 1 part；
Pore creating material be particle size range be the nano-carbon powder of 0.1 μm-1 μm；
Organic carrier includes the material of following weight portion: terpineol 58 parts, ethyl cellulose 25 parts, ethanol 2
Part；
Auxiliary agent includes the material of following weight portion: binding agent 6 parts, dispersant 3 parts, plasticizer 3 parts, stream
Flat agent 1 part；
In this step, by oxide, organic carrier and dispersant, the planetary ball mill is utilized with rotating speed to be
250r/min ball milling 12 hours, is subsequently adding binding agent, plasticizer and levelling agent, afterwards with rotating speed as 250r/min
Ball milling 12 hours, obtains protective paste, this protective paste temperature be viscosity when 25 DEG C be 300 ± 50Pa s,
Adhesive force is 12N/mm2.In the present embodiment, porous protective layer 1 hole aperture reaches 0.5-10 μm, hole
Degree reaches 5-50%, is a kind of single layer structure, has stronger adhesion with electrode, and its advantage is can be effective
Protection gasoline in harmful substance the corrosion of electrode surface is affected its catalytic action, and shock resistance is good,
Life-span is long, and cost supports, and processing technology is simple.
Embodiment 7:
In the present embodiment, in step S2, first with vacuum packing machine, each zirconium oxide curtain coating green compact upper,
Lower both sides add corrosion resistant plate, and recycling pellosil carries out vacuum coater, and utilization temperature isostatic pressing machine with pressure is
8-15MPa, temperature be 70 DEG C under the conditions of pressurize 10 minutes, more respectively to sensitive layer matrix 3, air duct
Layer 5, air duct supporter 6 and zone of heating matrix 9 carry out cut-parts, and the thickness of sensitive layer matrix 3 is:
0.5-0.7mm, the thickness of air duct layer 5 is 0.3-0.4mm, and the thickness of air duct supporter 6 is
0.2-0.3mm, the thickness of zone of heating matrix 9 is 0.5-0.7mm.
Embodiment 8:
In the present embodiment, in step S3, the thickness adding thermode 8 is 10-15 μm, outer working electrode 2 He
The thickness of interior working electrode 4 is 10-15 μm, the first insulating barrier the 12, second insulating barrier 7 and the 3rd insulation
The thickness of layer 10 is 30-35 μm, and porous protective layer thickness is 70-80 μm, and therein printing electrode makes guarantor
Card connects complete, without open circuit, short circuit, slurry prints halo-free dye phenomenon, printing printing insulating barrier, protective layer,
Keep any surface finish smooth during electrode layer, flawless, granule foreign；
In step S4, sensitive layer matrix 3, air duct layer 5, air duct supporter 6 and zone of heating base
After body 9 stacks gradually, carry out very with 0.4-0.6Mpa pressure precompressed, recycling pellosil with rustless steel clamping plate
Empty cladding, temperature isostatic pressing machine parameter is set to pressure 8-15Mpa, temperature 70 C, and the dwell time is 8-15min,
Becoming sensor green compact with blanking die stamping-out afterwards, a length of 60mm of these sensor green compact, width is 5mm；
In the present embodiment, use corrosion resistant plate to add pellosil upper and lower stake pad substrate when packaging, sky can be effectively ensured
Gas channel size is complete, and without filling the foreign body such as carbon dust, starch.
In step S5, porous hold burning pressing plate be thickness be the Woelm Alumina load bearing board of 0.5-0.8mm, sintering
Stove is Si-Mo rod sintering furnace, sinters 2 hours with temperature for 1450-1550 DEG C.
In oxygen sensor used in vehicle disclosed by the invention, sensitive layer matrix 3, air duct layer 5, air duct prop up
Support body 6 and zone of heating matrix 9 are made up of casting slurry, and casting slurry includes the material of following weight portion: oxygen
Change zirconium powder body 5-7 part, organic solvent 3-5 part, auxiliary agent 0.5-1.5 part；First insulating barrier 12, second insulate
Layer 7 and the 3rd insulating barrier 10 are made up of insulation paste, and insulation paste includes the material of following weight portion: inorganic
Powder body 4-6 part, organic carrier 2-4 part, auxiliary agent 1-3 part；Porous protective layer 1 is made up of protective paste, protects
Protect slurry and include the material of following weight portion: oxide 3-5 part, pore creating material 1-3 part, organic carrier 1-3 part,
Auxiliary agent 0.5-1.5 part.Each layer matrix of this oxygen sensor used in vehicle all uses zirconia material to make, sintering process
In, the sinter bonded degree that each base layer has had, especially air duct layer, it is not necessary to fill out in air duct
Fill the Organic substance such as carbon dust, starch, it is to avoid affect the sensitivity of sensor because residue is present in air duct.
Meanwhile, the organic solvent in the present invention, have employed avirulent acetic acid fat and/or acetic acid the third fat and ethanol
And/or isobutanol, its compared to existing technology in use the toxic solvent such as butanone, dimethylbenzene mode for, keep away
The pollution to environment and the harm to health are exempted from.
It is more than preferred embodiment of the present invention, is not limited to the present invention, all technology in the present invention
In the range of amendment, equivalent or the improvement etc. made, should be included in the range of the present invention protected.
Claims (2)
1. an oxygen sensor used in vehicle based on insulated by oxide slurry, it is characterized in that, include the sensitive layer matrix that stacking from top to bottom is arranged, air duct layer, air duct supporter and zone of heating matrix, the upper surface of described sensitive layer matrix is printed with outer working electrode and porous protective layer successively, the lower surface of this sensitive layer matrix is printed with interior working electrode, on described air duct layer, corresponding described interior working electrode offers air duct, the upper surface of described zone of heating matrix is printed with the first insulating barrier successively, add thermode and the second insulating barrier, the lower surface of described zone of heating matrix is printed with the 3rd insulating barrier and heating conductive pin successively, described outer working electrode draws hole with interior working electrode by conduction and is electrically connected with, the described thermode that adds draws hole electric connection with heating conductive pin by conduction, wherein,
Described first insulating barrier, the second insulating barrier and the 3rd insulating barrier are made up of insulation paste, and described insulation paste includes the material of following weight portion: inorganic particle 5 parts, organic carrier 3 parts, auxiliary agent 2 parts, wherein,
Described inorganic particle includes the material of following weight portion: aluminium oxide 20 parts, zirconium oxide 1 part, wherein aluminium oxide is the mixture of α phase low-temperature sintered alumina 6 parts and the aluminium oxide 14 parts of γ phase particle diameter ＜ 15nm；
Described organic carrier is the mixed liquor after water bath processing, and this organic carrier includes the material of following weight portion: terpineol 25 parts, ethyl cellulose 1 part；
Described auxiliary agent includes the material of following weight portion: dispersant 6 parts, binding agent 3 parts, levelling agent 3 parts, thixotropic agent 1 part；
The thickness of described sensitive layer matrix is: 0.5-0.7mm, and the thickness of described air duct layer is 0.3-0.4mm, and the thickness of described air duct supporter is 0.2-0.3mm, and the thickness of described zone of heating matrix is 0.5-0.7mm；
The described thickness adding thermode is 10-15 μm, and the thickness of described outer working electrode and interior working electrode is 10-15 μm, and the thickness of described first insulating barrier, the second insulating barrier and the 3rd insulating barrier is 30-35 μm, and protective layer thickness is 70-80 μm.
2. an oxygen sensor used in vehicle manufacture method based on insulated by oxide slurry, it is characterised in that comprise the steps:
Step S1, prepare insulation paste, described insulation paste includes the material of following weight portion: inorganic particle 5 parts, organic carrier 3 parts, auxiliary agent 2 parts, mixes inorganic particle, organic carrier and auxiliary agent, and obtains insulation paste after planetary ball mill ball milling, when its physical property is temperature 25 DEG C, viscosity is 100 ± 20Pa s, and adhesive force is 12N/mm2, resistivity is 3.1x 1012Ω·cm；
Step S2, utilizes blanking die, and by sensitive layer matrix, air duct layer, air duct supporter and zone of heating matrix respectively by preset thickness cut-parts, then stamping-out hole, location and conduction draw hole, afterwards to air duct layer stamping-out air duct respectively；
Step S3; utilize screen printing apparatus; upper surface at zone of heating matrix prints the first insulating barrier successively, adds thermode and the second insulating barrier; lower surface at zone of heating matrix prints the 3rd insulating barrier and heating conductive pin successively; upper surface at sensitive layer matrix prints outer working electrode and porous protective layer successively, working electrode in the lower surface of sensitive layer matrix prints；
Step S4, stacks gradually sensitive layer matrix, air duct layer, air duct supporter and zone of heating matrix, utilizes temperature isostatic pressing machine under vacuum with preset pressure lamination, becomes pre-set dimension with stamping-out grinding tool stamping-out afterwards, obtain sensor green compact；
Step S5, sensor green compact covers porous and holds burning pressing plate, sinter with sintering furnace；
In described step S1, described inorganic particle includes the material of following weight portion: aluminium oxide 20 parts, zirconium oxide 1 part, wherein aluminium oxide is the mixture of α phase low-temperature sintered alumina 6 parts and the aluminium oxide 14 parts of γ phase particle diameter ＜ 15nm；
Described organic carrier is the mixed liquor after water bath processing, and this organic carrier includes the material of following weight portion: terpineol 25 parts, ethyl cellulose 1 part；
Described auxiliary agent includes the material of following weight portion: dispersant 6 parts, binding agent 3 parts, levelling agent 3 parts, thixotropic agent 1 part；
In this step, first it is temperature 80 DEG C in water-bath, prepare the mixed solution of terpineol and ethyl cellulose under the conditions of time 8h or magnetic agitation 3h, add inorganic particle and dispersant afterwards, utilize planetary ball mill with rotating speed for 250r/min ball milling 12 hours, add binding agent, levelling agent and thixotropic agent afterwards, with rotating speed for 250r/min ball milling 24 hours, obtain insulation paste, when its physical property is temperature 25 DEG C, viscosity is 100 ± 20Pa s, and adhesive force is 12N/mm2, resistivity is 3.1x1012Ω·cm；
In described step S2, first with vacuum packing machine, corrosion resistant plate is added in the upper and lower both sides of each zirconium oxide curtain coating green compact, recycling pellosil carries out vacuum coater, utilize temperature isostatic pressing machine with pressure as 8-15MPa, temperature be 70 DEG C under the conditions of pressurize 10 minutes, more respectively sensitive layer matrix, air duct layer, air duct supporter and zone of heating matrix are carried out cut-parts；
In described step S2, the thickness of described sensitive layer matrix is: 0.5-0.7mm, and the thickness of described air duct layer is 0.3-0.4mm, and the thickness of described air duct supporter is 0.2-0.3mm, and the thickness of described zone of heating matrix is 0.5-0.7mm；
In described step S3; the described thickness adding thermode is 10-15 μm; the thickness of described outer working electrode and interior working electrode is 10-15 μm, and the thickness of described first insulating barrier, the second insulating barrier and the 3rd insulating barrier is 30-35 μm, and porous protective layer thickness is 70-80 μm；
In described step S4, after described sensitive layer matrix, air duct layer, air duct supporter and zone of heating matrix stack gradually, with rustless steel clamping plate with 0.4-0.6Mpa pressure precompressed, recycling pellosil carries out vacuum coater, and temperature isostatic pressing machine parameter is set to pressure 8-15Mpa, temperature 70 C, dwell time is 8-15min, becoming sensor green compact with blanking die stamping-out afterwards, a length of 60mm of these sensor green compact, width is 5mm；
In described step S5, described porous hold burning pressing plate be thickness be the Woelm Alumina load bearing board of 0.5-0.8mm, described sintering furnace is Si-Mo rod sintering furnace, with temperature for 1450-1550 DEG C sinter 2 hours.
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| CN106706743A (en) * | 2016-12-30 | 2017-05-24 | 莱鼎电子材料科技有限公司 | Novel chip type potentiometric automobile oxygen sensor and preparation method thereof |
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| CN102786294A (en) * | 2012-07-16 | 2012-11-21 | 中国科学院宁波材料技术与工程研究所 | Insulating layer slurry of chip-type oxygen sensor and insulating layer preparation method |
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| CN101042366A (en) * | 2007-04-24 | 2007-09-26 | 谢光远 | Manufacturing method of plate type oxygen sensor chip |
| CN101995426A (en) * | 2009-08-14 | 2011-03-30 | 比亚迪股份有限公司 | Chip type oxygen sensor and preparation method thereof |
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