WO2015100812A1 - 金属镁的预处理装置和方法 - Google Patents

金属镁的预处理装置和方法 Download PDF

Info

Publication number
WO2015100812A1
WO2015100812A1 PCT/CN2014/070934 CN2014070934W WO2015100812A1 WO 2015100812 A1 WO2015100812 A1 WO 2015100812A1 CN 2014070934 W CN2014070934 W CN 2014070934W WO 2015100812 A1 WO2015100812 A1 WO 2015100812A1
Authority
WO
WIPO (PCT)
Prior art keywords
cavity
magnesium
heating
air inlet
metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2014/070934
Other languages
English (en)
French (fr)
Inventor
邹清华
吴聪原
张鑫狄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TCL China Star Optoelectronics Technology Co Ltd
Original Assignee
Shenzhen China Star Optoelectronics Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen China Star Optoelectronics Technology Co Ltd filed Critical Shenzhen China Star Optoelectronics Technology Co Ltd
Priority to KR1020167014127A priority Critical patent/KR101746359B1/ko
Priority to JP2016533601A priority patent/JP6208871B2/ja
Priority to US14/348,703 priority patent/US9340851B2/en
Priority to GB1607192.0A priority patent/GB2535065B/en
Publication of WO2015100812A1 publication Critical patent/WO2015100812A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/02—Light metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/08—Apparatus
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/04—Refining by applying a vacuum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/04—Crucible or pot furnaces adapted for treating the charge in vacuum or special atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B21/00—Open or uncovered sintering apparatus; Other heat-treatment apparatus of like construction
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/04—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
    • F27B5/06—Details, accessories or equipment specially adapted for furnaces of these types
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D11/00—Arrangement of elements for electric heating in or on furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00—Arrangements of controlling devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D21/00—Arrangement of monitoring devices; Arrangement of safety devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D21/00—Arrangement of monitoring devices; Arrangement of safety devices
    • F27D21/0014—Devices for monitoring temperature
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D21/00—Arrangement of monitoring devices; Arrangement of safety devices
    • F27D21/02—Observation or illuminating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00—Arrangements of controlling devices
    • F27D2019/0006—Monitoring the characteristics (composition, quantities, temperature, pressure) of at least one of the gases of the kiln atmosphere and using it as a controlling value
    • F27D2019/0012—Monitoring the composition of the atmosphere or of one of their components
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00—Arrangements of controlling devices
    • F27D2019/0006—Monitoring the characteristics (composition, quantities, temperature, pressure) of at least one of the gases of the kiln atmosphere and using it as a controlling value
    • F27D2019/0018—Monitoring the temperature of the atmosphere of the kiln

Definitions

  • the present invention relates to the field of planar display processes, and more particularly to a pretreatment apparatus and method for magnesium metal as an OLED cathode. Background technique
  • Organic Light Emitting Diode Display also known as organic electroluminescent diode
  • OLED Organic Light Emitting Diode Display
  • organic electroluminescent diode is a new display technology developed since the mid-20th century. Compared with liquid crystal displays, organic electroluminescent diodes have all-solid-state, active illumination, high brightness, 3 ⁇ 4, j" ⁇ metamorphosis, ultra-thin, low cost, low power consumption, fast response, wide viewing angle, wide operating temperature range, It has many advantages such as easy flexible display.
  • the structure of the organic electroluminescent diode generally includes: a substrate, an anode, a cathode and an organic functional layer, and the principle of illumination is a very thin multilayer organic material vapor-deposited between the anode and the cathode, by a positive load.
  • the organic functional layer of the organic electroluminescent diode is generally composed of three functional layers, namely a hole transport layer (HTL) and a light-emitting function layer.
  • Emissive Layer EML
  • Electron Transport Layer ETL
  • Each functional layer can be one layer, or more than one layer, such as a hole transport function layer, sometimes subdivided into hole injection.
  • Layer and hole transport layer; electron transport functional layer which can be subdivided into an electron transport layer and an electron injection layer, but its work Are similar, it is referred to as a hole transport functional layer, an electron transport layer.
  • the production method of full-color organic electroluminescent diode is mainly composed of red, green and blue (RGB) three-color parallel independent illumination method, white light plus color filter method and color conversion method, among which red, green and blue are juxtaposed.
  • the independent illuminating method has the most potential and is the most practical application.
  • the manufacturing method is that the red, green and blue light materials of different subjects and objects are selected.
  • Organic electroluminescent diodes can be classified into passive driving and active driving depending on the driving method. That is, direct addressing and thin film transistor (TFT) matrix addressing.
  • the active-driven organic electroluminescent diode is an active matrix organic light emitting device (AMOLED).
  • the current technical route for small-size AMOLED displays is low-temperature polysilicon thin film transistors.
  • the back panel is equipped with a TOP Emission OLED.
  • the cathode uses a magnesium/silver (Mg/Ag) alloy.
  • the work function of Mg is -3,68ev
  • the work function of Ag is 4,26ev.
  • the alloy also has a very good penetration rate, so that the light energy emitted by the exciton transition inside the luminescent layer is more active from the metal with a higher work function in the device, such as the work function of lithium (li) - 2, lev; sodium (Na The work function - 2,28ev; the work function of calcium (Ca) - 2,9ev, the more active the metal is, the easier it is to be oxidized, the Na needs to be stored in kerosene, the reaction will occur when it encounters air and water vapor, Burning explosion. Therefore, for the convenience of use, a relatively high work function Mg is selected, but Mg is oxidized in the air, and a thin layer of dense magnesium oxide is formed on the surface.
  • Magnesium oxide is released in the form of very small particles during the heating and evaporation process in the coating machine, which is called "magnesium ash".
  • the quality of the magnesia is very light, and a large amount of cerium oxide is in the cavity of the coating machine, polluting the cavity, and most importantly, floating on the substrate, forming defects in the pixel, resulting in black spots in the illuminating region. Affect life and yield.
  • the object of the present invention is to provide a metal magnesium pretreatment device which has a simple structure, can effectively remove magnesium oxide on the surface of magnesium metal, and effectively reduces the exposed area of metal magnesium, thereby effectively reducing the area of reoxidation of metal magnesium. Improve the purity of magnesium metal.
  • Another object of the present invention is to provide a method for pretreating metallic magnesium, which is simple in operation, can effectively remove cerium oxide on the surface of metallic magnesium, and effectively reduce the exposed area of metallic magnesium, thereby effectively reducing the area of reoxidation of metallic magnesium. , improve the purity of metal ruthenium.
  • the present invention provides a metal magnesium pretreatment apparatus, comprising: a cavity, a heating device installed in the cavity, an air inlet disposed on the cavity, and an air suction port disposed on the cavity,
  • the air inlet is connected to an inert gas injection device of the outside, and is used for injecting an inert gas into the cavity
  • the air suction port is connected to the external vacuum pumping device for drawing a vacuum into the cavity
  • the heating device is used for The magnesium metal oxidized on the heated surface volatilizes a layer of magnesium oxide on the surface of the magnesium metal in a vacuum environment to obtain pure metallic magnesium.
  • the air inlet is provided with an intake valve for controlling opening and closing of the air inlet; and the air suction port is provided with an air suction valve for controlling opening and closing of the air suction port.
  • a control device is also included for controlling opening and closing of the intake and exhaust valves.
  • an oxygen sensor disposed within the chamber, a vacuum gauge disposed within the chamber, the oxygen sensor for detecting oxygen content within the chamber, and the vacuum gauge for detecting pressure within the chamber.
  • the heating device includes a base. a heating coil disposed on the base and a cover disposed on the base and located at a periphery of the heating wire pattern, wherein the heating coil is wound by an iron-chromium-aluminum alloy or a nickel-chromium alloy electric heating wire; the base and the cover are both Made of metal, the heating device is controlled by the control device No heating.
  • a temperature sensor is mounted in the cover for detecting the temperature of the heating device.
  • a lighting device is further disposed in the cavity, and a side opening of the cavity is provided with a transparent opening window for observing the molten state of the oxidized metal magnesium on the inner surface of the cavity.
  • a liner liner that is detachably mounted within the cavity.
  • the control device is mounted on the cavity or integrated on the coater.
  • the invention also provides a pretreatment device for a metal crucible, comprising: a cavity, a heating device installed in the cavity, an air inlet disposed on the cavity, and an air suction port disposed on the cavity, the air inlet In connection with an inert gas injection device of the outside, for injecting an inert gas into the cavity, the suction port is connected to an external vacuum pumping device for drawing a vacuum into the cavity, and the heating device is used to heat the surface Oxidized magnesium metal, in a vacuum environment, a layer of magnesium oxide on the surface of the magnesium metal is volatilized to obtain pure magnesium metal;
  • the air inlet is provided with an air intake wide door for controlling opening and closing of the air inlet;
  • the air suction port is provided with an air suction valve for controlling opening and closing of the air suction port;
  • the utility model further comprises: a control device for controlling opening and closing of the intake valve and the suction valve; further comprising: an oxygen sensor disposed in the cavity, a vacuum gauge disposed in the cavity, the oxygen sensor being used for detecting the cavity The oxygen content, the vacuum gauge is used to detect the pressure in the chamber;
  • the heating device comprises a base, a heating coil disposed on the base, and a cover body disposed on the base and located at a periphery of the heating coil, wherein the heating coil is made of iron-chromium-aluminum alloy or nickel-chromium alloy electric heating wire;
  • the base and the cover are both made of metal, and the heating device controls whether or not heating is performed by the control device.
  • a temperature sensor is mounted in the cover for detecting the temperature of the heating device.
  • a lighting device is further disposed in the cavity, and a side opening of the cavity is provided with a transparent opening window for observing the molten state of the oxidized metal magnesium on the inner surface of the cavity.
  • the control device is mounted on the cavity or integrated on the coater.
  • the invention also provides a method for pretreating metallic magnesium, comprising the following steps:
  • Step 1 providing a pretreatment device, the pretreatment device comprising: a cavity, a heating device installed in the cavity, an air inlet disposed on the cavity, and an air suction port disposed on the cavity, the air inlet and the air inlet
  • the external inert gas injection device is in communication, and the suction port is connected to the external vacuum pumping device;
  • Step 2 placing the surface oxidized magnesium metal in the crucible, and placing the crucible in the heating device;
  • Step 3 pumping the cavity into a vacuum through the air suction port;
  • Step 4 injecting an inert gas into the cavity through the air inlet
  • Step 5 repeat steps 3 and 4, the oxygen content in the cavity is less than 1 ppm;
  • Step 6 the chamber is evacuated through the suction port, so that the pressure in the chamber is less than or equal to 0 - 4 Pa;
  • Step 7 heating the surface of the oxidized magnesium metal by a heating device, so that the magnesium oxide is completely volatized;
  • Step 8 After cooling, obtaining pure magnesium metal
  • the air inlet is provided with an intake valve for controlling opening and closing of the air inlet;
  • the air suction port is provided with an air suction valve for controlling opening and closing of the air inlet;
  • the pretreatment device further includes control means for controlling opening and closing of the intake valve and the suction valve;
  • the pretreatment apparatus further includes an oxygen sensor disposed in the cavity, a vacuum gauge disposed in the cavity, the oxygen sensor is configured to detect an oxygen content in the cavity, and the vacuum gauge is configured to detect a pressure in the cavity;
  • the heating device includes a base, a heating coil disposed on the base, and a cover disposed on the base and located at a periphery of the heating coil, wherein the heating coil is wound by an iron-chromium-aluminum alloy or a nickel-chromium alloy electric heating wire;
  • the base and the cover are both made of metal, and the heating device controls whether heating is performed by the control device;
  • a temperature sensor is installed in the cover body for detecting the temperature of the heating device
  • the cavity is further provided with a lighting device, and a side wall of the cavity is provided with a transparent opening window for observing the molten state of the oxidized metal magnesium on the inner surface of the cavity;
  • the pretreatment device further includes a lining prevention plate detachably mounted in the cavity;
  • the control device is mounted on the cavity or integrated on the coater.
  • the pretreatment apparatus and method for metallic magnesium of the present invention can remove magnesium oxide on the surface of metallic magnesium particles by pre-treatment, and greatly reduce the surface area exposed by the metal ruthenium in the ruthenium, and reduce the content of magnesium oxide.
  • the coating chamber only a very small amount of magnesium oxide is pretreated, which can prevent the coating cavity from being contaminated by a large amount of magnesium oxide, and greatly reduce the probability of product defects caused by magnesium oxide; and the cavity does not have too much magnesium oxide, It can reduce the frequency of downtime maintenance, reduce the number of times the liner is replaced, increase the rate of machine utilization, and save costs.
  • FIG. 1 is a schematic perspective view showing a pretreatment apparatus for a metal magnesium according to the present invention
  • FIG. 2 is a schematic plan view showing a planar structure of a metal magnesium pretreatment apparatus of the present invention
  • FIG. 3 is a schematic cross-sectional structural view of a heating device for a metal magnesium pretreatment apparatus of the present invention
  • FIG. 4 is a flow chart of a method for pretreating metallic magnesium according to the present invention
  • Figure 5 is a solid-liquid-gas conversion curve of magnesium oxide. Specific travel mode
  • the present invention provides a pretreatment apparatus for magnesium metal, comprising: a cavity 20, and a heating device 22 installed in the cavity 20.
  • An inert gas is injected therein, and the suction port 26 is connected to an external vacuum pumping device (not shown) for drawing a vacuum into the cavity 20, and the heating device 22 is for heating the metal magnesium whose surface is oxidized.
  • a layer of magnesium oxide on the surface of the magnesium metal is volatilized in a vacuum environment to obtain a pure metal ruthenium.
  • the pretreatment device is formed by placing the surface oxidized magnesium metal in a crucible (not shown), after the pretreatment is completed, the exposed surface area of the pure metallic magnesium is less than or equal to the opening area of the crucible, even if exposed to the air. It can only oxidize the exposed surface, greatly reduce the oxidation area of the magnesium metal, reduce the content of magnesium oxide produced by the oxidation of the metal magnesium, and increase the purity of the magnesium metal.
  • the air inlet 24 is provided with an intake valve 242 for controlling opening and closing of the air inlet 24; and the pumping air ⁇ 26 is provided with an air suction valve 262 for controlling the air suction port 26
  • PLC programmable logic controller
  • the control device is a programmable logic controller (PLC), which can be directly mounted to the cavity 20
  • the control device is directly mounted on the cavity 20 and performs specific operations through the control panel 40.
  • the metal magnesium pretreatment apparatus further includes an oxygen sensor 21 disposed in the cavity 20, and a vacuum gauge 23 disposed in the cavity 20, wherein the oxygen sensor 21 is configured to detect the oxygen content in the cavity 20.
  • the vacuum gauge 23 is used to detect the pressure in the cavity 20, thereby ensuring that the oxygen content and pressure in the cavity 20 reach a predetermined standard to ensure the metal after pretreatment. Magnesium purity.
  • the heating device 22 includes a base 222, a heating coil 224 disposed on the base 222, and a cover 226 disposed on the base 222 and located at the periphery of the heating coil 224.
  • the heating coil 224 is made of iron-chromium-aluminum alloy or nickel-chromium alloy.
  • the heating wire is wound; the base 222 and the cover 226 are both made of metal having high thermal conductivity, and the heating device 22 controls whether heating is performed by the control device.
  • a temperature sensor 228 is mounted in the cover 226 for detecting the temperature of the heating device 22 so as to control the heating temperature within a predetermined range.
  • the cavity 20 is further provided with a lighting device 25, and a side wall of the cavity 20 is provided with a transparent opening window 27, which can be transparently opened by the illumination device 25.
  • the molten state of the oxidized metal magnesium on the inner surface of the cavity 20 was observed.
  • the metal magnesium pretreatment apparatus further includes a lining prevention plate 60 detachably mounted in the cavity 20, and the magnesium oxide is volatilized and adhered to prevent the magnesium oxide from directly contacting the inner wall of the cavity. on. Since the lining prevention plate 60 is detachable, when the magnesium oxide adheres to a certain amount, the lining prevention plate 60 can be removed for cleaning, thereby prolonging the service life of the metal magnesium pretreatment device.
  • the present invention also provides a method for pretreating metallic magnesium, comprising the following steps:
  • Step 1 Providing a pretreatment device, the pretreatment device comprising: a cavity 20, a heating device 22 installed in the cavity 20, an air inlet 24 disposed on the cavity 20, and an air suction port disposed on the cavity 20 26, the air inlet 24 is connected to an external inert gas injection device (not shown) for injecting an inert gas into the cavity 20, the air suction port 26 and an external vacuum pumping device (not shown)
  • the heating device 22 is for heating the metal magnesium whose surface is oxidized, and volatilizing a layer of magnesium oxide on the surface of the magnesium metal in a vacuum environment to obtain pure magnesium metal.
  • the pretreatment device is formed by placing the surface oxidized magnesium metal in a crucible (not shown), after the pretreatment is completed, the exposed surface area of the pure metallic magnesium is less than or equal to the opening area of the crucible, even if exposed to the air. It can only oxidize the exposed surface, greatly reduce the oxidation area of the magnesium metal, reduce the content of magnesium oxide produced by the oxidation of the metal magnesium, and increase the purity of the magnesium metal.
  • the air inlet 24 is provided with an intake valve 242 for controlling the opening and closing of the air inlet 24;
  • the air suction port 26 is provided with an air suction valve 262 for controlling the opening of the air suction port 26.
  • the opening and closing of the intake valve 242 and the suction valve 262 are controlled by a control device.
  • the control device is a programmable logic controller (PLC), which can be directly mounted on the cavity 20. Or integrated in a coating machine (not shown), in the present embodiment, the control device is directly mounted on the cavity 20 and performs a specific operation through the control panel 40.
  • PLC programmable logic controller
  • the metal magnesium pretreatment apparatus further includes an oxygen sensor 21 disposed in the cavity 20, and a vacuum gauge 23 disposed in the cavity 20, wherein the oxygen sensor 21 is configured to detect the oxygen content in the cavity 20.
  • the vacuum gauge 23 is used to detect the pressure in the cavity 20, thereby ensuring that the oxygen content and pressure in the cavity 20 reach a predetermined standard to ensure the purity of the pretreated magnesium metal.
  • the heating device 22 includes a base 222, a heating coil 224 disposed on the base 222, and a cover 226 disposed on the base 222 and located at the periphery of the heating coil 224.
  • the heating coil 224 is made of iron-chromium-aluminum alloy or nickel-chromium alloy.
  • the heating wire is wound; the base 222 and the cover 226 are both made of metal having high thermal conductivity, and the heating device 22 controls whether heating is performed by the control device.
  • a temperature sensor 228 is mounted in the cover 226 for detecting the temperature of the heating device 22 so as to control the heating temperature within a predetermined range.
  • the cavity 20 is further provided with a lighting device 25, and a side wall of the cavity 20 is provided with a transparent opening window 27, which can be transparently opened by the illumination device 25.
  • the molten state of the oxidized metal magnesium on the inner surface of the cavity 20 was observed.
  • the metal magnesium pretreatment apparatus further includes an inner village prevention plate 60 detachably mounted in the cavity 20, and the magnesium oxide is volatilized and attached to avoid direct adhesion of the magnesium oxide to the inner wall of the cavity. on. Since the lining prevention plate 60 is detachable, when the magnesium oxide adheres to a certain amount, the lining prevention plate 60 can be removed for cleaning, thereby prolonging the service life of the metal magnesium pretreatment device.
  • Step 2 placing the surface oxidized magnesium metal in the crucible, and placing the crucible on the heating device, the actual operation may be: filling the purchased magnesium metal particles into the magnesium crucible used in the coating machine, due to the production and processing of magnesium In the granule process, not in the whole process of vacuum and inert gas protection, the magnesium particles can be in contact with air. Since magnesium is a very active metal, it is easily oxidized by oxygen in the air, and a layer of cerium oxide is formed on the surface.
  • Step 3 The chamber 20 is evacuated through a suction port 26.
  • the chamber 4 can be injected into the chamber 20 through the inlet port 24 by means of a dry pump, a molecular pump, an oil pump, a cryopump or a combination of different pumps.
  • Step 5 Repeat steps 3 and 4 until the oxygen content in the chamber 20 is less than 1 ppm.
  • Step 6 The cavity 20 is evacuated by pumping ⁇ 26 so that the pressure in the cavity 20 is less than or equal to (T 4 Pa.
  • Step 7 Heating the surface oxidized magnesium metal by the heating device 22 so that the magnesium oxide is completely volatilized.
  • the OB and OC lines respectively represent the critical line of the transition between the gaseous state and the liquid and solid state.
  • OD stands for the adjacent line of liquid-solid transition, which is almost perpendicular to the temperature coordinate.
  • the pressure change has no effect on the liquid/solid transition temperature.
  • the magnesium oxide has a pressure of l (T 4 Pa, temperature of 450 - 600 ° C). Next, it will automatically evaporate.
  • the ruthenium containing the pretreated magnesium is placed in the heating source of the coating machine, and the vacuum of the chamber of the coating machine reaches below IE-4, the temperature is raised, the surface and a small amount of magnesium oxide are removed, and then Normally coated. At this time, there is no magnesium oxide in the crucible, and no magnesium oxide is deposited on the cathode during deposition to form a cathode, which substantially eliminates defects caused by magnesium oxide.
  • the metal magnesium pretreatment apparatus and method of the present invention can remove magnesium oxide on the surface of the magnesium metal particles by pre-treatment, and greatly reduce the surface area exposed by the metal magnesium in the crucible, and reduce the content of cerium oxide, thereby making In the coating chamber, only a very small amount of magnesium oxide is pretreated, which can prevent the coating cavity from being contaminated by a large amount of magnesium oxide, and greatly reduce the probability of product defects caused by magnesium oxide; and the cavity does not have too much magnesium oxide, Reduce the frequency of downtime maintenance, reduce the number of times the liner is replaced, increase the rate of machine utilization, and save costs.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • General Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Physical Vapour Deposition (AREA)
  • Furnace Details (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

提供一种金属镁的预处理装置及方法，所述装置包括：腔体（20）、安装于腔体（20）内的加热装置（22）、设于腔体（20）上的进气口（24）及设于腔体（20）上的抽气口（26），所述进气口（24）与外界的惰性气体注入设备相连通，用于向腔体（20）内注入惰性气体，所述抽气口（26）与外部真空抽气装置相连通，用于将腔体（20）内抽成真空，所述加热装置（22）用于加热表面被氧化的金属镁，在真空环境下使得金属镁表面的一层氧化镁挥发，得到纯金属镁。所述方法可以除去金属镁颗粒表面的氧化镁，降低氧化镁的含量，使得在镀膜腔体中，只需预处理极少量的氧化镁，可以防止镀膜腔体被大量氧化镁污染，并大大降低由氧化镁导致的产品不良的机率。

Description

本发明涉及平面显示制程领域， 尤其涉及一种用于作为 OLED阴极的 金属镁的预处理装置和方法。 背景技术
有机发光二极管或有机发光显示器 ( Organic Light Emitting Diode Display, OLED )又称为有机电致发光二极管， 是自 20世纪中期发展起来 的一种新型显示技术。 与液晶显示器相比， 有机电致发光二极管具有全固 态、 主动发光、 高亮度、 ¾ 、 j" ^匕变、 超薄、 低成本、 低功耗、 快速响应、 宽视角、 工作温度范围宽、 易于柔性显示等诸多优点。 有机电致发光二极 管的结构一般包括： 基板、 阳极、 阴极和有机功能层， 其发光原理是通过 阳极和阴极间蒸镀的非常薄的多层有机材料， 由正负载流子注入有机半导 体薄膜后复合产生发光。 有机电致发光二极管的有机功能层， 一般.由三个 功能层构成， 分别为空穴传输功能层 ( Hole Transport Layer, HTL ) 、 发 光功能.层 ( Emissive Layer, EML ) 、 电 ΐ 专愉功能.层 ( Electron Transport Layer, ETL ) 。 每个功能层可以是一层, 或者一层以上， 例如空穴传输功 能层， 有时可以细分为空穴注入层和空穴传输层； 电子传输功能层， 可以 细分为电子传输层和电子注入层， 但其功能相近， 故统称为空穴传输功能 层， 电子传输功能层。
目前， 全彩有机电致发光二极管的制作方法以红绿蓝 （RGB ) 三色并 列独立发光法、 白光加彩色滤光片法， 色转换法三种方式为主， 其中红绿 蓝三色并列独立发光法最有潜力， 实际应用最多， 其制作方法是红绿蓝选 用不同主体和客体的发光材料。
有机电致发光二极管， 根据其驱动方式， 可以分为无源驱动和有源驱 动两大类。 即直接寻址和薄膜晶体管 （TFT ) 矩阵寻址两类。 所述有源驱 动类有机电致发光二极管即是有源矩阵式有机电致发光二极管 （Active Matrix Organic Light Emitting Device, AMOLED ) 。
小尺寸 AMOLED 显示屏目前的技术路线是低温多晶硅薄膜晶体管
( LTPS TFT ) 背板搭载顶发光 ( TOP Emission ) 的 OLED, 其阴极使用镁 / 银（Mg/Ag )合金， Mg的功函数是- 3,68ev, Ag的功函数是 4,26ev， 这样 可以使电子能比较容易从阴极注入到电子传输层， 并且 10- 20mn的 Mg/Ag 合金也具有非常好的穿透率， 使发光层内部激子跃迁发出的光能从器件内 一般功函数越高的金属越活泼， 例如锂 （li ) 的功函数- 2, lev; 钠 ( Na ) 的功函数- 2,28ev; 钙 （ Ca ) 的功函数- 2,9ev， 越活泼的金属越容易 被氧化， Na 需要在煤油中保存， 遇到空气和水汽就会发生反应， 剧烈时 会燃烧爆炸。 所以为了便于使用选择了功函数相对较高的 Mg， 但是 Mg 在空气中^然会被氧化 , 其表面会形成一层致密的氧化镁薄层。
氧化镁在镀膜机里加热蒸镀过程中， 会以很小微粒形式鋒放出来， 简 称 "镁灰" 。 这种镁灰的质量很轻， 大量的氧化锾在镀膜机腔体中， 污染 腔体， 最重要的是可以漂浮到基板上， 在像素 （pixel ) 中形成缺陷， 导致 发光区呈现黑点， 影响寿命和良率。
' 本发明的目的在于提供一种金属镁的预处理装置， 其结构简单， 能有 效去除金属镁表面的氧化镁， 且有效减小金属镁外露面积， 进而有效减小 金属镁再次氧化的面积， 提高金属镁的纯度。
本发明的另一目的在于提供一种金属镁的预处理方法， 其操作简单， 能有效去除金属镁表面的氧化锾， 且有效减小金属镁外露面积， 进而有效 减小金属镁再次氧化的面积， 提高金属锾的纯度。
为实现上述目的， 本发明提供一种金属镁的预处理装置， 包括： 腔 体、 安装于腔体内的加热装置、 设于腔体上的进气口及设于腔体上的抽气 口， 所述进气口与外界的惰性气体注入设备相连通， 用于向腔体内注入惰 性气体， 所述抽气口与外部真空抽气装置相连通， 用于将腔体内抽成真 空， 所述加热装置用于加热表面被氧化的金属镁， 在真空环境下使得金属 镁表面的一层氧化镁挥发， 得到纯金属镁。
所述进气口上设置有进气阀门， 用于控制进气口的打开与关闭； 所述 抽气口上设有抽气阀门， 用于控制抽气口的打开与关闭。
还包括控制装置， 用于控制所述进气阔门与抽气阀门的开与关。
还包括设置于腔体内的氧气传感器、 设置于腔体内的真空计， 所述氧 气传感器用于检测腔体内的氧气含量， 所述真空计用于检测腔体内的压 力。
所述加热装置包括底座。 设于底座上的加热线圈及设于底座上且位于 加热线圖外围的罩体， 所述加热线圈由铁铬铝合金、 或镍铬合金电热丝缠 绕制成； 所述底座与罩体均由金属制成， 该加热装置通过控制装置控制是 否进行加热。
所述罩体内安装有温度传感器， 用于检测加热装置的温度。
所述腔体内还设有照明装置， 且该腔体的一个侧壁上， 设有透明开 窗， 用于观察腔体内表面被氧化的金属镁的熔融状况。
还包括可拆卸安装于腔体内的内衬防着板。
所述^ 制装置安装于腔体上或集成于镀膜机上。
本发明还提供一种金属锾的预处理装置， 包括： 腔体、 安装于腔体内 的加热装置、 设于腔体上的进气口及设于腔体上的抽气口， 所述进气口与 外界的惰性气体注入设备相连通， 用于向腔体内注入惰性气体， 所述抽气 口与外部真空抽气装置相连通， 用于将腔体内抽成真空， 所述加热装置用 于加热表面被氧化的金属镁， 在真空环境下使得金属镁表面的一层氧化镁 挥发， 得到纯金属镁；
其中， 所述进气口上设置有进气阔门， 用于控制进气口的打开与关 闭； 所述抽气口上设有抽气阀门， 用于控制抽气口的打开与关闭；
还包括 ·控制装置， 用于控制所述进气阀门与抽气阀门的开与关； 还包括设置于腔体内的氧气传感器、 设置于腔体内的真空计， 所述氧 气传感器用于检测腔体内的氧气含量， 所述真空计用于检测腔体内的压 力；
其中， 所述加热装置包括底座、 设于底座上的加热线圈及设于底座上 且位于加热线圈外围的罩体， 所述加热线圈由铁铬铝合金、 或镍铬合金电 热丝缠绕制成； 所述底座与罩体均由金属制成， 该加热装置通过控制装置 控制是否进行加热。
所述罩体内安装有温度传感器， 用于检测加热装置的温度。
所述腔体内还设有照明装置， 且该腔体的一个侧壁上， 设有透明开 窗， 用于观察腔体内表面被氧化的金属镁的熔融状况。
还包括可拆卸安装于腔体内的内村防着板。
所述控制装置安装于腔体上或集成于镀膜机上。
本发明还提供一种金属镁的预处理方法， 包括以下步骤：
步骤 1、 提供预处理装置， 该预处理装置包括： 腔体、 安装于腔体内 的加热装置、 设于腔体上的进气口及设于腔体上的抽气口， 所述进气口与 外界的惰性气体注入设备相连通， 所述抽气口与外部真空抽气装置相连 通；
步骤 2、 将表面被氧化的金属镁置于坩埚内， 并将坩埚放置于加热装 置内； 步骤 3、 通过抽气口将腔体内抽成真空；
步骤 4、 通过进气口向腔体内注入惰性气体；
步骤 5、 重复步驟 3与步骤 4， 至腔体内的氧气含量小于 Ippm;
步骤 6、 通过抽气口将腔体内抽成真空， 使得腔体内的压强小于或等 于】0- 4Pa;
步骤 7、 通过加热装置加热表面被氧化的金属镁， 使得氧化镁完全挥 发；
步骤 8、 进行冷却后， 得到纯金属镁；
所述进气口上设置有进气阀门， 用于控制进气口的打开与关闭； 所述 抽气口上设有抽气阀门， 用于控制抽气口的打开与关闭；
所述预处理装置还包括控制装置， 用于控制所述进气阀门与抽气阀门 的开与关；
所述预处理装置还包括设置于腔体内的氧气传感器、 设置于腔体内的 真空计， 所述氧气传感器用于检测腔体内的氧气含量， 所述真空计用于检 测腔体内的压力；
所述加热装置包括底座、 设于底座上的加热线圈及设于底座上且位于 加热线圈外围的罩体， 所述加热线圈由铁鉻铝合金、 或镍铬合金电热丝缠 绕制成； 所述底座与罩体均由金属制成， 该加热装置通过控制装置控制是 否进行加热；
所述罩体内安装有温度传感器， 用于检测加热装置的温度；
所述腔体内还设有照明装置， 且该腔体的一个侧壁上， 设有透明开 窗， 用于观察腔体内表面被氧化的金属镁的熔融状况；
所述预处理装置还包括可拆卸安装于腔体内的内衬防着板；
所述控制装置安装于腔体上或集成于镀膜机上。
本发明的有益效果： 本发明的金属镁的预处理装置和方法， 通过前期 预处理可以除去金属镁颗粒表面的氧化镁， 且大大减小坩埚中金属锾外露 的表面积， 降低氧化镁的含量， 使得在镀膜腔体中， 只需预处理极少量的 氧化镁， 可以防止镀膜腔体被大量氧化镁污染， 并大大降低由氧化镁导致 的产品不良的机率； 且腔体无太多氧化镁， 可以降低停机保养的频率， 减 少内衬防着板更换的次数， 提高机器稼动率， 节省成本。
为了能更进一步了解本发明的特征以及技术内容， 请参阔以下有关本 发明的详细说明与附图， 然而附图仅提供参考与说明用， 并非用来对本发 明加以限制。 附图说明
下面结合附图， 通过对本发明的具体实施方式详细描述， 将使本发明 的技术方案及其它有益效果显而易见。
附图中，
图 1为本发明金属镁的预处理装置的立体结构示意图；
图 2为本发明金属镁的预处理装置的平面结构示意图；
图 3为本发明金属镁的预处理装置的加热装置的剖面结构示意图； 图 4为本发明金属镁的预处理方法的流程图；
图 5为氧化镁的固液-气转化曲线图。 具体实旅方式
为更进一步阐述本发明所采取的技术手段及其效果， 以下结合本发明 的优选实施例及其附图进行详 ·细描述.
请参阅图 i 至图 3， 本发明提供一种金属镁的预处理装置， 包括： 腔 体 20、 安装于腔体 20内的加热装置 22。 设于腔体 20上的进气口 24及设 于腔体 20上的抽气口 26， 所述进气口 24与外界的惰性气体注入设备（未 图示）相连通， 用于向腔体 20内注入惰性气体， 所述抽气口 26与外部真 空抽气装置 （未图示）相连通， 用于将腔体 20 内抽成真空， 所述加热装 置 22 用于加热表面被氧化的金属镁， 在真空环境下使得金属镁表面的一 层氧化镁挥发， 得到纯金属锾。 由于该预处理装置是将表面被氧化的金属 镁置于坩埚 （未图示） 中进行的， 在预处理完成后， 纯金属镁外露的表面 积小于或等于坩埚的开口面积， 即使暴露在空气中， 其也只能氧化该外露 的表面， 大大减小金属镁的氧化面积， 降低金属镁再次被氧化产生的氧化 镁的含量， 提高金属镁的纯度。
具体地， 所述进气口 24上设置有进气阀门 242, 用于控制进气口 24 的打开与关闭； 所述抽气 α 26 上设有抽气阀门 262， 用于控制抽气口 26 的打开与关闭， 该进气阀门 242与抽气阀门 262的开与关通过控制装置进 行控制， 在本实施例中， 控制装置为可编程逻辑控制器 （PLC ) , 其可直 接安装于腔体 20 上或集成于镀膜机（未图示）上， 在本实施例中， 所述 控制装置直接安装于腔体 20上， 并通过控制面板 40进行具体操作。
进一步地， 所述金属镁的预处理装置还包括设置于腔体 20 内的氧气 传感器 21、 设置于腔体 20 内的真空计 23， 所述氧气传感器 21 用于检测 腔体 20 内的氧气含量， 所述真空计 23用于检测腔体 20 内的压力， 进而 保证腔体 20 内的氧气含量与压力达到预定标准， 以保证预处理后的金属 镁的纯度。
所述加热装置 22包括底座 222、 设于底座 222上的加热线圈 224及设 于底座 222上且位于加热线圈 224外围的罩体 226, 所述加热线圈 224由 铁铬铝合金、 或镍铬合金电热丝缠绕制成； 所述底座 222与罩体 226均由 导热性能较高的金属制成， 该加热装置 22 通过控制装置控制是否进行加 热。 且， 所述罩体 226内安装有温度传感器 228 , 用于检测加热装置 22的 温度， 以便控制加热温度在预定范围内。
值得一提的是， 所述腔体 20内还设有照明装置 25， 且该腔体 20的一 个侧壁上， 设有透明开窗 27， 通过照明装置 25 的照射， 可以通过透明开 窗 27观察腔体 20内表面被氧化的金属镁的熔融状况。
进一步地， 所述金属镁的預处理装置还包括可拆卸安装于腔体 20 内 的内衬防着板 60, 供所述氧化镁挥发后附着， 以避免氧化镁直接酎着于腔 体的内壁上。 由于该内衬防着板 60 可拆卸， 当氧化镁附着到一定的量 时， 可将该内衬防着板 60 拆下进行清洗， 有效延长金属镁的预处理装置 的使用寿命。
请参阅图 4， 并参考图 〗 至图 3 , 本发明还提供一种金属镁的预处理 方法， 包括以下步骤：
步骤 1、 提供预处理装置， 该预处理装置包括： 腔体 20、 安装于腔体 20内的加热装置 22、 设于腔体 20上的进气口 24及设于腔体 20上的抽气 口 26, 所述进气口 24 与外界的惰性气体注入设备（未图示）相连通， 用 于向腔体 20内注入惰性气体， 所述抽气口 26与外部真空抽气装置 （未图 示）相连通， 用于将腔体 20内抽成真空， 所述加热装置 22用于加热表面 被氧化的金属镁， 在真空环境下使得金属镁表面的一层氧化镁挥发， 得到 纯金属镁。 由于该预处理装置是将表面被氧化的金属镁置于坩埚 （未图 示） 中进行的， 在预处理完成后， 纯金属镁外露的表面积小于或等于坩埚 的开口面积， 即使暴露在空气中， 其也只能氧化该外露的表面， 大大减小 金属镁的氧化面积， 降低金属镁再次被氧化产生的氧化镁的含量， 提高金 属镁的純度。
具体地， 所述进气口 24上设置有进气阀门 242, 用于控制进气口 24 的打开与关闭； 所述抽气口 26上设有抽气阀门 262 , 用于控制抽气口 26 的打开与关闭， 该进气阀门 242与抽气阀门 262的开与关通过控制装置进 行控制， 在本实施例中， 控制装置为可编程逻辑控制器 （PLC ) ， 其可直 接安装于腔体 20 上或集成于镀膜机（未图示）上， 在本实施例中， 所述 控制装置直接安装于腔体 20上， 并通过控制面板 40进行具体操作。 进一步地， 所述金属镁的预处理装置还包括设置于腔体 20 内的氧气 传感器 21、 设置于腔体 20 内的真空计 23 , 所述氧气传感器 21 用于检测 腔体 20 内的氧气含量， 所述真空计 23用于检测腔体 20 内的压力， 进而 保证腔体 20 内的氧气含量与压力达到预定标准， 以保证预处理后的金属 镁的纯度。
所述加热装置 22包括底座 222、 设于底座 222上的加热线圈 224及设 于底座 222上且位于加热线圈 224外围的罩体 226, 所述加热线圈 224由 铁铬铝合金， 或镍铬合金电热丝缠绕制成； 所述底座 222与罩体 226均由 导热性能较高的金属制成， 该加热装置 22 通过控制装置控制是否进行加 热。 且， 所述罩体 226内安装有温度传感器 228， 用于检测加热装置 22的 温度， 以便控制加热温度在预定范围内。
值得一提的是， 所述腔体 20内还设有照明装置 25， 且该腔体 20的一 个侧壁上， 设有透明开窗 27, 通过照明装置 25 的照射， 可以通过透明开 窗 27观察腔体 20内表面被氧化的金属镁的熔融状况。
进一步地， 所述金属镁的预处理装置还包括可拆卸安装于腔体 20 内 的内村防着板 60， 供所述氧化镁挥发后附着， 以避.免氧化镁直接附着于腔 体的内壁上。 由于该内衬防着板 60 可拆卸， 当氧化镁附着到一定的量 时， 可将该内衬防着板 60拆下进行清洗， 有效延长金属镁的预处理装置 的使用寿命。
步骤 2、 将表面被氧化的金属镁置于坩埚内， 并将坩埚放置于加热装 实际操作可为： 将采购的金属镁颗粒填入镀膜机使用的镁泔埚中， 由 于在生产及加工镁颗粒过程中， 不是全程在真空及惰性气体保护环境下进 行, 镁颗粒能与空气接触， 由于镁是很活泼的金属， 很容易被空气中的氧 气氧化， 表面形成一层氧化锾。
步骤 3、 通过抽气口 26将腔体 20内抽成真空。
具体地， 可通过干泵、 分子泵、 油泵、 低温泵或者不同泵的组合对腔 步骤 4、 通过进气口 24向腔体 20内注入惰性气体。
步骤 5、 重复步骤 3与步骤 4， 至腔体 20内的氧气含量小于 lppm。 步骤 6。 通过.抽气 α 26将腔体 20内抽成真空， 使得腔体 20内的压强 小于或等于 (T4Pa。
步骤 7、 通过加热装置 22加热表面被氧化的金属镁， 使得氧化镁完全 挥发。 请参阋图 5 , 其中， OB和 OC线分别表示气态与液态和固态相互转变 的临界线， 当气 /液和气 /固转变时体积变化很大， 随压力身高， 转变温度 也显著升高； OD表示液态与固态相互转变的临近线， 几乎与温度坐标垂 直， 压力变化对液 /固转变温度没有影响， 可知， 氧化镁在压强为 l(T4Pa， 温度为 450 - 600°C的环境下， 会自动挥发。
步骤 8、 进行冷却后， 得到纯金属镁。
进一步地， 把装有预处理好的镁的坩埚放入镀膜机的加热源中， 待镀 膜机腔体真空度到达 IE- 4 以下， 开始升温， 把表面及少量的氧化镁去 除， 然后就可以正常镀膜了。 此时坩埚中已无氧化镁， 在沉积形成阴极 时， 亦无氧化镁沉积到阴极上， 基本上消除了氧化镁导致的缺陷。
综上所述， 本发明的金属镁的预处理装置和方法， 通过前期预处理可 以除去金属镁颗粒表面的氧化镁， 且大大减小坩埚中金属镁外露的表面 积， 降低氧化锾的含量， 使得在镀膜腔体中， 只需预处理极少量的氧化 镁， 可以防止镀膜腔体被大量氧化镁污染， 并大大降低由氧化镁导致的产 品不良的机率； 且腔体无太多氧化镁， 可以降低停机保养的频率， 减少内 衬防着板更换的次数， 提高机器稼动率， 节省成本。
以上所述， 对于本领域的普通技术人员来说， 可以根据本发明的技术 方案和技术构思作出其他各种相应的改变和变形， 而所有这些改变和变形 都应属于本发明权利要求的保护范围。

Claims

一种金属镁的预处理装置， 包括： 腔体、 安装于腔体内的加热装 置、 设于腔体上的进气口及设于腔体上的抽气口， 所述进气口与外界的惰 性气体注入设备相连通， 用于向腔体内注入惰性气体， 所述抽气口与外部 真空抽气装置相连通， 用于将腔体内抽成真空， 所述加热装置用于加热表 面被氧化的金属镁， 在真空环境下使得金属镁表面的一层氧化镁挥发， 得 到纯金属镁。
2、 如权利要求 所述的金属镁的預处理装置， 其中， 所述进气口上 设置有进气阀门， 用于控制进气口的打开与关闭； 所述抽气口上设有抽气 阀门， 用于控制抽气口的打开与关闭。
3、 如权利要求 2 所述的金属镁的预处理装置， 还包括控制装置， 用 于控制所述进气阔门与抽气阀门的开与关。
4、 如权利要求 3 所述的金属镁的预处理装置， 还包括设置于腔体内 的氧气传感器、 设置于腔体内的真空计， 所述氧气传感器用于检测腔体内 的氧气含量， 所述真空计用于检测腔体内的压力。
5、 如权利要求 3 所述的金属镁的预处理装置， 其中， 所述加热装置 包括底座、 设于底座上的加热线圈及设于底座上且位于加热线圈外围的罩 体， 所述加热线圈由铁铬铝合金或镍铬合金电热丝缠绕制成； 所述底座与 罩体均由金属制成， 该加热装置通过控制装置控制是否进行加热。
6、 如权利要求 5 所述的金属镁的预处理装置， 其中， 所述罩体内安 装有温度传感器， 用于检测加热装置的温度。
7、 如权利要求 1 所述的金属镁的预处理装置， 其中， 所述腔体内还 设有照明装置， 且该腔体的一个侧壁上设有透明开窗， 用于观察腔体内表 面被氧化的金属镁的熔融状况。
8、 如权利要求 所述的金属镁的預处理装置， 还包括可拆卸安装于 腔体内的内衬防着板。
9、 如权利要求 3 所述的金属镁的预处理装置， 其中， 所述控制装置 安装于腔体上或集成于镀膜机上。
10、 一种金属镁的预处理装置， 包括： 腔体、 安装于腔体内的加热装 置、 设于腔体上的进气口及设于腔体上的抽气口， 所述进气口与外界的惰 性气体注入设备相连通， 用于向腔体内注入惰性气体， 所述抽气口与外部 真空抽气装置相连通， 用于将腔体内抽成真空， 所述加热装置用于加热表 面被氧化的金属镁， 在真空环境下使得金属镁表面的一层氧化镁挥发， 得 到纯金属镁；
其中， 所述进气口上设置有进气阀门， 用于控制进气口的打开与关 闭； 所述抽气口上设有抽气阀门， 用于控制抽气口的打开与关闭；
还包括控制装置， 用于控制所述进气阀门与抽气阀 Π的开与关； 还包括设置于腔体内的氧气传感器、 设置于腔体内的真空计， 所述氧 气传感器用于检测腔体内的氧气含量， 所述真空计用于检测腔体内的压 力；
其中， 所述加热装置包括底座、 设于底座上的加热线圈及设于底座上 且位于加热线圈外围的罩体， 所述加热线圈由铁铬铝合金或镍铬合金电热 丝缠绕制成； 所述底座与罩体均由金属制成， 该加热装置通过控制装置控 制是否进行加热。
11、 如权利要求 10 所述的金属镁的预处理装置， 其中， 所述罩体内 安装^ Γ温度传感器， 用于检测加热装置的温度。
12、 如权利要求 10 所述的金属镁的预处理装置， 其中， 所述腔体内 还设有照明装置， 且该腔体的一个侧壁上设有透明开窗， 用于观察腔体内 表面被氧化的金属镁的熔融状况。
13、 如权利要求 10 所述的金属锾的预处理装置， 还包括可拆卸安装 于腔体内的内衬防着板。
14、 如权利要求 10 所述的金属镁的预处理装置， 其中， 所述控制装 置安装于腔体上或集成于镀膜机上。
15 , 一种金属镁的预处理方法， 包括以下步骤：
步骤 1、 提供预处理装置， 该预处理装置包括： 腔体 安装于腔体内 的加热装置， 设于腔体上的进气口及设于腔体上的抽气口， 所述进气口与 外界的'隋性气体注入设备相连通， 所述抽气口与外部真空抽气装置相连 通；
步骤 2、 将表面被氧化的金属镁置于坩埚内， 并将坩埚放置于加热装
3：-' L .
L ,
步糠 3、 通过抽气口将腔体内抽成真空；
步骤 4、 通过进气口向腔体内注入惰性气体；
步骤 5、 重复步骤 3与步骤 4， 至腔体内的氧气含量小于 Ippm;
步骤 6、 通过抽气口将腔体内抽成真空， 使得腔体内的压强小于或等 于 liO-4Pa;
步骤 7、 通过加热装置加热表面被氧化的金属镁， 使得氧化镁完全挥 发；
步骤 8、 进行冷却后， 得到纯金属镁；
所述进气口上设置有进气阀门， 用于控制进气口的打开与关闭； 所述 抽气口上设有抽气阀 Π， 用于控制抽气口的打开与关闭；
所述预处理装置还包括控制装置， 用于控制所述进气阀门与抽气阀门 的开与关；
所述预处理装置还包括设置于腔体内的氧气传感器、 设置于腔体内的 真空计， 所述氧气传感器用于检测腔体内的氧气含量， 所述真空计用于检 测月空体内的压力；
所述加热装置包括底座、 设于底座上的加热线圈及设于底座上且位于 加热线圖外围的罩体， 所述加热线圈由铁铬铝合金、 或镍铬合金电热丝缠 绕制成； 所述底座与罩体均由金属制成， 该加热装置通过控制装置控制是 否进行加热；
所述罩体内安装有温度传感器， 用于检测加热装置的温度；
所述腔体内还设有照明装置， 且该腔体的一个侧壁上设有透明开窗， 用于观察腔体内表面被氧化的金属镁的熔融状¾;
所述预处理装置还包括可拆卸安装于腔体内的内村防着板；
所述.控制装置安装于腔体上或集成于镀膜机上。
PCT/CN2014/070934 2013-12-31 2014-01-21 金属镁的预处理装置和方法 Ceased WO2015100812A1 (zh)

Priority Applications (4)

Application Number Priority Date Filing Date Title
KR1020167014127A KR101746359B1 (ko) 2013-12-31 2014-01-21 금속 마그네슘의 전처리 장치 및 방법
JP2016533601A JP6208871B2 (ja) 2013-12-31 2014-01-21 金属マグネシウムの予備処理装置と方法
US14/348,703 US9340851B2 (en) 2013-12-31 2014-01-21 Device and method for preprocessing metallic magnesium
GB1607192.0A GB2535065B (en) 2013-12-31 2014-01-21 Method for preprocessing metallic magnesium

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201310753927.8 2013-12-31
CN201310753927.8A CN103740949B (zh) 2013-12-31 2013-12-31 金属镁的预处理装置和方法

Publications (1)

Publication Number Publication Date
WO2015100812A1 true WO2015100812A1 (zh) 2015-07-09

Family

ID=50498013

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2014/070934 Ceased WO2015100812A1 (zh) 2013-12-31 2014-01-21 金属镁的预处理装置和方法

Country Status (6)

Country Link
US (1) US9340851B2 (zh)
JP (1) JP6208871B2 (zh)
KR (1) KR101746359B1 (zh)
CN (1) CN103740949B (zh)
GB (1) GB2535065B (zh)
WO (1) WO2015100812A1 (zh)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11459651B2 (en) 2017-02-07 2022-10-04 Applied Materials, Inc. Paste method to reduce defects in dielectric sputtering
CN106957968B (zh) * 2017-05-27 2019-09-10 郑州大学 一种冶炼镁金属的还原罐
CN113091413B (zh) * 2021-04-30 2022-06-10 Tcl华星光电技术有限公司 真空干燥装置
CN114959628A (zh) * 2022-06-18 2022-08-30 安徽纯源镀膜科技有限公司 一种真空离子镀膜预处理设备

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4238224A (en) * 1979-06-25 1980-12-09 Societa Italiana per Il Magnesesio E Leghe Di Magnesio S.p.A. Continuous extraction of magnesium from magnesium oxides
US4518425A (en) * 1983-12-20 1985-05-21 University Of Waterloo Production of magnesium metal
US5090996A (en) * 1987-07-10 1992-02-25 University Of Manchester Institute Of Science And Technology Magnesium production
CN101386919A (zh) * 2008-10-24 2009-03-18 贵阳铝镁设计研究院 一种高纯镁的制备方法及装置
WO2011153683A1 (zh) * 2010-06-07 2011-12-15 Niu Qiang 一种真空环流硅热法制金属镁的方法及其设备

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2309644A (en) * 1938-12-24 1943-02-02 Anglo California Nat Bank Sublimation apparatus
US3565410A (en) * 1968-09-06 1971-02-23 Midland Ross Corp Vacuum furnace
GB1480778A (en) * 1974-10-03 1977-07-27 Gray & Co Inc R Method of treating articles under vacuum conditions with external gas flow
US5128515A (en) * 1990-05-21 1992-07-07 Tokyo Electron Sagami Limited Heating apparatus
JP3338757B2 (ja) * 1997-01-23 2002-10-28 神鋼電機株式会社 真空溶解装置の蒸着防止板
JP4734852B2 (ja) * 2004-06-02 2011-07-27 シンフォニアテクノロジー株式会社 精錬方法及び精錬装置
DE112008002890T5 (de) * 2007-10-31 2010-09-16 ULVAC, Inc., Chigasaki-shi Verfahren zur Herstellung eines Permanentmagneten und Permanentmagnet
CN104204306A (zh) * 2011-10-07 2014-12-10 英菲纽姆股份有限公司 用氧化物电解有效生产金属和蒸馏的方法和设备
EP2804964B1 (de) * 2012-01-19 2019-07-31 ETH Zuerich Verfahren und vorrichtung zur vakuumdestillation von hochreinem magnesium

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4238224A (en) * 1979-06-25 1980-12-09 Societa Italiana per Il Magnesesio E Leghe Di Magnesio S.p.A. Continuous extraction of magnesium from magnesium oxides
US4518425A (en) * 1983-12-20 1985-05-21 University Of Waterloo Production of magnesium metal
US5090996A (en) * 1987-07-10 1992-02-25 University Of Manchester Institute Of Science And Technology Magnesium production
CN101386919A (zh) * 2008-10-24 2009-03-18 贵阳铝镁设计研究院 一种高纯镁的制备方法及装置
WO2011153683A1 (zh) * 2010-06-07 2011-12-15 Niu Qiang 一种真空环流硅热法制金属镁的方法及其设备

Also Published As

Publication number Publication date
KR101746359B1 (ko) 2017-06-12
GB2535065B (en) 2021-02-10
KR20160077177A (ko) 2016-07-01
CN103740949B (zh) 2015-02-04
JP2017508062A (ja) 2017-03-23
JP6208871B2 (ja) 2017-10-04
GB2535065A (en) 2016-08-10
US20150247217A1 (en) 2015-09-03
CN103740949A (zh) 2014-04-23
US9340851B2 (en) 2016-05-17

Similar Documents

Publication Publication Date Title
JP6117998B2 (ja) フレキシブルｏｌｅｄパネルの製造方法
JP2007227086A (ja) 成膜装置および発光素子の製造方法
WO2015100812A1 (zh) 金属镁的预处理装置和方法
JP6280234B2 (ja) 有機電界発光素子及びその制作方法
WO2020258395A1 (zh) 一种有机电致发光器件及显示面板
CN102983284A (zh) 一种具有弱视角效应的顶发射白光有机电致发光器件
CN102185120B (zh) 手套箱装置及工件传输的方法
CN107267920A (zh) 蒸镀设备、坩埚及蒸镀方法
CN201243391Y (zh) 一种有机电致发光显示器
WO2016123853A1 (zh) 蒸镀换料一体化设备及其使用方法
US20170222185A1 (en) Organic electroluminescent display substrate, organic electroluminescent display apparatus, and method for manufacturing organic electroluminescent display apparatus
CN203956935U (zh) 手套箱密封装置
TWI569492B (zh) 有機發光元件
CN201778107U (zh) 镀膜基片前置处理装置
KR20110124429A (ko) 유기박막 증착장치 및 이를 이용한 유기전계발광소자의 제조방법
CN112063988A (zh) 一种金属处理设备及驱动方法
JP2012156073A (ja) 真空蒸着装置、有機エレクトロルミネッセンス素子の製造方法及び有機エレクトロルミネッセンス素子
JP6228444B2 (ja) 有機ｅｌ表示装置およびその製造方法
CN104593730B (zh) 防止oled材料裂解的坩埚
CN104752621B (zh) 一种提高有源矩阵有机发光显示器显示质量的方法
KR100773403B1 (ko) 증착 장치 및 그 증착 장치의 점증발원 배열 방법
KR20150025730A (ko) 유기전계 발광소자 제조방법
KR101920759B1 (ko) 유기 발광 표시장치의 제조방법
CN103296059A (zh) 有源矩阵有机电致发光显示器件及其制备方法
KR102045374B1 (ko) 상부 발광형 유기 발광 소자 및 그의 제조방법

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 14348703

Country of ref document: US

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 14876170

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 201607192

Country of ref document: GB

Kind code of ref document: A

Free format text: PCT FILING DATE = 20140121

WWE Wipo information: entry into national phase

Ref document number: 1607192

Country of ref document: GB

ENP Entry into the national phase

Ref document number: 2016533601

Country of ref document: JP

Kind code of ref document: A

ENP Entry into the national phase

Ref document number: 20167014127

Country of ref document: KR

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 14876170

Country of ref document: EP

Kind code of ref document: A1