CN113314250A - Nitrogen-oxygen sensor main pump electrode slurry - Google Patents
Nitrogen-oxygen sensor main pump electrode slurry Download PDFInfo
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- CN113314250A CN113314250A CN202110491873.7A CN202110491873A CN113314250A CN 113314250 A CN113314250 A CN 113314250A CN 202110491873 A CN202110491873 A CN 202110491873A CN 113314250 A CN113314250 A CN 113314250A
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Abstract
The invention discloses a main pump electrode slurry of a nitrogen-oxygen sensor, which is characterized by comprising the following raw materials: 35-65% of Pt powder, 3-5% of 5Y composite powder, 0.5-2.5% of gamma-alumina, 5-15% of inorganic adhesive and 20-40% of organic adhesive, and the invention has the following beneficial effects: according to the invention, the 5Y composite powder is added into the Pt electrode slurry, and the cheap ceramic powder is used for partially replacing expensive Pt powder, so that the consumption of noble metal is reduced, the cost is reduced, and the oxygen pumping capacity of the nitrogen-oxygen sensor is not influenced; meanwhile, the main pump electrode slurry has high adhesive force with the substrate.
Description
The technical field is as follows:
the invention belongs to the technical field of sensor slurry, and particularly relates to main pump electrode slurry of a nitrogen-oxygen sensor.
Background art:
nitrogen oxygen gas, including nitric oxide, nitrogen dioxide, not only can lead to photochemistry smog and acid rain, destroy the ozone layer, still can cause serious harm to human respiratory track, along with the sharp increase of car quantity, when giving people's life and bringing convenience, the nitrogen oxygen gas that the car produced has also brought serious pollution for the atmosphere, nitrogen oxygen sensor ceramic chip is with zirconia as the base member, based on two kinds of battery rationale of concentration type, limiting current type, cooperation electrode electrochemical catalytic reaction, the nitrogen oxide in the separation tail gas, and turn into the measurement of the O2 of nitrogen oxide decomposition with the measurement of nitrogen oxide.
The slurry used by the main pump electrode of the ceramic chip of the oxynitride sensor is required to have higher oxygen pumping capacity and good adhesion capacity with a matrix material (ZrO2), the oxygen pumping capacity of the slurry of the main pump electrode which is commercially used at present can meet the performance requirement of the national hexaoxynitride sensor, but the used pure platinum has high manufacturing cost, and has the problems of poor basic adhesion, falling off of the main pump electrode and the like in the preparation process of the oxynitride sensor chip, the process qualification rate of the oxynitride sensor is seriously influenced, and the long-term working stability and consistency of the oxynitride sensor are also influenced.
The invention content is as follows:
the invention aims to solve the problems and provide a main pump electrode slurry of a nitrogen-oxygen sensor.
In order to solve the problems, the invention provides a technical scheme of electrode slurry of a main pump of a nitrogen-oxygen sensor, which comprises the following steps:
a main pump electrode slurry of a nitrogen-oxygen sensor comprises the following raw materials: 35-65% of Pt powder, 3-5% of 5Y composite powder, 0.5-2.5% of gamma-alumina, 5-15% of inorganic adhesive and 20-40% of organic adhesive.
Preferably, the Pt powder is a mixture of nano-scale Pt powder and micron-scale Pt powder, the mass ratio is 5:5, wherein the grain size of the nano-scale Pt powder is 100-500 nm, and the grain size of the micron-scale Pt powder is 1-1.5 um.
Preferably, the 5Y composite powder is a mixture of Y2O3 and ZrO2 in a molar ratio of 4: 96-6: 94, the particle size of the 5Y composite powder is 100-800 nm, 0.1mol/L yttrium nitrate aqueous solution and 100-300 nm zirconium oxide nano powder are placed in a high-pressure reaction kettle in a molar ratio of 1: 8-12, the mixture reacts for 2-5 hours at 100-200 ℃, the product is centrifugally separated to obtain a precipitate after being naturally cooled to room temperature, the precipitate is washed with deionized water, dried in vacuum, and then roasted for 5-8 hours at 600-800 ℃, and the 5Y composite powder with the size of 100-800 nm is obtained.
Preferably, the particle size distribution of the gamma-alumina is 50 to 200 nm.
Preferably, the inorganic binder comprises the following components in percentage by mass: 1 to 6 percent of CaO, 5 to 10 percent of MgO, 15 to 40 percent of SiO2, 15 to 25 percent of Al2O3, 30 to 45 percent of Bi2O3, 1 to 3 percent of TiO2, 1 to 3 percent of B2O3 and 0.5 to 1.5 percent of Na 2O.
Preferably, the organic binder comprises the following components in percentage by mass: 5 to 10 percent of ethyl cellulose and 90 to 95 percent of organic solvent.
Preferably, the method comprises the following preparation steps:
s1, the composition by mass percent is as follows: weighing raw materials of 1-6% of CaO, 5-10% of MgO, 15-40% of SiO2, 15-25% of Al2O3, 30-45% of Bi2O3, 1-3% of TiO2, 1-3% of B2O3 and 0.5-1.5% of Na2O, ball-milling and mixing for 3-5 h by a planetary ball mill, drying, preserving heat for 1h at 1350-1500 ℃, taking out molten liquid, quenching, crushing and drying to obtain an inorganic binder with the particle size of 1-2 um;
s2, the composition by mass percent is as follows: weighing raw materials of 5-10% of ethyl cellulose and 90-95% of organic solvent, adding the ethyl cellulose into the organic solvent at the temperature of 60-80 ℃, and stirring until the ethyl cellulose is completely dissolved to obtain the organic binder;
and S3, sequentially adding an inorganic binder, 5Y composite powder, gamma-alumina and Pt powder into the organic binder according to the mass percentage of the main pump electrode slurry, fully stirring and uniformly dispersing, then rolling by using a three-roll mill, removing agglomerated particles, and uniformly stirring again to obtain the uniformly dispersed main pump electrode slurry.
The invention has the beneficial effects that: according to the invention, the 5Y composite powder is added into the Pt electrode slurry, and the cheap ceramic powder is used for partially replacing expensive Pt powder, so that the consumption of noble metal is reduced, the cost is reduced, and the oxygen pumping capacity of the nitrogen-oxygen sensor is not influenced; meanwhile, the main pump electrode slurry has high adhesive force with the substrate.
Description of the drawings:
for ease of illustration, the invention is described in detail by the following detailed description and the accompanying drawings.
FIG. 1 is a graph comparing the oxygen pumping capacity of the present invention.
The specific implementation mode is as follows:
the specific implementation mode adopts the following technical scheme: a main pump electrode slurry of a nitrogen-oxygen sensor comprises the following raw materials: 35-65% of Pt powder, 3-5% of 5Y composite powder, 0.5-2.5% of gamma-alumina, 5-15% of inorganic adhesive and 20-40% of organic adhesive.
The Pt powder is a mixture of nano-grade Pt powder and micron-grade Pt powder, and the mass ratio is 5:5, wherein the grain size of the nano-grade Pt powder is 100-500 nm, and the grain size of the micron-grade Pt powder is 1-1.5 um.
The 5Y composite powder is a mixture of Y2O3 and ZrO2 in a molar ratio of 4: 96-6: 94, the particle size of the 5Y composite powder is 100-800 nm, 0.1mol/L yttrium nitrate aqueous solution and 100-300 nm zirconium oxide nano powder are placed in a high-pressure reaction kettle in a molar ratio of 1: 8-12, the mixture reacts for 2-5 hours at 100-200 ℃, the product is centrifugally separated to obtain a precipitate after being naturally cooled to room temperature, the precipitate is washed with deionized water, dried in vacuum, and then roasted for 5-8 hours at 600-800 ℃, and the 5Y composite powder with the size of 100-800 nm is obtained.
Wherein the particle size distribution of the gamma-alumina is 50-200 nm.
Wherein the inorganic binder comprises the following components in percentage by mass: 1 to 6 percent of CaO, 5 to 10 percent of MgO, 15 to 40 percent of SiO2, 15 to 25 percent of Al2O3, 30 to 45 percent of Bi2O3, 1 to 3 percent of TiO2, 1 to 3 percent of B2O3 and 0.5 to 1.5 percent of Na 2O.
Wherein the organic binder comprises the following components in percentage by mass: 5 to 10 percent of ethyl cellulose and 90 to 95 percent of organic solvent.
Example one
100mL of 0.1mol/L yttrium nitrate aqueous solution and 123.2g (1mol) of zirconium oxide nano powder with the particle size of 100nm are placed in a high-pressure reaction kettle, react for 3h at 150 ℃, after the zirconium oxide nano powder is naturally cooled to room temperature, the product is centrifugally separated to obtain precipitate, the precipitate is washed for 2 times by deionized water, dried for 5h in vacuum at 80 ℃, and then roasted for 6h at 800 ℃ to obtain 5Y composite powder with the size of 250 nm.
Weighing 5g of CaO, 8g of MgO, 25g of SiO2, 20g of Al2O3, 37g of Bi2O3, 2g of TiO2, 2g B2O3 and 1g of Na2O, putting the materials into a ball milling tank, adding 100g of deionized water, ball milling and mixing for 4 hours by a planetary ball mill, pouring the mixture out, putting the mixture into an oven at 80 ℃ for drying for 12 hours, putting the dried material block into a crucible, putting the crucible into a boiling furnace for heating to 1500 ℃, preserving the heat for 1 hour, taking out the molten liquid, quenching, crushing and drying to obtain the inorganic binder with the particle size of 1.5 um.
Weighing 10g of ethyl cellulose, adding the ethyl cellulose into 90g of terpineol solution, and stirring until the ethyl cellulose is completely dissolved to obtain the organic binder.
Sequentially adding 10g of inorganic binder, 4g of 5Y composite powder, 1.5g of gamma-alumina (average particle size is 100nm) and 54.5g of Pt powder into 30g of organic binder, wherein the Pt powder is a mixture of nanoscale Pt powder and micron-sized Pt powder in a mass ratio of 5:5, the average particle size of the nanoscale Pt powder is 250nm, the average particle size of the micron-sized Pt powder is 1.0um, fully stirring and uniformly dispersing, rolling by using a three-roll mill, removing agglomerated particles, and uniformly stirring to obtain uniformly dispersed main pump electrode slurry.
Example two
Putting 100mL of 0.1mol/L yttrium nitrate aqueous solution and 147.84g (1.2mol) of zirconium oxide nano powder with the particle size of 300nm into a high-pressure reaction kettle, reacting for 2h at 200 ℃, naturally cooling to room temperature, carrying out centrifugal separation on a product to obtain a precipitate, washing for 2 times with deionized water, carrying out vacuum drying for 5h at 80 ℃, and then roasting for 8h at 700 ℃ to obtain 5Y composite powder with the size of 500 nm.
Weighing 6g of CaO, 10g of MgO, 30g of SiO2, 15g of Al2O3, 36.5g of Bi2O3, 1g of TiO2, 1g B2O3 and 0.5g of Na2O, putting the materials into a ball milling tank, adding 100g of deionized water, ball milling and mixing for 4 hours by a planetary ball mill, pouring the mixture into an oven at 80 ℃ for drying for 12 hours, putting the dried material blocks into a crucible, heating the material blocks to 1500 ℃ in a muffle furnace, preserving the heat for 1 hour, taking out the molten liquid, quenching, crushing and drying to obtain the inorganic binder with the average particle size of 1.8 um.
5g of ethyl cellulose is weighed and added into a mixed solution of 85g of terpineol and 10g of acetone, and the mixture is stirred until the ethyl cellulose is completely dissolved, so that the organic binder is obtained.
Adding 15g of inorganic binder, 5g of 5Y composite powder, 2.5g of gamma-alumina (average particle size of 200nm) and 37.5g of Pt powder into 40g of organic binder in sequence, wherein the Pt powder is a mixture of nanoscale Pt powder and micron-sized Pt powder in a mass ratio of 5:5, the average particle size of the nanoscale Pt powder is 500nm, and the average particle size of the micron-sized Pt powder is 1.5 um. Fully stirring and uniformly dispersing, then rolling by using a three-roll mill, removing agglomerated particles, and uniformly stirring to obtain the uniformly dispersed main pump electrode slurry.
In order to prove the beneficial effects of the invention, the main pump electrode slurry prepared in the first embodiment and the main pump electrode slurry of the commercial nitrogen-oxygen sensor are respectively adopted to prepare the nitrogen oxide sensor ceramic chip by the same screen printing process; the results of the pump oxygen capacity comparison are shown in fig. 1.
As can be seen from fig. 1, the intensity of the output current signal of the nitrogen-oxygen sensor of the main pump electrode prepared by the electrode paste of example one is equivalent to that of the commercial main pump electrode, and the adhesion between the main pump electrode and the substrate (ZrO2) is significantly enhanced, which shows that the main pump electrode prepared by the electrode paste of the present invention can satisfy the higher oxygen pumping capability of the nitrogen-oxygen sensor, and the expensive Pt powder is partially replaced by the cheap ceramic powder, so that the cost is reduced, and meanwhile, the main pump electrode paste has higher adhesion with the substrate (ZrO2), so that the present invention has great practical value.
While there have been shown and described what are at present considered to be the fundamental principles of the invention and its essential features and advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (7)
1. The main pump electrode slurry of the nitrogen-oxygen sensor is characterized by comprising the following raw materials: 35-65% of Pt powder, 3-5% of 5Y composite powder, 0.5-2.5% of gamma-alumina, 5-15% of inorganic adhesive and 20-40% of organic adhesive.
2. The electrode slurry for a main pump of a nitrogen-oxygen sensor according to claim 1, characterized in that: the Pt powder is a mixture of nano-grade Pt powder and micron-grade Pt powder, and the mass ratio is 5:5, wherein the grain size of the nano-grade Pt powder is 100-500 nm, and the grain size of the micron-grade Pt powder is 1-1.5 um.
3. The electrode slurry for a main pump of a nitrogen-oxygen sensor according to claim 1, characterized in that: the 5Y composite powder is a mixture of Y2O3 and ZrO2 in a molar ratio of 4: 96-6: 94, the particle size of the 5Y composite powder is 100-800 nm, 0.1mol/L yttrium nitrate aqueous solution and 100-300 nm zirconium oxide nano powder are placed in a high-pressure reaction kettle in a molar ratio of 1: 8-12, the mixture reacts for 2-5 hours at 100-200 ℃, the product is naturally cooled to room temperature, then the product is centrifugally separated to obtain precipitate, washed by deionized water, dried in vacuum, and then roasted for 5-8 hours at 600-800 ℃, and the 5Y composite powder with the size of 100-800 nm is obtained.
4. The electrode slurry for a main pump of a nitrogen-oxygen sensor according to claim 1, characterized in that: the particle size distribution of the gamma-alumina is 50-200 nm.
5. The electrode slurry for a main pump of a nitrogen-oxygen sensor according to claim 1, characterized in that: the inorganic binder comprises the following components in percentage by mass: 1 to 6 percent of CaO, 5 to 10 percent of MgO, 15 to 40 percent of SiO2, 15 to 25 percent of Al2O3, 30 to 45 percent of Bi2O3, 1 to 3 percent of TiO2, 1 to 3 percent of B2O3 and 0.5 to 1.5 percent of Na 2O.
6. The electrode slurry for a main pump of a nitrogen-oxygen sensor according to claim 1, characterized in that: the organic binder comprises the following components in percentage by mass: 5 to 10 percent of ethyl cellulose and 90 to 95 percent of organic solvent.
7. The method for preparing electrode slurry of a main pump of a nitrogen-oxygen sensor according to claim 1, wherein the method comprises the following steps: the preparation method comprises the following preparation steps:
s1, the composition by mass percent is as follows: weighing raw materials of 1-6% of CaO, 5-10% of MgO, 15-40% of SiO2, 15-25% of Al2O3, 30-45% of Bi2O3, 1-3% of TiO2, 1-3% of B2O3 and 0.5-1.5% of Na2O, ball-milling and mixing for 3-5 h by a planetary ball mill, drying, preserving heat for 1h at 1350-1500 ℃, taking out molten liquid, quenching, crushing and drying to obtain an inorganic binder with the particle size of 1-2 um;
s2, the composition by mass percent is as follows: weighing raw materials of 5-10% of ethyl cellulose and 90-95% of organic solvent, adding the ethyl cellulose into the organic solvent at the temperature of 60-80 ℃, and stirring until the ethyl cellulose is completely dissolved to obtain the organic binder;
and S3, sequentially adding an inorganic binder, 5Y composite powder, gamma-alumina and Pt powder into the organic binder according to the mass percentage of the main pump electrode slurry, fully stirring and uniformly dispersing, then rolling by using a three-roll mill, removing agglomerated particles, and uniformly stirring again to obtain the uniformly dispersed main pump electrode slurry.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114414640A (en) * | 2022-01-24 | 2022-04-29 | 深圳市富济新材料科技有限公司 | Pt-Au composite electrode for nitrogen-oxygen sensor chip, preparation method and chip |
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| JPS5752853A (en) * | 1980-09-16 | 1982-03-29 | Matsushita Electric Ind Co Ltd | Manufacture of oxygen sensor |
| JPS6154444A (en) * | 1984-08-27 | 1986-03-18 | Hitachi Chem Co Ltd | Element for detecting oxygen concentration |
| JPH036449A (en) * | 1989-06-02 | 1991-01-11 | Fujikura Ltd | Manufacture of oxygen sensor |
| CN102109485A (en) * | 2009-12-29 | 2011-06-29 | 比亚迪股份有限公司 | Oxygen sensor electrode slurry and oxygen sensor sensing layer and preparation methods thereof |
| CN103217469A (en) * | 2013-01-21 | 2013-07-24 | 武汉天榜氧传感器有限公司 | Tubular automotive oxygen sensor structure and manufacturing method thereof |
| CN108932989A (en) * | 2018-06-13 | 2018-12-04 | 西安创联电气科技（集团）有限责任公司 | A kind of NOx sensor measuring electrode high activity electrode slurry |
| CN108956699A (en) * | 2018-06-22 | 2018-12-07 | 西安创联电气科技（集团）有限责任公司 | A kind of NOXSensor ceramic chip insulating film band and insulating layer preparation process |
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2021
- 2021-05-06 CN CN202110491873.7A patent/CN113314250A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5752853A (en) * | 1980-09-16 | 1982-03-29 | Matsushita Electric Ind Co Ltd | Manufacture of oxygen sensor |
| JPS6154444A (en) * | 1984-08-27 | 1986-03-18 | Hitachi Chem Co Ltd | Element for detecting oxygen concentration |
| JPH036449A (en) * | 1989-06-02 | 1991-01-11 | Fujikura Ltd | Manufacture of oxygen sensor |
| CN102109485A (en) * | 2009-12-29 | 2011-06-29 | 比亚迪股份有限公司 | Oxygen sensor electrode slurry and oxygen sensor sensing layer and preparation methods thereof |
| CN103217469A (en) * | 2013-01-21 | 2013-07-24 | 武汉天榜氧传感器有限公司 | Tubular automotive oxygen sensor structure and manufacturing method thereof |
| CN108932989A (en) * | 2018-06-13 | 2018-12-04 | 西安创联电气科技（集团）有限责任公司 | A kind of NOx sensor measuring electrode high activity electrode slurry |
| CN108956699A (en) * | 2018-06-22 | 2018-12-07 | 西安创联电气科技（集团）有限责任公司 | A kind of NOXSensor ceramic chip insulating film band and insulating layer preparation process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114414640A (en) * | 2022-01-24 | 2022-04-29 | 深圳市富济新材料科技有限公司 | Pt-Au composite electrode for nitrogen-oxygen sensor chip, preparation method and chip |
| CN114414640B (en) * | 2022-01-24 | 2024-08-02 | 深圳汇北川科技股份有限公司 | Pt-Au composite electrode for nitrogen-oxygen sensor chip, preparation method and chip |
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