微波烧结ITO靶材研究
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摘要
微波烧结具有节能、缩短烧结周期等一系列优点,获得的材料表现出高致密度、组织均匀等特征,在近20年来备受关注。随着现代工业向高效节能方向的发展,微波烧结将会有更为广阔的应用前景。ITO靶材作为制备透明导电氧化物薄膜的材料,在军用和民用领域有着广泛应用。鉴于微波烧结的特殊优势和ITO靶材的重要价值,论文首次应用微波烧结技术制备ITO靶材,并研究了微波烧结制备ITO靶材的工艺、致密化行为、以及靶材显微组织,得到以下结论：
(1)微波烧结能快速制备高致密度、显微组织均匀的的ITO靶材。研究发现,靶材的相对密度随着烧结温度升高而增大；在1580℃进行微波烧结时,靶材的相对密度随着保温时间的延长先增大后减小,在保温1.5h时相对密度达到最大值(99.58%),高温更长时间烧结对ITO靶材的致密化不利。另外,微波烧结促进了ITO靶材的致密化,即以更低的烧结温度或更短的保温时间均能获得综合性能较好的材料,是一种活化烧结模式。升温速度是微波烧结的一个重要参数,ITO靶材可以在10-65℃/min升温速度范围内烧结出相对密度和收缩率均较高的ITO靶材,而最佳升温速度约为45℃/min;
(2)在微波烧结制备ITO靶材的过程中,压制压力也有着重要的影响。压坯和ITO靶材的密度均随着压制压力的升高而增加,在压制压力为500MPa时达到最高。提高压制压力有利于靶材的致密化；在最佳的微波烧结工艺参数(1580℃×1.5h×500MPa)条件下,ITO靶材密度达到7.12g/cm3,与常规烧结(7.13g/cm3)几乎相当,但与常规烧结相比,微波烧结温度略低,但烧结时间仅是常规烧结的1/8,可以明显缩短烧结周期,有利于节约能源,降低成本。这对工业生产有积极意义；
(3)微波烧结制备的高密度ITO靶材显微组织均匀,失氧率比商用靶材低,晶粒尺寸较均匀,晶粒尺寸大致为3.5-7.3μm,而且晶粒尺寸较商用靶材要小,不同温度下制备的ITO靶材均无Sn02相析出,仍是单一的固溶体相,不存在第二相。
Microwave sintering has gained a lot of acceptance in resent decades because of its dramatic advantages such as energy efficiency, reduced fabricating cycle, rapid densification, and homogeneous microstructure.And microwave sintering would expand its applications in modern industries as it can meet the high efficiency and energy saving demands trend.ITO(Indiμm Tin Oxide)target as an important material that can be made into transparent conductive film,have broad application in ordnance and civilian. Based on the nμmerous advantages of microwave sintering and the great significance of ITO,our experiment fabricates the ITO targets by microwave process first,researches in terms of sintering process,microstructure and densification behaviors.The major conclusions of this paper were sμmmarized as following:
(1) The resulted evidence shows microwave sintering technique possesses ITO targets with full density and homogeneous microstructure in short cycle. The results indicated that the relative density of samples increased with the increasing of the temperature. The relative density of samples increased then decreased with the time increasing when sintered at 1580℃. The relative density reached the maximμm value (99.58%) when 1.5 hours soaking. It is shown that high temperature and long soaking deteriorate densification of the ITO targets.In addition, the microwave sintering promotes densification of ITO targets, which can lower the sintering temperature and shorter soaking time to obtain High performance ITO targets,is activated sintering model. Heating rate is an important parameter in microwave sintering, high density and shrinkage ITO target can be sintered at the heating rate of 10-65℃/min,but the best heating rate is about 45℃/min;
(2) In the process of microwave sintering ITO targets, the compaction pressure also has an important impact. The relative density of green body and ITO targets increased with the compacting pressure increasing,and reach the maximμm at the pressure 500MPa. Compacting pressure is conducive to improve the densification of targets;in the best condition of microwave sintering process parameters(1580℃×1.5h×500MPa), the ITO target density reaches 7.12g/cm3,which is almost equivalent to the conventional sintering (7.13 g/cm3),but in comparison with conventional sintering, microwave sintering temperature is slightly lower,and the sintering time is only 1/8 of the conventional sintering. Microwave sintering can significantly reduce the sintering cycle, help save energy and reduce costs,which has positive significance in industrial application;
(3) ITO targets microstructure sintered by microwave sintering are homogeneous, Oxygen loss rate lower than the commercial target.The grain size is uniform,3.5-7.3μm approximately,which is smaller than the commercial target.The XRD analysis indicates that no SnO2 precipitation is observed under different sintering temperature, and ITO targets still are single-phase, without the second phase.
(1)微波烧结能快速制备高致密度、显微组织均匀的的ITO靶材。研究发现,靶材的相对密度随着烧结温度升高而增大；在1580℃进行微波烧结时,靶材的相对密度随着保温时间的延长先增大后减小,在保温1.5h时相对密度达到最大值(99.58%),高温更长时间烧结对ITO靶材的致密化不利。另外,微波烧结促进了ITO靶材的致密化,即以更低的烧结温度或更短的保温时间均能获得综合性能较好的材料,是一种活化烧结模式。升温速度是微波烧结的一个重要参数,ITO靶材可以在10-65℃/min升温速度范围内烧结出相对密度和收缩率均较高的ITO靶材,而最佳升温速度约为45℃/min;
(2)在微波烧结制备ITO靶材的过程中,压制压力也有着重要的影响。压坯和ITO靶材的密度均随着压制压力的升高而增加,在压制压力为500MPa时达到最高。提高压制压力有利于靶材的致密化；在最佳的微波烧结工艺参数(1580℃×1.5h×500MPa)条件下,ITO靶材密度达到7.12g/cm3,与常规烧结(7.13g/cm3)几乎相当,但与常规烧结相比,微波烧结温度略低,但烧结时间仅是常规烧结的1/8,可以明显缩短烧结周期,有利于节约能源,降低成本。这对工业生产有积极意义；
(3)微波烧结制备的高密度ITO靶材显微组织均匀,失氧率比商用靶材低,晶粒尺寸较均匀,晶粒尺寸大致为3.5-7.3μm,而且晶粒尺寸较商用靶材要小,不同温度下制备的ITO靶材均无Sn02相析出,仍是单一的固溶体相,不存在第二相。
Microwave sintering has gained a lot of acceptance in resent decades because of its dramatic advantages such as energy efficiency, reduced fabricating cycle, rapid densification, and homogeneous microstructure.And microwave sintering would expand its applications in modern industries as it can meet the high efficiency and energy saving demands trend.ITO(Indiμm Tin Oxide)target as an important material that can be made into transparent conductive film,have broad application in ordnance and civilian. Based on the nμmerous advantages of microwave sintering and the great significance of ITO,our experiment fabricates the ITO targets by microwave process first,researches in terms of sintering process,microstructure and densification behaviors.The major conclusions of this paper were sμmmarized as following:
(1) The resulted evidence shows microwave sintering technique possesses ITO targets with full density and homogeneous microstructure in short cycle. The results indicated that the relative density of samples increased with the increasing of the temperature. The relative density of samples increased then decreased with the time increasing when sintered at 1580℃. The relative density reached the maximμm value (99.58%) when 1.5 hours soaking. It is shown that high temperature and long soaking deteriorate densification of the ITO targets.In addition, the microwave sintering promotes densification of ITO targets, which can lower the sintering temperature and shorter soaking time to obtain High performance ITO targets,is activated sintering model. Heating rate is an important parameter in microwave sintering, high density and shrinkage ITO target can be sintered at the heating rate of 10-65℃/min,but the best heating rate is about 45℃/min;
(2) In the process of microwave sintering ITO targets, the compaction pressure also has an important impact. The relative density of green body and ITO targets increased with the compacting pressure increasing,and reach the maximμm at the pressure 500MPa. Compacting pressure is conducive to improve the densification of targets;in the best condition of microwave sintering process parameters(1580℃×1.5h×500MPa), the ITO target density reaches 7.12g/cm3,which is almost equivalent to the conventional sintering (7.13 g/cm3),but in comparison with conventional sintering, microwave sintering temperature is slightly lower,and the sintering time is only 1/8 of the conventional sintering. Microwave sintering can significantly reduce the sintering cycle, help save energy and reduce costs,which has positive significance in industrial application;
(3) ITO targets microstructure sintered by microwave sintering are homogeneous, Oxygen loss rate lower than the commercial target.The grain size is uniform,3.5-7.3μm approximately,which is smaller than the commercial target.The XRD analysis indicates that no SnO2 precipitation is observed under different sintering temperature, and ITO targets still are single-phase, without the second phase.
引文
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