CN111617702A - Oxide powder manufacturing apparatus - Google Patents
Oxide powder manufacturing apparatus Download PDFInfo
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- CN111617702A CN111617702A CN201910215973.XA CN201910215973A CN111617702A CN 111617702 A CN111617702 A CN 111617702A CN 201910215973 A CN201910215973 A CN 201910215973A CN 111617702 A CN111617702 A CN 111617702A
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- 239000000843 powder Substances 0.000 title claims abstract description 71
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- 238000001704 evaporation Methods 0.000 claims abstract description 73
- 230000008020 evaporation Effects 0.000 claims abstract description 72
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 27
- 239000001301 oxygen Substances 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 239000011261 inert gas Substances 0.000 claims description 20
- 230000003647 oxidation Effects 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 19
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 239000002245 particle Substances 0.000 description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 11
- 238000004544 sputter deposition Methods 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 229910001887 tin oxide Inorganic materials 0.000 description 9
- 229910052786 argon Inorganic materials 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910003437 indium oxide Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000002902 bimodal effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- AZWHFTKIBIQKCA-UHFFFAOYSA-N [Sn+2]=O.[O-2].[In+3] Chemical compound [Sn+2]=O.[O-2].[In+3] AZWHFTKIBIQKCA-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/06—Solidifying liquids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
- B01J2219/00277—Apparatus
- B01J2219/00351—Means for dispensing and evacuation of reagents
- B01J2219/0036—Nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
Abstract
The present invention provides an oxide powder manufacturing apparatus, an oxide powder manufacturing apparatus of an embodiment of the present invention includes: the method comprises the following steps: an evaporation chamber as a reaction unit for heating a reaction substance in a solid state to perform evaporation, the reaction substance being accommodated in the evaporation chamber; an oxidation reaction chamber disposed above the evaporation chamber, for oxidizing a liquid reaction substance moving from the evaporation chamber; at least one trap for trapping oxide powder generated from the oxidation reaction chamber; a transport pipe disposed between the catcher and the reaction unit, for transporting the oxide in a droplet state; and a controller for controlling the evaporation chamber, the oxidation reaction chamber, the transport pipe, and the trap.
Description
Technical Field
The present invention relates to an apparatus for producing an oxide powder, and more particularly, to an apparatus for producing an oxide powder having small aggregation and uniform size, particularly, a nano-oxide powder having small aggregation and small size, by evaporating a solid reaction substance into a droplet state.
Background
Generally, the sputtering method is known as one of methods for manufacturing a thin film. The sputtering method is a method for forming a thin film on a substrate by sputtering a sputtering target, and has advantages that a large area can be easily realized and a high-performance thin film can be efficiently produced.
Recently, as a sputtering method, there have been proposed a reactive sputtering method in which sputtering is performed with a reactive gas, a magnetron sputtering method in which a magnet is provided on the inner surface of a target material to accelerate the speed of thin film formation, and the like.
Among the thin films used In such a sputtering method, indium oxide-tin oxide (In) is particularly preferable2O3-SnO2The composite oxide of (1), hereinafter referred to as "ITO") film has high visible light transmittance and high conductivity, and thus is widely used as a transparent conductive film, for example, as a heat generating film for preventing dew condensation of liquid crystal display devices or glass, or an infrared ray reflective film.
Because of this, in order to form a film more efficiently, studies on sputtering conditions, sputtering apparatuses, and the like have been actively conducted. Further, such ITO sputtering has a problem that the time from when a new sputtering target is installed to when the initial arc (abnormal discharge) disappears and a product can be manufactured is short, and the time to which the target can be used after installation once (total sputtering time: target life).
Such an ITO sputtering target is produced by mixing indium oxide powder and tin oxide powder at a predetermined ratio and then performing a dry or wet process, and in order to obtain an ITO sintered body having a high density, it is necessary to provide indium oxide powder and tin oxide powder having high dispersibility.
Most of the methods for producing oxide powders as described above employ a method in which a hydroxide is obtained in an aqueous solution state and then calcined to obtain an oxide powder, or a method in which a hydroxide is synthesized by applying ultrasonic waves to an aqueous solution and then subjected to a wet synthesis process of precipitation, washing, and calcination.
However, in the above-described oxide powder production method, since the intermediate compound having a logarithmic nm to several tens of nm is subjected to a calcination treatment for the purpose of separation, oxidation, and crystallization of metal ions, a bottleneck (Neck) due to a diffusion phenomenon is formed between activated particles, thereby increasing the cohesion between powders and lowering the characteristics of the oxide powder.
Disclosure of Invention
An object of the present invention is to provide an oxide powder manufacturing apparatus that heats a solid reaction material to evaporate an oxide into a droplet state, collects the oxide powder, and injects an inert gas into an evaporation chamber to reduce collision between evaporated metal gases, thereby manufacturing oxide powder having a smaller particle size.
Further, an object of the present invention is to provide an oxide powder manufacturing apparatus capable of manufacturing a nano oxide powder having a small particle aggregation ratio by reducing a flow rate of a metal and an oxide vapor ascending in an evaporation chamber when the metal and the oxide vapor flow into an oxidation reaction chamber, thereby increasing a mean free path by reducing the flow rate, and by such a change in the flow rate, a high degree of oxidation homogeneity can be secured.
In order to achieve the above-described object, an oxide powder manufacturing apparatus of an embodiment of the present invention includes: the method comprises the following steps: an evaporation chamber as a reaction unit for heating a reaction substance in a solid state to perform evaporation, the reaction substance being accommodated in the evaporation chamber; an oxidation reaction chamber disposed above the evaporation chamber, for oxidizing a liquid reaction substance moving from the evaporation chamber; at least one trap for trapping oxide powder generated from the oxidation reaction chamber; a transport pipe disposed between the catcher and the reaction unit, for transporting the oxide in a droplet state; and a controller for controlling the evaporation chamber, the oxidation reaction chamber, the transport pipe, and the trap.
Drawings
Fig. 1 is a diagram showing the overall configuration of an oxide powder manufacturing apparatus of the present invention.
Fig. 2 is a diagram for explaining in detail the structures of the evaporation chamber and the oxidation reaction chamber constituting the apparatus of the present invention.
Fig. 3 is a view showing an oxygen supply unit configured in the oxidation reaction chamber of the present invention and used to effect oxidation of the reaction substance.
Fig. 4 is a diagram showing a heating unit configured in the evaporation chamber of the present invention.
Fig. 5 is a graph showing the yield of oxide powder corresponding to inert gas when the apparatus of the present invention performs an oxidation process.
Fig. 6 is a graph showing a comparison of particle sizes of oxide powders corresponding to inert gases when the apparatus of the present invention performs an oxidation process.
Fig. 7 is a graph showing particle analysis in the case where argon gas is fed when the apparatus of the present invention performs an oxidation process.
Fig. 8 is a graph showing particle analysis in the case where nitrogen gas is fed when the apparatus of the present invention performs an oxidation process.
Fig. 9 is a graph showing the result of XRD analysis of the tin oxide powder manufactured using the apparatus of the present invention.
Fig. 10 and 11 are SEM photographs of the tin oxide powder manufactured by the apparatus of the present invention.
Detailed Description
Fig. 1 is a diagram showing the overall configuration of an oxide powder manufacturing apparatus of the present invention. Referring to fig. 1, an oxide powder manufacturing apparatus 100 of the present invention includes: an evaporation chamber 200 that heats the solid reaction substance to evaporate it into an oxide in a droplet state; an oxidation reaction chamber 300 disposed at an upper side of the evaporation chamber 200, for powdering vapor of a reaction substance generated in the evaporation chamber 200; a transfer pipe 130 for transferring the powder generated in the oxidation reaction chamber 300; at least one trapping unit 120 for trapping the moving oxide powder.
The transport pipe 130 is disposed between the oxidation reaction chamber 300 and the trap units 120, and when a plurality of trap units 120 are provided, the transport pipe 130 is also disposed between the trap units to perform a function of transporting the oxide in a droplet state.
In addition, the one or more trap units 120 may be connected in series or in parallel. Further, the trap unit 120 includes: a circulation unit 120a for circulating the oxide in the form of droplets supplied through the transport pipe 130; and a trap part 120b for trapping the oxide powder under the circulation part 120 a.
Further, a motor part 140a for supplying power to circulate the oxide in a liquid crystal state is further included, and a filter part 140b may be further disposed between the circulation part 120a and the trap part 120 b.
The evaporation chamber 200, the oxidation reaction chamber 300, the trap unit 120, and the transfer pipe 130 may be controlled by the controller 180. For example, the controller 180 may control flow rate, pressure, and time conditions related to air discharge and gas introduction by the vacuum pump 210 and the gas introduction unit 240 included in the evaporation chamber 200, heating, temperature, and pressure conditions of the evaporation chamber 200, operations of the circulation unit 120a and the capture unit 120b of the capture unit 120, and temperature conditions of the transport pipe 130 for transporting the oxide in the droplet state to the capture unit 120.
The method for producing an oxide powder by using the oxide powder production apparatus 100 of the present invention having the above-described structure is as follows.
Wherein, the oxide is assumed to be tin oxide SnO2The case (b) is described as an example, but the present invention is not limited thereto. Thus, the oxide may refer to indium oxide In2O3Gallium oxideGa2O3These can be trapped in a powder state in the same manner as in the production of tin oxide powder.
First, the evaporation chamber 200 and the oxidation reaction chamber 300 for producing solid tin into powder in a droplet state will be described with reference to fig. 2 to 4, for example, as a reaction substance in a solid state.
Fig. 2 is a diagram for explaining in detail the structures of an evaporation chamber and an oxidation reaction chamber constituting the apparatus of the present invention, fig. 3 is a diagram showing an oxygen supply unit configured in the oxidation reaction chamber of the present invention to effect oxidation of a reaction substance, and fig. 4 is a diagram showing a heating unit configured in the evaporation chamber of the present invention.
First, a reaction unit in which solid tin is powdered in a droplet (liquid) state and oxidized according to an embodiment of the present invention will be described. The reaction unit includes an evaporation chamber 200 and an oxidation reaction chamber 300.
The evaporation chamber 200 is a reaction unit, is formed below the oxidation reaction chamber 300, and has a larger size than the oxidation reaction chamber 300.
The evaporation chamber 200 includes: a first chamber body 201 for forming a profile; a first heating unit 230 formed in the first chamber body 201 and including a heating element for generating heat; a container 220 formed in the chamber interior 202 for containing solid reaction substances; a vacuum pump 210 for exhausting air from the interior 202 of the evaporation chamber 200; and exhaust ports 212 and 213 for providing a passage for allowing air in the chamber interior 202 to escape to the vacuum pump 210 side.
In addition, the method also comprises injecting inert gas (Ar or N) into the evaporation chamber 2002) The gas introducing part 240 of (a) and including an inlet 241 for introducing the inert gas supplied through the gas introducing part 240.
In addition, an oxidation reaction chamber 300 is formed at an upper side of the evaporation chamber 200, and the oxidation reaction chamber 300 serves as a reaction unit for oxidizing the powder in a droplet state.
In order to sufficiently impart an oxidation reaction time to the powder in a droplet state moving to the upper side of the evaporation chamber 200 and moving into the oxidation reaction chamber 300 and ensure a high degree of oxidation homogeneity, the inside of the oxidation reaction chamber 300 includes a first inlet 301a and a second inlet 301b having a larger diameter (size) than the first inlet 301 a.
That is, the first inlet 301a is provided closer to the evaporation chamber 200 than the second inlet 301b, and the flow rate of the powder in the form of droplets flowing into the oxidation reaction chamber 300 through the first inlet 301a is reduced by the larger inner diameter of the second inlet 301 b.
Also, the oxidation reaction chamber 300 includes: a second chamber body 301 having internal dimensions of different sizes 301a, 301b from each other; a second heating unit 330 formed in the second chamber body 301 and including a heating element for heating the temperature inside the oxidation reaction chamber 300; an oxygen supply unit 310 is formed inside the oxidation reaction chamber 300, and is used for supplying oxygen to oxidize the powder in the droplet state.
Further, a transfer pipe 130 is connected to the oxidation reaction chamber 300 to transfer the powder oxidized in the oxidation reaction chamber 300.
The operation of the reaction unit in which the reaction substance (tin) in a solid state is changed into a droplet state and oxidized to produce a powder will be described in more detail.
First, a solid reaction substance (e.g., tin) is contained within the evaporation chamber 200. For example, the container 220 in the form of a furnace contains solid tin.
Next, the vacuum pump 210 is operated to discharge the air inside the evaporation chamber 200. The removal of the air in the evaporation chamber by the vacuum pump 210 is to suppress the oxidation of tin, and is a step for reducing oxygen in the vacuum pump 210 although the inside of the vacuum pump is not completely vacuum.
This is because tin tends to be produced as tin oxide powder when it comes into contact with oxygen at a high temperature, and when solid tin is charged into the evaporation chamber 200, the inside of the evaporation chamber 200 is filled with air/atmosphere, and the solid tin may react due to oxygen in the atmosphere. Therefore, only liquid tin can be generated by operating the vacuum pump 210 to remove or reduce oxygen inside the evaporation chamber 200 and then increasing the temperature inside the evaporation chamber 200.
That is, after the air or oxygen inside the evaporation chamber 200 is removed by the vacuum pump 210, the first heating unit 230 of the evaporation chamber 200 is operated to heat the solid tin into liquid tin. The heating temperature of the evaporation chamber 200 may be in the range of 1000 to 1600 ℃.
In addition, the evaporation chamber 200 may be divided into a plurality of zones (zones) and heated, and the same heating temperature may be maintained throughout the entire Zone inside the evaporation chamber 200.
As shown in fig. 4, heating units 230 each including a heating element are stacked in the vertical direction to keep the temperature inside the evaporation chamber 200 constant. In the case of vertically dividing the inner region of the evaporation chamber 200 into three regions, the heating unit 230 is disposed in the first, second, and third regions such that the edges of the respective heating elements intersect with each other. Thereby, the inside of the evaporation chamber 200 can maintain a predetermined reaction temperature in the entire region. Such an arrangement of the heating units is not only the evaporation chamber 200, but also in the case of the second heating unit 330 constructed in the oxidation reaction chamber 300.
In addition, after the inside of the evaporation chamber 200 is raised to a preset temperature by the heating of the first heating unit 230 configured by such an arrangement, the operation of the vacuum pump 210 is turned off, thereby interrupting the process of removing the air inside the evaporation chamber 200.
Next, as the gas injection part 240 connected to the upper side of the evaporation chamber 200 operates, an inert gas is injected into the evaporation chamber 200.
The inert gas is supplied and simultaneously oxygen is supplied through the oxygen supply unit 310 formed in the oxidation reaction chamber 300.
The motor unit 140a operates to start powdering by transferring and collecting oxide powder.
Specifically, the reason why the inert gas is introduced into the evaporation chamber 200 in which the tin in the liquid state is generated is to move only the pure tin crystal grains (seed) upward and to oxidize the tin crystal grains by the supplied oxygen.
The inert gas may be, for example, argon or nitrogen, and other inert gases may be used.
Table 1 below shows experimental data on the type of inert gas to be fed into the evaporation chamber when the apparatus of the present invention produces oxide powder, the size of powder produced according to the injection pressure, and the production yield.
[ TABLE 1 ]
Gas species | Pressure (MPa) | Size (D)10) | Size (D)50) | Size (D)90) | BET(m2/g) | Production yield (%) |
Atmosphere (es) | - | 0.9 | 1.2 | 6.2 | 8.25 | 85 |
Ar | 0.2 | 0.1 | 0.7 | 3.2 | 8.75 | 91 |
Ar | 0.3 | 0.2 | 0.9 | 4.1 | 8.67 | 92 |
N2 | 0.1 | 0.1 | 0.8 | 3.4 | 9.36 | 89 |
N2 | 0.2 | 0.2 | 1.0 | 4.5 | 9.16 | 91 |
N2 | 0.25 | 0.1 | 0.7 | 4.0 | 9.29 | 92 |
N2 | 0.3 | 0.2 | 0.9 | 4.6 | 9.15 | 92 |
By injecting an inert gas, a powder having a particle size of D100.2 μm, DS01.0 μm or D905.0 μm or less can be produced, and when argon gas is injected, 8.5m can be obtained2Specific surface area of 9.0m or more when nitrogen gas is injected2Powder with specific surface area of more than g. It was confirmed that when a gas of 0.2MPa or more was injected, a production yield of 90% or more could be obtained.
As the characteristics of the produced powder, data measured by a specific surface area analyzer and a particle size analyzer will be described later together with the attached drawings.
In addition, in the process of injecting the inert gas into the evaporation chamber 200, oxygen is supplied by the oxygen supply unit 310 in the upper oxidation reaction chamber 300, and the liquid tin meets the oxygen supplied through the oxygen supply holes 312 of the oxygen supply nozzle 311 to cause an oxidation reaction, and thus homogeneous oxide powder is produced.
Further, in the process of forming the oxidation reaction, the heating unit is controlled by the controller so that the temperature inside the oxidation reaction chamber 300 is the same as the temperature inside the evaporation chamber 200 or maintained lower than the temperature inside the evaporation chamber 200 (e.g., 50 ℃), thereby preventing the oxygen supplied into the oxidation reaction chamber 300 from moving into the evaporation chamber 200 below.
Further, the heater 313 operates to prevent the oxide powder from condensing around the oxygen supply hole 312 in the process of performing the oxidation reaction based on the oxygen supplied through the oxygen supply unit 310.
As described above, the generated oxide powder is supplied to the adjacent trap unit 120 through the transfer pipe 130, and the oxide powder is circulated by the circulation unit 120a in the trap unit 120 to be suppressed from being condensed, and is trapped in the trap unit 120b disposed at the lower portion.
Fig. 5 is a graph showing the yield of oxide powder corresponding to inert gas when the apparatus of the present invention performs an oxidation process.
As can be seen from the graph of fig. 5, as the injection amount of the inert gas increases, the production yield increases, but the maximum specific surface area can be achieved when injecting N0.1. When the production yield and the specific surface area are considered together, the case of injecting N0.25 when the oxidation is carried out will be most preferable.
The reason why the production yield is improved as the injection amount of the inert gas is increased is that the amount of the powder adsorbed in the evaporation chamber 200 can be significantly reduced, and thus the production yield is improved.
In addition, the reason for the increase of the specific surface area is that the oxidation reaction chamber 300 reacts with pure oxygen, and thus there is no contact with other impurities or defects corresponding to the contact.
Fig. 6 is a graph showing a comparison of particle sizes of oxide powders corresponding to inert gases when the apparatus of the present invention performs an oxidation process.
In which experimental data showing particle sizes when the same amount of argon and nitrogen was injected, particles having a slightly larger size were produced when nitrogen was injected, and if an optimum amount was selected with reference to the aforementioned graph of fig. 5 and with reference to the production yield, an optimum particle size could be obtained at a nitrogen of 0.25.
Fig. 7 is a graph showing particle analysis in the case where argon gas is fed when the apparatus of the present invention performs the oxidation process, and fig. 8 is a graph showing particle analysis in the case where nitrogen gas is fed when the apparatus of the present invention performs the oxidation process.
From the graphs of fig. 7 and 8, a bimodal distribution (bimodal distribution) or a multimodal distribution was confirmed, and in the case of production with nitrogen 0.2 and nitrogen 0.25, it was confirmed that the distribution of the fine powder was larger than that of argon. Nitrogen 0.1 and nitrogen 0.3 exhibit a similar profile to that of argon.
The type and amount of inert gas may be selected according to the objective/purpose to be produced.
Fig. 9 is a graph showing the result of XRD analysis of the tin oxide powder manufactured using the apparatus of the present invention.
Fig. 10 and 11 are SEM photographs of the tin oxide powder produced by the apparatus of the present invention, and it was confirmed that the powder having a size of less than 200nm could be produced.
Claims (6)
1. An oxide powder manufacturing apparatus, wherein,
the method comprises the following steps:
an evaporation chamber as a reaction unit for heating a reaction substance in a solid state to perform evaporation, the reaction substance being accommodated in the evaporation chamber;
an oxidation reaction chamber disposed above the evaporation chamber, for oxidizing a liquid reaction substance moving from the evaporation chamber;
at least one trap for trapping oxide powder generated from the oxidation reaction chamber;
a transport pipe disposed between the catcher and the reaction unit, for transporting the oxide in a droplet state; and
a controller for controlling the evaporation chamber, the oxidation reaction chamber, the transport pipe, and the trap.
2. The oxide powder manufacturing apparatus according to claim 1,
the evaporation chamber includes:
a first chamber body for forming a profile;
a first heating unit formed in the first chamber body and including a heating body for generating heat;
a vacuum pump for exhausting air inside the evaporation chamber; and
a discharge port formed in the first chamber body, providing a passage for air to escape.
3. The oxide powder manufacturing apparatus according to claim 2,
further comprising:
a gas injection unit for injecting an inert gas into the evaporation chamber; and
and an input port for inputting the inert gas supplied by the gas input part.
4. The oxide powder manufacturing apparatus according to claim 1,
the oxidation reaction chamber includes:
a second chamber body disposed on an upper side of the first chamber body to form an outer shape;
a second heating unit formed in the second chamber body and including a heating element for heating a temperature inside the oxidation reaction chamber; and
and the oxygen supply unit is formed inside the oxidation reaction chamber and used for supplying oxygen to realize the oxidation of the powder in a liquid drop state.
5. The oxide powder manufacturing apparatus according to claim 4, wherein,
the oxidation reaction chamber having a first inlet and a second inlet for moving a reaction substance in a liquid state generated from the evaporation chamber, the second inlet having a larger size than the first inlet,
the oxygen supply unit includes:
an oxygen supply nozzle formed with an oxygen supply hole; and
and a heater formed inside the oxygen supply nozzle and heating at a predetermined temperature.
6. The oxide powder manufacturing apparatus according to claim 1,
controlling, with the controller, the temperature inside the oxidation reaction chamber to reach the same temperature as or lower than the temperature inside the evaporation chamber while the oxidation reaction chamber and the evaporation chamber are heated.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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KR1020190023561A KR102202399B1 (en) | 2019-02-28 | 2019-02-28 | Apparatus for a oxide powder |
KR10-2019-0023561 | 2019-02-28 |
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CN111617702A true CN111617702A (en) | 2020-09-04 |
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CN114177856A (en) * | 2021-12-09 | 2022-03-15 | 安徽骏马新材料科技股份有限公司 | Red lead production facility of environmental protection |
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KR102084524B1 (en) * | 2018-05-28 | 2020-03-04 | 주식회사 더방신소재 | Apparatus for a oxide powder |
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US20040065170A1 (en) * | 2002-10-07 | 2004-04-08 | L. W. Wu | Method for producing nano-structured materials |
CN1946476A (en) * | 2004-02-28 | 2007-04-11 | 库尔尼亚·维拉 | Fine particle powder production |
KR100839020B1 (en) * | 2006-12-20 | 2008-06-17 | 대주전자재료 주식회사 | Method and equipment for production of magnesium oxide nanopowder |
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CN114177856A (en) * | 2021-12-09 | 2022-03-15 | 安徽骏马新材料科技股份有限公司 | Red lead production facility of environmental protection |
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