CN103645221A - Slurry for slits in zirconia base electrochemical NOx sensor chip, and manufacturing method thereof - Google Patents
Slurry for slits in zirconia base electrochemical NOx sensor chip, and manufacturing method thereof Download PDFInfo
- Publication number
- CN103645221A CN103645221A CN201310606881.7A CN201310606881A CN103645221A CN 103645221 A CN103645221 A CN 103645221A CN 201310606881 A CN201310606881 A CN 201310606881A CN 103645221 A CN103645221 A CN 103645221A
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- Prior art keywords
- slit
- sensor chip
- nox sensor
- printing
- filling paste
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title abstract description 3
- 239000002002 slurry Substances 0.000 title abstract 7
- 238000007639 printing Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000000314 lubricant Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical group CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 238000013461 design Methods 0.000 claims description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 5
- 229920002472 Starch Polymers 0.000 claims description 3
- 229920000151 polyglycol Polymers 0.000 claims description 3
- 239000010695 polyglycol Substances 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000001856 Ethyl cellulose Substances 0.000 claims description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 2
- 229920001249 ethyl cellulose Polymers 0.000 claims description 2
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 abstract description 7
- 239000004014 plasticizer Substances 0.000 abstract description 2
- 238000007650 screen-printing Methods 0.000 abstract 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 15
- 239000001301 oxygen Substances 0.000 description 15
- 239000007789 gas Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007784 solid electrolyte Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 101700004678 SLIT3 Proteins 0.000 description 1
- 102100027339 Slit homolog 3 protein Human genes 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention relates to a filling slurry for slits in zirconia base electrochemical NOx sensor chip, and a manufacturing method thereof. The filling slurry is composed of the following components in percentage by weight: 30 to 50% of solvent, 20 to 40% of adhesive, 10 to 20% of filling agent, 10 to 20% of plasticizer, and 10 to 20% of lubricant. The components mentioned above are evenly mixed, and at the temperature of 25 DEG C, the viscosity of the mixture is 4000 to 20000 Pa.s. The preparation method comprises the following steps: in the premise that the slit printing height and the printing thickness of a NOx sensor chip are in a proportional relationship, carrying out printing tests so as to determine the corresponding relationship between the printing thickness of the filling slurry and the slit, determining the printing thickness according to the slit of the NOx sensor chip, designing a screen printing plate according to the printing height so as to obtain the required slit thickness, printing the prepared filling slurry into the slit of the NOx sensor chip through the designed screen printing plate, and then co-sintering the sensor chip and the filling slurry in a furnace, wherein the filling slurry are totally burned off during the co-sintering process. The invention adjusts the diffusion resistance by adjusting the height of the slit.
Description
Technical field
The present invention relates to a kind of zirconia base oxides of nitrogen (NO
x) filling paste and the method for making of sensor chip slit.
Background technology
The detection method of NOx has: ion-selective electrode method, chemoluminescence method, biochemical sensor method, semiconductor transducer method, solid electrolyte amperometric sensor method etc.There have been at present some mechanisms to develop solid electrolyte amperometric sensor industrialization abroad, have been mainly used in the exhaust emissions disposal system of heavy duty diesel engine.The structure of this NOx sensor is slice structure, by six layers of even more multi-layered yttrium stable zirconium oxide YSZ and Al
2o
3potsherd is formed by stacking, and structure and manufacture craft are all very complicated.
A kind of structure and the method for making of inventing before inventor introduced in patented claim 201010525727.3, wherein about control and the preparation of slit size, do not carry out concrete research.
The size of slit directly affects the size of pump current signal, and the size of three slits in NOx sensor how controlled well is very important, and slit is excessive, and the speed of oxygen pump has little time pump and walks oxygen, can not occur limiting current; Slit is too small, and gas diffusion is too slow, and limiting current value is too low, low to the resolution of gas concentration, and the oxygen of low concentration is changed to not reaction.
Summary of the invention
The object of the invention provides a kind of filling paste and method for making of zirconia base galvanochemistry NOx sensor chip slit.
First according to a kind of computing method of slit, according to oxygen pump work Current calculation, limiting current is expressed as: I=4FD/R
0t*S/L* (Po-Pe) is wherein: D is NO
xcoefficient of diffusion, S is the sectional area of effective the evolving path, L is the length of effective the evolving path, Po is partial pressure of oxygen in diffusion pre-test gas, Pe is the partial pressure of oxygen of measuring chamber after diffusion, R
0be gas law constant, F is Faraday constant, and T is absolute temperature.F=96490C/mol and D=1.68cm
2/ sec, R
0=82.05atm*cm
3/ mol*K, T=1073K, can adjust diffusional resistance R=L/S by adjusting the size of slit, due to NO
xsensor chip compact conformation, slit width and the adjustable scope of diffusion length L are smaller, so the present invention adjusts diffusional resistance by adjusting the height of slit.
Technical scheme of the present invention is:
The filling paste of zirconia base galvanochemistry NOx sensor chip slit, it is characterized in that: filling paste is by following components based on weight percentage solvent 30～50%, cementing agent 20～40%, filling agent 10～20%, plastifier 10～20%, lubricant 10～20%; Said components is mixed, and at 25 ℃, viscosity is 4000～20000Pa.s.NOx sensor chip of the present invention is the disclosed structure of application number 201010525727.3.
Described solvent is one or two or more kinds potpourri in toluene, ethanol, butanone.
Described cementing agent is polyvinyl butyral PVB, ethyl cellulose is a kind of or two kinds of potpourris.
Described filling agent is graphite or starch.
Described plastifier is dibutyl phthalate.
Described lubricant is polyglycol.
A kind of method for making of zirconia base galvanochemistry NOx sensor chip slit, it is characterized in that carrying out according to the following steps: the preparation of the filling paste of (1) slit: filling paste is by following components based on weight percentage solvent 30～50%, cementing agent 20～40%, filling agent 10～20%, plastifier 10～20%, lubricant 10～20%; Said components is mixed, and at 25 ℃, viscosity is 4000～20000Pa.s; (2) slit printing height and the print thickness due to NOx sensor chip is directly proportional, the printing test preparation print thickness of filling paste and the corresponding relation of slit, and determine print thickness according to the slit of NOx sensor chip, by printing height design and printing half tone, thereby obtain needed slit thickness; (3) filling paste by the printing screen plate designing, step (1) being made is printed onto in the slit of NOx sensor chip, puts into stove sintering together, and printed filling paste whole burn offs after co-sintering do not have residual.
When the viscosity of described filling paste changes, the print thickness that same printing screen plate parameter obtains also can change, so while changing formula of size, tested and redefined the preparation print thickness of filling paste and the corresponding relation of slit by printing at every turn.
The present invention adjusts diffusional resistance R=L/S by adjusting the size of slit, due to NO
xsensor chip compact conformation, slit width and the adjustable scope of diffusion length L are smaller, and the present invention adjusts diffusional resistance by adjusting the height of slit.
Accompanying drawing explanation
Fig. 1 is the one-piece construction sectional view of Nox sensor chip.
Fig. 2 is the vertical view of Nox sensor chip second layer substrate.
Fig. 3 is that the pump electric current of 6 kinds of samples is with the changing condition figure of pump voltage.
Fig. 4 is that the pump electric current of 1# sample is with the changing condition figure of pump voltage.
Fig. 5 is that the pump electric current of 2# sample is with the changing condition figure of pump voltage.
Fig. 6 is that the pump electric current of 3# sample is with the changing condition figure of pump voltage.
Fig. 7 is pump electric current and the pump voltage corresponding relation figure of gamut different oxygen.
Fig. 8 is oxygen content and limiting current matching graph of a relation.
Embodiment
The present invention will be described in detail by reference to the accompanying drawings:
If Fig. 1 is the structure of Nox sensor, 5 layers of substrate are respectively 2, 11, 21, 13, 14, tail gas is by tail gas import 22, slit 3 enters surge chamber 20, by slit 4, enter the first Room 6 again, through slit 7, entering the second Room 9, the first indoor disactivation electrode 5 and external electrode 1 forms main oxygen pump, the second indoor activated electrode 8 and external electrode 1 forms auxiliary oxygen pump, the second indoor potential electrode 10 and external electrode 1 forms measurement oxygen pump, contrast electrode 17 and external electrode 1 are drawn electromotive force as the reference of system works, 15, 16 and the 12 common passages that form reference air, the common needed heating condition of system works that forms of insulation course 19 and heating resistor 18.Calculate theoretically slit magnitude range, I=4FD/RT*S/L* (Po-Pe), establishes limiting current corresponding to 2500ppm oxygen concentration difference and is: 20-50uA; Suppose in addition slit width 1mm, length 5mm, calculates accordingly and estimates that the height of slit is as follows:
1), during corresponding 20uA, relevant data substitution formula has:
h=3.4(μm)
2), during corresponding 50um, relevant data substitution formula has:
h=8.5(μm)
The scope that the thickness that we design slit is thus 2-20um, with 10um, for approaching most design reference, the slit of design can be so that the limiting current resolution of work be higher like this, and measurement range is wider.
Each components based on weight percentage of the proportioning of the filling paste of slit: solvent 40%, described solvent is toluene: ethanol: the mass ratio of butanone is 4:4:2; Cementing agent polyvinyl butyral PVB20%, filler starch 15%, plasticizer phthalic acid dibutyl ester 15%, polyglycol 10%; At 25 ℃, viscosity reaches 8000Pa.s.Test show that final slit height is 80% of print thickness, and print thickness is 50% of screen thickness, so will obtain the slit of 10um, screen thickness is 25um.
In standard air chamber, join 1% O
2, all the other are N
2, the sample of every kind of different slit heights to be tested, the slit height that 1#～6# sample is corresponding is respectively 2um, 5um, 10um, 15um, 20um, 30um, test result is as shown in Figure 3, as can be seen from the figure, can not there is limiting current in 6#, and 4# and 5# limiting current platform are not very smooth, slightly upcast phenomenon, all can there is limiting current in 1#, 2#, 3# sample, and slit is larger, and limiting current value is just larger.Then to 1#, 2#, 3# sample at O
2content is 1000ppm, 1500ppm, 2000ppm and 2500ppm, and all the other are N
2standard air chamber in test, test result is respectively as Fig. 4, shown in Fig. 5 and Fig. 6.
As can be seen from Figure 3, can there is stable limiting current platform in 1# sample, but the variable quantity of limiting current is not proportional to the variable quantity of oxygen concentration, and limiting current value is all very little, so can judge that the slit of 1# sample is too small; 2# becomes good linear relationship with the variable quantity of the limiting current of 3# sample and the variable quantity of oxygen concentration as can be seen from Figure 4 and Figure 5, and the resolution that 3# sample changes oxygen concentration than 2# sample is higher.
3# sample main pump has been carried out to gamut O
2the measurement of concentration, test result as shown in Figure 7 and Figure 8.
Claims (8)
1. the filling paste of zirconia base galvanochemistry NOx sensor chip slit, it is characterized in that: filling paste is by following components based on weight percentage solvent 30～50%, cementing agent 20～40%, filling agent 10～20%, plastifier 10～20%, lubricant 10～20%; Said components is mixed, and at 25 ℃, viscosity is 4000～20000Pa.s.
2. the filling paste of zirconia base galvanochemistry NOx sensor chip slit according to claim 1, is characterized in that: described solvent is one or two or more kinds potpourri in toluene, ethanol, butanone.
3. the filling paste of zirconia base galvanochemistry NOx sensor chip slit according to claim 1, is characterized in that: described cementing agent is polyvinyl butyral PVB, ethyl cellulose is a kind of or two kinds of potpourris.
4. the filling paste of zirconia base galvanochemistry NOx sensor chip slit according to claim 1, is characterized in that: described filling agent is graphite or starch.
5. the filling paste of zirconia base galvanochemistry NOx sensor chip slit according to claim 1, is characterized in that: described plastifier is dibutyl phthalate.
6. the filling paste of zirconia base galvanochemistry NOx sensor chip slit according to claim 1, is characterized in that: described lubricant is polyglycol.
7. the method for making of zirconia base galvanochemistry NOx sensor chip slit, it is characterized in that carrying out according to the following steps: the preparation of the filling paste of (1) slit: filling paste is by following components based on weight percentage solvent 30～50%, cementing agent 20～40%, filling agent 10～20%, plastifier 10～20%, lubricant 10～20%; Said components is mixed, and at 25 ℃, viscosity is 4000～20000Pa.s; (2) slit printing height and the print thickness due to NOx sensor chip is directly proportional, the printing test preparation print thickness of filling paste and the corresponding relation of slit, and determine print thickness according to the slit of NOx sensor chip, by printing height design and printing half tone, thereby obtain needed slit thickness; (3) filling paste by the printing screen plate designing, step (1) being made is printed onto in the slit of NOx sensor chip, puts into stove sintering together, and printed filling paste whole burn offs after co-sintering do not have residual.
8. the method for making of zirconia base galvanochemistry NOx sensor chip slit according to claim 7, it is characterized in that: when the viscosity of described filling paste changes, the print thickness that same printing screen plate parameter obtains also can change, so while changing formula of size, test and redefine the preparation print thickness of filling paste and the corresponding relation of slit by printing at every turn.
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|---|---|---|---|
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|---|---|---|---|
| CN201310606881.7A CN103645221B (en) | 2013-11-26 | 2013-11-26 | The filling paste of zirconia base galvanochemistry NOx sensor chip slit and method for making |
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| CN103645221B CN103645221B (en) | 2015-11-18 |
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Cited By (7)
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| CN104764785A (en) * | 2015-03-31 | 2015-07-08 | 北京博曼迪汽车科技有限公司 | Sizing agent, reference gas layer and preparation method of reference gas layer as well as oxygen sensor |
| CN111331677A (en) * | 2020-03-30 | 2020-06-26 | 镇江锆源传感科技有限公司 | Blanking and filling method of cast membrane |
| CN113321526A (en) * | 2021-05-28 | 2021-08-31 | 深圳顺络电子股份有限公司 | Sacrificial slurry preparation material, preparation method thereof and preparation method of gas sensor |
| CN113466308A (en) * | 2020-03-31 | 2021-10-01 | 日本碍子株式会社 | Gas sensor |
| CN115388752A (en) * | 2022-09-20 | 2022-11-25 | 徐州芯源诚达传感科技有限公司 | A Nitrogen Oxygen Sensor Chip Slit Testing Method |
| CN115598189A (en) * | 2022-10-08 | 2023-01-13 | 浙江百岸科技有限公司（Cn） | Nitrogen-oxygen sensor chip with hidden circuit |
| CN115746750A (en) * | 2022-11-22 | 2023-03-07 | 苏州博材贵金新材料有限公司 | Binder slurry for nitrogen-oxygen sensor, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115388752A (en) * | 2022-09-20 | 2022-11-25 | 徐州芯源诚达传感科技有限公司 | A Nitrogen Oxygen Sensor Chip Slit Testing Method |
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| CN115746750A (en) * | 2022-11-22 | 2023-03-07 | 苏州博材贵金新材料有限公司 | Binder slurry for nitrogen-oxygen sensor, and preparation method and application thereof |
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Effective date of registration: 20170626 Address after: 441004, No. A58, No. A58, Jia Hai Industrial Park, hi tech Zone, Hubei, Xiangyang, China Patentee after: Xiangyang core sensor technology Co., Ltd. Address before: 430040 Wuhan, East and West Lake District, the Fifth Ring Road, No. 31, Hubei Patentee before: WUHAN HAOYUAN SENSING TECHNOLOGY CO., LTD. |