Preparation method of novel ITO target material

Abstract

The application relates to the field of ITO thin films, and particularly discloses a novel ITO target material and a preparation method thereof, the target material comprising indium oxide and tin oxide, and the two kinds of proportions being 90:10; the preparation method comprises the following steps: calcining indium oxide and tin oxide with different proportions at different temperatures respectively, then recombining the two kinds of mixed powders into a third mixed powder with the mass proportion of indium oxide and tin oxide being 90:10, adding 0.5%-1% of an additive in the third mixed powder, and resintering. The ITO target material prepared by the preparation method significantly reduces the second phase, the proportion of which in the microstructure image is not more than 5%, and the conductivity of the target material and the uniformity of sputtering are optimized.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of ITO thin film, and particularly relates to a preparation method of a new type of ITO target material. BACKGROUND

[0002] Indium tin oxide (ITO) target material is a kind of semiconductor ceramic functional material, which is used for magnetron sputtering to deposit ITO thin film. As a kind of transparent conductive material, ITO thin film is widely used in display, touch and other fields. Indium tin oxide material is essentially indium oxide doped with tin element. The solid solubility of tin oxide in indium oxide is about 5%, but the commonly used indium tin oxide material contains 10% of tin oxide. This results in a large number of second phases in the ITO target material, such as Figure 2 as shown in the figure, Figure 2 small squares are distributed in the middle of the second phase. The existence of the second phase will affect the conductivity of the target material on the one hand, and will affect the uniformity of sputtering on the other hand. SUMMARY

[0003] The purpose of the present application is to provide a preparation method of a new type of ITO target material which reduces the proportion of the second phase.

[0004] To achieve the above purpose, the present application provides a preparation method of a new type of ITO target material, comprising the following steps:

[0005] (1) uniformly mix and grind the nano-powder of indium oxide and tin oxide to form a first mixed powder, wherein the mass proportion of tin oxide is 43.9%-45.9%, and the first mixed powder is calcined at a first set temperature;

[0006] (2) uniformly mix and grind the nano-powder of indium oxide and tin oxide to form a second mixed powder, wherein the mass proportion of tin oxide is 5%-7%, and the second mixed powder is calcined at a second set temperature;

[0007] (3) mix the above two mixed powders again to ensure that the mass proportion of tin oxide reaches 10%, then add 0.5%-1% of the total mass of the mixed powder to the mixed powder, and uniformly mix and grind, the additive includes one or more of zirconium oxide, gallium oxide, niobium oxide, antimony oxide and tantalum oxide;

[0008] (4) after the above mixed powder is formed, sintering is carried out in an oxygen atmosphere at a third set temperature, and a new type of ITO target material with a ratio of indium oxide to tin oxide of 90:10 is obtained after cooling, and the proportion of the second phase in the microstructure thereof is less than 5%.

[0009] As an improvement of the above scheme, the first set temperature is 1430-1450℃, the second set temperature is 800-880℃, and the third set temperature is 1550-1580℃.

[0010] The present application has the following beneficial effects: the ITO target material prepared by the preparation method has a second phase which is reduced significantly, and the proportion of the second phase in the microscopic component image is not more than 5%, and the conductivity of the target material and the uniformity of sputtering are optimized. Figure 2 The second phase in the prior art, Figure 1 The second phase in the prior art is significantly reduced. BRIEF DESCRIPTION OF DRAWINGS

[0011] Figure 1 is the microscopic structure of a new ITO target material;

[0012] Figure 2 is the microscopic structure of a conventional ITO target material.

[0013] Reference signs: 1, second phase. DETAILED DESCRIPTION

[0014] In the description of the present application, it should be noted that the orientations or positional relationships indicated by the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "top", "bottom", "top surface", "bottom surface", "inner", "outer", "inner side", "outer side" and the like are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the devices or elements indicated must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0015] In the description of the present application, the meaning of several is one or more, the meaning of multiple is two or more, greater than, less than, more than, etc. are understood as not including the number, above, below, within, etc. are understood as including the number. If the terms "first", "second", "third" are described, they are only for the purpose of description and distinguishing technical features, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features or the sequence of indicated technical features.

[0016] In the description of the present application, it should be noted that, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connection", "setting" should be understood broadly, for example, it can be fixedly connected, or it can be detachably connected, or integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the communication between two elements inside. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances. The embodiments will be described below according to the overall structure of the present application.

[0017] ReferenceFigure 1 and Figure 2 The application discloses a new ITO target material, the ITO target material comprises indium oxide and tin oxide, the mass ratio of the indium oxide and the tin oxide is 90:10, and the second phase 1 accounts for less than 5% in the microstructure of the ITO target material.

[0018] The application further discloses a preparation method of the new ITO target material.

[0019] (1) uniformly mixing and grinding nano-powders of the indium oxide and the tin oxide to form a first mixed powder, wherein the mass ratio of the tin oxide is 43.9%-45.9%, and the mass ratio of the indium oxide is 54.1%-56.1% correspondingly, and the first mixed powder is calcined at 1430-1450 DEG C.

[0020] (2) uniformly mixing and grinding nano-powders of the indium oxide and the tin oxide to form a second mixed powder, wherein the mass ratio of the tin oxide is 5%-7%, and the mass ratio of the indium oxide is 93%-95% correspondingly, and the second mixed powder is calcined at 800-880 DEG C.

[0021] (3) mixing the two mixed powders again, ensuring that the mass ratio of the tin oxide is 10% and the mass ratio of the indium oxide is 90% after the two different mixed powders are mixed again, for example, taking a small part of the mixed powder in the step (1), taking a large part of the mixed powder in the step (2), then adding 0.5%-1% of an additive to the mixed powder, and uniformly mixing and grinding, the additive comprises one or more of zirconium oxide, gallium oxide, niobium oxide, antimony oxide and tantalum oxide.

[0022] (4) after the mixed powder is formed, sintering is carried out at 1550-1580 DEG C in an oxygen atmosphere, and the new ITO target material with the mass ratio of the indium oxide and the tin oxide being 90:10 is obtained after cooling.

[0023] Embodiment 1

[0024] Nano-powders of the indium oxide and the tin oxide are uniformly mixed and ground according to the mass ratio of 55.1:44.9, and are calcined at 1430 DEG C.

[0025] Nano-powders of the indium oxide and the tin oxide are uniformly mixed and ground according to the mass ratio of 55.1:44.9, and are calcined at 1430 DEG C.

[0026] The two mixed powders are mixed again to form a mixed powder containing the indium oxide and the tin oxide with the mass ratio of 90:10, and then 0.5% of zirconium oxide is added to the mixed powder, and the mixed powder is uniformly mixed and ground.

[0027] The mixed powder is formed, sintered at 1565°C in an oxygen atmosphere, and cooled to obtain an ITO target material with a mass ratio of indium oxide to tin oxide of 90:10. The microstructure of the target material is detected, and the second phase 1 accounts for 3%.

[0028] Example 2:

[0029] The nanometer powders of indium oxide and tin oxide are uniformly mixed and ground in a mass ratio of 56.1:45.9, and calcined at 1440°C.

[0030] The nanometer powders of indium oxide and tin oxide are uniformly mixed and ground in a mass ratio of 56.1:45.9, and calcined at 1440°C.

[0031] The two mixed powders are re-mixed to a mixed powder containing indium oxide and tin oxide in a mass ratio of 90:10, and then 0.5% of zirconium oxide and 0.5% of antimony oxide are added to the total mass of the mixed powder, and uniformly mixed and ground.

[0032] The mixed powder is formed, sintered at 1565°C in an oxygen atmosphere, and cooled to obtain an ITO target material with a mass ratio of indium oxide to tin oxide of 90:10. The microstructure of the target material is detected, and the second phase 1 accounts for 3%.

[0033] Example 3:

[0034] The nanometer powders of indium oxide and tin oxide are uniformly mixed and ground in a mass ratio of 56.1:45.9, and calcined at 1440°C.

[0035] The nanometer powders of indium oxide and tin oxide are uniformly mixed and ground in a mass ratio of 56.1:45.9, and calcined at 1440°C.

[0036] The two mixed powders are re-mixed to a mixed powder containing indium oxide and tin oxide in a mass ratio of 90:10, and then 0.5% of zirconium oxide and 0.5% of antimony oxide are added to the total mass of the mixed powder, and uniformly mixed and ground.

[0037] The mixed powder is formed, sintered at 1565°C in an oxygen atmosphere, and cooled to obtain an ITO target material with a mass ratio of indium oxide to tin oxide of 90:10. The microstructure of the target material is detected, and the second phase 1 accounts for 3%.

[0038] The foregoing description of specific exemplary embodiments of the application has been presented for the purposes of illustration and description. It is not intended to be exhaustive or to limit the application to the precise forms disclosed, and obviously many modifications and variations are possible in light of the above teaching. It is intended that the scope of the application be limited not with this detailed description, but rather by the claims appended hereto.

Claims

1. A method for preparing a novel ITO target material, characterized in that The method comprises the following steps: (1) uniformly mixing and grinding nano-powders of indium oxide and tin oxide to form a first mixed powder, wherein the mass percentage of tin oxide is 43.9%-45.9%, and the first mixed powder is calcined at a first set temperature of 1430-1450 ℃; (2) uniformly mixing and grinding nano-powders of indium oxide and tin oxide to form a second mixed powder, wherein the mass percentage of tin oxide is 5%-7%, and the second mixed powder is calcined at a second set temperature of 800-880 ℃; (3) mixing the two mixed powders again to ensure that the mass percentage of tin oxide is 10%, then adding an additive accounting for 0.5%-1% of the total mass of the mixed powder, and uniformly mixing and grinding, wherein the additive comprises one or more of zirconium oxide, gallium oxide, niobium oxide, antimony oxide and tantalum oxide; (4) after forming the mixed powder, sintering in an oxygen atmosphere at a third set temperature of 1550-1580 ℃, and cooling to obtain a new ITO target material with a ratio of indium oxide to tin oxide of 90:10, wherein the second phase accounts for less than 5% in the microstructure thereof.

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