CN117285343B - LaErCe co-doped ITO target material and preparation method and application thereof - Google Patents

LaErCe co-doped ITO target material and preparation method and application thereof Download PDF

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CN117285343B
CN117285343B CN202311141928.7A CN202311141928A CN117285343B CN 117285343 B CN117285343 B CN 117285343B CN 202311141928 A CN202311141928 A CN 202311141928A CN 117285343 B CN117285343 B CN 117285343B
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oxide
laerce
sintering
mixing
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CN117285343A (en
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唐智勇
唐安泰
程波
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Zhuzhou Torch Antai New Materials Co ltd
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Zhuzhou Torch Antai New Materials Co ltd
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Abstract

The invention discloses LaErCe co-doped ITO target material, a preparation method and application thereof, relating to the technical field of target material, and comprising the following preparation raw materials in parts by weight: 100 parts of indium oxide, 10-12 parts of tin oxide, 1-2 parts of lanthanum oxide, 4-5 parts of erbium oxide, 0.1-0.2 part of cerium oxide, 1-2 parts of silane coupling agent, 3-4 parts of titanate coupling agent, 10-20 parts of polyvinylpyrrolidone, 0.3-0.4 part of acid, 1000-1500 parts of water and 100-200 parts of alcohol. According to the invention, the preparation raw materials of the target are controlled, so that the target with high light transmittance and small resistance is prepared.

Description

LaErCe co-doped ITO target material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of targets, and particularly relates to a LaErCe co-doped ITO target, and a preparation method and application thereof.
Background
The Indium Tin Oxide target, indium Tin Oxide target for short, is a ceramic functional material formed by mixing the powder of two metal oxides of Indium Oxide and Tin Oxide, processing the mixed powder into ITO composite powder, and then pressing and sintering the ITO composite powder at high temperature. After vacuum magnetron sputtering coating, the ITO target material can form an ITO transparent conductive film on a substrate such as glass, and the ITO film has high visible light transmittance, high infrared light area reflectivity, high ultraviolet light area absorptivity, good conductivity, substrate adhesiveness and chemical stability, and has been widely applied in industry in recent years.
The preparation methods of the ITO target are various, the sintering method for preparing the ITO target currently mainly comprises normal pressure sintering and hot pressing sintering, and the two sintering preparation methods have advantages, and the preparation of the ITO target by any sintering method is key to obtaining the ITO target with high density and low resistance.
The existing ITO nano powder preparation method comprises a sol-gel method, a mixed ball milling method and a chemical precipitation method, wherein the sol-gel method is used for producing indium tin organic salt by adding alkali liquor into an organic solution containing In and Sn, and the ITO nano powder is obtained through heat treatment; the chemical coprecipitation method has the advantages that raw materials are easy to obtain, the process is simple and widely used, but in the process of preparing the ITO nano powder by adopting the method in the prior art, coprecipitated starch is easy to agglomerate, the particle size range is wide in distribution, the relative density of a target material can be influenced by particle agglomeration and non-uniformity, further, the electron mobility is reduced, the conductivity of the ITO target material can be reduced when the mobility is reduced, and the conductivity of a subsequent photoelectric film is influenced.
Disclosure of Invention
The present invention is directed to a LaErCe co-doped ITO target that overcomes at least one of the problems and disadvantages set forth in the background art described above.
The invention also provides a preparation method of the LaErCe co-doped ITO target.
The invention also provides application of the LaErCe co-doped ITO target.
The invention discloses a LaErCe co-doped ITO target in a first aspect, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10-12 parts of tin oxide, 1-2 parts of lanthanum oxide, 4-5 parts of erbium oxide, 0.1-0.2 part of cerium oxide, 1-2 parts of silane coupling agent, 3-4 parts of titanate coupling agent, 10-20 parts of polyvinylpyrrolidone, 0.3-0.4 part of acid, 1000-1500 parts of water and 100-200 parts of alcohol.
According to one of the target technical schemes, the invention has at least the following beneficial effects:
According to the application, erbium in the erbium oxide is doped into the target material, so that the defect state of the target material is effectively restrained; lanthanum oxide is favorable for reducing the sintering temperature of the target material, and can promote the compactness of the target material; cerium oxide can greatly improve the compactness of the target; namely, the light transmittance of the target material is improved and the resistivity of the target material is reduced through the synergistic effect among lanthanum oxide, erbium oxide and cerium oxide.
Meanwhile, the dispersibility of the oxide is improved through the silane coupling agent, the titanate coupling agent and the polyvinylpyrrolidone, so that the uniformity of the sintered target is improved; and the titanate coupling agent can also play a role in titanium doping, so that the visible light transmittance of the target is further improved.
According to some embodiments of the invention, the silane coupling agent is KH550 or KH560.
According to some embodiments of the invention, the titanate coupling agent is TC-27.
According to some embodiments of the invention, the acid is sulfuric acid.
According to some embodiments of the invention, the alcohol is ethanol.
According to some embodiments of the invention, the indium oxide has a particle size of 20nm to 70nm.
According to some embodiments of the invention, the particle size of the tin oxide is 40nm to 50nm.
According to some embodiments of the invention, the lanthanum oxide has a particle size of 30nm to 50nm.
According to some embodiments of the invention, the cerium oxide has a particle size of 20nm to 40nm.
According to some embodiments of the invention, the average particle size of the erbium oxide is 45nm.
The particle size of the metal oxide is equivalent, namely the activity of the oxide in the solution is equivalent, the difference of the reactivity is smaller, and the uniform target is formed.
According to some embodiments of the invention, the polyvinylpyrrolidone has a number average molecular weight of 8000 to 10000.
The second aspect of the invention discloses a preparation method of the LaErCe co-doped ITO target, which comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, a silane coupling agent, polyvinylpyrrolidone, part of water and part of alcohol to prepare a first mixture;
Mixing erbium oxide, cerium oxide, acid and part of water, carrying out solid-liquid separation, and collecting a solid phase;
Mixing the solid phase, the titanate coupling agent, the remaining portion of water and the remaining portion of alcohol to produce a second mixture;
s2, mixing the first mixture and the second mixture, and then ball milling and spray granulating; preparing a precursor;
s3, pre-treating the precursor and sintering the precursor;
The sintering temperature is 1100-1200 ℃.
According to one of the technical schemes of the preparation method, the preparation method at least has the following beneficial effects:
In the invention, the oxide is pre-dispersed, so that the yield of the target blank is greatly improved; according to the invention, the silane coupling agent is used for modifying the indium oxide, the tin oxide and the lanthanum oxide, so that the dispersion effect of the oxide is greatly improved; the invention also adopts acid to carry out preliminary treatment on the erbium oxide and the cerium oxide, so as to carry out preliminary surface treatment on the erbium oxide and the cerium oxide, adopts titanate coupling agent to carry out surface modification on the cerium oxide and the erbium oxide, and carries out coupling through chemical action of alkoxy groups which are easy to carry out with hydroxyl groups adsorbed on the surfaces of the cerium oxide and the erbium oxide, so that an organic active molecular layer is formed on the surfaces of the cerium oxide and the erbium oxide, and the dispersibility of metal oxide is improved.
According to some embodiments of the invention, the first mixture has a mixing temperature of 70 ℃ to 80 ℃.
According to some embodiments of the invention, the first mixture is mixed for a time period of 1h to 2h.
According to some embodiments of the invention, the temperature of the mixed treatment of erbium oxide, cerium oxide, acid and part of the water is between 40 ℃ and 50 ℃.
According to some embodiments of the invention, the mixing treatment of erbium oxide, cerium oxide, acid and part of water takes 1min to 2min.
According to some embodiments of the invention, the second mixture has a mixing temperature of 80 ℃ to 90 ℃.
According to some embodiments of the invention, the second mixture is mixed for a time of 4h to 5h.
According to some embodiments of the invention, the rotational speed of the ball mill is 500r/min to 1500r/min.
According to some embodiments of the invention, the ball milling time is 3-5 hours.
According to some embodiments of the invention, the spray drying temperature is 160 ℃ to 180 ℃.
According to some embodiments of the invention, the pretreatment is oxygen pressure sintering; the temperature of the oxygen pressure sintering is 900-1000 ℃.
According to some embodiments of the invention, the oxygen pressure sintering pressure is between 10MPa and 20MPa.
According to some embodiments of the invention, the oxygen pressure sintering has an oxygen volume concentration of 20% to 30%.
According to some embodiments of the invention, the oxygen pressure sintering time is 2h to 4h.
According to some embodiments of the invention, the sintering pressure in step S3 is 100MPa to 200MPa.
According to some embodiments of the invention, the sintering time in step S3 is 3h to 5h.
The third aspect of the invention discloses application of the LaErCe co-doped ITO target in preparing an oxide film.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The manufacturer and model of the metal oxide selected in the embodiment of the invention are as follows:
indium oxide (In 2O3) was purchased from beijing jia An Heng technologies limited (nano indium oxide); the grain diameter is 20 nm-70 nm.
Tin oxide (SnO 2) was purchased from Hangzhou Hengna New materials Co., ltd. (trade name is HN-Sn 50); the grain diameter is 40 nm-50 nm.
Lanthanum oxide (La 2O3) is purchased from Hangzhou Hengna New materials Co., ltd (trade name is HN-La 01) and has a particle size of 30 nm-50 nm.
Cerium oxide (CeO 2) is purchased from Hangzhou Hengna New materials Co., ltd (trade name is HN-Ce 01) and has a particle size of 20 nm-40 nm.
Erbium oxide (Er 2O3) was purchased from Shanghai funang New Material technologies Co., ltd (trade mark: HL-Er 2O3 -50); the average particle diameter was 45nm.
In an embodiment of the invention the polyvinylpyrrolidone has a number average molecular weight of 10000.
Example 1
The embodiment is a LaErCe co-doped ITO target, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 11.5 parts of tin oxide, 1.2 parts of lanthanum oxide, 4.8 parts of erbium oxide, 0.15 part of cerium oxide, 1.2 parts of a silane coupling agent (KH 560), 3.2 parts of a titanate coupling agent (TC-27), 15 parts of polyvinylpyrrolidone, 0.31 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the embodiment comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, a silane coupling agent, polyvinylpyrrolidone, 1/3 of total volume of water and 1/2 of total volume of alcohol (the mixing temperature is 70 ℃, the time is 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
mixing erbium oxide, cerium oxide, acid and water with total volume of 1/3 (mixing temperature of 40deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
mixing the solid phase, the titanate coupling agent, the rest of water and the rest of alcohol (the mixing temperature is 80 ℃, the time is 4 hours, and the dispersion speed is 120 r/min) to prepare a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 950 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 15MPa, the oxygen volume concentration is 30%, and the time of the oxygen pressure sintering is 3 h);
the sintering temperature after pretreatment is 1150 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 180MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
Example 2
The embodiment is a LaErCe co-doped ITO target, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 2 parts of lanthanum oxide, 5 parts of erbium oxide, 0.1 part of cerium oxide, 1 part of a silane coupling agent (KH 560), 4 parts of a titanate coupling agent (TC-27), 20 parts of polyvinylpyrrolidone, 0.4 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in this example was performed as described in example 1.
Example 3
The embodiment is a LaErCe co-doped ITO target, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 12 parts of tin oxide, 1 part of lanthanum oxide, 4 parts of erbium oxide, 0.2 part of cerium oxide, 2 parts of a silane coupling agent (KH 560), 3 parts of a titanate coupling agent (TC-27), 10 parts of polyvinylpyrrolidone, 0.3 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in this example was performed as described in example 1.
Example 4
The embodiment is a LaErCe co-doped ITO target, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10.8 parts of tin oxide, 1.5 parts of lanthanum oxide, 4.2 parts of erbium oxide, 0.12 part of cerium oxide, 1.8 parts of a silane coupling agent (KH 560), 3.5 parts of a titanate coupling agent (TC-27), 14 parts of polyvinylpyrrolidone, 0.36 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in this example was performed as described in example 1.
Example 5
The embodiment is a LaErCe co-doped ITO target, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 1 part of lanthanum oxide, 4 parts of erbium oxide, 0.1 part of cerium oxide, 1 part of a silane coupling agent (KH 560), 3 parts of a titanate coupling agent (TC-27), 10 parts of polyvinylpyrrolidone, 0.3 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the embodiment comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, a silane coupling agent, polyvinylpyrrolidone, 1/3 of total volume of water and 1/2 of total volume of alcohol (the mixing temperature is 75 ℃, the time is 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
Mixing erbium oxide, cerium oxide, acid and water with total volume of 1/3 (mixing temperature of 50deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
Mixing the solid phase, the titanate coupling agent, the rest of water and the rest of alcohol (the mixing temperature is 75 ℃, the time is 4 hours, and the dispersion speed is 120 r/min) to prepare a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 900 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 20MPa, the oxygen volume concentration is 20%, and the time of the oxygen pressure sintering is 3 h);
The sintering temperature after pretreatment is 1100 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 100MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
Comparative example 1
The comparative example is LaErCe co-doped ITO target material, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 1 part of lanthanum oxide, 4 parts of erbium oxide, 0.1 part of cerium oxide, 10 parts of polyvinylpyrrolidone, 0.3 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the comparative example comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, polyvinylpyrrolidone, water with the total volume of 1/3 and alcohol with the total volume of 1/2 (the mixing temperature is 75 ℃ for 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
Mixing erbium oxide, cerium oxide, acid and water with total volume of 1/3 (mixing temperature of 50deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
mixing the solid phase, the remaining part of water and the remaining part of alcohol (mixing temperature is 75 ℃, time is 4h, and dispersion speed is 120 r/min) to prepare a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 900 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 20MPa, the oxygen volume concentration is 20%, and the time of the oxygen pressure sintering is 3 h);
The sintering temperature after pretreatment is 1100 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 100MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
Comparative example 2
The comparative example is LaErCe co-doped ITO target material, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 1 part of lanthanum oxide, 4 parts of erbium oxide, 0.1 part of cerium oxide, 1 part of a silane coupling agent (KH 560), 10 parts of polyvinylpyrrolidone, 0.3 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the comparative example comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, a silane coupling agent, polyvinylpyrrolidone, 1/3 of total volume of water and 1/2 of total volume of alcohol (the mixing temperature is 75 ℃, the time is 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
Mixing erbium oxide, cerium oxide, acid and water with total volume of 1/3 (mixing temperature of 50deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
Mixing the remaining water and the remaining alcohol (mixing temperature of 75deg.C for 4h, dispersion speed of 120 r/min) to obtain a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 900 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 20MPa, the oxygen volume concentration is 20%, and the time of the oxygen pressure sintering is 3 h);
The sintering temperature after pretreatment is 1100 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 100MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
Comparative example 3
The comparative example is LaErCe co-doped ITO target material, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 0.1 part of cerium oxide, 1 part of a silane coupling agent (KH 560), 3 parts of a titanate coupling agent (TC-27), 10 parts of polyvinylpyrrolidone, 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the comparative example comprises the following steps:
s1, mixing indium oxide, tin oxide, a silane coupling agent, polyvinylpyrrolidone, water with the total volume of 1/3 and alcohol with the total volume of 1/2 (the mixing temperature is 75 ℃ for 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
Mixing cerium oxide with water with total volume of 1/3 (mixing temperature of 50deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
Mixing the solid phase, the titanate coupling agent, the rest of water and the rest of alcohol (the mixing temperature is 75 ℃, the time is 4 hours, and the dispersion speed is 120 r/min) to prepare a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 900 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 20MPa, the oxygen volume concentration is 20%, and the time of the oxygen pressure sintering is 3 h);
The sintering temperature after pretreatment is 1100 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 100MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
Comparative example 4
The comparative example is LaErCe co-doped ITO target material, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 4 parts of erbium oxide, 1 part of a silane coupling agent (KH 560), 3 parts of a titanate coupling agent (TC-27), 10 parts of polyvinylpyrrolidone, 0.3 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the comparative example comprises the following steps:
s1, mixing indium oxide, tin oxide, a silane coupling agent, polyvinylpyrrolidone, water with the total volume of 1/3 and alcohol with the total volume of 1/2 (the mixing temperature is 75 ℃ for 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
Mixing erbium oxide, acid and water with total volume of 1/3 (mixing temperature of 50deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
Mixing the solid phase, the titanate coupling agent, the rest of water and the rest of alcohol (the mixing temperature is 75 ℃, the time is 4 hours, and the dispersion speed is 120 r/min) to prepare a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 900 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 20MPa, the oxygen volume concentration is 20%, and the time of the oxygen pressure sintering is 3 h);
The sintering temperature after pretreatment is 1100 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 100MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
Comparative example 5
The comparative example is LaErCe co-doped ITO target material, which comprises the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10 parts of tin oxide, 1 part of lanthanum oxide, 0.1 part of cerium oxide, 1 part of a silane coupling agent (KH 560), 3 parts of a titanate coupling agent (TC-27), 10 parts of polyvinylpyrrolidone, 0.3 part of acid (sulfuric acid), 1500 parts of water and 150 parts of alcohol (ethanol).
The preparation method of LaErCe co-doped ITO target in the comparative example comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, a silane coupling agent, polyvinylpyrrolidone, 1/3 of total volume of water and 1/2 of total volume of alcohol (the mixing temperature is 75 ℃, the time is 2 hours, and the mixing dispersion speed is 100 r/min) to prepare a first mixture;
mixing cerium oxide, acid and water with total volume of 1/3 (mixing temperature of 50deg.C, time of 1.5min, dispersion speed of 20 r/min), solid-liquid separating, and collecting solid phase;
Mixing the solid phase, the titanate coupling agent, the rest of water and the rest of alcohol (the mixing temperature is 75 ℃, the time is 4 hours, and the dispersion speed is 120 r/min) to prepare a second mixture;
S2, mixing the first mixture and the second mixture (the mixing time is 15min, the dispersion speed is 100 r/min), ball milling (the ball milling rotating speed is 1000r/min, the ball milling time is 4 h), and spray granulation (the spray granulation temperature is 170 ℃); preparing a precursor;
S3, pre-treating the precursor and sintering;
the pretreatment is oxygen pressure sintering (the temperature of the oxygen pressure sintering is 900 ℃ (the temperature rising speed is 15 ℃/min), the pressure of the oxygen pressure sintering is 20MPa, the oxygen volume concentration is 20%, and the time of the oxygen pressure sintering is 3 h);
The sintering temperature after pretreatment is 1100 ℃ (the heating speed is 15 ℃/min), the sintering pressure is 100MPa, and the sintering time is 4 hours;
Cooling after sintering (cooling speed is 10 ℃/min, cooling final temperature is 50 ℃).
The light transmittance (visible light) and the conductivity of the films prepared from the targets of examples 1 to 5 and comparative examples 1 to 5 are shown in Table 1.
TABLE 1 Performance test results of the targets produced in examples 1 to 5 and comparative examples 1 to 5 of the present invention
In summary, according to the application, erbium in the erbium oxide is doped into the target material, so that the defect state of the target material is effectively inhibited; lanthanum oxide is favorable for reducing the sintering temperature of the target material, and can promote the compactness of the target material; cerium oxide can greatly improve the compactness of the target; namely, the light transmittance of the target material is improved and the resistivity of the target material is reduced through the synergistic effect among lanthanum oxide, erbium oxide and cerium oxide. Meanwhile, the dispersibility of the oxide is improved through the silane coupling agent, the titanate coupling agent and the polyvinylpyrrolidone, so that the uniformity of the sintered target is improved; and the titanate coupling agent can also play a role in titanium doping, so that the visible light transmittance of the target is further improved.
While the foregoing is directed to embodiments of the present invention, other and further details of the invention may be had by the present invention, it should be understood that the foregoing description is merely illustrative of the present invention and that no limitations are intended to the scope of the invention, except insofar as modifications, equivalents, improvements or modifications are within the spirit and principles of the invention.

Claims (9)

1. LaErCe co-doped ITO target is characterized by comprising the following preparation raw materials in parts by weight:
100 parts of indium oxide, 10-12 parts of tin oxide, 1-2 parts of lanthanum oxide, 4-5 parts of erbium oxide, 0.1-0.2 part of cerium oxide, 1-2 parts of silane coupling agent, 3-4 parts of titanate coupling agent, 10-20 parts of polyvinylpyrrolidone, 0.3-0.4 part of acid, 1000-1500 parts of water and 100-200 parts of alcohol;
The preparation method of the LaErCe co-doped ITO target comprises the following steps:
S1, mixing indium oxide, tin oxide, lanthanum oxide, a silane coupling agent, polyvinylpyrrolidone, part of water and part of alcohol to prepare a first mixture;
Mixing erbium oxide, cerium oxide, acid and part of water, carrying out solid-liquid separation, and collecting a solid phase;
Mixing the solid phase, the titanate coupling agent, the remaining portion of water and the remaining portion of alcohol to produce a second mixture;
s2, mixing the first mixture and the second mixture, and then ball milling and spray granulating; preparing a precursor;
s3, pre-treating the precursor and sintering the precursor;
the sintering temperature is 1100-1200 ℃.
2. The LaErCe co-doped ITO target of claim 1, wherein the silane coupling agent is KH550 or KH560.
3. The LaErCe co-doped ITO target of claim 1, wherein the titanate coupling agent is TC-27.
4. The LaErCe co-doped ITO target of claim 1, wherein the acid is sulfuric acid.
5. The LaErCe co-doped ITO target of claim 1, wherein the pretreatment is oxygen pressure sintering; the temperature of the oxygen pressure sintering is 900-1000 ℃.
6. The LaErCe co-doped ITO target of claim 5, wherein the oxygen pressure sintering pressure is 10mpa to 20mpa.
7. The LaErCe co-doped ITO target of claim 1, wherein the sintering pressure is 100mpa to 200mpa.
8. The LaErCe co-doped ITO target of claim 1, wherein the sintering time is 3h to 5h.
9. Use of LaErCe co-doped ITO target as claimed in any one of claims 1 to 8 in the preparation of an oxide film.
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CN114883025A (en) * 2022-05-05 2022-08-09 株洲火炬安泰新材料有限公司 Low-resistance high-transmittance ITO conductive film

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