CN112062150A - Method for preparing high-purity nano indium oxide powder - Google Patents
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- CN112062150A CN112062150A CN202010967571.8A CN202010967571A CN112062150A CN 112062150 A CN112062150 A CN 112062150A CN 202010967571 A CN202010967571 A CN 202010967571A CN 112062150 A CN112062150 A CN 112062150A
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a method for preparing high-purity nano indium oxide powder, which comprises a reaction box body for providing a purification reaction site, wherein the reaction box body is provided with a bin door, a crucible for containing indium powder is arranged in the reaction box body, a high-frequency induction coil for heating the crucible is arranged below the crucible, and O2The gas cylinder is connected with the reaction box body through a pipeline provided with a ball valve switch, the vacuum pump is connected with the reaction box body through a pipeline provided with a ball valve switch, and the reaction box body is further provided with a vacuum degree meter. The scheme does not need to specially arrange a special high-temperature reaction chamber and an atomizer. Compared with a precipitation method, the method does not produce waste liquid, does not need washing and centrifuging processes, does not need a high-temperature calcination link, and is beneficial to environmental protection and water and energy conservation. In contrast to the solid phase method, indium vapor is reacted with oxygen at high temperatureThe nano indium oxide powder with higher purity, uniform particle size and high sintering activity can be prepared by gas oxidation.
Description
Technical Field
The invention belongs to the field of ITO target preparation, and particularly relates to a method for preparing high-purity nano indium oxide powder by a sublimation method.
Background
Most of transparent electrodes used in flat panel display devices are ITO thin films, which require few defects, uniform quality, high flatness, and good conductivity. The ITO film is prepared by an ITO target material through a magnetron sputtering method, so that the high-quality ITO film is obtained, and the used ITO target material has high density, high purity, few defects and uniform grain size. The ITO target material is prepared from the following components in percentage by mass of 9: 1, the indium oxide powder and the tin oxide powder are mixed, granulated, molded and sintered, and the indium oxide powder occupies most of raw materials. Therefore, the prepared indium oxide powder with high purity, uniform particle size and high sintering activity is very important for preparing the high-end ITO target material. The melting point of indium metal is 156.61 ℃, and indium metal sublimes when heated in a vacuum environment. The current methods for producing high-purity nano indium oxide mainly include three methods, namely a gas phase method, a liquid phase method and a solid phase method according to the state of reactants, wherein the gas phase method is represented by a spray pyrolysis method and a spray combustion method, the spray pyrolysis method refers to a method in which a precursor containing an indium salt solution is made into liquid mist through an atomizer and is introduced into a high-temperature reaction chamber to perform pyrolysis reaction to prepare indium oxide powder, and the spray combustion method refers to a method in which molten indium metal is made into liquid mist through an atomizer and is introduced into a high-temperature reaction chamber to be combusted with oxygen or air to prepare indium oxide powder. The two methods are characterized in that special equipment such as an atomizer and a high-temperature reaction chamber are needed, the preparation process is complex, the temperature of the high-temperature reaction is difficult to control, the reaction is possibly insufficient, and the safety is slightly low. The liquid phase method is represented by a precipitation method, wherein the reaction raw material is metal indium or soluble indium salt, a salt solution of the metal indium is prepared firstly, then excessive ammonia water is dripped to obtain a colloidal precipitate of indium hydroxide, and the precipitate is washed and dried for several times and then calcined at high temperature to obtain indium oxide powder. The method is common, but has more steps, needs a high-temperature calcination process and has more complex process control. In addition, more waste liquid is generated, the environment is polluted, precipitates need to be washed for several times, and water sources are wasted. The solid phase method is classified into a high temperature solid phase reaction method, a room temperature solid phase reaction method, and the like, and the solid phase method has disadvantages that the purity of the produced indium oxide powder is difficult to be ensured, the reaction is difficult to reach a nano scale, and the particles of the produced powder are large.
Disclosure of Invention
In order to solve the technical problems, the method uses a principle similar to a spray combustion method to enable sublimed indium vapor to be oxidized and reused with oxygen at high temperature, and indium oxide powder with high purity, uniform particle size and high sintering activity is generated.
In order to achieve the aim, the invention provides a method for preparing high-purity nano indium oxide powder, which comprises the steps of arranging a reaction box body, arranging a bin door with an observation window on the reaction box body, arranging a crucible for containing indium powder in the reaction box body, arranging a high-frequency induction coil for heating the crucible below the crucible, and forming O2The gas cylinder is connected with the reaction box through the pipeline that is equipped with ball valve switch, and a vacuum pump is connected with the reaction box through the pipeline that is equipped with ball valve switch, the reaction box on still be provided with the vacuum gauge, concrete preparation step:
a. ball-milling reaction raw material indium powder through a screen;
b. placing indium powder in a crucible, opening a bin door of a box body, and erecting the crucible on a high-frequency heating coil;
c. closing the bin door of the box body, closing the ball valve switch, opening the vacuum pump for pumping vacuum, and closing the ball valve switch and closing the vacuum pump after the vacuum degree meter shows that the required vacuum degree is reached;
d. turning on a switch of a high-frequency induction coil power supply, starting to heat the crucible, setting a heating rate and a heating temperature for sublimating the indium powder, and starting to heat the indium powder in the crucible;
e. heating temperature for indium powder sublimationThen, open O2A ball valve switch on the gas cylinder is provided with an O2The flow rate of the indium powder is 0.1-5 m/s, and the indium powder is kept at the sublimation temperature of the indium powder for 10-60 min, so that the indium powder is fully sublimated, and the indium vapor and O2Fully oxidizing, observing the conditions in the reaction box body through the observation window until no indium powder is left in the crucible, depositing no indium powder in the reaction box body, closing a power switch of the high-frequency induction coil, stopping heating, and keeping O2Then continuously entering the reaction box for a period of time and closing the ball valve switch;
f. after the temperature in the reaction box body is reduced to the room temperature, the ball valve switch (2) is opened to lead O2And (4) entering a reaction box body, opening a bin door of the reaction box body after the vacuum degree gauge is restored to the atmospheric pressure, and collecting the indium oxide powder deposited in the reaction box body, thereby obtaining the high-purity nano indium oxide powder.
The theoretical basis is as follows: indium metal can be heated to sublimate under vacuum conditions, and the melting point of indium metal is 156.61 ℃. The heating temperature should be set below the melting point of the indium metal so that the indium metal sublimes. Opening O in the cylinder2Sublimed indium vapour at elevated temperature with O2And carrying out oxidation reaction to generate indium oxide powder, depositing the indium oxide powder in the box body, and collecting the indium oxide powder to obtain the high-purity nano indium oxide powder.
By adopting the technical scheme, compared with the existing spray thermal decomposition method and spray combustion method, the preparation method is simple, the temperature control is simpler, and a special high-temperature reaction chamber and an atomizer are not required to be specially arranged. Compared with a precipitation method, the method does not produce waste liquid, does not need washing and centrifuging processes, does not need a high-temperature calcination link, and is beneficial to environmental protection and water and energy conservation. Compared with a solid phase method, the method has the advantages that the indium vapor is oxidized with oxygen at high temperature, and the nano indium oxide powder with higher purity, uniform particle size and high sintering activity can be prepared. The scanning electron microscope photo of the prepared nano indium oxide powder can show that the granularity range is 20-100 nm, the granularity is uniform, and no obvious agglomeration phenomenon exists. The method is simple and efficient, has no pollution, and the prepared nano indium oxide powder has high purity, uniform particle size and high sintering activity.
In order to better realize the purpose of the invention, the invention also has the following better technical scheme:
in some embodiments, the reaction raw material indium powder is ball-milled for 1-2 hours, and the mesh number of the powder passing through a screen is 60-200 meshes.
In some embodiments, for more complete reaction, the vacuum pump is required to have a power of more than 2KW, and the ultimate vacuum degree can be 5 x 10^ c～2pa is more than; the ball valve switch is closed when the vacuum degree in the reaction box body is 2-20 pa, and the vacuum degree is kept to be 20-3000 pa in the sublimation and oxidation processes.
In some embodiments, the heating rate of the medium-high frequency induction coil is 0.5-10 ℃/min and the heating temperature is 50-150 ℃ for sufficient heating of the reaction raw material indium powder.
In some embodiments, to allow sufficient oxidation to occur, O2The flow rate of the indium powder is 0.1-5 m/s, the time of keeping at the sublimation temperature of the indium powder is 10-60 min, and the heating is stopped and then O is kept2And then continuously circulating for 5-15 min.
In some embodiments, to increase the heating efficiency while preventing the deposited indium oxide powder from falling into the crucible, the crucible is provided with a perforated cover.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing high-purity nano indium oxide powder by a sublimation method;
fig. 2 is a scanning electron micrograph of the prepared nano indium oxide powder.
The reference numbers are: o2 gas cylinder 1, ball valve switch 2, gas pipeline 3, vacuum degree meter 4, reaction box 5, box door 6, infundibulate air cock 7, transparent observation window 8, crucible 9, high frequency induction coil 10, high frequency induction coil's power 11, high frequency induction coil's switch 12, ball valve switch 13, vacuum pump 14.
Detailed Description
The present invention will be described in further detail with reference to examples.
As shown in figures 1 and 2, the invention provides a method for preparing high-purity nano oxideThe method for preparing indium powder comprises providing a reaction box 5, providing a door 6 with an observation window 8 on the reaction box 5, providing a crucible 9 for containing indium powder in the reaction box 5, providing a high-frequency induction coil 10 below the crucible 9 for heating the crucible 9, and providing an O2The gas cylinder 1 is connected with the reaction box body 5 through a pipeline provided with a ball valve switch 2, a vacuum pump 14 is connected with the reaction box body 5 through a pipeline provided with a ball valve switch 13, and a vacuum degree meter 4 is further arranged on the reaction box body 5.
The preparation method comprises the following specific steps: ball-milling reaction raw material indium powder for 1-2 h, wherein the mesh number of the reaction raw material indium powder passing through a screen is 60, 100, 150 or 200 meshes, and ball-milling the reaction raw material indium powder passing through the screen; placing indium powder in a crucible 9, opening a bin door 6 of a box body, and erecting the crucible 9 on a high-frequency heating coil 10; the heating rate of the high-frequency induction coil 10 is 0.5, 3, 6 and 10 ℃/min, and the heating temperature is 50, 100, 120 and 150 ℃; closing the bin gate 6 of the box body, closing the ball valve switch 2, opening the ball valve switch 13, opening the vacuum pump 14 for vacuumizing, and closing the ball valve switch 13 and the vacuum pump 14 after the vacuum degree meter 4 shows that the required vacuum degree is reached; the power of the vacuum pump 14 is more than 2KW in the reaction process, and the ultimate vacuum degree which can be reached is 5 multiplied by 10^ s～2pa is more than; the degree of vacuum in the reaction chamber body 5 is 5, 15, 20pa, the ball valve switch 13 is closed, and the degree of vacuum is maintained at 20, 150, 500, 1000, 2000, 3000pa during the sublimation and oxidation process.
Turning on a switch 12 of a high-frequency induction coil power supply 11, starting to heat the crucible 9, setting a heating rate and a heating temperature for sublimating the indium powder, and starting to heat the indium powder in the crucible 9; after reaching the heating temperature for indium powder sublimation, opening O2A ball valve switch 2 on the gas cylinder 1 is provided with O2The flow rate of the indium powder is 0.1, 2, 3, 5m/s, the sublimation temperature of the indium powder is kept for 10, 20, 30, 50, 60min, the indium powder is fully sublimated, and the indium vapor and O are mixed2Fully oxidizing, observing the conditions in the reaction box body 5 through the observation window 8 until no indium powder is left in the crucible 9, no indium powder is deposited in the reaction box body 5, closing a power switch 12 of the high-frequency induction coil 10, stopping heating, and keeping O2Continuously entering the reaction box 5 for 5-15 min and then closing the ball valve switch 2; to be treatedAfter the temperature in the reaction box body 5 is reduced to the room temperature, the ball valve switch 2 is opened to lead O2And (3) entering a reaction box body 5, opening a bin gate 6 of the reaction box body 5 after the vacuum degree meter is restored to the atmospheric pressure, and collecting the indium oxide powder deposited in the reaction box body 5, thereby obtaining the high-purity nano indium oxide powder.
The theoretical basis is as follows: indium metal can be heated to sublimate under vacuum conditions, and the melting point of indium metal is 156.61 ℃. The heating temperature should be set below the melting point of the indium metal so that the indium metal sublimes. Opening O in the cylinder2Sublimed indium vapour at elevated temperature with O2And carrying out oxidation reaction to generate indium oxide powder, depositing the indium oxide powder in the box body, and collecting the indium oxide powder to obtain the high-purity nano indium oxide powder. The scanning electron microscope photo of the prepared nano indium oxide powder can show that the granularity ranges from 20 nm, 40 nm, 60 nm, 80 nm and 100nm, the granularity is uniform, and no obvious agglomeration phenomenon exists. The method is simple and efficient, has no pollution, and the prepared nano indium oxide powder has high purity, uniform particle size and high sintering activity. What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (6)
1. The method for preparing high-purity nano indium oxide powder is characterized by comprising a reaction box body (5), a bin door (6) with an observation window (8) is arranged on the reaction box body (5), a crucible (9) for containing indium powder is arranged in the reaction box body (5), a high-frequency induction coil (10) for heating the crucible (9) is arranged below the crucible (9), and O2Gas cylinder (1) is connected through the pipeline that is equipped with ball valve switch (2) with reaction box (5), and a vacuum pump (14) is connected with reaction box (5) through the pipeline that is equipped with ball valve switch (13), reaction box (5) on still be provided with vacuum gauge (4), concrete preparation step:
a. ball-milling reaction raw material indium powder through a screen;
b. indium powder is placed in a crucible (9), a bin door (6) of a box body is opened, and the crucible (9) is erected on a high-frequency heating coil (10);
c. closing a bin door (6) of the box body, closing a ball valve switch (2), opening a ball valve switch (13), opening a vacuum pump (14) for vacuumizing, and closing the ball valve switch (13) and the vacuum pump (14) after a vacuum degree meter (4) displays that the required vacuum degree is reached;
d. turning on a switch (12) of a high-frequency induction coil power supply (11), starting to heat the crucible (9), setting a heating rate and a heating temperature for sublimating the indium powder, and starting to heat the indium powder in the crucible (9);
e. after reaching the heating temperature for indium powder sublimation, opening O2A ball valve switch (2) on the gas cylinder (1) is provided with O2The flow rate of the indium powder is 0.1-5 m/s, and the indium powder is kept at the sublimation temperature of the indium powder for 10-60 min, so that the indium powder is fully sublimated, and the indium vapor and O2Fully oxidizing, observing the conditions in the reaction box body (5) through the observation window (8) until no indium powder is left in the crucible 9 and no indium oxide powder is deposited in the reaction box body (5), closing a power switch (12) of the high-frequency induction coil (10), stopping heating, and keeping O2Then continuously enters a reaction box (5)
Closing the ball valve switch (2) after a period of time;
f. after the temperature in the reaction box body (5) is reduced to the room temperature, the ball valve switch (2) is opened to lead O2And (3) entering a reaction box body (5), opening a bin gate (6) of the reaction box body (5) after the vacuum degree meter is restored to the atmospheric pressure, and collecting the indium oxide powder deposited in the reaction box body (5) so as to obtain the high-purity nano indium oxide powder.
2. The method for preparing high-purity nano indium oxide powder according to claim 1, wherein the reaction raw material indium powder is subjected to ball milling for 1-2 h, and the mesh number of the reaction raw material indium powder passing through a screen is 60-200 meshes.
3. The method for preparing high-purity nano indium oxide powder according to claim 1, wherein the power of the vacuum pump (14) is more than 2KW, and the ultimate vacuum degree which can be achieved is 5 x 10^ e2pa is more than; the ball valve switch (13) is closed when the vacuum degree in the reaction box body (5) is 2-20 pa, and the vacuum degree is kept to be 2 in the sublimation and oxidation processes0～3000pa。
4. The method for preparing high-purity nano indium oxide powder according to claim 1, wherein the temperature rise rate of the medium-high frequency induction coil (10) is 0.5-10 ℃/min, and the heating temperature is 50-150 ℃.
5. The method for preparing high purity nano indium oxide powder according to claim 1, wherein O is2The flow rate of the indium powder is 0.1-5 m/s, the time of keeping at the sublimation temperature of the indium powder is 10-60 min, and the heating is stopped and then O is kept2And then continuously circulating for 5-15 min.
6. The method for preparing high purity nano indium oxide powder according to claim 1, wherein the crucible (9) is provided with a crucible cover cap having a hole on the upper surface thereof.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106757323A (en) * | 2016-12-05 | 2017-05-31 | 南京大学 | A kind of unstressed InN nanowire growth methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106757323A (en) * | 2016-12-05 | 2017-05-31 | 南京大学 | A kind of unstressed InN nanowire growth methods |
Non-Patent Citations (2)
| Title |
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| LI ZHANG ET AL.: "Effect of Carrier Gas Flow Rate on In2O3 Nanostructure Morphology and Growth Mechanism", 《JOURNAL OF NANO RESEARCH》 * |
| 张莉等: "《分离检测实训》", 31 January 2013, 中国科学技术大学出版社 * |
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Application publication date: 20201211 |