CN106929809A - A kind of continuous producing apparatus for micro-nano powder plated film and preparation method thereof - Google Patents

A kind of continuous producing apparatus for micro-nano powder plated film and preparation method thereof Download PDF

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Publication number
CN106929809A
CN106929809A CN201511020346.9A CN201511020346A CN106929809A CN 106929809 A CN106929809 A CN 106929809A CN 201511020346 A CN201511020346 A CN 201511020346A CN 106929809 A CN106929809 A CN 106929809A
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CN
China
Prior art keywords
plated film
micro
belt
nano powder
target
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Pending
Application number
CN201511020346.9A
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Chinese (zh)
Inventor
唐晓峰
逯琪
董建廷
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SHANGHAI LANGYI NEW MATERIAL TECHNOLOGY Co Ltd
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SHANGHAI LANGYI NEW MATERIAL TECHNOLOGY Co Ltd
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Priority to CN201511020346.9A priority Critical patent/CN106929809A/en
Publication of CN106929809A publication Critical patent/CN106929809A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks

Abstract

The present invention relates to a kind of continuous producing apparatus for micro-nano powder plated film and preparation method thereof, the equipment includes storage bin (1), continuous blanking device (2), Transmission system (3), magnetic control sputtering device (4), vacuum cavity (5), receiving warehouse (6), extract system (7) and gas handling system (8).Can realize that technique diversity changes and product coating stability to micro-nano powder plated film by the equipment.

Description

A kind of continuous producing apparatus for micro-nano powder plated film and preparation method thereof
Technical field:
The present invention relates to a kind of continuous producing apparatus of powder plated film and preparation method thereof, it is particularly suited for micro-nano Continuous producing apparatus of powder magnetic control sputtering single or multiple lift plated film and preparation method thereof.
Background technology:
With the progress and the development of material industry of science and technology, the surface coating modification technology of micro-nano powder is gradually It is applied to the every aspect of industry, such as cell catalyst, powder photocatalyst.Conventional powder surface plated film Handling process is including chemical plating, chemical gel method, magnetron sputtering plating etc..The plated film sides such as chemical plating, gel method Formula, due to the particularity of its technique, inevitably produces the pollutants such as waste gas, waste water in production process, right The harm of environment is serious, is disagreed with the national environmental protection theory advocated at present, certainly will be taken by other techniques Generation.Magnetron sputtering technique is a kind of physical gas-phase deposite method, and coating medium is in vacuum system by sputtering Process deposits form coating in powder surface, and pilot process is produced without waste liquid or waste gas, is a kind of safety and environmental protection Production technology.
But the specific surface area and surface due to micro-nano powder itself can be than larger, and radius of curvature is small, powder it Between be susceptible to reunite etc. phenomenon, if pass through simple dispersing mode, it is impossible to realize the uniformity of powder plated film, Thus realize that uniform coated treatment has certain difficulty on micro-nano powder surface.
In existing powder filming equipment, more using drum-type plated film mode, plating is realized during separation descends slowly and lightly Film.The coating process reappearance is not high, belongs to semi-successive cultivation device, and pilot process monitoring means are limited, nothing Method ensures the homogeneity of powder plated film;Simultaneously because inside configuration target Limited Number, it is impossible to realize multicoating Technique.Therefore seek a kind of to realize that the change of technique diversity and the equipment of product coating stability are a necessity And promising work.
The content of the invention:
The present invention proposes a kind of continuous production device of single or multiple lift plated film for micro-nano powder, laterally On powder is laid in conveyer belt, control plated film time using the speed of conveyer belt;On longitudinal direction, using vibration The shake and dispersion of motor and ultrasonic wave co- controlling powder, the effective homogeneity for improving powder plated film.Due to It is that two dimensions are individually controlled, is more beneficial for realizing diversity change and the stability of product coating of technique.Target The species of material and position can be changed easily, realize MULTILAYER COMPOSITE plated film.
A kind of continuous producing apparatus for micro-nano powder plated film of the present invention, as shown in Figure 1.This sets It is standby to include storage bin (1), continuous blanking device (2), Transmission system (3), magnetic control sputtering device (4), vacuum Cavity (5), receiving warehouse (6), extract system (7) and gas handling system (8).
Transmission system (3) includes belt conveyor and belt vibration device, is installed in vacuum cavity (5) The lower section of the magnetic control sputtering device (4) in portion.Belt conveyor by frame, roller bearing, motor, speed changer, Liner plate is constituted.Belt vibration device is assemblied in belt conveyor liner plate or frame, and vibration can be by vibrating electricity Machine or ultrasonic vibration generator are realized.
Magnetic control sputtering device (4) includes sputtering target, shielding power supply, cooling water channel, sealing system.Magnetic control splashes Injection device (4) is assemblied in vacuum cavity (5) upper wall.Sputtering target is assemblied in vacuum cavity top, number side by side And species can be changed according to demand.
Storage bin (1) and receiving warehouse (6) are realized equipped with slightly taking out room, essence takes out room and corresponding vacuum system Continuous feed and storing in production process.Storage bin is equipped with corresponding control blanking velocity device, can be by regulation Feed opening bore gap or screw feeding device realize control.
Extract system (7) includes diffusion pump, molecular pump, lobe pump, sliding vane rotary pump, vacuum suction pipeline, gas Movable valve etc., gas handling system (8) includes gas cylinder, gas piping, gas flowmeter.
Set using a kind of continuous prodution of single or multiple lift plated film for micro-nano powder proposed by the present invention The process of standby plated film is as follows:
1) species and number of target needed for the position assembling in magnetic control sputtering device (4) magnetic control target;
2) to the micro-nano powder base-material that target grain size is added in storage bin (1);
3) vacuum cavity (5) chamber door is closed, extract system (7) is opened, pressure needed for technique is evacuated to, Gas cylinder needed for opening, adjusting gas flow technological parameter controls cavity vacuum, opens shielding power supply, regulation The sputtering current size of each magnetic control handle;
4) belt conveyor is opened, belt horizontal feed speed is controlled, vertical direction belt vibration device is opened Power supply.Powder is trickled down to Belt Conveying belt surface, belt drive powder from storage bin (1) with certain speed It is delivered to sputter area;During Belt Conveying, in the presence of vibrating device, realization is rolled up and down, it is ensured that Each face of all powders can realize uniform coated;
5) after the completion of plated film, powder drops down onto receiving warehouse (6) under conveyor belt surface.
Wherein, step 1) structure of the target can be divided into piece type, rotational circle column type;The material of target includes Metal simple-substance target, alloys target and other targets.Metal simple-substance target include gold, silver, copper, iron, aluminium, platinum, chromium, Nickel, zinc, titanium, zirconium, tin, lead, magnesium, antimony, cobalt, indium etc., alloys target are mixed with by all kinds of elemental metals Obtain;Other targets include the compound that above-mentioned one or more elemental metals are formed with oxygen, nitrogen, carbon.
Step 2) the micro-nano powder base-material include man-made glass, quartz sand, enamel, alundum (Al2O3), Aluminium nitride, cubic boron nitride, carborundum, calcite etc..The particle size range of the micro-nano powder is 100 Nanometer~60 microns.
Step 3) gaseous species include helium, neon, argon gas, Krypton, nitrogen, oxygen, methane, Acetylene, chlorination fluorine etc..The chamber vacuum degree control is 1.5~6.1 × 10-1Pa.The shielding power supply includes straight Stream power supply, intermediate frequency power supply, radio-frequency power supply, multi sphere ion power supply etc..The sputtering current size is 5A~8A.
Step 4) the belt horizontal feed velocity interval spills for powder described in 0.01~10m/min from storage bin The speed for dropping down onto Belt Conveying belt surface is 200~1500g/min.
The operation that raw material is required supplementation with coating process or finished product is taken out can smoke room and cavity by slightly smoking room, essence With the use of realization.Meanwhile, if MULTILAYER COMPOSITE plated film need to be realized, can be by changing position and the species reality of target It is existing.
Brief description of the drawings
Fig. 1 is equipment schematic diagram.
1. storage bin;2. continuous blanking device;3. Transmission system;4. magnetic control sputtering device;5. vacuum cavity;6. rewinding Storehouse.
Fig. 2 is vacuum system figure.
5. vacuum cavity;7. extract system;8. gas handling system.
Specific embodiment
Embodiment 1
In 1~No. 8 assembling slice type aluminium target of magnetic control target, to the quartz sand that 10~30 microns of particle diameter is added in storage bin, Vacuum cavity chamber door is closed, vacuum-pumping system is opened, 4.3 × 10 are evacuated to-3Pa, is passed through 50sccm pure The argon gas for 99.999% is spent, chamber vacuum degree is controlled 1.5 × 10-1Pa.1~No. 8 aluminium target intermediate frequency power supply is opened, Regulation electric current is 8A.Belt conveyor is opened, belt horizontal feed speed is controlled for 0.5m/min, control Blanking velocity is 250g/min, opens vertical vibration motor power, and powder passes through aluminium target by tape transport Sputtering zone.After the completion of powder plated film, shielding power supply, vacuum system, conveying device and vibrating device, chamber are closed Body leads to air, opens chamber door, and 10~30 microns of quartz sand particles of aluminizing are obtained by receiving warehouse.
Embodiment 2
In 1~No. 4 assembling cylindrical type aluminium target of magnetic control target, 5~No. 8 assembling cylindrical type copper targets are added in storage bin The calcite that 20~50 microns of particle diameter, closes vacuum cavity chamber door, opens vacuum-pumping system, is evacuated to 6.7×10-3Pa, is passed through the argon gas that 60sccm purity is 99.999%, and chamber vacuum degree is controlled 2.1 × 10-1Pa。 1~No. 4 aluminium target dc source is opened, regulation electric current is 6A;Open 5~No. 8 copper target dc sources, regulation electricity It is 5A to flow.Belt conveyor is opened, belt horizontal feed speed is controlled for 0.25m/min, control blanking speed It is 300g/min to spend, and opens vertical direction ultrasonic vibration generator power supply, and powder is led to successively by tape transport Cross aluminium target sputtering zone and copper target sputtering zone.After the completion of powder plated film, shielding power supply, vacuum system, conveying are closed Device and vibrating device, cavity lead to air, open chamber door, and obtaining 20~50 microns of Solder for Al-Cu Joint Welding by receiving warehouse is combined Plating calcite particle.
Embodiment 3
In 1~No. 6 assembling cylindrical type titanium target of magnetic control target, to three oxidations that 40~60 microns of particle diameter is added in storage bin Two aluminium, close vacuum cavity chamber door, open vacuum-pumping system, are evacuated to 6.7 × 10-3Pa, is passed through 60sccm Purity is 99.999% argon gas, and 50sccm purity is 99.999% nitrogen, and the control of chamber vacuum degree exists 6.1×10-1Pa.1~No. 6 titanium target dc source is opened, regulation electric current is 6A, opens belt conveyor, control Belt horizontal feed speed processed is 0.25m/min, controls blanking velocity for 200g/min, opens vertical direction and shakes Dynamic motor power, titanium target sputtering zone is passed sequentially through by tape transport.In sputter procedure, titanium metal ions and nitrogen Solid/liquid/gas reactions, in particle form of expression titanium nitride coating.After the completion of powder plated film, shielding power supply, vacuum system are closed System, conveying device and vibrating device, cavity lead to air, open chamber door, and 40~60 microns of nitrogen are obtained by receiving warehouse Change titanium plated film alundum (Al2O3) particle.
Embodiment 4
In 1~No. 8 assembling slice type titanium dioxide titanium target of magnetic control target, to adding the vertical of 10~30 microns of particle diameter in storage bin Square boron nitride, closes vacuum cavity chamber door, opens vacuum-pumping system, is evacuated to 4.3 × 10-3Pa, is passed through 50sccm purity is 99.999% argon gas, and chamber vacuum degree is controlled 1.5 × 10-1Pa.Open 1~No. 8 aluminium target Radio-frequency power supply, regulation electric current is 8A, opens belt conveyor, controls the belt horizontal feed speed to be 0.5m/min, controls blanking velocity for 250g/min, opens vertical vibration motor power, defeated by conveyer belt Send and pass sequentially through titanium dioxide titanium target sputtering zone.After the completion of powder plated film, shielding power supply, vacuum system, defeated is closed Send device and vibrating device, cavity to lead to air, open chamber door, 10~30 hum silicon dioxide titaniums are obtained by receiving warehouse Plated film cubic boron nitride particle.

Claims (6)

1. a kind of continuous producing apparatus for micro-nano powder plated film, including storage bin (1), continuous blanking device (2), magnetic control sputtering device (4), vacuum cavity (5), receiving warehouse (6), extract system (7), air inlet system System (8), it is characterised in that:Also include the Transmission system with belt conveyor and belt vibration device (3), the Transmission system (3) is installed under the internal magnetic control sputtering device (4) of vacuum cavity (5) Side.
2. a kind of continuous producing apparatus for micro-nano powder plated film according to claim 1, its feature exists In:The gas handling system (8) includes gas cylinder, gas piping, gas flowmeter, and the species of air inlet is included Helium, neon, argon gas, Krypton, nitrogen, oxygen, methane, acetylene, chlorination fluorine.
3. a kind of continuous producing apparatus for micro-nano powder plated film according to claim 1, its feature exists In:The belt conveyor includes frame, roller bearing, motor, speed changer and liner plate.
4. a kind of continuous producing apparatus for micro-nano powder plated film according to claim 1, its feature exists In:The belt vibration device is assemblied in the liner plate of belt conveyor or frame, and vibrating device includes Vibrating motor or ultrasonic vibration generator.
5. a kind of continuous producing apparatus for micro-nano powder plated film according to claim 1, its feature exists In:The magnetic control sputtering device (4) is assemblied in vacuum cavity (5) top, including target, target side by side Frame, shielding power supply, cooling water channel and sealing system.
6. equipment described in a kind of utilization claim 1 is as follows to the preparation method of micro-nano powder plated film:
1) species and number of target needed for the position assembling in magnetic control sputtering device (4) magnetic control target;
2) to the micro-nano powder base-material that target grain size is added in storage bin (1);
3) vacuum cavity (5) chamber door is closed, extract system (7) is opened, pressure needed for technique is evacuated to, Gas cylinder needed for opening, adjusting gas flow technological parameter controls cavity vacuum, opens shielding power supply, Adjust the sputtering current size of each magnetic control handle;
4) belt conveyor is opened, belt horizontal feed speed is controlled, vertical direction belt vibration device is opened Power supply, powder is trickled down to Belt Conveying belt surface, belt drive powder from storage bin (1) with certain speed Body is delivered to sputter area;During Belt Conveying, in the presence of vibrating device, realization is rolled up and down, Ensure that each face of all powders can realize uniform coated;
5) after the completion of plated film, powder drops down onto receiving warehouse (6) under conveyor belt surface.
CN201511020346.9A 2015-12-30 2015-12-30 A kind of continuous producing apparatus for micro-nano powder plated film and preparation method thereof Pending CN106929809A (en)

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Application Number Priority Date Filing Date Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108483557A (en) * 2018-05-09 2018-09-04 天津大学 High energy ionizes the device of cooperative photocatalysis processing electroplating wastewater
CN109702344A (en) * 2019-01-25 2019-05-03 大连理工大学 Hot arc and laser composite heat power supply evaporate Multicarity nano powder preparing device
CN112992690A (en) * 2021-02-08 2021-06-18 杭州航鹏机电科技有限公司 Integrated circuit manufacturing process
CN113445018A (en) * 2021-06-29 2021-09-28 山东三齐能源有限公司 Magnetron sputtering-based shielding conductive film layer preparation equipment and method
CN114855126A (en) * 2022-06-02 2022-08-05 西安稀有金属材料研究院有限公司 Device and method for modifying surface of micro-nano powder

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010042839A1 (en) * 2010-10-22 2012-04-26 Von Ardenne Anlagentechnik Gmbh Method for operating target in continuous vacuum coating installation, has movable covering that is provided above the transport unit, for covering the substrate provided on the transport unit
CN202246846U (en) * 2011-07-08 2012-05-30 王殿儒 Horizontal reciprocating type ion film plating machine for plating ceramics by physical vapor deposition method
CN205275692U (en) * 2015-12-30 2016-06-01 上海朗亿功能材料有限公司 A continuous production equipment for declining nanometer powder coating film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102010042839A1 (en) * 2010-10-22 2012-04-26 Von Ardenne Anlagentechnik Gmbh Method for operating target in continuous vacuum coating installation, has movable covering that is provided above the transport unit, for covering the substrate provided on the transport unit
CN202246846U (en) * 2011-07-08 2012-05-30 王殿儒 Horizontal reciprocating type ion film plating machine for plating ceramics by physical vapor deposition method
CN205275692U (en) * 2015-12-30 2016-06-01 上海朗亿功能材料有限公司 A continuous production equipment for declining nanometer powder coating film

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴宏富: "《中国粉体工业通鉴 第3卷 2007版》", 31 August 2007 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108483557A (en) * 2018-05-09 2018-09-04 天津大学 High energy ionizes the device of cooperative photocatalysis processing electroplating wastewater
CN109702344A (en) * 2019-01-25 2019-05-03 大连理工大学 Hot arc and laser composite heat power supply evaporate Multicarity nano powder preparing device
CN109702344B (en) * 2019-01-25 2023-12-29 大连理工大学 Thermal arc and laser composite heat source evaporation multi-cavity nano powder preparation device
CN112992690A (en) * 2021-02-08 2021-06-18 杭州航鹏机电科技有限公司 Integrated circuit manufacturing process
CN112992690B (en) * 2021-02-08 2024-03-19 杭州航鹏机电科技有限公司 Integrated circuit manufacturing process
CN113445018A (en) * 2021-06-29 2021-09-28 山东三齐能源有限公司 Magnetron sputtering-based shielding conductive film layer preparation equipment and method
CN114855126A (en) * 2022-06-02 2022-08-05 西安稀有金属材料研究院有限公司 Device and method for modifying surface of micro-nano powder
CN114855126B (en) * 2022-06-02 2023-10-27 西安稀有金属材料研究院有限公司 Device and method for modifying surface of micro-nano powder

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Application publication date: 20170707