片式氧传感器的ZrO_2陶瓷的水基流延方法的研究
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摘要
本文主要研究的是应用于片式汽车氧传感器的二氧化锆陶瓷的制备,所选用的实验方法是水基流延工艺。为了节省实验原料和实践,首先采用氧化铝为粉体熟悉水基流延的工艺过程,摸索出陶瓷浆料的参考配方,在此基础上再进行对二氧化锆陶瓷浆料的进一步研究。
在本文中,分别采用了粒径为41nm的ZrO_2(记为ZrO_2 A)与粒径为26nm的ZrO_2(记为ZrO_2 B)为粉体,重点研究了在水基流延工艺过程中,各种有机添加剂对二氧化锆陶瓷浆料的影响,并得出最终配制方案。实验表明,在PH值为9.36时,以ZrO_2 B为粉体的浆料各项性能稍好一些,在浆料中,其最佳固含量为45wt.%;分散剂聚丙烯酸铵的含量为1.5wt.%时,ZrO_2 B陶瓷浆料的分散性能做好,其粘度与沉降体积同时达到最低值;采用PVA--S-07作为复合粘结剂时,在其加入量为5.5wt. %的条件下,浆料的流延、稳定性能最好;在增塑剂的选择上,本文对比了三种常用的增塑剂(DBP、GLY、PEG)对浆料粘度的影响,最终选择了质量比为1:1的DBP和PEG作为复合增塑剂,其总的加入量为3.0wt.%。此外本文还分别探讨了一次、二次球磨时间和剪切速率等因素对浆料粘度的影响。最终将所制的ZrO_2陶瓷浆料流延,得到表面较为光滑、平整的素坯,自然干燥24h后将素坯进行程序升温烧结,制得所需的二氧化锆陶瓷,并对该样品进行XRD测试分析。
As the fast development of the automotive industry in china, more and more problems come out, including the problem of the car-exhaust induced environmental pollution, being highlighted for special attention. Especially as the gradual upgrade of the international emission control regulations , more and more requirements for the oxygen sensor are raised for the detection and control of the car exhaust, resulting in many urgent theoretical and technical problems, meanwhile, the market of oxygen sensor in china is just starting, far behind the international companies. Thus there is not only the academic value but also the economic and strategy value for china in the study of the car oxygen sensor.
Nowadays, the chip-style oxygen sensor has dominated the market for the characteristics of the small size, the long life, and the flexibility for tough environments. Materials for the chip-style oxygen sensor include aluminum oxide, titanium carbide, calcium titanate, zirconium oxide and so on, resulting in different characteristics of the oxygen sensor. The zirconium oxide ceramic of 8mol% fraction of Y2O3 stabilize ZrO2 (YSZ) has gain growing concern and has been selected to be the basic material of the oxygen sensor studied in this paper for its advantages of the high oxygen ion conductivity and the stability in oxidation and reduction atmosphere.
The manufacture technologies for the zirconium oxide ceramic chip include sol-gel method, extrusion molding method, injection molding method, spray forming method and tape casting method, etc., and the tape casting method is applied broadly for the high efficiency due to the simplicity of equipments, high level of automation, continuity of operation, and for the uniform performance of cast biscuit due to the stable casting process. The tape casting method includes water based method and non-water based method, which having the same technical process. But the non-water tape casting method using a large number of organic solvents, causes great environmental pollution, and its technology has not improved. Therefore, this paper studies the zirconium oxide ceramic slurry using the water based tape casting method, discussing the technical process of the slurry preparation and the tape casting method, giving the standard for the choice of the dispersant, the binder and the plasticizer, while the factors determining the thickness and the quality of the cast film are also analyzed, with the scheme for the enhancement of the quality of the cast film proposed.
Considering the high price of the 8mol% fraction of Y2O3 stabilize ZrO2 (YSZ), the cheaper Al2O3 is first chose as the powder to study the specified factor in the water based tape casting process. Referring to the charge ratio in relative references, this paper choosing water as solvent, debugs the composition and dosage of the dispersant, the binder and the plasticizer, and get the best ratio of stable casting slurry. Finally, this paper gets the alumina ceramic slurry which is suitable for the water based tape casting and does the casting. Specifically, this paper prepares the Al2O3 40wt.% slurry for water based tape casting, determines the best value for the amount of the dispersant is 1.0wt.%, chooses dibutyl phthalate plasticizers and polyethylene glycol as the compound with a ratio of 1:1 and a mount of 3.6wt.%, chooses polyvinyl alcohol (PVA) as the binder with the mount of 3.9wt.%. This paper deal the prepared slurry with manual tape-casting operations, and after natural drying for 20h, the relatively flat tape-casting biscuit of Al2O3 is got.
Based on the manufacture technology of Al2O3 slurry, this paper replaces Al2O3 with ZrO2 as the powder to prepare the tape casting slurry, and studies the affects of the dispersant, the binder, the plasticizer and other organic additives to the stability of tape casting slurry, getting the formula of the ZrO2 tape casting slurry. Specifically, this paper prepares two different tape casting slurry of the ZrO2 powder with different particle sizes (DA=0.41nm,DB=0.26nm), determines the best ratio of the water-based tape casting slurry as the solid content of ZrO2 A to be 40.0wt.%, determines the amount of the dispersant Ammonium to be 2.0wt.%, uses the PVA as the binder alone with a amount of 3.84wt.%, uses the polyethylene glycol and dibutyl phthalate as the plasticizer with a ratio of 1:1 and a amount of 2.52wt.%. Thus, this paper has prepared the water-based tape casting slurry with good flow properties, and after casting and drying, smooth casting film with scalability is punched, sintering in the conditions of 1550℃, to get the zirconium oxide ceramic with good density, but, the shrinkage of sintering is more than 20% both in the length and width direction, which is not conducive to control the size of zirconium oxide ceramic, and that is due to the low solid content in the slurry. When PVA is used as a binder alone, due to the existence of the organic side chain, after adsorbed on the ceramic surface, PVA increases the viscosity of the slurry, and therefore the solid content of ZrO2 A is very difficult to continue to improve, while when acrylic emulsion S-07 is used as a binder alone, the solid content is enhanced effectively, with the drawback of decreasing the green strength of casting plan films.
Considering the factors above, this paper for the first time chooses acrylic emulsion S-07 and PVA as the composite binder, and chooses polyethylene glycol and dibutyl phthalate as the composite plasticizer, increasing the solid content of ZrO2 casting slurry to 45wt.%, thus the Shrinkage in the length direction and the width direction of the sintered samples is reduced by 16.72% and 14.58% respectively, to meet the requirements of production of zirconium oxide ceramic chips. When the ratio of PVA and acrylic emulsion adhesive S-07 is 1.2, the slurry has a good rheological property.
In addition, the paper also studies the affects of the first and the second ball mill time to the viscosity of two different zirconium oxide casting slurry with different particle sizes, showing that the ball mill time should get the optimal time, instead as long as possible. For ZrO2 A, the optimal times of the first and the second ball milling time are 10h and 20h, while for ZrO2 B, the optimal times are 8h and 18h. The smaller the particle size of zirconium oxide powder, the shorter the time required for slurry achieving good flow properties.
在本文中,分别采用了粒径为41nm的ZrO_2(记为ZrO_2 A)与粒径为26nm的ZrO_2(记为ZrO_2 B)为粉体,重点研究了在水基流延工艺过程中,各种有机添加剂对二氧化锆陶瓷浆料的影响,并得出最终配制方案。实验表明,在PH值为9.36时,以ZrO_2 B为粉体的浆料各项性能稍好一些,在浆料中,其最佳固含量为45wt.%;分散剂聚丙烯酸铵的含量为1.5wt.%时,ZrO_2 B陶瓷浆料的分散性能做好,其粘度与沉降体积同时达到最低值;采用PVA--S-07作为复合粘结剂时,在其加入量为5.5wt. %的条件下,浆料的流延、稳定性能最好;在增塑剂的选择上,本文对比了三种常用的增塑剂(DBP、GLY、PEG)对浆料粘度的影响,最终选择了质量比为1:1的DBP和PEG作为复合增塑剂,其总的加入量为3.0wt.%。此外本文还分别探讨了一次、二次球磨时间和剪切速率等因素对浆料粘度的影响。最终将所制的ZrO_2陶瓷浆料流延,得到表面较为光滑、平整的素坯,自然干燥24h后将素坯进行程序升温烧结,制得所需的二氧化锆陶瓷,并对该样品进行XRD测试分析。
As the fast development of the automotive industry in china, more and more problems come out, including the problem of the car-exhaust induced environmental pollution, being highlighted for special attention. Especially as the gradual upgrade of the international emission control regulations , more and more requirements for the oxygen sensor are raised for the detection and control of the car exhaust, resulting in many urgent theoretical and technical problems, meanwhile, the market of oxygen sensor in china is just starting, far behind the international companies. Thus there is not only the academic value but also the economic and strategy value for china in the study of the car oxygen sensor.
Nowadays, the chip-style oxygen sensor has dominated the market for the characteristics of the small size, the long life, and the flexibility for tough environments. Materials for the chip-style oxygen sensor include aluminum oxide, titanium carbide, calcium titanate, zirconium oxide and so on, resulting in different characteristics of the oxygen sensor. The zirconium oxide ceramic of 8mol% fraction of Y2O3 stabilize ZrO2 (YSZ) has gain growing concern and has been selected to be the basic material of the oxygen sensor studied in this paper for its advantages of the high oxygen ion conductivity and the stability in oxidation and reduction atmosphere.
The manufacture technologies for the zirconium oxide ceramic chip include sol-gel method, extrusion molding method, injection molding method, spray forming method and tape casting method, etc., and the tape casting method is applied broadly for the high efficiency due to the simplicity of equipments, high level of automation, continuity of operation, and for the uniform performance of cast biscuit due to the stable casting process. The tape casting method includes water based method and non-water based method, which having the same technical process. But the non-water tape casting method using a large number of organic solvents, causes great environmental pollution, and its technology has not improved. Therefore, this paper studies the zirconium oxide ceramic slurry using the water based tape casting method, discussing the technical process of the slurry preparation and the tape casting method, giving the standard for the choice of the dispersant, the binder and the plasticizer, while the factors determining the thickness and the quality of the cast film are also analyzed, with the scheme for the enhancement of the quality of the cast film proposed.
Considering the high price of the 8mol% fraction of Y2O3 stabilize ZrO2 (YSZ), the cheaper Al2O3 is first chose as the powder to study the specified factor in the water based tape casting process. Referring to the charge ratio in relative references, this paper choosing water as solvent, debugs the composition and dosage of the dispersant, the binder and the plasticizer, and get the best ratio of stable casting slurry. Finally, this paper gets the alumina ceramic slurry which is suitable for the water based tape casting and does the casting. Specifically, this paper prepares the Al2O3 40wt.% slurry for water based tape casting, determines the best value for the amount of the dispersant is 1.0wt.%, chooses dibutyl phthalate plasticizers and polyethylene glycol as the compound with a ratio of 1:1 and a mount of 3.6wt.%, chooses polyvinyl alcohol (PVA) as the binder with the mount of 3.9wt.%. This paper deal the prepared slurry with manual tape-casting operations, and after natural drying for 20h, the relatively flat tape-casting biscuit of Al2O3 is got.
Based on the manufacture technology of Al2O3 slurry, this paper replaces Al2O3 with ZrO2 as the powder to prepare the tape casting slurry, and studies the affects of the dispersant, the binder, the plasticizer and other organic additives to the stability of tape casting slurry, getting the formula of the ZrO2 tape casting slurry. Specifically, this paper prepares two different tape casting slurry of the ZrO2 powder with different particle sizes (DA=0.41nm,DB=0.26nm), determines the best ratio of the water-based tape casting slurry as the solid content of ZrO2 A to be 40.0wt.%, determines the amount of the dispersant Ammonium to be 2.0wt.%, uses the PVA as the binder alone with a amount of 3.84wt.%, uses the polyethylene glycol and dibutyl phthalate as the plasticizer with a ratio of 1:1 and a amount of 2.52wt.%. Thus, this paper has prepared the water-based tape casting slurry with good flow properties, and after casting and drying, smooth casting film with scalability is punched, sintering in the conditions of 1550℃, to get the zirconium oxide ceramic with good density, but, the shrinkage of sintering is more than 20% both in the length and width direction, which is not conducive to control the size of zirconium oxide ceramic, and that is due to the low solid content in the slurry. When PVA is used as a binder alone, due to the existence of the organic side chain, after adsorbed on the ceramic surface, PVA increases the viscosity of the slurry, and therefore the solid content of ZrO2 A is very difficult to continue to improve, while when acrylic emulsion S-07 is used as a binder alone, the solid content is enhanced effectively, with the drawback of decreasing the green strength of casting plan films.
Considering the factors above, this paper for the first time chooses acrylic emulsion S-07 and PVA as the composite binder, and chooses polyethylene glycol and dibutyl phthalate as the composite plasticizer, increasing the solid content of ZrO2 casting slurry to 45wt.%, thus the Shrinkage in the length direction and the width direction of the sintered samples is reduced by 16.72% and 14.58% respectively, to meet the requirements of production of zirconium oxide ceramic chips. When the ratio of PVA and acrylic emulsion adhesive S-07 is 1.2, the slurry has a good rheological property.
In addition, the paper also studies the affects of the first and the second ball mill time to the viscosity of two different zirconium oxide casting slurry with different particle sizes, showing that the ball mill time should get the optimal time, instead as long as possible. For ZrO2 A, the optimal times of the first and the second ball milling time are 10h and 20h, while for ZrO2 B, the optimal times are 8h and 18h. The smaller the particle size of zirconium oxide powder, the shorter the time required for slurry achieving good flow properties.
引文
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