TW527241B - Method for forming metal oxide powder by means of spray of pressurized water containing oxygen dissolved therein - Google Patents

Abstract

The present invention relates to a method for forming metal oxide powder by means of the spray of pressurized water containing oxygen dissolved therein wherein a metal melt is formed with metal components with desired composition and a pressurized water jet that contain oxygen dissolved therein impacts onto the metal melt to form spray of metallic drips. By means of oxygen dissolved in the pressurized pure water and forming oxygen atmosphere to add oxygen thereto, the spray of metallic drips is exposed to oxidation condition for cooling and drying in order to form desired metal oxide powder. Subsequent heat treatment can be taken to more precisely control oxidation thereof.

Description

527241 V. Description of the invention (1) [Scope of application of the invention] The present invention relates to a method using dissolved aerobic paleo-oxide powder, especially θ p = between rolling € water condensate manufacturing gold pressure water spray manufacturing transparent Conduction is all oxygen: = method of using / combining lice [Background of the invention] method of powder. In the industry of bell film (.ptlcal coatlng) products and the liquid crystal display (LCD), which is more important today, the so-called transparent conductive chip is used to hang the towel from B and it is used in Dali ^ ^ ^ The surface of the special spicy glass nozzle used by various products is plated with a layer of transparent lightning guide _, Μ, # 日 日 道 H electrical materials. Currently most commonly used = Ming :: The emulsion material is indium tin oxide (indlum—Tin—_ and then is sputtered or evaporated on the special glass surface, and the two types of J film M are required and required. The transparent I oxide powder is first manufactured, and then directly evaporated or high pressure sintered to form the sputtering target. In terms of White 4 technology, the transparent conductive oxide powder is manufactured chemically using related salts, including chemical Both reduction and chemical thermal decomposition methods have the problems of tedious production process and high production cost. Taking the US patent No. 54 1 78 1 6 owned by Nikko Matenal of Japan as an example, the steps for manufacturing indium oxide powder are: First, the indium metal raw material is smelted to form an indium ingot, and then the indium ingot is electrolytically produced to produce indium hydroxide (Indlum Hydronde); then, indium hydroxide (Ιη (Ηι ^

Hydroxide) for solid-liquid separation (piiter); the separated solid indium hydroxide is washed with a large amount of pure water and made into an indium hydroxide mud table, and the indium hydroxide mud is dried and then pulverized; The subsequent hydroxide steel powder is heat-treated.

II

I rpf m ΓΛΐ'Ρ

I 527241

V. Description of the invention (2) The conventional chemical process is used to manufacture transparent conductive oxide powder. The production steps are tedious and the process is long, and it requires multiple process equipment and cooperation to increase the manufacturing cost. In addition, the chemical process institute The large amount of industrial waste water produced, if not properly treated, will even cause environmental pollution. The current trend of environmental protection is inconsistent. , T 〃 [Objective and summary of the invention] In order to change the principle of the present invention, the present invention uses a dissolving method and the degree of formulation. After a guided beam impacts the required shape of the metal, it is exempted from the use of high-pressure pure molten metal. The metal is oxidized and oxidized to achieve the required oxide. The above-mentioned transparent conductive physical method is well-known. The high pressure is combined with a water spray method pipe formed by pure water under the pressure of South to form a metal powder. Water spray powder. The method of the present invention manufactures oxygen in water, oxygen in liquid, and powder in the atomization process. The above-mentioned various tritium-based powders of conductive metal rhenium have different problems in the prior art, and the present invention provides a process for making oxide powder; and, because of the manufacturing process, it does not cause pollution to the environment. The water spray method in the powder metallurgy process provides a method for manufacturing a metal oxide powder by a water spray = a method of dissolving oxygen to increase the oxygen of the powder. After the metal or non-metal is heated and melted, the f-fluid is flowed. The high-pressure water is used to atomize the particles into high-pressure water, and it is cooled to form particles. Generally, it is used to make bows of powder metallurgy. Use the principle of "physical method to pulverize powder" to avoid chemical powder. High pollution from π, combined with oxygen addition methods such as chanting X h _, oxygen atmosphere, etc., make BE $, +, + rupture in an oxidizing environment during the process, and produce powder made of catty as an incomplete compound. Fangu & 1 '

Resentments, such as K ,, ^, can more precisely control the emulsified p b redness of transparent conductive gold. In addition, such as the incomplete five, the description of the invention (3) gasification of reading BB, * ^ " material, phase ^ ^ ^ electric metal oxide powder ancient ten systems ρ # father Yu use completely air + future Making a transparent conductive sputtering target 4 cars is easy. The transparent conductive metal oxide powder of L is used in the ancient invention to dissolve, h two, f method, its steps include; 2 t ^ pressurized water spray to produce metal oxide connection / Gu Rong metal solution; The metal raw material is heated to a molten state and connected to the osmium. Jiu Yu 1 Metal Nozzle: ,, right φ >, .. Freezing point) V barrels need to be added to J, its container ""), in order to maintain the metal solution to the appropriate * temperature (over the metal raw materials, The melting state of oxygen and oxygen; the metal solution flows into the metal solution to form atomization, and pure water impacts it, and the high pressure water is used to form the metal oxide powder to oxidize the metal droplets; the atomized oxidized metal liquid The impact pressure of the water is determined. The particle size is determined by the diameter of the nozzle and the high pressure is one of indium, tin, and zinc. The metal raw material used in the present invention is zinc. In addition, the metal raw material can form oxidation. Indium, tin oxide and oxidized indium tin oxide are produced using an appropriate ratio of indium and tin. In addition, the present invention also includes a step of ~ to increase the metal gas = ^, at the final forming stage, after the oxygen atmosphere is passed, it further contains Subsequent heat treatment ^, the degree of oxidation. After the powder is formed, the temperature is oxidized to adjust the gold. The degree of oxidation of the powder obtained by reoxidizing the metal oxide powder can be slowly reduced by the degree of oxidation of the non-gasified powder. The same heat treatment To control the degree and time [] using the described preferred embodiments of the present invention, the gas dissolved powder method 5, 21 and two conventional pressurized water spray producing metal oxide promoter to compare, in addition to the low cost

527241

ί 本 ί: Will ίίί The problem of water. • Re-advanced-detailed steps ^, the implementation examples of this ^ Ming are illustrated as follows: Contains the right: Γ test Figure 1 'It is a schematic diagram of dissolved oxygen water spray milling equipment, bag, 1 bucket 10' Used to hold the molten metal solution 11. And it shows the melting state of the metal solution 11 in the right-handed material blessing, * k symbol sparse barrel.妾 First-rate mouth 30, metal solution 11 flows into spray seat through flow nozzle 30. 1 Dissolved oxygen high-pressure pure water 40 to impact and oxidize metal solution 11, dissolved oxygen pressure pure water 40 is provided during the transmission of pure water—oxygen source 70, complex: pressure: 1 kg per square centimeter (lKg / Cm2) to increase the water droplets of dissolved oxygen lice diku t t t After cooling, the oxygen atmosphere in the cavity 50 is controlled by the cavity oxygen source. The pressure of the cavity oxygen source 90 is 0.1 kg per square centimeter of water: tail: 22 :: chemical oxygen 1 metal liquid After dropping 12 to form a metal oxide powder and adding this mouth makeup, the metal oxide powder will gradually settle to the bottom of the powder collector. After the powder is collected, the powder collector 60 is fitted with a pressure cap; j Bar worker lice, Water is pressed out to form metal oxide sludge. The metal oxide mud block is put into a heating furnace and dried, and metal oxides with different degrees of oxidation can be formed through the control of temperature, time and atmosphere. The specific implementation method of the present invention can be described in conjunction with the schematic diagram of the water spray powder making equipment shown in FIG. 丨, and the steps are detailed as follows: firstly, pure indium metal and pure tin metal with a purity of 9 9.9 9% are prepared in a ratio of 1 to 1. The earrings are scaled and weighed to prepare the metal materials. Next, the metal raw materials are placed in a smelting reel and heated to between 600 and 800 degrees Celsius to form a molten metal solution u, and then the metal solution U is placed in a hopper 10 and the hopper Need to warm up to about

Page 7 527241

Page 8 527241 V. Description of the invention (6) The oxidized file is a container placed in an atmospheric furnace, air is passed in and the heat treatment temperature is set to 850 ° C, and the heat treatment time is two hours. The oxygen content of the indium tin oxide powder after further heat treatment was 17.8 wt% after chemical analysis. Although the preferred embodiment of the present invention is disclosed as described above, it is not intended to limit the present invention. Any person skilled in the art can make some changes and retouching without departing from the spirit and scope of the present invention. The scope of patent protection of an invention shall be determined by the scope of patent application attached to this specification.

Page 9 527241 Brief description of the drawings Figure 1 is a schematic diagram of the dissolved oxygen water spray powder making equipment; and Figure 2 is an enlarged schematic view of a spray holder in the embodiment of the present invention.

Page 10 [Illustration of Symbols] 10 Container 11 Metal solution 12 Oxidized metal droplets 20 Induction furnace 30 Flow nozzle 40 Dissolved oxygen high-pressure pure water 50 Cavity 60 Powder collector 70 Oxygen source 80 Spray base 90 Cavity Oxygen source

Claims (1)

527241 / 、 The scope of the patent application is a high-pressure method using dissolved oxygen, which comprises: heating a metal raw material to a molten state to make metal oxide powder for clothing, so that the metal solution is produced into a metal solution through a spray holder; House pure water impinges on the metal solution, and injects a high droplet of dissolved oxygen; and genus> Valley fluid formation-the oxidized metal cools the oxidized metal droplet to form a metal Xuan &丨 Guanggang μ, 'Guangxi oxidation powder. The method described in item 1 of the Ming patent consumes a method of manufacturing metal oxide powder by dissolving a mist of sense gas. One of the methods is to spray one of indium, tin, and indium. /. The metal raw material is the method for manufacturing metal oxide powder by using the high service of dissolved oxygen as described in item 1 of the scope of the patent application, wherein, and tin. /, Τ The metal raw material is indium 4. The method for manufacturing metal powder by using high-pressure water mold in which oxygen is dissolved as described in item i of the scope of the patent application, further comprising flowing the metal solution into the spray nozzle through a first-class nozzle. Steps to re-flow the fog seat. 5. The method for manufacturing metal oxide powder using high-pressure water sprayed with oxygen as described in item 4 of the scope of patent application, wherein the particle size of the metal oxide powder is determined by the diameter of the nozzle. 6. The method for manufacturing metal compound powder by using high-pressure water sprayed with oxygen as described in item 1 of the scope of the patent application, wherein the particles of the metal oxide powder are produced by the impact pressure of the high-pressure pure water with dissolved oxygen. control. Ming, '... one method for spraying metal oxide powder from high-pressure water of Sichuan / Hega lice gas, one by one 丄 1 plant A ~ one, which further includes the use of oxygen as described in item 1 of the scope of patent application Oxygen-soluble high-pressure water spraying is costly, but also nitrogen and nitrogen? Cong Shi Cong, Tu, Gan A. _ Page 11 527241 VI. Patent Application Steps in the atmosphere to increase the degree of oxidation of the metal oxide powder. 8. The method for manufacturing metal oxide powder by using high-pressure water spray in which oxygen is dissolved as described in item 1 of the scope of the patent application, further comprising a heat treatment step, and the prepared metal oxide powder is subjected to high temperature oxidation to adjust The degree of oxidation of the metal oxide powder. 9. The method for manufacturing metal oxide powder by using high-pressure water spray in which oxygen is dissolved as described in item 8 of the scope of patent application, wherein the degree of oxidation of the metal oxide powder is controlled by the temperature, time and atmosphere of the heat treatment step . 1 0. A method for manufacturing metal oxide powder by using high-pressure water spray in which oxygen is dissolved, comprising: heating a metal raw material to a molten state to form a metal solution, and placing the metal solution in a hopper The container is connected to the nozzle; the metal solution is flowed into the spray seat through the flow nozzle, and a high-pressure pure water of dissolved oxygen is injected to impact and oxidize the metal solution to form metal oxide droplets; and The metal oxide droplets are cooled to form a metal oxide powder. 1 1. The method for manufacturing metal oxide powder by spraying with high pressure water in which oxygen is dissolved as described in item 10 of the scope of patent application, wherein the metal raw material is one of indium, tin, and zinc. 1 2. The method for manufacturing metal oxide powder by spraying high-pressure water in which oxygen is dissolved as described in item 10 of the scope of patent application, wherein the metal raw material is Page 12 527241 6. The scope of patent application is indium and tin. 1 3. The method for manufacturing metal oxide powder by using high-pressure water spray dissolved with oxygen as described in item 10 of the scope of patent application, wherein the bucket needs to be heated to an appropriate temperature to maintain the molten state of the metal solution . 14. The method for manufacturing a metal oxide powder by using high-pressure water sprayed with oxygen as described in item 10 of the scope of the patent application, wherein the particle diameter of the metal oxide powder is transmitted through the orifice of the nozzle and the dissolved oxygen The impact pressure of high-pressure pure water is controlled. 15 · The method for manufacturing metal oxide powder by using high-pressure water spray in which oxygen is dissolved as described in item 10 of the scope of patent application, further comprising a step of introducing an oxygen atmosphere to increase the oxidation degree of the metal oxide powder . 16. The method for manufacturing a metal oxide powder by using high-pressure water spray in which oxygen is dissolved as described in item 10 of the scope of the patent application, further comprising a heat treatment step, and then subjecting the prepared metal oxide powder to high-temperature oxidation. To adjust the degree of oxidation of the metal oxide powder. 1 7. The method for manufacturing metal oxide powder by using high-pressure water spray in which oxygen is dissolved as described in item 10 of the scope of patent application, wherein the degree of oxidation of the metal oxide powder is the temperature, time and atmosphere through the heat treatment step To control.