CN116444263A - Sintering process of indium tin oxide target - Google Patents

Sintering process of indium tin oxide target Download PDF

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Publication number
CN116444263A
CN116444263A CN202310248397.5A CN202310248397A CN116444263A CN 116444263 A CN116444263 A CN 116444263A CN 202310248397 A CN202310248397 A CN 202310248397A CN 116444263 A CN116444263 A CN 116444263A
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tin oxide
indium tin
temperature
sintering
blank
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CN202310248397.5A
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CN116444263B (en
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高建成
张莉兰
徐涛
汪强
钟小华
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Leading Film Materials Anhui Co ltd
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Leading Film Materials Anhui Co ltd
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    • 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
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Abstract

The invention discloses a sintering process of an indium tin oxide target, which belongs to the technical field of preparation of indium tin oxide targets, and is characterized in that after indium oxide and tin oxide raw materials are prepared into a blank, a target sintering system is adopted for pre-degreasing, degreasing and sintering, and finally the indium tin oxide target is prepared; the blank is pre-degreased in the argon atmosphere, the argon is inert gas and does not react with components in the blank, so that the blank is completely solidified and formed, then the temperature is increased to continuously degrease, components such as polyvinyl alcohol in the blank are decomposed at high temperature, and the gas dissipation amount in unit time of the blank can be reduced by a mode of step-by-step removal of water and organic cohesive substances, so that the blank is prevented from cracking; the atmosphere conversion is controlled by a target sintering system, so that the pressure and the temperature in a hearth are prevented from floating too much; the accurate temperature rise and temperature reduction adjustment is beneficial to controlling the crystal grains and the compactness of the indium tin oxide target material to reach the optimal state, and is beneficial to improving the product quality.

Description

Sintering process of indium tin oxide target
Technical Field
The invention belongs to the technical field of preparation of indium tin oxide targets, and particularly relates to a sintering process of an indium tin oxide target.
Background
The target material is also called sputtering film material, and is a sputtering source for forming various functional films on a substrate by magnetron sputtering, multi-arc ion plating or other types of coating systems under proper process conditions. According to the material division, targets can be classified into metal targets, ceramic targets and alloy targets, and various types of targets are widely used in the fields of semiconductor integrated circuits, optical discs, flat panel displays and surface coatings of workpieces, for example, copper conductor films with lower resistivity are used for replacing aluminum film wiring in the manufacturing process of semiconductor integrated circuits; in the flat panel display industry, some have been used for the manufacture of computers and displays for computers.
The ceramic targets comprise indium oxide (ITO) targets, magnesium oxide targets, ferric oxide targets, silicon oxide targets, titanium nitride targets, zinc sulfide targets and the like, wherein the indium tin oxide targets are black gray ceramic semiconductors formed by mixing indium oxide and tin oxide powder according to a certain proportion and then processing and forming, and sintering at high temperature, belong to oxide ceramic targets and are common targets in advanced ceramic sputtering targets. The oxide ceramic targets are formed by sintering one or more oxides at high temperature, and most of the oxide ceramic targets have high melting point, excellent heat resistance and corrosion resistance, so that the oxide ceramic targets can be exposed to high temperature and oxidation environment for a long time and are worthy of being widely applied in the engineering field.
The indium tin oxide target material is an important raw material for preparing indium oxide conductive glass, and can be applied to a touch screen, an organic light emitting flat display (OLED), a Plasma Display Panel (PDP), automobile heat-proof defogging glass, a photoelectric converter and the like besides a liquid crystal display panel (LCD). The indium tin oxide target material can form a transparent indium oxide conductive film on glass after sputtering, and the performance of the transparent indium oxide conductive film is a key factor for determining the quality, the production efficiency and the yield of conductive glass products, and the indium tin oxide target material needs to be ensured to keep unchanged in the whole film plating process.
The indium tin oxide powder raw material needs to be sintered to prepare the indium tin oxide target material after being pressed into a green body, obvious shrinkage can occur in the preparation process of the indium tin oxide target material, cracks can be possibly caused by internal stress, and slight cracks can not generate great influence, but when obvious cracks occur in the indium tin oxide target material, charges are easily concentrated at the edges of the cracks in the use process, so that abnormal discharge is caused on the surface of the indium tin oxide target material, and the defective rate is increased. In order to avoid cracks in the preparation process of the indium tin oxide target, a sintering process of the indium tin oxide target is provided.
Disclosure of Invention
The invention aims to provide a sintering process of an indium tin oxide target material, which aims to solve the problems in the background technology.
The aim of the invention can be achieved by the following technical scheme:
the sintering process of the indium tin oxide target material comprises the following steps:
step one: indium oxide with purity not less than 99.99% and tin oxide with purity not less than 99.99% are mixed according to 9:1, and fully grinding, sieving to obtain powder with specific surface area of 5-15m 2 Indium tin oxide powder/g; uniformly mixing polyvinyl alcohol, polyacrylamide and a polyether type defoamer, then adding indium tin oxide powder, uniformly mixing to obtain slurry, and regulating the viscosity of the slurry to 1000-3000 mPa.s; setting the casting pressure to be 0.2-1.5MPa, maintaining the pressure for 10-30min, and casting and molding the slurry to obtain a blank;
step two: placing the blank into a hearth of a vacuum atmosphere furnace by adopting a target sintering system, closing the vacuum atmosphere furnace, introducing argon, controlling the flow of the argon to be 5-20L/min, discharging air, keeping the temperature of the hearth to be 200-250 ℃ according to the heating rate of 0.1-1 ℃/min, and preserving the temperature for 10-30h to finish pre-degreasing;
step three: maintaining the flow of argon at 5-20L/min, then raising the temperature of a hearth to 550-600 ℃ according to the heating rate of 0.1-1 ℃/min, and preserving heat for 20-50h to finish degreasing;
step four: argon in the vacuum atmosphere furnace is pumped out, oxygen is introduced, the flow of the oxygen is regulated to be 20-50L/min, the temperature of a hearth is increased to 1500-1600 ℃ according to the heating rate of 0.5-1 ℃/min, sintering is completed after heat preservation is carried out for 5-20h, the introduction of the oxygen is stopped, the temperature of the hearth is reduced to 150-250 ℃ according to the cooling rate of 1-3 ℃/min, then the air is introduced to cool to room temperature, and the indium tin oxide target is obtained, and the sintering process of the indium tin oxide target is completed.
Further, the amount of polyvinyl alcohol in the first step is 0.5-1wt% of indium tin oxide powder, the amount of polyacrylamide is 0.05-0.1wt% of indium tin oxide powder, and the amount of polyether defoamer is 0.05-0.1wt% of indium tin oxide powder.
The target sintering system comprises a vacuum atmosphere furnace, a main controller, a vacuum system, an argon control system and an oxygen control system.
The vacuum system comprises a vacuumizing device and a vacuum controller, the vacuumizing device is connected with the vacuum atmosphere furnace in a matched mode, gas in the vacuum atmosphere furnace is conveniently pumped out, and the vacuum controller is connected with the main controller and the vacuumizing device in a telecommunication mode respectively.
The argon control system comprises an argon source and an argon heater, wherein the argon source conveys argon to the vacuum atmosphere furnace through the argon heater; the argon heater telecom is connected with an argon flow controller and an argon temperature controller, and the argon flow controller and the argon temperature controller are also in telecom connection with the main controller.
The oxygen control system comprises an oxygen source and an oxygen heater, wherein the oxygen source is used for conveying oxygen to the vacuum atmosphere furnace through the oxygen heater; the oxygen heater is in telecommunication connection with an oxygen flow controller and an oxygen temperature controller, and the oxygen flow controller and the oxygen temperature controller are also in telecommunication connection with the main controller.
The vacuum atmosphere furnace is internally provided with a hearth, a temperature detection device and a water cooling device, the main controller is also in telecommunication connection with a hearth temperature controller and a water cooling controller, and the water cooling controller is in telecommunication connection with the water cooling device; the hearth temperature controller is in telecommunication connection with the temperature monitoring device, the temperature data detected in real time are fed back to the hearth temperature controller by the temperature detecting device, and then the power is adjusted through the power regulator so as to control the hearth temperature.
The invention has the beneficial effects that:
according to the sintering process of the indium tin oxide target material, firstly, indium oxide and tin oxide raw materials are prepared into slurry, and then pressed into a green body, so that the forming is easy, and the bonding strength of the green body is ensured.
The green body is pre-degreased in the argon atmosphere in the sintering process, the argon is inert gas and cannot react with components in the green body, moisture in the green body is thoroughly removed at a lower temperature, the green body is completely solidified and molded, then the temperature is increased to continue degreasing, components such as polyvinyl alcohol in the green body are decomposed at a high temperature, the amount of gas dissipation in unit time of the green body can be reduced by means of step-by-step removal of moisture and organic cohesive substances, the green body is contracted more uniformly in the degreasing process, and accordingly cracks of the green body are avoided.
In the degreasing and sintering steps, the atmosphere conversion is controlled by a target sintering system, so that the pressure and temperature in a hearth are prevented from floating too much, and the blank is prevented from cracking. In the sintering process of the green body, the crystal grains and the densification degree of the indium tin oxide target material are controlled to reach the optimal state by accurate temperature rise and temperature reduction adjustment, and the product quality is improved.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a control schematic of the target sintering system of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the target sintering system comprises a vacuum atmosphere furnace, a main controller, a vacuum system, an argon gas control system and an oxygen gas control system.
The target sintering system comprises a vacuum atmosphere furnace, a main controller, a vacuum system, an argon control system and an oxygen control system.
The argon control system comprises an argon source and an argon heater, wherein the argon source conveys argon to the vacuum atmosphere furnace through the argon heater; the argon heater telecom is connected with an argon flow controller and an argon temperature controller, and the argon flow controller and the argon temperature controller are also in telecom connection with the main controller. The oxygen control system comprises an oxygen source and an oxygen heater, wherein the oxygen source is used for conveying oxygen to the vacuum atmosphere furnace through the oxygen heater; the oxygen heater is in telecommunication connection with an oxygen flow controller and an oxygen temperature controller, and the oxygen flow controller and the oxygen temperature controller are also in telecommunication connection with the main controller. The argon heater and the oxygen heater can heat the other corresponding materials conveyed into the vacuum atmosphere furnace to the same temperature as the hearth, so that the blank body is prevented from shrinking when encountering cold.
The vacuum atmosphere furnace is internally provided with a hearth, a temperature detection device and a water cooling device, the main controller is also in telecommunication connection with a hearth temperature controller and a water cooling controller, and the water cooling controller is in telecommunication connection with the water cooling device; the hearth temperature controller is in telecommunication connection with the temperature monitoring device, the temperature data detected in real time are fed back to the hearth temperature controller by the temperature detecting device, and then the power is adjusted through the power regulator so as to control the hearth temperature.
The vacuum system comprises a vacuumizing device and a vacuum controller, the vacuumizing device is connected with the vacuum atmosphere furnace in a matched mode, gas in the vacuum atmosphere furnace is conveniently pumped out, and the vacuum controller is connected with the main controller and the vacuumizing device in a telecommunication mode respectively.
The main controller controls the corresponding controllers according to the set parameters, and under the cooperation of the water cooling controller, the hearth temperature controller and the vacuum controller, the pressure change in the vacuum atmosphere furnace is prevented from being too large, and the blank body is prevented from cracking.
Example 1
The preparation method of the indium tin oxide target material by sintering comprises the following steps:
step one: indium oxide with purity not less than 99.99% and tin oxide with purity not less than 99.99% are mixed according to 9:1, and fully grinding, sieving to obtain powder with specific surface area of 5m 2 Indium tin oxide powder/g; uniformly mixing polyvinyl alcohol, polyacrylamide and a polyether type defoamer, then adding indium tin oxide powder, uniformly mixing to obtain slurry, and regulating the viscosity of the slurry to 1000 mPa.s; setting the casting pressure to be 0.2MPa, maintaining the pressure for 10min, and casting and forming the slurry to obtain a blank;
step two: placing the blank into a hearth of a vacuum atmosphere furnace by adopting a target sintering system, closing the vacuum atmosphere furnace, introducing argon, controlling the flow of the argon to be 5L/min, discharging air, keeping the temperature of the hearth at 200 ℃ according to the heating rate of 0.1 ℃/min, and preserving the temperature for 10 hours to finish pre-degreasing;
step three: maintaining the flow of argon at 5L/min, then raising the temperature of a hearth to 550 ℃ according to the heating rate of 0.1 ℃/min, and preserving heat for 20h to finish degreasing;
step four: argon in the vacuum atmosphere furnace is pumped out through a vacuumizing device, oxygen is introduced, the flow rate of the oxygen is adjusted to be 20L/min, the temperature of a hearth is increased to 1500 ℃ according to the heating rate of 0.5 ℃/min, sintering is completed after heat preservation is carried out for 5 hours, the introduction of the oxygen is stopped, the temperature of the hearth is reduced to 150 ℃ according to the cooling rate of 1 ℃/min, and then the air is introduced and cooled to room temperature, so that the indium tin oxide target is obtained.
Observing the surface of the indium tin oxide target material with a 50-time magnifying glass, measuring the average size of crystal grains of the indium tin oxide target material to be 4.5 mu m by using a scanning electron microscope, and measuring the relative density of the target material to be 99.76g/cm by using an Archimedes drainage method 3 。
Example 2
The preparation method of the indium tin oxide target material by sintering comprises the following steps:
step one: indium oxide with purity not less than 99.99% and tin oxide with purity not less than 99.99% are mixed according to 9:1, and fully grinding, sieving to obtain powder with specific surface area of 10m 2 Indium tin oxide powder/g; uniformly mixing polyvinyl alcohol, polyacrylamide and a polyether type defoamer, then adding indium tin oxide powder, uniformly mixing to obtain slurry, and regulating the viscosity of the slurry to 2000 mPa.s; setting casting pressure to be 1MPa, maintaining pressure for 20min, and casting and forming the slurry to obtain a blank;
step two: placing the blank into a hearth of a vacuum atmosphere furnace by adopting a target sintering system, closing the vacuum atmosphere furnace, introducing argon, controlling the flow of the argon to be 10L/min, discharging air, keeping the temperature of the hearth at 225 ℃ at a heating rate of 0.5 ℃/min, and preserving the temperature for 20 hours to finish pre-degreasing;
step three: maintaining the flow of argon at 10L/min, then raising the temperature of a hearth to 580 ℃ according to the heating rate of 0.5 ℃/min, and preserving the heat for 35h to finish degreasing;
step four: argon in the vacuum atmosphere furnace is pumped out through a vacuumizing device, oxygen is introduced, the flow rate of the oxygen is regulated to be 35L/min, the temperature of a furnace chamber is increased to 1550 ℃ according to the heating rate of 0.8 ℃/min, sintering is completed after heat preservation is carried out for 10 hours, the introduction of the oxygen is stopped, the temperature of the furnace chamber is reduced to 200 ℃ according to the cooling rate of 2 ℃/min, and then the air is introduced and cooled to room temperature, so that the indium tin oxide target material is obtained.
The surface of the indium tin oxide target material is observed to have no crack by using a 50-time magnifying glass, the average size of crystal grains of the indium tin oxide target material is measured to be 4.6 mu m by using a scanning electron microscope, and the relative density of the target material is measured to be 99.76g/cm by using an Archimedes drainage method 3 。
Example 3
The preparation method of the indium tin oxide target material by sintering comprises the following steps:
step one: indium oxide with purity not less than 99.99% and tin oxide with purity not less than 99.99% are mixed according to 9:1, and fully grinding, sieving to obtain powder with specific surface area of 15m 2 Indium tin oxide powder/g; polyvinyl alcohol, polyacrylamide and polyether typeUniformly mixing the foaming agent, adding indium tin oxide powder, uniformly mixing to obtain slurry, and regulating the viscosity of the slurry to 3000 mPa.s; setting the casting pressure to be 1.5MPa, maintaining the pressure for 30min, and casting and forming the slurry to obtain a blank;
step two: placing the blank into a hearth of a vacuum atmosphere furnace by adopting a target sintering system, closing the vacuum atmosphere furnace, introducing argon, controlling the flow of the argon to be 20L/min, discharging air, keeping the temperature of the hearth at 250 ℃ according to the heating rate of 1 ℃/min, and preserving the temperature for 30 hours to finish pre-degreasing;
step three: maintaining the flow of argon at 20L/min, then raising the temperature of a hearth to 600 ℃ according to the heating rate of 1 ℃/min, and preserving the heat for 50h to finish degreasing;
step four: argon in the vacuum atmosphere furnace is pumped out through a vacuumizing device, oxygen is introduced, the flow rate of the oxygen is regulated to be 50L/min, the temperature of a hearth is increased to 1600 ℃ according to the heating rate of 1 ℃/min, sintering is completed after heat preservation is carried out for 20 hours, the introduction of the oxygen is stopped, the temperature of the hearth is reduced to 250 ℃ according to the cooling rate of 3 ℃/min, and then the air is introduced and cooled to room temperature, so that the indium tin oxide target is obtained.
Observing the surface of the indium tin oxide target material with a 50-time magnifying glass, measuring the average size of crystal grains of the indium tin oxide target material to be 4.8 mu m by using a scanning electron microscope, and measuring the relative density of the target material to be 99.75g/cm by using an Archimedes drainage method 3 。
The polyether defoamer is purchased from Shenzhen ocean New Material Co., ltd, and the model is A-922.
It should be noted that in this document, terms such as "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. The sintering process of the indium tin oxide target material is characterized by comprising the following steps of:
step one: mixing, grinding and sieving indium oxide and tin oxide to obtain indium tin oxide powder; mixing polyvinyl alcohol, polyacrylamide, polyether defoamer and indium tin oxide powder into slurry, and casting the slurry to obtain a blank;
step two: adopting a target sintering system, controlling the flow of argon to be 5-20L/min, discharging air, heating, and preserving heat for 10-30h at 200-250 ℃ to finish pre-degreasing;
step three: maintaining the flow of argon at 5-20L/min, heating, and maintaining the temperature at 550-600deg.C for 20-50h to finish degreasing;
step four: argon is pumped out and oxygen is introduced, the flow of the oxygen is regulated to be 20-50L/min, the temperature is raised to 1500-1600 ℃, the heat is preserved for 5-20h, and the sintering process of the indium tin oxide target material is completed after cooling.
2. The sintering process of an indium tin oxide target according to claim 1, wherein in the first step, the mass ratio of indium oxide to zinc oxide is 9:1.
3. the process according to claim 1, wherein the specific surface area of the indium tin oxide powder is 5-15m 2 /g。
4. The sintering process of an indium tin oxide target according to claim 1, wherein the amount of the polyvinyl alcohol in the first step is 0.5-1wt% of the indium tin oxide powder, and the amounts of the polyacrylamide and the polyether defoamer are respectively 0.05-0.1wt% of the indium tin oxide powder.
5. The process according to claim 1, wherein the slurry in step one has a viscosity of 1000-3000 mPa-s.
6. The sintering process of an indium tin oxide target according to claim 1, wherein the casting pressure of the casting molding in the first step is 0.2-1.5MPa.
7. The sintering process of an indium tin oxide target according to claim 1, wherein the pre-degreasing temperature rise rate in the second step is 0.1-1 ℃/min.
8. The sintering process of an indium tin oxide target according to claim 1, wherein the degreasing temperature rise rate in the third step is 0.1-1 ℃/min.
9. The process for sintering an indium tin oxide target according to claim 1, wherein the temperature rising rate of sintering in the fourth step is 0.5-1 ℃/min.
10. The sintering process of an indium tin oxide target according to claim 1, wherein the specific step of cooling in the fourth step is: stopping introducing oxygen, cooling to 150-250deg.C at a rate of 1-3deg.C/min, and cooling to room temperature.
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CN114835485A (en) * 2022-04-20 2022-08-02 柳州华锡有色设计研究院有限责任公司 Method for deeply reducing resistivity of ITO target by accurately proportioning oxygen and argon
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JPS6287464A (en) * 1985-10-12 1987-04-21 トヨタ自動車株式会社 Method of dewaxing ceramic formed body
US20070031633A1 (en) * 2005-07-08 2007-02-08 Kabushiki Kaisha Toshiba Sputtering target, optical thin film and manufacturing method thereof using the sputtering target, and optical recording medium
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