固相反应型复相陶瓷涂层制备工艺、反应机理及性能研究
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摘要
以Al-TiO_2-B_2O_3为反应体系,经机械球磨制成超细粉体,采用固相反应法,在金属(Q235钢、AZ31B镁合金)基体表面,制备了Al_2O_3-TiB_2复相陶瓷涂层。采用EET理论对涂层体系进行了理论设计与性能预测;采用SEM、激光粒度分布仪、XRD、DTA等设备和手段研究了Al-TiO_2-B_2O_3体系的机械力化学和热化学行为;采用热力学、动力学方法研究了涂层的形成机理,并对涂层的物相组成、界面特征进行了分析,对涂层的硬度、结合强度、热震、耐磨、耐蚀等性能进行了测试。
EET理论计算结果表明:在Q235钢和AZ31B镁合金基底上制备Al_2O_3-TiB_2复相陶瓷涂层具有科学性和合理性,涂层与基底之间可形成较强的界面结合,涂层本身强度和韧性可得到适当的配合。热力学计算结果表明:Al-TiO_2-B_2O_3体系在实际条件下,反应可以发生,生成的最终产物为Al_2O_3和TiB_2。机械球磨可使Al-TiO_2-B_2O_3复合粉体得到充分细化,颗粒度呈正态分布,粉体加入PCA球磨20h后,颗粒中位径可达到4.35μm,晶粒度可达到纳米级,形状近乎球形,并有少量Al_2O_3、TiB_2等新相生成。机械力化学作用可使反应体系的活性显著增强,球磨20h粉体在400℃左右就可发生缓慢的固相反应,670℃反应最为剧烈,粉体经700℃热处理,产物大部分为Al_2O_3、TiB_2,经1000℃热处理,产物基本全部为Al_2O_3和TiB_2。动力学分析表明,Al-TiO_2-B_2O_3体系反应激活能E_a随着粉体球磨时间的延长而降低,其动力学机制属于反应-扩散模型。
采用固相反应涂覆法在Q235钢表面制备的Al_2O_3-TiB_2复相陶瓷涂层,其综合性能随热固化温度的提高而提高,随骨料和粘结剂之比的增大先提高后降低,当骨料:粘结剂=1.5:1时,涂层综合性能最佳。700℃热固化涂层界面结合方式主要为化学、冶金和扩散结合,最高显微硬度值可达HV_(0.1)1000,结合强度可达13.4MPa,热震次数可达45次,耐磨性提高为基底的3.21倍,润滑和封孔后可使耐磨性分别提高为基底的4.00和3.38倍。700℃热固化涂层耐蚀性能优异,在15wt.%H_2SO_4溶液中的平均腐蚀速率为1.06,耐蚀性提高为Q235钢基体的19.52倍,封孔后提高为基体的36.48倍。
采用固相反应涂覆法在AZ31B镁合金表面于400℃热固化制备的Al_2O_3-TiB_2复相陶瓷涂层,其综合性能随骨料和粘结剂之比和纳米Al_2O_3加入量的增大先提高后降低,当骨料:粘结剂=1.35:1,纳米Al_2O_3加入量为50%时,涂层综合性能最佳,其界面结合方式主要为化学、冶金和扩散结合,结合强度可达11.28MP,热震次数可达35次,显微硬度最大值可达HV_(0.1)750,封孔处理后,涂层的抗磨粒磨损和抗粘着磨损性能分别提高为基体的6.27和6.41倍。涂层耐蚀性能优异,在3.5wt%醋酸溶液中的平均腐蚀速率为0.2254g·m~(-2)·h~(-1),提高为基体的40.12倍,封孔后平均腐蚀速率仅为0.1488 g·m~(-2)·h~(-1),提高为基体的60.79倍。
采用固相反应热喷涂法在AZ31B镁合金表面制备的Al_2O_3-TiB_2复相陶瓷涂层综合性能优于固相反应涂覆法,涂层主要的结合方式除了机械结合外,还有化学冶金结合,热震次数可达到49次,显微硬度可达到,重熔处理后可达到HV_(0.1)1400;涂层粘着干磨损和粘着油磨损的耐磨性分别比AZ31B基体提高了10.07和11.48倍,磨粒磨损的耐磨性比AZ31B基体提高了9.3倍,明显优于普通热喷涂陶瓷涂层,重熔处理可进一步提高涂层的耐磨性。涂层在5wt.%的醋酸腐蚀溶液中的平均腐蚀速率为26.10909 g·m~(-2)·h~(-1)耐蚀性提高为基体的42.25倍,涂层封孔后,平均腐蚀速率为15.96028g·m~(-2)·h~(-1)提高为基体的67.48倍,并表现出较好的抗氧化性。
The ultra-fine powders of Al-TiO_2-B_2O_3 system were prepared by ball milling.The multiphase ceramic coating of Al_2O_3-TiB_2 on the surface of Q235 and AZ31B bases were made by solid-phase reaction method.The reaction systems of coatings were designed and properties of the coating were predicted through the Empirical Electronic Theory(EET) in solid and molecules.Behaviors of mechanochemistry and thermal chemistry of Al-TiO_2-B_2O_3 system were investigated by scanning electron microscopy(SEM), differential thermal analysis(DTA),X-rays diffraction(XRD) and laser granularity distributing apparatus.The forming mechanisms of coatings were studied through kinetics and thermodynamics.The phase composition and the characteristic of interface between coating and base were analyzed.The properties of coatings,such as hardness,bonding strength,thermal shock,wear resistance,corrosion resistance,etc.,were test too.
The calculation of EET showed that the multiphase ceramic coating of Al_2O_3-TiB_2 on the bases of Q235 and AZ31B are scientific and reasonable.A higher interface bonding can be obtained between the coating and the base,the strength and toughen of coating itself could be adjustable for the base.The calculation of thermodynamic showed that the reaction of Al-TiO_2-B_2O_3 system will happen in practice and the ultimate products are Al_2O_3 and TiB_2.The composite powders of Al-TiO_2-B_2O_3 were refined enough by ball milling and the granularity appeared in normal distribution.The medium particle diameter of powders with 4.35μm in diameter added by process control agent(PCA) could be obtained after 20h ball milling and the grain size was in nanometer degree.The shapes of particles were close to spherical and a few of new phases,such as Al_2O_3,TiB_2,etc., appeared.The system could be activated obviously by the mechanochemistry reaction. The solid reaction would happen slowly at 400℃in powders with 20h ball milling and severely at 670℃.The final products are mostly Al_2O_3 and TiB_2 after heat treatment at 700℃and completely Al_2O_3 and TiB_2 at 1000℃.The kinetics analysis showed that the activation energy E_a in Al-TiO_2-B_2O_3 system decreased with the increased ball milling time and the kinetics mechanism belonged to the reaction-diffusion model.
The comprehensive properties of Al_2O_3-TiB_2 multiphase ceramic coatings on the surface of Q235 bases prepared with coated solid-state reaction method improved with the increasing of thermal curing temperature.The properties increased firstly with the ratio of aggregates and binders and then decreased.The comprehensive properties of coatings were best when the ratio of aggregates and binders is 1.5:1. The mode of interface bonding was mainly in chemical,metallurgical and diffusional bonding.The highest microhardness of coating was HV_(0.1)1000 and the bonding strength of coatings on Q235 bases was 13.4MPa;the thermal shock times of them was 45 and the wear-resistance improved 3.21 times than the bases. The wear-resistance of coating improved 4.00 times than the bases after lubricated and 3.38 times after sealed.The corrosion resistance was best after thermal curing at 700℃.The average corrosion ratio was 1.06 g·m~(-2)·h~(-1) in aqueous solution with 15wt.%H_2SO_4.The corrosion resistance improved 19.52 times than Q235 bases and 36.48 times after sealed.
The Al_2O_3-TiB_2 multiphase ceramic coatings on the surface of AZ31B bases were prepared with coated solid-state reaction method at 400℃thermal curing temperature.The comprehensive properties increased firstly with the ratio of aggregates and binders and the added amount of Al_2O_3 in nanometer and then decreased.When the ratio of aggregates and binders is 1.35:1 and the added amount of Al_2O_3 in nanometer is 50%,the comprehensive properties of coatings were best.The mode of interface bonding was mainly in chemical,metallurgical and diffusional bonding.The bonding strength of coatings on AZ31B bases was 11.28MPa and the thermal shock times of them was 45.The highest microhardness of coating was HV_(0.1)750.The abrasive wear-resistance and the adhesive wear-resistance improved 6.27,6.41 times than the bases,respectively.The corrosion resistance was superior to the bases.The average corrosion ratio was 0.2254 g·m~(-2)·h~(-1) in aqueous solution with 3.5wt.%acetic acid.The corrosion resistance improved 40.12 times than AZ31B bases.The average corrosion ratio was 0.1488 g·m~(-2)·h~(-1) and the corrosion resistance improved 60.79 times after sealed.
The comprehensive properties of Al_2O_3-TiB_2 multiphase ceramic coatings on the surface of AZ31B bases prepared with thermal spraying were superior to that prepared with coated solid-state reaction method.The mainly mode of interface bonding included mechanical,chemical and metallurgical bonding.The thermal shock times was 49.The highest microhardness is HV_(0.1)1200 and it was HV_(0.1)1400 after remelted;the dry adhesive wear-resistance and the oil adhesive wear-resistance improved 10.07,11.48 times than the AZ31B bases,respectively; the abrasive wear-resistance improved 9.3 times than the AZ31B bases,which were superior to the common ceramic coating made by thermal spraying method. The remelted treatment could further improve the wear-resistance of coatings.The average corrosion ratio was 26.10909 g·m~(-2)·h~(-1) in aqueous solution with 5wt.% acetic acid.The corrosion resistance improved 42.25 times than AZ31B bases.The average corrosion ratio was 15.96028 g·m~(-2)·h~(-1) and the corrosion resistance improved 67.48 times after sealed.A better oxidation resistance appeared in the coatings too.
EET理论计算结果表明:在Q235钢和AZ31B镁合金基底上制备Al_2O_3-TiB_2复相陶瓷涂层具有科学性和合理性,涂层与基底之间可形成较强的界面结合,涂层本身强度和韧性可得到适当的配合。热力学计算结果表明:Al-TiO_2-B_2O_3体系在实际条件下,反应可以发生,生成的最终产物为Al_2O_3和TiB_2。机械球磨可使Al-TiO_2-B_2O_3复合粉体得到充分细化,颗粒度呈正态分布,粉体加入PCA球磨20h后,颗粒中位径可达到4.35μm,晶粒度可达到纳米级,形状近乎球形,并有少量Al_2O_3、TiB_2等新相生成。机械力化学作用可使反应体系的活性显著增强,球磨20h粉体在400℃左右就可发生缓慢的固相反应,670℃反应最为剧烈,粉体经700℃热处理,产物大部分为Al_2O_3、TiB_2,经1000℃热处理,产物基本全部为Al_2O_3和TiB_2。动力学分析表明,Al-TiO_2-B_2O_3体系反应激活能E_a随着粉体球磨时间的延长而降低,其动力学机制属于反应-扩散模型。
采用固相反应涂覆法在Q235钢表面制备的Al_2O_3-TiB_2复相陶瓷涂层,其综合性能随热固化温度的提高而提高,随骨料和粘结剂之比的增大先提高后降低,当骨料:粘结剂=1.5:1时,涂层综合性能最佳。700℃热固化涂层界面结合方式主要为化学、冶金和扩散结合,最高显微硬度值可达HV_(0.1)1000,结合强度可达13.4MPa,热震次数可达45次,耐磨性提高为基底的3.21倍,润滑和封孔后可使耐磨性分别提高为基底的4.00和3.38倍。700℃热固化涂层耐蚀性能优异,在15wt.%H_2SO_4溶液中的平均腐蚀速率为1.06,耐蚀性提高为Q235钢基体的19.52倍,封孔后提高为基体的36.48倍。
采用固相反应涂覆法在AZ31B镁合金表面于400℃热固化制备的Al_2O_3-TiB_2复相陶瓷涂层,其综合性能随骨料和粘结剂之比和纳米Al_2O_3加入量的增大先提高后降低,当骨料:粘结剂=1.35:1,纳米Al_2O_3加入量为50%时,涂层综合性能最佳,其界面结合方式主要为化学、冶金和扩散结合,结合强度可达11.28MP,热震次数可达35次,显微硬度最大值可达HV_(0.1)750,封孔处理后,涂层的抗磨粒磨损和抗粘着磨损性能分别提高为基体的6.27和6.41倍。涂层耐蚀性能优异,在3.5wt%醋酸溶液中的平均腐蚀速率为0.2254g·m~(-2)·h~(-1),提高为基体的40.12倍,封孔后平均腐蚀速率仅为0.1488 g·m~(-2)·h~(-1),提高为基体的60.79倍。
采用固相反应热喷涂法在AZ31B镁合金表面制备的Al_2O_3-TiB_2复相陶瓷涂层综合性能优于固相反应涂覆法,涂层主要的结合方式除了机械结合外,还有化学冶金结合,热震次数可达到49次,显微硬度可达到,重熔处理后可达到HV_(0.1)1400;涂层粘着干磨损和粘着油磨损的耐磨性分别比AZ31B基体提高了10.07和11.48倍,磨粒磨损的耐磨性比AZ31B基体提高了9.3倍,明显优于普通热喷涂陶瓷涂层,重熔处理可进一步提高涂层的耐磨性。涂层在5wt.%的醋酸腐蚀溶液中的平均腐蚀速率为26.10909 g·m~(-2)·h~(-1)耐蚀性提高为基体的42.25倍,涂层封孔后,平均腐蚀速率为15.96028g·m~(-2)·h~(-1)提高为基体的67.48倍,并表现出较好的抗氧化性。
The ultra-fine powders of Al-TiO_2-B_2O_3 system were prepared by ball milling.The multiphase ceramic coating of Al_2O_3-TiB_2 on the surface of Q235 and AZ31B bases were made by solid-phase reaction method.The reaction systems of coatings were designed and properties of the coating were predicted through the Empirical Electronic Theory(EET) in solid and molecules.Behaviors of mechanochemistry and thermal chemistry of Al-TiO_2-B_2O_3 system were investigated by scanning electron microscopy(SEM), differential thermal analysis(DTA),X-rays diffraction(XRD) and laser granularity distributing apparatus.The forming mechanisms of coatings were studied through kinetics and thermodynamics.The phase composition and the characteristic of interface between coating and base were analyzed.The properties of coatings,such as hardness,bonding strength,thermal shock,wear resistance,corrosion resistance,etc.,were test too.
The calculation of EET showed that the multiphase ceramic coating of Al_2O_3-TiB_2 on the bases of Q235 and AZ31B are scientific and reasonable.A higher interface bonding can be obtained between the coating and the base,the strength and toughen of coating itself could be adjustable for the base.The calculation of thermodynamic showed that the reaction of Al-TiO_2-B_2O_3 system will happen in practice and the ultimate products are Al_2O_3 and TiB_2.The composite powders of Al-TiO_2-B_2O_3 were refined enough by ball milling and the granularity appeared in normal distribution.The medium particle diameter of powders with 4.35μm in diameter added by process control agent(PCA) could be obtained after 20h ball milling and the grain size was in nanometer degree.The shapes of particles were close to spherical and a few of new phases,such as Al_2O_3,TiB_2,etc., appeared.The system could be activated obviously by the mechanochemistry reaction. The solid reaction would happen slowly at 400℃in powders with 20h ball milling and severely at 670℃.The final products are mostly Al_2O_3 and TiB_2 after heat treatment at 700℃and completely Al_2O_3 and TiB_2 at 1000℃.The kinetics analysis showed that the activation energy E_a in Al-TiO_2-B_2O_3 system decreased with the increased ball milling time and the kinetics mechanism belonged to the reaction-diffusion model.
The comprehensive properties of Al_2O_3-TiB_2 multiphase ceramic coatings on the surface of Q235 bases prepared with coated solid-state reaction method improved with the increasing of thermal curing temperature.The properties increased firstly with the ratio of aggregates and binders and then decreased.The comprehensive properties of coatings were best when the ratio of aggregates and binders is 1.5:1. The mode of interface bonding was mainly in chemical,metallurgical and diffusional bonding.The highest microhardness of coating was HV_(0.1)1000 and the bonding strength of coatings on Q235 bases was 13.4MPa;the thermal shock times of them was 45 and the wear-resistance improved 3.21 times than the bases. The wear-resistance of coating improved 4.00 times than the bases after lubricated and 3.38 times after sealed.The corrosion resistance was best after thermal curing at 700℃.The average corrosion ratio was 1.06 g·m~(-2)·h~(-1) in aqueous solution with 15wt.%H_2SO_4.The corrosion resistance improved 19.52 times than Q235 bases and 36.48 times after sealed.
The Al_2O_3-TiB_2 multiphase ceramic coatings on the surface of AZ31B bases were prepared with coated solid-state reaction method at 400℃thermal curing temperature.The comprehensive properties increased firstly with the ratio of aggregates and binders and the added amount of Al_2O_3 in nanometer and then decreased.When the ratio of aggregates and binders is 1.35:1 and the added amount of Al_2O_3 in nanometer is 50%,the comprehensive properties of coatings were best.The mode of interface bonding was mainly in chemical,metallurgical and diffusional bonding.The bonding strength of coatings on AZ31B bases was 11.28MPa and the thermal shock times of them was 45.The highest microhardness of coating was HV_(0.1)750.The abrasive wear-resistance and the adhesive wear-resistance improved 6.27,6.41 times than the bases,respectively.The corrosion resistance was superior to the bases.The average corrosion ratio was 0.2254 g·m~(-2)·h~(-1) in aqueous solution with 3.5wt.%acetic acid.The corrosion resistance improved 40.12 times than AZ31B bases.The average corrosion ratio was 0.1488 g·m~(-2)·h~(-1) and the corrosion resistance improved 60.79 times after sealed.
The comprehensive properties of Al_2O_3-TiB_2 multiphase ceramic coatings on the surface of AZ31B bases prepared with thermal spraying were superior to that prepared with coated solid-state reaction method.The mainly mode of interface bonding included mechanical,chemical and metallurgical bonding.The thermal shock times was 49.The highest microhardness is HV_(0.1)1200 and it was HV_(0.1)1400 after remelted;the dry adhesive wear-resistance and the oil adhesive wear-resistance improved 10.07,11.48 times than the AZ31B bases,respectively; the abrasive wear-resistance improved 9.3 times than the AZ31B bases,which were superior to the common ceramic coating made by thermal spraying method. The remelted treatment could further improve the wear-resistance of coatings.The average corrosion ratio was 26.10909 g·m~(-2)·h~(-1) in aqueous solution with 5wt.% acetic acid.The corrosion resistance improved 42.25 times than AZ31B bases.The average corrosion ratio was 15.96028 g·m~(-2)·h~(-1) and the corrosion resistance improved 67.48 times after sealed.A better oxidation resistance appeared in the coatings too.
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