CN111707712A - Manufacturing method for increasing ceramic strength of nitrogen-oxygen sensor chip - Google Patents
Manufacturing method for increasing ceramic strength of nitrogen-oxygen sensor chip Download PDFInfo
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Abstract
The invention relates to a manufacturing method for increasing the strength of a porcelain body of a nitrogen-oxygen sensor chip. According to the manufacturing method for increasing the ceramic strength of the oxynitride sensor chip, the ceramic strength enhancement layer is manufactured on the surface of the ceramic body by printing the enhancement slurry in the non-functional area of the ceramic body green body, and the anti-bending capability of the oxynitride sensor chip manufactured by de-gluing and sintering is greatly improved, so that the reliability of the oxynitride sensor is improved.
Description
Technical Field
The invention relates to the field of automobile oxynitride sensor chips, in particular to a manufacturing method for increasing the strength of a porcelain body by using an oxynitride sensor chip.
Background
The nitrogen oxide is a gas pollutant, and the nation lists nitrogen oxide and ammonia nitrogen as restrictive indexes according to the requirement of environmental protection, wherein the most important is the nitrogen oxide emission of motor vehicles. The scheme of China heavy-duty vehicles, national IV and national V, mostly adopts a Selective Catalytic Reduction (SCR) scheme, nitrogen and oxygen in tail gas can be selectively adsorbed on a catalyst, urea is sprayed to the catalyst to decompose the nitrogen and oxygen into nitrogen and water through a reduction reaction and then discharge, the spraying amount of the urea is determined by the real-time content of the nitrogen and oxygen detected by a nitrogen and oxygen sensor, and the environment is polluted when the spraying amount is too large or too small, so that the nitrogen and oxygen sensor is used as one of key technologies and key parts of the SCR scheme and plays a crucial role in controlling and reducing the emission of the nitrogen and oxygen.
At present, the oxynitride sensor is mainly of a sheet type and is formed by overlapping six layers of yttria-stabilized zirconia ceramic sheets, each functional layer is printed with an electrode and an insulating layer, chambers or cavities with different shapes are clamped in the functional layers, and the structure and the process are very complex. The electrodes and the insulating layers are printed, chambers or cavities with different shapes are clamped in the middle of the electrodes or the insulating layers, the strength of the oxynitride chip is greatly influenced, and the oxynitride chip is easily damaged during testing or assembling.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for manufacturing a nitrogen-oxygen sensor chip to increase the strength of a ceramic body.
The technical scheme adopted by the invention for solving the technical problems is as follows: a manufacturing method for increasing the strength of a porcelain body of a nitrogen-oxygen sensor chip comprises the steps of printing reinforcing slurry on a non-functional area on a green porcelain body of the nitrogen-oxygen sensor chip, and then performing a nitrogen-oxygen sensor chip manufacturing procedure to obtain the nitrogen-oxygen sensor chip.
Further, the reinforced slurry is prepared from 15-35 parts of alumina powder, 65-85 parts of zirconia powder, 20-25 parts of solvent, 0.5-1 part of dispersing agent, 0.2-1 part of flatting agent, 0.5-1 part of coupling agent and 5-7 parts of resin according to parts by weight.
Further, the preparation method of the reinforced slurry specifically comprises the following steps: adding a solvent, a dispersing agent, a flatting agent, a coupling agent and resin into a batching tank, and then heating for 20-30 minutes at 70-80 ℃ under a sealed condition to uniformly mix the resin, the solvent and the additive; and adding zirconia powder and alumina powder into the mixed material, stirring and defoaming, and finally rolling the stirred material, and filtering the rolled material by a 200-mesh and 600-mesh filter screen to obtain filter slurry, namely the reinforced slurry.
Further, the particle size of the alumina powder is not more than 0.1 μm; the zirconia powder is 3Y tetragonal crystal zirconia powder, and the granularity of the zirconia powder is not more than 50 nm.
Further, the solvent is terpineol or ethylene glycol butyl ether acetate; the resin is polyvinyl butyral or ethyl cellulose.
Further, the dispersant is tributyl phosphate or span 80.
Further, the leveling agent is ethylene glycol monomethyl ether.
Further, the coupling agent is a silane coupling agent.
Further, the reinforcing slurry is printed on a non-functional area on the surface of the ceramic green body.
Further, after the ceramic chip printed with the enhanced slurry is subjected to binder removal, high-temperature sintering is carried out, and the nitrogen-oxygen sensor chip can be obtained; wherein the glue discharging is carried out at the temperature of 300-450 ℃ for 48-96h, and is used for discharging the resin and the solvent of the ceramic plate; the high-temperature sintering is carried out at the temperature of 1400 ℃ and 1450 ℃ and the temperature is kept for 1.5-3 h.
The invention has the advantages that: according to the manufacturing method for increasing the ceramic strength of the oxynitride sensor chip, the ceramic strength enhancement layer is manufactured on the surface of the ceramic body by printing the enhancement slurry in the non-functional area of the ceramic body green body, and the anti-bending capability of the oxynitride sensor chip manufactured by de-gluing and sintering is greatly improved, so that the reliability of the oxynitride sensor is improved.
Drawings
FIG. 1 is a schematic diagram of a printing area of the front side of a ceramic green body in the manufacturing method of the nitrogen-oxygen sensor chip for increasing the strength of a ceramic body;
FIG. 2 is a schematic diagram of a printing area on the reverse side of a ceramic green body in the manufacturing method of the nitrogen-oxygen sensor chip for increasing the strength of a ceramic body;
FIG. 3 is a schematic diagram of a printing area of the side surface of a ceramic green body in the manufacturing method of the nitrogen-oxygen sensor chip for increasing the strength of the ceramic body.
Detailed Description
For the purpose of enhancing the understanding of the present invention, the present invention will be described in further detail with reference to the accompanying drawings and examples, which are provided for the purpose of illustration only and are not intended to limit the scope of the present invention.
Example one
This example provides a reinforcement slurry: adding 20 parts of terpineol, 1 part of tributyl phosphate, 1 part of ethylene glycol monomethyl ether, 1 part of silane coupling agent KH550 and 7 parts of ethyl cellulose into a mixing tank, sealing and heating at 80 ℃ for 20 minutes until the ethyl cellulose, the terpineol, the tributyl phosphate, the ethylene glycol monomethyl ether and the silane coupling agent KH550 are fully and uniformly mixed; then adding 15 parts of alumina powder and 85 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
Example two
This example provides a reinforcement slurry: adding 22 parts of ethylene glycol butyl ether acetate, 0.5 part of span 80, 1 part of ethylene glycol methyl ether, 0.5 part of silane coupling agent KH560 and 5 parts of polyvinyl butyral into a preparation tank, sealing and heating at 70 ℃ for 30 minutes until the polyvinyl butyral, the ethylene glycol butyl ether acetate, the span 80, the ethylene glycol methyl ether and the silane coupling agent KH560 are fully and uniformly mixed; then adding 15 parts of alumina powder and 85 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
EXAMPLE III
This example provides a reinforcement slurry: adding 20 parts of terpineol, 1 part of tributyl phosphate, 1 part of ethylene glycol monomethyl ether, 1 part of silane coupling agent KH550 and 7 parts of ethyl cellulose into a mixing tank, sealing and heating at 80 ℃ for 20 minutes until the ethyl cellulose, the terpineol, the tributyl phosphate, the ethylene glycol monomethyl ether and the silane coupling agent KH550 are fully and uniformly mixed; then adding 20 parts of alumina powder and 80 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
Example four
This example provides a reinforcement slurry: adding 22 parts of ethylene glycol butyl ether acetate, 0.5 part of span 80, 1 part of ethylene glycol methyl ether, 0.5 part of silane coupling agent KH560 and 5 parts of polyvinyl butyral into a preparation tank, sealing and heating at 70 ℃ for 30 minutes until the polyvinyl butyral, the ethylene glycol butyl ether acetate, the span 80, the ethylene glycol methyl ether and the silane coupling agent KH560 are fully and uniformly mixed; then adding 20 parts of alumina powder and 80 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
EXAMPLE five
This example provides a reinforcement slurry: adding 20 parts of terpineol, 1 part of tributyl phosphate, 1 part of ethylene glycol monomethyl ether, 1 part of silane coupling agent KH550 and 7 parts of ethyl cellulose into a mixing tank, sealing and heating at 80 ℃ for 20 minutes until the ethyl cellulose, the terpineol, the tributyl phosphate, the ethylene glycol monomethyl ether and the silane coupling agent KH550 are fully and uniformly mixed; then adding 25 parts of alumina powder and 75 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
EXAMPLE six
This example provides a reinforcement slurry: adding 22 parts of ethylene glycol butyl ether acetate, 0.5 part of span 80, 1 part of ethylene glycol methyl ether, 0.5 part of silane coupling agent KH560 and 5 parts of polyvinyl butyral into a preparation tank, sealing and heating at 70 ℃ for 30 minutes until the polyvinyl butyral, the ethylene glycol butyl ether acetate, the span 80, the ethylene glycol methyl ether and the silane coupling agent KH560 are fully and uniformly mixed; then adding 25 parts of alumina powder and 75 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
EXAMPLE seven
This example provides a reinforcement slurry: adding 20 parts of terpineol, 1 part of tributyl phosphate, 1 part of ethylene glycol monomethyl ether, 1 part of silane coupling agent KH550 and 7 parts of ethyl cellulose into a mixing tank, sealing and heating at 80 ℃ for 20 minutes until the ethyl cellulose, the terpineol, the tributyl phosphate, the ethylene glycol monomethyl ether and the silane coupling agent KH550 are fully and uniformly mixed; then adding 30 parts of alumina powder and 70 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
Example eight
This example provides a reinforcement slurry: adding 22 parts of ethylene glycol butyl ether acetate, 0.5 part of span 80, 1 part of ethylene glycol methyl ether, 0.5 part of silane coupling agent KH560 and 5 parts of polyvinyl butyral into a preparation tank, sealing and heating at 70 ℃ for 30 minutes until the polyvinyl butyral, the ethylene glycol butyl ether acetate, the span 80, the ethylene glycol methyl ether and the silane coupling agent KH560 are fully and uniformly mixed; then adding 30 parts of alumina powder and 70 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
Example nine
This example provides a reinforcement slurry: adding 20 parts of terpineol, 1 part of tributyl phosphate, 1 part of ethylene glycol monomethyl ether, 1 part of silane coupling agent KH550 and 7 parts of ethyl cellulose into a mixing tank, sealing and heating at 80 ℃ for 20 minutes until the ethyl cellulose, the terpineol, the tributyl phosphate, the ethylene glycol monomethyl ether and the silane coupling agent KH550 are fully and uniformly mixed; then adding 35 parts of alumina powder and 65 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
Example ten
This example provides a reinforcement slurry: adding 22 parts of ethylene glycol butyl ether acetate, 0.5 part of span 80, 1 part of ethylene glycol methyl ether, 0.5 part of silane coupling agent KH560 and 5 parts of polyvinyl butyral into a preparation tank, sealing and heating at 70 ℃ for 30 minutes until the polyvinyl butyral, the ethylene glycol butyl ether acetate, the span 80, the ethylene glycol methyl ether and the silane coupling agent KH560 are fully and uniformly mixed; then adding 35 parts of alumina powder and 65 parts of zirconia powder into a stirring and defoaming machine for stirring; filtering with a 400-mesh filter screen after rolling by a three-roller mill to obtain the slurry.
The reinforced slurry prepared by the embodiment is used for processing a green ceramic body of the oxynitride sensor, and the specific operation is as follows:
printing: after the functional layers (electrodes and the like) on the front and back surfaces of the green ceramic body of the oxynitride sensor core are printed, the reinforcing slurry prepared in the embodiment is subjected to screen printing of slurry with the thickness of 100um on the front and back surfaces of the green ceramic body except the electrodes; then, the reinforcing paste prepared in the above example was screen-printed with a paste having a thickness of 100um on both sides of the oxynitride sensor core on the green ceramic green body, and as shown in fig. 1 to 3, the reinforcing paste was printed in the non-functional region 2 excluding the functional printed region 1 (electrode region) while avoiding the functional printed region 1 (electrode region) during printing.
Rubber discharging: and (3) filling the green ceramic blank printed with the reinforcing slurry into a glue discharging pot by using a circulating hot air drying box, raising the temperature to 400 ℃, preserving the heat for 72 hours, and discharging the resin, the organic solvent and the like in the ceramic.
And (3) firing: and (3) utilizing a high-temperature firing furnace, raising the temperature to 1450 ℃, preserving the temperature for 2h, and firing the oxynitride sensor green ceramic blank into the oxynitride sensor chip.
A comparative example is also introduced, namely, only a functional area is printed on the green ceramic body, the reinforcing slurry is not printed, then, the green ceramic body without the reinforcing slurry is filled into a glue discharging bowl by utilizing a circulating hot air drying box, the temperature is raised to 400 ℃, the temperature is kept for 72 hours, and resin, organic solvent and the like in the ceramic are discharged; and then, a high-temperature firing furnace is utilized, the temperature is raised to 1450 ℃, the temperature is kept for 2h, and the oxynitride sensor green ceramic blank is sintered into the oxynitride sensor chip.
The oxynitride sensor core obtained by testing the slurry of the above example after printing and the oxynitride sensor core of the comparative example were subjected to a three-point bending test, and the test data were compared as shown in the following table.
The bending strength of the oxynitride sensor chip of the comparative example was 7 kg; the oxynitride sensor chip of the invention can reach 10-12 kg.
The reinforced slurry mainly comprises alumina powder and zirconia powder, and the alumina powder and the zirconia powder are proportioned in a certain proportion and can achieve the effect of toughening ceramics after being fired, so that the strength of the oxynitride sensor chip is increased. In the reinforced slurry, alumina powder and zirconia powder are main components of the ceramic body reinforcing layer of the oxynitride sensor chip; the solvent, the dispersant, the leveling agent, the coupling agent and the resin are used for fully mixing the alumina powder and the zirconia powder and enabling the mixture to be in a printable slurry state.
In the above embodiments, the proportion of the alumina powder and the zirconia powder has a decisive influence on the flexural strength performance of the reinforced slurry; wherein, the reinforced slurry prepared from 30 parts of alumina powder and 70 parts of zirconia powder has the best bending strength after reinforcing the oxynitride sensor chip.
The above embodiments should not limit the present invention in any way, and all technical solutions obtained by using equivalent alternatives or equivalent transformations fall within the protection scope of the present invention.
Claims (9)
1. A manufacturing method for increasing the strength of a porcelain body of a nitrogen-oxygen sensor chip is characterized by comprising the following steps: and (3) printing the reinforced slurry on the non-functional area on the green ceramic body of the oxynitride sensor chip, and then performing the fabrication process of the oxynitride sensor chip to obtain the oxynitride sensor chip.
2. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 1, characterized in that: the reinforced slurry is prepared from 15-35 parts of alumina powder, 65-85 parts of zirconia powder, 20-25 parts of solvent, 0.5-1 part of dispersant, 0.2-1 part of flatting agent, 0.5-1 part of coupling agent and 5-7 parts of resin by mass.
3. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 2, characterized in that: the preparation method of the reinforced slurry specifically comprises the following steps: adding a solvent, a dispersing agent, a flatting agent, a coupling agent and resin into a batching tank, and then heating for 20-30 minutes at 70-80 ℃ under a sealed condition to uniformly mix the resin, the solvent and the additive; and adding zirconia powder and alumina powder into the mixed material, stirring and defoaming, and finally rolling the stirred material, and filtering the rolled material by a 200-mesh and 600-mesh filter screen to obtain filter slurry, namely the reinforced slurry.
4. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 2, characterized in that: the granularity of the alumina powder is not more than 0.1 mu m; the zirconia powder is 3Y tetragonal crystal zirconia powder, and the granularity of the zirconia powder is not more than 50 nm.
5. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 2, characterized in that: the solvent is terpineol or ethylene glycol monobutyl ether acetate; the resin is polyvinyl butyral or ethyl cellulose.
6. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 2, characterized in that: the dispersant is tributyl phosphate or span 80.
7. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 2, characterized in that: the leveling agent is ethylene glycol monomethyl ether.
8. The manufacturing method for increasing the strength of the porcelain body of the oxynitride sensor chip according to claim 1, characterized in that: the coupling agent is a silane coupling agent.
9. The manufacturing method of the oxynitride sensor chip for increasing the strength of the ceramic body according to any one of claims 2 to 8, wherein: the manufacturing process of the nitrogen-oxygen sensor chip at least comprises the following steps: a glue discharging procedure and a high-temperature sintering procedure; after the ceramic chip printed with the enhanced slurry is subjected to glue removal, high-temperature sintering is carried out, and the nitrogen-oxygen sensor chip can be obtained; wherein the glue discharging is carried out at the temperature of 300-450 ℃ for 48-96h, and is used for discharging the resin and the solvent of the ceramic plate; the high-temperature sintering is carried out at the temperature of 1400 ℃ and 1450 ℃ and the temperature is kept for 1.5-3 h.
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