CN103951421A - Casting slurry and method for preparing zirconia substrate for NOx sensor by using same - Google Patents
Casting slurry and method for preparing zirconia substrate for NOx sensor by using same Download PDFInfo
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- CN103951421A CN103951421A CN201410169463.0A CN201410169463A CN103951421A CN 103951421 A CN103951421 A CN 103951421A CN 201410169463 A CN201410169463 A CN 201410169463A CN 103951421 A CN103951421 A CN 103951421A
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Abstract
The invention relates to casting slurry. The casting slurry is characterized by comprising the following components: ceramic powder, a solvent, a binder, a dispersing agent and a plasticizer in a mass ratio of 100:(60-75):(8-20):(1-8):(5-10). A casting substrate of an NOx sensor, which has better surface conditions, has thickness of 0.15-0.5mm and is suitable for a six-layer structure, can be formed by applying the casting slurry to preparation of a zirconia substrate for the NOx sensor, thus meeting the operating requirements of the sensor. The invention also provides a method for preparing the zirconia substrate for the NOx sensor by using the casting slurry. The method is simple in preparation process, provides a key sensitive part and a support for the NOx sensor for cars, can be used for preparing casting substrates in different thickness, and is applied to other fields needing ceramic laminated structures.
Description
Technical field
The present invention relates to automobile NOx sensor development field, be particularly directed to the material of NOx sensor, relate in particular to a kind of casting slurry and use this casting slurry to prepare the method for the zirconium oxide substrate that NOx sensor uses.
Background technology
Current automobile industry develops rapidly, and problem of environmental pollution is day by day serious, and people's environmental consciousness and the specification of quality of living environment is improved day by day, therefore also thereupon further strict for the standard of motor vehicle exhaust.Propelling along with China state four emission standards, standard for particulate matter in vehicle exhaust (PM2.5) and NOx gas purging is more and more tighter, general automotive oxygen sensor can not meet emission standard, therefore need special NOx sensor accurately to detect the NOx gas in vehicle exhaust, and then signal is passed to automobile ECU, then instruct SCR system to process vehicle exhaust, and then reduce NOx gas purging.When preparation NOx sensor, the good crucial sensitive compressible members-zirconium oxide substrate of over-all properties is the basis of whole sensor, and the well behaved zirconium oxide substrate of development research is very important.
The structure of the NOx sensor that application is at present maximum as shown in Figure 1, is comprised of 1～6 stack of six layers of zirconium oxide substrate, and it includes two gas compartments, a reference gas passage, a heating member, three blocking buffer layers, 3 oxygen pumping cells, 3 these special batteries of energy.
In the first gas compartment, there are an oxygen pumping cell and this special battery of energy, tail gas enters the first gas compartment by first and second blocking buffer layer, at the first gas compartment, by this special battery feedback control first oxygen pumping cell of energy, worked, make the oxygen concentration of the first gas compartment lower than 50ppm, following reaction occur:
There is the very tail gas of low oxygen concentration and through the 3rd blocking buffer layer, enter the second gas compartment again, in the second gas compartment, there are 2 oxygen pumping cells and 2 these special batteries of energy, one of them oxygen pumping cell is service pump oxygen cell, further makes the oxygen concentration of the second Room reduce, to 6*10-3ppm left and right, second oxygen pumping cell is exactly the test battery of NOx sensor, because the oxygen of the second Room is constantly walked by pump, the balance of NO and O2 is broken, there is following reaction:
Near the potential electrode of the second gas compartment, the oxygen of decomposition is constantly pumped out, and will produce like this pump oxygen electric current, i.e. Ip2, and this electric current also just corresponds to the concentration of NOx gas.
And in order to obtain the test result that tolerance range is high, higher to the requirement of the properties of zirconium oxide substrate, the specific conductivity of requirement is also higher, therefore develop the zirconium oxide substrate of a kind of NOx of being applicable to sensor requirement, is very important.
At present, the method of preparing zirconium oxide substrate generally adopts doctor-blade casting process, because this method is simple to operate, be easy to industrialization, be widely used, but be all much to adopt curtain coating to become the biscuit sheet of thinner (20-70 μ m), and then prepared by the method that laminates into the biscuit substrate of desired thickness, complex process so not only, efficiency is low, and substrate is easily layering also.
So a kind of technique is simple, efficiency is high, can one time the curtain coating surfacing that goes out cast sheet and the cast sheet of desired thickness, the casting slurry that properties meets the service requirements of NOx sensor is extremely to have practical value.
Summary of the invention:
To an object of the present invention is in order addressing the above problem, a kind of cast sheet that can be used in zirconium oxide substrate that preparation NOx sensor uses, can form the good thickness of surface appearance the NOx sensor that is 0.15～0.5mm, be applicable to six layers of structure to be provided, to meet the casting slurry of sensor service requirements.
The casting slurry of the zirconium oxide substrate of using for the preparation of NOx sensor provided by the invention, has following characteristics, comprises following composition:
Ceramic powder, solvent, binding agent, dispersion agent, softening agent, the mass ratio of these described compositions is 100:60～75:8～20:1～8:5～10.
Preferably, the Zirconium powder that described ceramic powder is 4～8% for doped yttrium oxide molar fraction, the mean particle size of described Zirconium powder is 0.1～1.5 μ m, specific surface area is 7～9m
2/ g, purity is more than 99%.
More preferably, in described casting slurry, zirconic solid content is 70%～85%, is 75%～80% best.
Preferably, described solvent is the mixture of butanone and dehydrated alcohol, and the mass ratio of described butanone and described dehydrated alcohol is 0.5～1.
Preferably, described dispersion agent is trolamine.
Preferably, described binding agent is the mixture of ethyl cellulose and polyvinyl butyral acetal, and the mass ratio of polyvinyl butyral acetal and ethyl cellulose is 5～10.Preferably, described softening agent is polyoxyethylene glycol and dibutyl phthalate azeotropic mixture, and the mass ratio of described polyoxyethylene glycol and described dibutyl phthalate is 1:1.
Beneficial effect of the present invention is specifically: the solid content of Zirconium powder in casting slurry adjustment of the present invention, the features such as viscosity, also to the Zirconium powder in slurry, dispersion agent, solvent, binding agent, the usage ratio of fluidizer is adjusted, cooperation in conjunction with casting machine parameter, obtain and a kind ofly can prepare the slurry that goes for the cast sheet that the thickness of six layers of structure NOx sensor (as shown in Figure 1) is 0.15～0.5mm, can one time the curtain coating surfacing that goes out cast sheet and the cast sheet of desired thickness, properties meets the service requirements of NOx sensor, the good zirconium oxide substrate of over-all properties after binder removal sintering, operation is simple.
Another object of the present invention is to provide a kind of simple method of using above-mentioned casting slurry to prepare the zirconium oxide substrate that NOx sensor uses of preparation process.
The above-mentioned casting slurry of use provided by the invention is prepared the method for the zirconium oxide substrate that NOx sensor uses, and comprises following steps:
Step 1: adopt the method for ball milling that the ceramic powder of said components, solvent, dispersion agent are mixed, Ball-milling Time is 12～20h, then adds the binding agent of said components, and softening agent carries out ball milling, and Ball-milling Time is 10～18h, obtains described casting slurry;
Step 2: after described casting slurry vacuum defoamation is processed, on casting machine, to become thickness be the zirconium white green compact film of 0.15～0.5mm to curtain coating, described zirconium white green compact film, according to the scantlings of the structure design requirements cutting of NOx sensor, is prepared to rectangular ceramic green sheet;
Step 3: described zirconium white green sheet, through binder removal, is obtained to ceramic substrate after high temperature sintering.
Preferably, described slurry, after vacuum defoamation is processed, is used rotational viscosimeter to carry out viscosity test, and viscosity is 6000～10000mPas.
Preferably, the thickness of the zirconium white green compact film making is 0.15～0.5mm, and the later stage also can be adjusted into the zirconia film that is applicable to thickness according to actual needs.
Preferably, described rectangular zirconium white green sheet, is positioned on smooth zirconium white substrate, carries out aluminum oxide powder buried powder, puts into draft glue discharging furnace, according to the binder removal program of setting, carries out binder removal.
More preferably, described binder removal program, can be with the temperature rise rate lower than 1 ℃/min, to be warmed up to 400 ℃ from room temperature (25 ℃), insulation, then temperature is risen to 800 ℃, insulation 2h.After binder removal completes, can insert in temperature control high temperature sintering furnace and carry out sintering, according to the sintering procedure of setting.
After sintering, obtain zirconium oxide substrate smooth, shrinking percentage is 15～22%, and thickness is 0.15～0.5mm.The folding strength of zirconium oxide substrate reaches 500～750MPa.Under a normal atmosphere, 800 ℃ time, ceramic substrate resistivity is less than 10 Ω m.
Preparation method's manufacture craft of the present invention is simple, for preparing the NOx sensor that automobile uses, provides crucial sensitive compressible members and supporter, but also can be produced according to the present invention goes out the cast sheet of different thickness, is applied to the field that other need laminated ceramic.
Accompanying drawing explanation
Fig. 1 is six layers of structure of the NOx sensor that formed by zirconium oxide substrate in prior art.
Embodiment
Below in conjunction with accompanying drawing, specific embodiment of the invention method is described further.
Embodiment
A curtain coating preparation method for the zirconium oxide substrate that NOx sensor is used, concrete steps are as follows:
Step 1: getting Zirconium powder 1000g that doping oxidation Yttrium molar fraction is 5% and the zirconia ball of a certain amount of different diameter and putting into the ball grinder that liner is tetrafluoroethylene, by example prepares for 1:1 in mass ratio butanone and dehydrated alcohol 700g, add and account for powder quality than the triethanolamine solution that is 1%～8%, ball milling 18h on planetary ball mill.
Step 2: in the slurry after ball milling 18h, put into the binding agent of 100g, binding agent is the mixture that polyvinyl butyral acetal and ethyl cellulose mass ratio are 5～10.Then put into the azeotropic mixture that polyoxyethylene glycol and dibutyl phthalate mass ratio are 1:1 some, on planetary ball mill, carry out again ball milling 10h.
Step 3: the slurry after ball milling 10h aftertreatment, through standing, after cool to room temperature, poured in vacuum defoamation machine and vacuumized, stirs, and deaeration, until slurry does not observe bubble.
Step 4: get the above-mentioned slurry of a little, carry out viscosity test on rotational viscosimeter, viscosity is 7000mPas.As improper in viscosity, need repeat step 3.
Step 5: the casting slurry preparing is put into the slurry tank of the film band casting machine of long 4.5 meters, adjusted knife up and film tape speed to desired value, open air exhausting device, carry out flow casting molding.The thickness of the film after curtain coating is 0.2mm, and smooth surface, no significant defect.
Step 6: curtain coating each diaphragm is out carried out to gas compartment moulding, and reference gas Slot shaping etc. carry out the printing of each electrode and protective layer insulation layer after processing.
Step 7: the above-mentioned satisfactory diaphragm processing is carried out to lamination processing, wait static pressure to process.
Step 8: wait the lamination after static pressure is processed to cut into single NOx sensor chip according to NOx size sensor profile.
Step 9: above-mentioned NOx sensor chip is carried out to the degreasing sintered NOx sensor ceramic chip that is shaped to according to certain program.Wide 4.2～the 4.5mm of being of NOx sensor making, length is 67.5～68.5mm, and thickness is roughly 1.45～1.55mm, by carrying out function contrast with the NOx sensor of market purchase, can substantially reach NOx gas test function, and precision is ± 25%.
In this specification sheets, the present invention is described with reference to its specific embodiment.But, still can make various modifications and conversion obviously and not deviate from the spirit and scope of the present invention.Therefore, specification sheets is regarded in an illustrative, rather than a restrictive.
Claims (8)
1. a casting slurry, is characterized in that, comprises following composition:
Ceramic powder, solvent, binding agent, dispersion agent, softening agent, the mass ratio of wherein said ceramic powder, described solvent, described binding agent, described dispersion agent, described softening agent is 100:60～75:8～20:1～8:5～10.
2. casting slurry according to claim 1, is characterized in that, described ceramic powder is that doped yttrium oxide molar fraction is 4～8% Zirconium powder, and the mean particle size of described Zirconium powder is 0.1～1.5 μ m, and specific surface area is 7～9m
2/ g, purity is more than 99%.
3. casting slurry according to claim 1, is characterized in that, described solvent is the mixture of butanone and dehydrated alcohol, and the mass ratio of described butanone and described dehydrated alcohol is 0.5～1.
4. casting slurry according to claim 1, is characterized in that, described dispersion agent is trolamine.
5. casting slurry according to claim 1, is characterized in that, described binding agent is the mixture of ethyl cellulose and polyvinyl butyral acetal, and wherein, the mass ratio of described polyvinyl butyral acetal and described ethyl cellulose is 5～10.
6. casting slurry according to claim 1, is characterized in that, described softening agent is polyoxyethylene glycol and dibutyl phthalate azeotropic mixture, and the mass ratio of described polyoxyethylene glycol and described dibutyl phthalate is 1:1.
7. right to use requires 1～6 casting slurry to prepare a method for the zirconium oxide substrate that NOx sensor uses, it is characterized in that:
Step 1: adopt the method for ball milling that the ceramic powder of said components, solvent, dispersion agent are mixed, Ball-milling Time is 12～20h, then adds the binding agent of said components, and softening agent carries out ball milling, and Ball-milling Time is 10～18h, obtains described casting slurry;
Step 2: after described casting slurry vacuum defoamation is processed, on casting machine, to become thickness be the zirconium white green compact film of 0.15～0.5mm to curtain coating, described zirconium white green compact film, according to the scantlings of the structure design requirements cutting of NOx sensor, is prepared to rectangular zirconium white green sheet;
Step 3: described zirconium white green sheet, through binder removal, is obtained to zirconia ceramics substrate after high temperature sintering.
8. method according to claim 7, is characterized in that, described slurry, after vacuum defoamation is processed, is used rotational viscosimeter to carry out viscosity test, and viscosity is 6000～10000mPas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410169463.0A CN103951421A (en) | 2014-04-25 | 2014-04-25 | Casting slurry and method for preparing zirconia substrate for NOx sensor by using same |
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|---|---|---|---|
| CN201410169463.0A CN103951421A (en) | 2014-04-25 | 2014-04-25 | Casting slurry and method for preparing zirconia substrate for NOx sensor by using same |
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| CN104261809A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | Processing method of electronic ceramic tape-casting slurry |
| CN104788096A (en) * | 2015-03-31 | 2015-07-22 | 北京博曼迪汽车科技有限公司 | Tape-casting slurry and preparation method thereof as well as base material, ceramic matrix and oxygen sensor |
| CN105503182A (en) * | 2015-12-18 | 2016-04-20 | 珠海市香之君科技股份有限公司 | Cutter blank forming technology of ceramic surgical blade |
| CN107235716A (en) * | 2017-08-01 | 2017-10-10 | 郑州联冠科技有限公司 | SMD ceramic base casting slurries |
| CN107433670A (en) * | 2017-06-22 | 2017-12-05 | 瑞声科技(新加坡)有限公司 | The preparation method of mobile communication equipment shell |
| CN107433672A (en) * | 2017-06-22 | 2017-12-05 | 瑞声科技(新加坡)有限公司 | The preparation method of mobile communication equipment shell |
| CN107652601A (en) * | 2017-11-02 | 2018-02-02 | 哈尔滨工业大学 | A kind of preparation method of the composite sheet comprising low damage and the SiC nanowire aligned |
| CN107686379A (en) * | 2017-07-25 | 2018-02-13 | 歌尔股份有限公司 | The preparation method of zirconia ceramics with porous layer |
| CN108218422A (en) * | 2018-01-18 | 2018-06-29 | 东莞信柏结构陶瓷股份有限公司 | Wear-resistant ceramic tape casting slurry and its application process |
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| CN110028319A (en) * | 2019-03-28 | 2019-07-19 | 湖北熙田科技有限公司 | Powder granule grading method and Zirconium powder casting slurry and preparation method thereof |
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| CN104261809A (en) * | 2014-09-09 | 2015-01-07 | 登封福中特种电器元件有限公司 | Processing method of electronic ceramic tape-casting slurry |
| CN104788096A (en) * | 2015-03-31 | 2015-07-22 | 北京博曼迪汽车科技有限公司 | Tape-casting slurry and preparation method thereof as well as base material, ceramic matrix and oxygen sensor |
| CN105503182A (en) * | 2015-12-18 | 2016-04-20 | 珠海市香之君科技股份有限公司 | Cutter blank forming technology of ceramic surgical blade |
| CN107433670A (en) * | 2017-06-22 | 2017-12-05 | 瑞声科技(新加坡)有限公司 | The preparation method of mobile communication equipment shell |
| CN107433672A (en) * | 2017-06-22 | 2017-12-05 | 瑞声科技(新加坡)有限公司 | The preparation method of mobile communication equipment shell |
| CN107686379A (en) * | 2017-07-25 | 2018-02-13 | 歌尔股份有限公司 | The preparation method of zirconia ceramics with porous layer |
| CN107235716A (en) * | 2017-08-01 | 2017-10-10 | 郑州联冠科技有限公司 | SMD ceramic base casting slurries |
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| CN110028319A (en) * | 2019-03-28 | 2019-07-19 | 湖北熙田科技有限公司 | Powder granule grading method and Zirconium powder casting slurry and preparation method thereof |
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| CN114685164A (en) * | 2022-04-28 | 2022-07-01 | 武汉市浦翔电子有限公司 | Casting membrane for preparing oxygen sensor chip and preparation process thereof |
| CN115838284A (en) * | 2022-10-08 | 2023-03-24 | 浙江百岸科技有限公司 | Preparation method of water-based casting film belt for nitrogen-oxygen sensor |
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Application publication date: 20140730 |