WO2013082822A1 - 玻璃基板薄膜溅射靶材及其制备方法 - Google Patents

玻璃基板薄膜溅射靶材及其制备方法 Download PDF

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WO2013082822A1
WO2013082822A1 PCT/CN2011/083799 CN2011083799W WO2013082822A1 WO 2013082822 A1 WO2013082822 A1 WO 2013082822A1 CN 2011083799 W CN2011083799 W CN 2011083799W WO 2013082822 A1 WO2013082822 A1 WO 2013082822A1
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sintering
target
glass substrate
preparation
alloy material
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French (fr)
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寇浩
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TCL China Star Optoelectronics Technology Co Ltd
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Shenzhen China Star Optoelectronics Technology Co Ltd
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Priority to US13/380,861 priority Critical patent/US9162286B2/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering
    • H01J37/3488—Constructional details of particle beam apparatus not otherwise provided for, e.g. arrangement, mounting, housing, environment; special provisions for cleaning or maintenance of the apparatus
    • H01J37/3491—Manufacturing of targets
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
    • C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density

Definitions

  • the embodiment of the invention relates to a preparation method, in particular to a glass substrate thin film sputtering target and a preparation method thereof.
  • the preparation process of the large-scale glass substrate thin film sputtering target used in the TFT-LCD (thin film transistor liquid crystal display device) industry mainly includes the steps of weighing ⁇ mixing granulation ⁇ forming ⁇ drying ⁇ sintering ⁇ processing.
  • the most important influence on the use of the sputtering target in the later panel factory is the forming step and the sintering step.
  • the main forming and sintering methods include hot pressing (Hot). Press) and Cool Press, the two main methods are the following:
  • the targets prepared by the two methods all have the problem that the relative density of the target is insufficient and gas impurities such as oxygen are present inside the grain and at the grain boundary.
  • the surface of the target has micro-cavities so that the electric field on the surface of the target is unevenly distributed, and it is easy to generate a strong electric field on the surface.
  • the local ability of Ar (argon) to hit the target is too high, so that the oxygen atoms are impinged on the free, forming a high-resistance region and gradually forming film-forming deposits and protrusions, resulting in poor film formation uniformity and a large surface roughness of the film;
  • the sintering time is too long, and the sintering relies mainly on the conduction heat transfer and the radiation heat transfer of the heating body, resulting in excessive grain size of the target; therefore, the physical organization caused by physical vapor deposition (PVD) in the panel factory The genetic effect" will make the grain size of the film deposited larger and the uniformity is poor, which is not conducive to the development of large-sized panels;
  • PVD physical vapor deposition
  • the technical problem to be solved by the present invention is to provide a glass substrate thin film sputtering target and a preparation method thereof, which can improve the target quality and shorten the target preparation time.
  • an embodiment of the present invention discloses a method for preparing a glass substrate thin film sputtering target, comprising: weighing an alloy material for preparing a glass substrate thin film sputtering target, and the particle diameter of the alloy material Less than or equal to 100 nm; the weighed alloy material is added to the plasma pressure forming sintering cavity for sintering, and the plasma pressure forming sintering cavity is externally pressurized to obtain a target sintered body, and the sintering temperature is The sintering time is 5-20 minutes at 500 ° C ⁇ 1600 ° C; the sintered body of the target obtained by sintering is post-processed.
  • the sintering temperature is from 1400 ° C to 1500 ° C and the sintering time is from 10 to 15 minutes.
  • the target sintered body obtained by the sintering has a relative density of greater than or equal to 99.5% and an oxygen content of less than or equal to 500 ppm.
  • the sintering temperature is from 600 ° C to 700 ° C and the sintering time is 10 minutes.
  • the target sintered body obtained by the sintering has a relative density of greater than or equal to 99.8% and an oxygen content of less than or equal to 1000 ppm.
  • an embodiment of the present invention discloses a method for preparing a glass substrate thin film sputtering target, comprising: weighing an alloy material for forming a glass substrate thin film sputtering target; adding the weighed alloy material To plasma pressure forming (P2C, Plasma Pressure Sintering is performed in the sintered chamber of the compaction to obtain a sintered body of the target, the sintering temperature is 500 ° C to 1600 ° C, and the sintering time is 5 to 20 minutes; and the sintered body of the target obtained by sintering is subjected to post processing.
  • P2C Plasma Pressure Sintering is performed in the sintered chamber of the compaction to obtain a sintered body of the target, the sintering temperature is 500 ° C to 1600 ° C, and the sintering time is 5 to 20 minutes; and the sintered body of the target obtained by sintering is subjected to post processing.
  • the alloy material has a particle size of less than or equal to 100 nanometers.
  • the sintering temperature is from 1400 ° C to 1500 ° C and the sintering time is from 10 to 15 minutes.
  • the target sintered body obtained by the sintering has a relative density of greater than or equal to 99.5% and an oxygen content of less than or equal to 500 ppm.
  • the sintering temperature is from 600 ° C to 700 ° C and the sintering time is 10 minutes.
  • the target sintered body obtained by the sintering has a relative density of greater than or equal to 99.8% and an oxygen content of less than or equal to 1000 ppm.
  • the method when sintering is performed in the plasma pressure forming sintering cavity, the method further comprises pressurizing the plasma pressure forming sintering cavity from the outside.
  • the embodiment of the invention further discloses a glass substrate thin film sputtering target, which is prepared by the following preparation method, the preparation method comprises: weighing an alloy material for preparing a glass substrate thin film sputtering target; The amount of alloy material is added to the plasma pressure forming sintering cavity for sintering to obtain a target sintered body, the sintering temperature is 500 ° C ⁇ 1600 ° C, the sintering time is 5 ⁇ 20 minutes; the sintered body obtained by sintering is late Processing.
  • the invention has the beneficial effects that the method for preparing a glass substrate thin film sputtering target and the glass substrate thin film sputtering target adopt a rapid sintering method of plasma pressure forming, which is different from the prior art. Therefore, the target quality can be improved and the target preparation time can be shortened.
  • Figure 1 is a schematic view showing the steps of a method for preparing a glass substrate thin film sputtering target according to a preferred embodiment of the present invention.
  • FIG. 1 is a schematic diagram showing the steps of a method for preparing a glass substrate thin film sputtering target according to a preferred embodiment of the present invention.
  • the preparation method includes:
  • Step S1 weighing an alloy material for preparing a glass substrate thin film sputtering target
  • step S2 the weighed alloy material is added to the plasma pressure forming sintering cavity for sintering to obtain a target sintered body, and the sintered body of the target sintered body is sintered at a temperature of 500 ° C to 1600 ° C and a sintering time of 5 to 20 minutes. ;
  • step S3 the sintered body of the target obtained by sintering is subjected to post-processing.
  • the alloy material has a particle diameter of less than or equal to 100 nm, and when sintering is performed in the plasma pressure forming sintering cavity, the method further comprises pressurizing the plasma pressure forming sintering cavity from the outside.
  • the sintering temperature is 1400 ° C to 1500 ° C
  • the sintering time is 10 to 15 minutes
  • the sintered body obtained by the sintering has a relative density of 99.5% or more and an oxygen content of 500 ppm or less.
  • the sintering temperature is 600 ° C to 700 ° C, and the sintering time is 10 minutes.
  • the sintered body obtained by the sintering has a relative density of 99.8% or more and an oxygen content of 1000 ppm or less.
  • the target sintered body is obtained, the sintering temperature is 1400 ⁇ 1500 ° C, and the sintering time is 10-15 minutes.
  • the relative density of the target sintered body is ⁇ 99.5%, and the oxygen content is ⁇ 500ppm.
  • the target sintered body is obtained, the sintering temperature is 1500-1600 ° C, and the sintering time is 16-20 minutes, and the relative density of the target sintered body is ⁇ 99.3%, and the oxygen content is ⁇ 400 ppm.
  • the target sintered body is obtained by sintering, the sintering temperature is 600-700 ° C, and the sintering time is 5-9 minutes.
  • the relative density of the target sintered body is ⁇ 99.6%, and the oxygen content is ⁇ 800 ppm.
  • the embodiment of the invention further provides a glass substrate thin film sputtering target which can be obtained by the above preparation method and can be used for the fabrication of a large TFT-LCD.
  • the specific preparation method will not be described here.
  • the method for preparing a glass substrate thin film sputtering target according to an embodiment of the present invention and the glass substrate thin film sputtering target adopt a rapid sintering method of plasma pressure forming instead of the conventional hot press sintering and cold pressing sintering method.
  • the rapid sintering method of pressure forming is applied to the preparation of a glass substrate thin film sputtering target with the following characteristics:
  • the use of plasma in the initial activation phase destroys and removes the surface oxide and impurity layers of the sintered alloy material, while providing the partial activation energy required for the micro-nano bond of the internal cleaning material of the alloy material particles, reducing the necessary Processing temperature, which is critical to prevent particle growth during sintering, thereby protecting the nano-sized properties of the particles;
  • the sintering time in the present invention only takes about 10 to 15 minutes, which greatly shortens the sintering time and the target preparation time, and also reduces the sintered alloy material. It is easy to oxidize or unstable, and it is not necessary to add excessive oxidizable part of the material during the weighing process, so that the composition points of the alloy material are more fine and controllable, and the purity of the target is improved;
  • the method for preparing a glass substrate thin film sputtering target according to the embodiment of the present invention and the glass substrate thin film sputtering target adopt a rapid sintering method of plasma pressure forming, thereby improving the target quality and shortening the target. Material preparation time and other advantages.

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Abstract

一种玻璃基板薄膜溅射靶材的制备方法，包括：称量用于制作玻璃基板薄膜溅射靶材的合金材料；将称量的合金材料添加到等离子体压力成型烧结腔体中进行烧结，得到靶材烧结体，烧结温度为500°C〜1600°C，烧结时间为5〜20分钟；将烧结获得的靶材烧结体进行后期加工处理。还提供了一种玻璃基板薄膜溅射靶材。由于采用了等离子体压力成型的快速烧结方法，因此能够提高靶材品质和缩短靶材制备时间。

Description

玻璃基板薄膜溅射靶材及其制备方法
【技术领域】
本发明实施例涉及一种制备方法，尤其涉及一种玻璃基板薄膜溅射靶材及其制备方法。
【背景技术】
目前TFT-LCD（薄膜晶体管液晶显示装置）行业采用的大型玻璃基板薄膜溅射靶材的制备流程主要包括称量→混合造粒→成形→干燥→烧结→加工等步骤。其中，对溅射靶材在后期面板厂使用中影响最大的为成形步骤与烧结步骤，目前主要采用的成形与烧结方式包括热压（Hot Press）与冷压（Cool Press），这两种方式主要存在以下不足：
第一，这两种方式所制备的靶材均体现出靶材相对密度不足及晶粒内部及晶界存在氧气等气体杂质的问题。其中，靶材表面具有微空洞使得靶材表面的电场分布不均，极容易产生表面较强电场。此外，Ar（氩）撞击靶材局部能力太高，从而将氧原子撞击游离，形成高阻区域并逐渐形成成膜堆积及凸起，造成成膜均匀性差且膜层表面的粗糙度较大；
第二，烧结时间过长，烧结时主要依靠加热体的传导传热及辐射传热，致使靶材晶粒尺寸过大；因此在面板厂进行物理气相沉积（PVD）时，所引起的“组织遗传效应”会使得薄膜沉积的晶粒尺寸较大且均匀性较差，不利于开发大尺寸面板；
第三，在较长时间烧结过程中，由于烧结粉体越细小，吸附的杂质元素越多，长时间烧结产生的扩散作用，会在晶界出现团聚的杂质离子或吸附气体，在面板厂进行物理气相沉积成膜时同样也会产生污染影响良率及产品品质等问题。
因此，综上所述，提出一种可以解决上述问题的玻璃基板薄膜溅射靶材的制备方法显得较为必需。
【发明内容】
本发明主要解决的技术问题是提供一种玻璃基板薄膜溅射靶材及其制备方法，能够提高靶材品质和缩短靶材制备时间。
为了解决上述技术问题，本发明实施例公开了一种玻璃基板薄膜溅射靶材的制备方法，包括：称量用于制作玻璃基板薄膜溅射靶材的合金材料，所述合金材料的粒径小于或等于100纳米；将称量的合金材料添加到等离子体压力成型烧结腔体中进行烧结，并对所述等离子体压力成型烧结腔体从外部加压，获得靶材烧结体，烧结温度为500℃~1600℃，烧结时间为5~20分钟；将烧结获得的靶材烧结体进行后期加工处理。
在本发明一个较佳实施例中，所述合金材料的成分配比为MoxCuyTiz，其中x，y，z均介于0-100%之间，且x+y+z=100%。
在本发明一个较佳实施例中，所述烧结温度为1400℃~1500℃，烧结时间为10~15分钟。
在本发明一个较佳实施例中，所述烧结获得的靶材烧结体的相对密度大于或等于99.5%，氧含量小于或等于500ppm。
在本发明一个较佳实施例中，所述合金材料的成分配比为（In2O3）x（SnO2）y，其中y介于0~7%之间，且x+y=100%。
在本发明一个较佳实施例中，所述烧结温度为600℃~700℃，烧结时间为10分钟。
在本发明一个较佳实施例中，所述烧结获得的靶材烧结体的相对密度大于或等于99.8%，氧含量小于或等于1000ppm。
为了解决上述技术问题，本发明实施例公开了一种玻璃基板薄膜溅射靶材的制备方法，包括：称量用于制作玻璃基板薄膜溅射靶材的合金材料；将称量的合金材料添加到等离子体压力成型（P2C，Plasma Pressure Compaction）烧结腔体中进行烧结，得到靶材烧结体，烧结温度为500℃~1600℃，烧结时间为5~20分钟；将烧结获得的靶材烧结体进行后期加工处理。
在本发明一个较佳实施例中，所述合金材料的粒径小于或等于100纳米。
在本发明一个较佳实施例中，所述合金材料的成分配比为MoxCuyTiz，其中x，y，z均介于0-100%之间，且x+y+z=100%。
在本发明一个较佳实施例中，所述烧结温度为1400℃~1500℃，烧结时间为10~15分钟。
在本发明一个较佳实施例中，所述烧结获得的靶材烧结体的相对密度大于或等于99.5%，氧含量小于或等于500ppm。
在本发明一个较佳实施例中，所述合金材料的成分配比为（In2O3）x（SnO2）y，其中y介于0~7%之间，且x+y=100%。
在本发明一个较佳实施例中，所述烧结温度为600℃~700℃，烧结时间为10分钟。
在本发明一个较佳实施例中，所述烧结获得的靶材烧结体的相对密度大于或等于99.8%，氧含量小于或等于1000ppm。
在本发明一个较佳实施例中，在等离子体压力成型烧结腔体中进行烧结时，还包括对所述等离子体压力成型烧结腔体从外部加压。
本发明实施例还公开了一种玻璃基板薄膜溅射靶材，其由下述制备方法制得，所述制备方法包括：称量用于制作玻璃基板薄膜溅射靶材的合金材料；将称量的合金材料添加到等离子体压力成型烧结腔体中进行烧结，得到靶材烧结体，烧结温度为500℃~1600℃，烧结时间为5~20分钟；将烧结获得的靶材烧结体进行后期加工处理。
本发明的有益效果是：区别于现有技术的情况，本发明实施例的玻璃基板薄膜溅射靶材的制备方法及玻璃基板薄膜溅射靶材由于采用了等离子体压力成型的快速烧结方法，因此能够提高靶材品质和缩短靶材制备时间。
【附图说明】
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其它的附图，其中：
图1是 本发明优选实施例玻璃基板薄膜溅射靶材的制备方法的步骤示意图。
【具体实施方式】
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
请参阅图1，图1是本发明优选实施例玻璃基板薄膜溅射靶材的制备方法的步骤示意图，所述制备方法包括：
步骤S1，称量用于制作玻璃基板薄膜溅射靶材的合金材料；
步骤S2，将称量的合金材料添加到等离子体压力成型烧结腔体中进行烧结，得到靶材烧结体，烧结获得靶材烧结体烧结温度为500℃~1600℃，烧结时间为5~20分钟；
步骤S3，将烧结获得的靶材烧结体进行后期加工处理。
其中，所述合金材料的粒径小于或等于100纳米，在等离子体压力成型烧结腔体中进行烧结时，还包括对所述等离子体压力成型烧结腔体从外部加压。
所述合金材料的成分配比可以为MoxCuyTiz，其中x，y，z均介于0-100%之间，且x+y+z=100%。此时，烧结温度为1400℃~1500℃，烧结时间为10~15分钟，所述烧结获得的靶材烧结体的相对密度大于或等于99.5%，氧含量小于或等于500ppm。
所述合金材料的成分配比还可以为（In2O3）x（SnO2）y，其中y介于0~7%之间，且x+y=100%。此时，所述烧结温度为600℃~700℃，烧结时间为10分钟，所述烧结获得的靶材烧结体的相对密度大于或等于99.8%，氧含量小于或等于1000ppm。
以下以多个实施例对本发明玻璃基板薄膜溅射靶材的制备方法进行说明。
实施例1：
将经过称量的成分配比为MoxCuyTiz（x，y，z均介于0-100%之间，且x+y+z=100%）合金添加入等离子体压力成型烧结腔体中，进行烧结获得靶材烧结体，烧结温度为1400~1500℃，烧结时间为10~15分钟，可以测得靶材烧结体相对密度≥99.5%，氧含量≤500ppm。
实施例2：
将经过称量的成分配比为MoxCuyTiz（x，y，z均介于0-100%之间，且x+y+z=100%）合金添加入等离子体压力成型烧结腔体中，进行烧结获得靶材烧结体，烧结温度为1500~1600℃，烧结时间为16~20分钟，可以测得靶材烧结体相对密度≥99.3%，氧含量≤400ppm。
实施例3：
将经过称量的成分配比为（In2O3）x（SnO2）y - ITO合金（y介于0-7%之间，且x+y=100%）添加入等离子体压力成型烧结腔体中，进行烧结获得靶材烧结体，烧结温度为600~700℃，烧结时间为10分钟，可以测得靶材烧结体相对密度≥99.8%，氧含量≤1000ppm。
实施例4：
将经过称量的成分配比为（In2O3）x（SnO2）y（y介于0-7%之间，且x+y=100%）ITO合金添加入等离子体压力成型烧结腔体中，进行烧结获得靶材烧结体，烧结温度为600~700℃，烧结时间为5~9分钟，可以测得靶材烧结体相对密度≥99.6%，氧含量≤800ppm。
本发明实施例还提供了一种玻璃基板薄膜溅射靶材，所述玻璃基板薄膜溅射靶材可以由上述制备方法制得，并能用于大型TFT-LCD的制作。具体制备方法在此不再赘述。
本发明实施例的玻璃基板薄膜溅射靶材的制备方法及玻璃基板薄膜溅射靶材采用了等离子体压力成型的快速烧结方法来取代传统的热压烧结和冷压烧结方式，所述等离子体压力成型的快速烧结方法应用于制备玻璃基板薄膜溅射靶材中具有如下特点：
第一，利用等离子体在初始的活化阶段破坏并去除了烧结的合金材料的表面氧化物和杂质层，同时提供合金材料微粒内部清洁材料的微纳结合所需的部分活化能，降低了必要的处理温度，这对于防止烧结过程中的微粒生长，从而保护微粒的纳米尺寸属性来说至关重要；
第二，在外部加压的协同作用下，加速烧结的合金材料的致密化，有利于提升相对密度和降低氧含量；
第三，如果使用传统烧结方式需要耗时2~3小时，本发明中的烧结时间仅需10~15分钟左右，极大的缩短烧结时间和靶材制备时间，还可以降低了烧结的合金材料中易于氧化或不稳定因素，无需在称量过程中添加过量易氧化部分材料，使合金材料的成分点更加精细可控，提高了靶材的纯净度；
第四，提高靶材的相对密度、合金纯净度、降低靶材烧结的合金材料尺寸、使合金成分细微可控，有利于提高面板厂物理气相沉积进行溅射成膜的均匀性、工艺良率和产品品质。
综上所述，本发明实施例的玻璃基板薄膜溅射靶材的制备方法及玻璃基板薄膜溅射靶材由于采用了等离子体压力成型的快速烧结方法，因此具有能够提高靶材品质、缩短靶材制备时间等优点。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换，或直接或间接运用在其它相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (17)

  1. 一种玻璃基板薄膜溅射靶材的制备方法，其特征在于，包括：
    称量用于制作玻璃基板薄膜溅射靶材的合金材料，所述合金材料的粒径小于或等于100纳米；
    将称量的合金材料添加到等离子体压力成型烧结腔体中进行烧结，并对所述等离子体压力成型烧结腔体从外部加压，获得靶材烧结体，烧结温度为500℃~1600℃，烧 结时间为5~20分钟；
    将烧结获得的靶材烧结体进行后期加工处理。
  2. 根据权利要求1所述的制备方法，其特征在于，所述合金材料的成分配比为MoxCuyTiz，其中x，y，z均介于0-100%之间，且x+y+z=100%。
  3. 根据权利要求2所述的制备方法，其特征在于，所述烧结温度为1400℃~1500℃，烧结时间为10~15分钟。
  4. 根据权利要求3所述的制备方法，其特征在于，所述烧结获得的靶材烧结体的相对密度大于或等于99.5%，氧含量小于或等于500ppm。
  5. 根据权利要求1所述的制备方法，其特征在于，所述合金材料的成分配比为（In2O3）x（SnO2）y，其中y介于0~7%之间，且x+y=100%。
  6. 根据权利要求5所述的制备方法，其特征在于，所述烧结温度为600℃~700℃，烧结时间为10分钟。
  7. 根据权利要求6所述的制备方法，其特征在于，所述烧结获得的靶材烧结体的相对密度大于或等于99.8%，氧含量小于或等于1000ppm。
  8. 一种玻璃基板薄膜溅射靶材的制备方法，其特征在于，包括：
    称量用于制作玻璃基板薄膜溅射靶材的合金材料；
    将称量的合金材料添加到等离子体压力成型烧结腔体中进行烧结，得到靶材烧结体，烧结温度为500℃~1600℃，烧结时间为5~20分钟；
    将烧结获得的靶材烧结体进行后期加工处理。
  9. 根据权利要求8所述的制备方法，其特征在于，所述合金材料的粒径小于或等于100纳米。
  10. 根据权利要求8所述的制备方法，其特征在于，所述合金材料的成分配比为MoxCuyTiz，其中x，y，z均介于0-100%之间，且x+y+z=100%。
  11. 根据权利要求10所述的制备方法，其特征在于，所述烧结温度为1400℃~1500℃，烧结时间为10~15分钟。
  12. 根据权利要求11所述的制备方法，其特征在于，所述烧结获得的靶材烧结体的相对密度大于或等于99.5%，氧含量小于或等于500ppm。
  13. 根据权利要求8所述的制备方法，其特征在于，所述合金材料的成分配比为（In2O3）x（SnO2）y，其中y介于0~7%之间，且x+y=100%。
  14. 根据权利要求13所述的制备方法，其特征在于，所述烧结温度为600℃~700℃，烧结时间为10分钟。
  15. 根据权利要求14所述的制备方法，其特征在于，所述烧结获得的靶材烧结体的相对密度大于或等于99.8%，氧含量小于或等于1000ppm。
  16. 根据权利要求8所述的制备方法，其特征在于，在等离子体压力成型烧结腔体中进行烧结时，还包括对所述等离子体压力成型烧结腔体从外部加压。
  17. 一种玻璃基板薄膜溅射靶材，其特征在于，所述玻璃基板薄膜溅射靶材由权利要求8所述的制备方法制得。
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CN102703869A (zh) * 2012-05-30 2012-10-03 深圳市华星光电技术有限公司 制备tft-lcd阵列基板铜导线用靶材的方法及靶材
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04341504A (ja) * 1991-05-20 1992-11-27 Seiko Epson Corp 焼結体
JP2003081673A (ja) * 2001-09-05 2003-03-19 National Institute Of Advanced Industrial & Technology インジウム−錫酸化物焼結体の製造方法
CN1829820A (zh) * 2003-08-05 2006-09-06 株式会社日矿材料 溅射靶及其制造方法
CN101775578A (zh) * 2009-01-12 2010-07-14 E.I.内穆尔杜邦公司 制备ZnAl靶材的方法以及制得的ZnAl靶材
CN101942591A (zh) * 2010-07-31 2011-01-12 湖南科技大学 一种快速制备钼铜合金的方法
CN102137826A (zh) * 2008-08-29 2011-07-27 Skf股份公司 陶瓷部件的制造方法
CN102139371A (zh) * 2011-05-04 2011-08-03 佛山市钜仕泰粉末冶金有限公司 一种钨合金靶材及其制备方法
CN102260802A (zh) * 2011-07-20 2011-11-30 佛山市钜仕泰粉末冶金有限公司 一种靶材制备装置及其靶材加工方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001276208A (ja) * 2000-04-04 2001-10-09 Asahi Optical Co Ltd リン酸カルシウム系多孔体と金属との複合焼結体及びその製造方法

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04341504A (ja) * 1991-05-20 1992-11-27 Seiko Epson Corp 焼結体
JP2003081673A (ja) * 2001-09-05 2003-03-19 National Institute Of Advanced Industrial & Technology インジウム−錫酸化物焼結体の製造方法
CN1829820A (zh) * 2003-08-05 2006-09-06 株式会社日矿材料 溅射靶及其制造方法
CN102137826A (zh) * 2008-08-29 2011-07-27 Skf股份公司 陶瓷部件的制造方法
CN101775578A (zh) * 2009-01-12 2010-07-14 E.I.内穆尔杜邦公司 制备ZnAl靶材的方法以及制得的ZnAl靶材
CN101942591A (zh) * 2010-07-31 2011-01-12 湖南科技大学 一种快速制备钼铜合金的方法
CN102139371A (zh) * 2011-05-04 2011-08-03 佛山市钜仕泰粉末冶金有限公司 一种钨合金靶材及其制备方法
CN102260802A (zh) * 2011-07-20 2011-11-30 佛山市钜仕泰粉末冶金有限公司 一种靶材制备装置及其靶材加工方法

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
GUO WEI ET AL.: "Preparation of Indium Tin Oxide Sputtering Targets by Spark Plasma Sintering", RARE METAL MATERIALS AND ENGINEERING, vol. 38, no. SP. 2, pages 407 - 410 *
TOMONARI TAKEUCHI: "Preparation of Fluorine-Containing Indium Tin Oxide Targets using Spark Plasma Sintering Process Sputtering", J. AM. CERAM. SOC., vol. 91, no. 8, August 2008 (2008-08-01), pages 2495 - 2500, XP055071080 *
WANG HAIBING ET AL.: "Development trend of spark plasma sintering", MATERIALS SCIENCE AND ENGINEERING OF POWDER METALLURGY, vol. 10, no. 3, pages 138 - 143 *

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