CN110747493B - Method for producing electrolytic nickel material by barrel plating method - Google Patents

Method for producing electrolytic nickel material by barrel plating method Download PDF

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Publication number
CN110747493B
CN110747493B CN201810820772.8A CN201810820772A CN110747493B CN 110747493 B CN110747493 B CN 110747493B CN 201810820772 A CN201810820772 A CN 201810820772A CN 110747493 B CN110747493 B CN 110747493B
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electrolytic
nickel
barrel plating
main
electrolytic nickel
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CN110747493A (en
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张�浩
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Shanghai Ruifu Nonferrous Metal Co ltd
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Shanghai Ruifu Nonferrous Metal Co ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/16Apparatus for electrolytic coating of small objects in bulk
    • C25D17/18Apparatus for electrolytic coating of small objects in bulk having closed containers
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/06Filtering particles other than ions
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/12Process control or regulation
    • C25D21/14Controlled addition of electrolyte components
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/562Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Automation & Control Theory (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Abstract

The conventional rack plating electroplating method needs to use a cathode template in production, but the cathode plate cannot be recycled and the labor cost is high in the process of processing and manufacturing the cathode plate. The invention provides a novel production method, which is used for producing electrolytic nickel materials by a barrel plating method. And adding the configured electrolyte into a main electrolytic tank of the barrel plating device, controlling voltage and current, taking out the electrolytic nickel material when the starting material of the electrolytic nickel material grows to a specified size, and cleaning, drying and packaging the electrolytic nickel material.

Description

Method for producing electrolytic nickel material by barrel plating method
Technical Field
The invention relates to a method for preparing an electrolytic nickel material with a nickel cake, a nickel button or other shapes by using a barrel plating method, which belongs to the field of nonferrous metal processing and is mainly applied to the industry of producing metal materials by an electrolytic method.
Background
At present, the electrolytic nickel anode material is mainly produced by a rack plating method. Taking the preparation of the button-shaped nickel anode material as an example, the process is approximately as follows: the method comprises the steps of taking a nickel material as an anode, adding the nickel material into a titanium anode basket, taking a stainless steel plate or a titanium plate as a cathode substrate, designing and processing a special cathode template according to the shape and growth rule of the button-shaped nickel anode material, carrying out electroplating production in an electrolyte in a rack plating mode, hanging out the cathode plate after the product grows to the required size or weight, cleaning and packaging.
The rack plating method for producing the nickel anode material requires the preparation of a cathode plate in advance, and the cathode plate is usually disposable. After the electroplating production is finished once, the insulating material on the surface of the cathode plate needs to be processed and remanufactured again before being used again. The manufacturing and processing of the cathode plate are a very complicated process, and waste time and materials, which causes the increase of the production cost. And the nickel buttons grown on the treated cathode plate may also cause problems such as poor local conductivity of the metal substrate, irregular growth shape of the nickel buttons, and the like due to the difficulty in controlling the coating quality. Resulting in the problems of low finished product qualification rate, high production cost, lack of market competitiveness and the like.
Disclosure of Invention
Technical problem to be solved by the invention
The invention provides a novel production method, which is used for producing electrolytic nickel materials by a barrel plating method.
Means for solving the problems
To solve the above problems, the present invention comprises:
a method for producing an electrolytic nickel material by a barrel plating method is characterized by comprising the following steps:
(1) adding the electrolyte into a main electrolytic bath of a barrel plating device, and starting circulating filtration and heating;
(2) adding a starting electrode seed material for electrolytic nickel to be plated into a roller of a barrel plating device, wherein the roller is connected with a circuit cathode, and a main electrolytic bath anode is connected with a circuit anode;
(3) and controlling the voltage interval of the main electrolytic tank to be 1-4V, and gradually increasing the voltage along with the growth time of the starting electrode seed material for the electrolytic nickel after keeping for 24 hours, wherein the voltage interval is 4-8V.
Furthermore, the barrel plating device comprises a main electrolytic tank, a roller and a motor, wherein the roller is obliquely arranged in the main electrolytic tank, and the motor is connected with the roller.
Furthermore, the barrel plating device also comprises an auxiliary electrolytic tank.
Furthermore, the electrolyte is subjected to chemical impurity removal or low-current electrolytic impurity removal and then is added into the auxiliary electrolytic tank and the main electrolytic tank.
Further, the small current electrolysis impurity removal process comprises the following steps: electrolysis with a corrugated cathode plate with a cathodic current density of: 0.2-0.8A/dm 2.
Further, the electrolyte used in the production method for producing the electrolytic nickel material by the barrel plating method is as follows: the nickel sulfamate system electrolytic solution comprises the following components: nickel sulfamate: 200-600g/L, nickel chloride: 3-20g/L, boric acid: 25-40 g/L. Regulating pH value of the solution to 2.5-4.5 with sulfamic acid or nickel carbonate at 40-60 deg.c.
Further, the electrolyte used in the production method for producing the electrolytic nickel material by the barrel plating method is as follows: nickel sulfate system electrolytic solution: the main components are as follows: nickel sulfate: 200-400g/L, nickel chloride: 3-20g/L, boric acid: 25-40 g/L. The pH value is controlled between 2.0 and 4.5 and the temperature is controlled between 40 and 65 ℃ when the device works.
Furthermore, the electrolytic nickel material can be sulfur-containing electrolytic nickel, and the sulfur content in the sulfur-containing electrolytic nickel is controlled to be 0.015-0.040%.
Further, the content of sulfur in the electrolytic nickel material is controlled by adding additives into the auxiliary electrolytic tank.
Further, the auxiliary electrolytic cell may be used to purify the electrolyte.
The beneficial effects of the invention are:
1. the barrel plating mode is adopted for production, the use of a negative plate is avoided, and a large amount of labor hour is reduced.
2. The roller is specially designed, and continuous production can be realized by screening the sizes of cathode materials such as nickel cakes and the like.
3. By adopting the barrel plating production method, the cathode material continuously rolls in the deposition process, the solution is stirred, and no bubbles and the like are left on the surface of the material, so that the wetting agent can not be used.
4. The electrolytic nickel material with different shapes which is suitable for the requirements of users can be produced by designing the shape of the starting sheet according to the requirements of the users.
Drawings
FIG. 1 is a schematic view showing the structure of a barrel plating apparatus according to the present invention.
In the figure, 1, a barrel plating cylinder, 2, a helical blade, 3, a main electrolytic tank, 4, an opening on the barrel plating cylinder, 5, an opening on the helical blade, 6, a driving motor, 7 and an anode.
FIG. 2 is a schematic view showing the structure of the barrel plating apparatus of the present invention.
In the figure, 1, a barrel plating cylinder, 2, a helical blade, 3, a main electrolytic tank, 4, an opening on the barrel plating cylinder, 5, an opening on the helical blade, 6, a driving motor, 7 and an anode.
Detailed Description
As shown in fig. 1, a barrel plating apparatus for producing a nickel material by barrel plating mainly comprises the following devices: the barrel plating device comprises a barrel plating barrel 1, a helical blade 2 and a main electrolytic tank 3, wherein holes 4 are distributed on the barrel plating barrel 1, the helical blade 2 is provided with a hole 5, a driving motor 6 drives the barrel plating barrel 1 to rotate, and the driving motor 6 can be connected with the barrel plating barrel through a transmission gear. The anode 7 in the main electrolytic tank 3, the anode material is nickel horn, can put and use in the titanium anode basket. The anode of the auxiliary plating bath is also a nickel horn. The distance between the barrel plating barrel 1 and the anode 7 is set to be 100-250mm, and the preferred distance is 200 mm.
The barrel plating barrel 1 is arranged obliquely in the main plating tank 3, preferably at an angle of between 10 and 30 degrees.
An anode and a cathode conductive contact line are arranged in the main electrolytic tank 3. Wherein the barrel plating barrel 1 is provided with holes with the aperture ratio of 50-95% different; the distance between the barrel plating barrel 1 and the anode 7 is set to be 100-200 mm.
The barrel plating apparatus shown in FIG. 1 may further include an auxiliary electrolytic bath communicating with the main electrolytic bath, and an electrolytic solution may be circulated between the two baths. Heating device can be set up in the supplementary electrolysis trough, positive pole electrolysis board, in the production process, can be through the circulating filter pump, squeeze into main electrolysis trough with electrolyte by supplementary electrolysis trough after filtering, play the effect of purifying electrolyte. Additives required in the production process can be added in the auxiliary electrolytic cell.
Preparing a starting electrode material for producing electrolytic nickel. Injecting the prepared electrolytic solution into a plating bath, and producing the starting electrode seed material for electrolytic nickel in the plating bath by using a plating method. The shape of the starting electrode material can be customized according to the requirements of customers, and the starting electrode material of the electrolytic nickel material can also be processed by a cutting method and the like.
Preparing the electrolyte required by production. The electrolytic solution can be specifically configured as a nickel sulfamate system electrolytic solution, and comprises: nickel sulfamate: 200-600g/L, nickel chloride: 3-20g/L, boric acid: 25-40g/L, regulating the pH value of the solution to 2.0-4.5 by using sulfamic acid or nickel carbonate, adding 2ml/L of sulfur-containing additive, heating the solution to 40-50 ℃, and using a waveform cathode electrolytic solution under the filtering condition, wherein the cathode current density is as follows: 0.2-0.8A/dm2
The following electrolytes may also be provided as alternatives: nickel sulfate: 200-400g/L, nickel chloride: 3-20g/L, boric acid: 25-40g/L, 2ml/L of sulfur-containing additive is added. Adjusting the pH value of the solution to 2.0-4.5 by using sulfuric acid or nickel carbonate, heating the solution to 40-55 ℃, and using a low-current electrolytic solution under the filtering condition, wherein the cathode current density is as follows: 0.2-0.8A/dm2
The nickel button is produced by barrel plating. The prepared electrolytic solution is injected into a main electrolytic bath (a roll plating bath), and a nickel anode is filled in an anode titanium basket. The circulation filtration was started and the solution was heated to 50 ℃. Loading the starting electrode seed material of the electrolytic nickel button into a roller of a barrel plating machine, connecting a switching power supply, adjusting the voltage to be 2V-3V, and increasing the voltage to 4V after keeping for 24 hours. Adjusting an electrolysis power supply in the electrolytic cell to enable the electric quantity of the electrolytic cell to account for about 1-50% of the total electric quantity.
Sampling every 2-24 hours to detect the additive content in the electrolyte and the sulfur content in the cathode nickel material, and controlling the sulfur content to be 0.01-0.040%.
The growth cycle is divided into 1-5 stages, each stage needs a roller corresponding to the stage, and the cycle of each stage is 1-15 days.
And when the starting electrode seed material of the electrolytic nickel material grows to the specified size, taking out, cleaning, drying and packaging.
The nickel button produced by the method can be in the shape of button, block or ball. The components of the alloy comprise 0.015-0.040% of sulfur, 0.005-0.03% of impurities and the balance of nickel and cobalt.
Other components are less than or equal to 0.15 percent of cobalt. The impurities include: less than or equal to 0.03 percent of carbon, less than or equal to 0.01 percent of copper, less than or equal to 0.01 percent of iron, less than 0.005 percent of zinc, less than 0.005 percent of lead, less than 0.005 percent of phosphorus, less than 0.005 percent of silicon, less than 0.005 percent of bismuth, less than 0.005 percent of tin, less than 0.005 percent of manganese, less than 0.005 percent of arsenic and less than 0.005 percent of antimony.
The sulfur-containing active nickel anode material can be prepared by adopting an electrolytic method in the barrel plating device.
As shown in FIG. 2, the barrel plating device for producing nickel material by barrel plating mainly comprises the following equipment: the device comprises a barrel plating cylinder 1, a helical blade 2 and a main electrolytic tank 3, wherein openings 4 are distributed on the barrel plating cylinder 1, openings 5 are formed in the helical blade 2, a driving motor 6 drives the barrel plating cylinder 1 to rotate, and the driving motor 6 can be connected with the barrel plating cylinder through a transmission gear.
The helical blade in fig. 1 is a cross-sectional view, and a complete schematic diagram of the helical blade can be seen from fig. 2, when in operation, after a nickel material (sulfur-containing active nickel anode material) grows to a set size in a roller through electroplating, the nickel material cannot pass through the opening 4 on the helical blade, and then is automatically sent out from the barrel along with the rotation of the helical blade, and the full automation of barrel plating production can be realized through the cooperation of devices such as a conveyor belt and the like outside barrel plating equipment.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.

Claims (10)

1. A method for producing electrolytic nickel material by barrel plating is characterized by comprising the following steps:
(1) adding the electrolyte into a main electrolytic bath of a barrel plating device, and starting circulating filtration and heating;
(2) adding an initial electrode seed material for electrolytic nickel to be plated into a roller of a barrel plating device, wherein the roller is connected with a circuit cathode, and a main electrolytic tank anode is connected with a circuit anode;
(3) controlling the voltage interval of the main electrolytic tank to be 1-4V, after keeping for 24 hours, gradually increasing the voltage along with the lengthening of the growth time of the starting material for the electrolytic nickel, wherein the voltage interval is 4-8V,
the electrolytic nickel material is a nickel button.
2. The method as claimed in claim 1, wherein the barrel plating device comprises a main electrolytic bath, a roller and a motor, the roller is obliquely arranged in the main electrolytic bath, and the motor is connected with the roller.
3. The method of claim 2, wherein the barrel plating apparatus further comprises an auxiliary electrolytic bath.
4. The method as claimed in claim 3, wherein the electrolyte is subjected to chemical impurity removal or low-current electrolytic impurity removal and then is added to the auxiliary electrolytic tank and the main electrolytic tank.
5. The method according to claim 4, wherein the low-current electrolytic impurity removal process comprises the following steps: electrolysis was carried out using a corrugated cathode plate with a cathode current density of: 0.2-0.8A/dm 2.
6. The method according to claim 1, wherein the electrolyte used in the production method of electrolytic nickel material by barrel plating is: the nickel sulfamate system electrolytic solution comprises the following components: nickel sulfamate: 200-600g/L, nickel chloride: 3-20g/L, boric acid: 25-40g/L, regulating pH value of the solution to 2.5-4.5 with sulfamic acid or nickel carbonate, and controlling the temperature to 40-60 ℃.
7. The method according to claim 1, wherein the electrolyte used in the production method of electrolytic nickel material by barrel plating is: nickel sulfate system electrolytic solution: the main components are as follows: nickel sulfate: 200-400g/L, nickel chloride: 3-20g/L, boric acid: 25-40g/L, the pH value is controlled between 2.0-4.5 when the device works, and the temperature is 40-65 ℃.
8. The method of claim 3, wherein the electrolytic nickel material is sulfur-containing electrolytic nickel, and the sulfur content in the sulfur-containing electrolytic nickel is controlled to be 0.015-0.040%.
9. The method of claim 8, wherein the amount of sulfur in the electrolytic nickel material is controlled by adding an additive to the auxiliary cell.
10. A method according to claim 9, wherein the auxiliary cell is used to purify the electrolyte.
CN201810820772.8A 2018-07-24 2018-07-24 Method for producing electrolytic nickel material by barrel plating method Active CN110747493B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61194200A (en) * 1985-02-23 1986-08-28 Yoshihisa Ichio Barrel device for plating or the like
JPH05214597A (en) * 1992-01-30 1993-08-24 Fuji Plant Kogyo Kk Barrel planting method and plating drum
JPH06272095A (en) * 1993-03-19 1994-09-27 Taiyo Yuden Co Ltd Barrel plating device
CN106507857B (en) * 2008-11-25 2011-07-27 中核北方核燃料元件有限公司 Cobalt block nickel plating technology
CN102719868A (en) * 2012-07-20 2012-10-10 滨中元川金属制品(昆山)有限公司 Nickel plating process of stainless steel fastener
CN202808983U (en) * 2012-07-30 2013-03-20 保定市普天奥电子科技设备有限公司 Synergia rotary barrel for barrel plating machine
CN104047044A (en) * 2014-07-04 2014-09-17 旺诠科技(昆山)有限公司 Circulation mechanism for filling electroplating liquid into electroplating barrel

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT1181469B (en) * 1983-11-07 1987-09-30 Luciano Folco Continuous electroplating plant for small articles

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61194200A (en) * 1985-02-23 1986-08-28 Yoshihisa Ichio Barrel device for plating or the like
JPH05214597A (en) * 1992-01-30 1993-08-24 Fuji Plant Kogyo Kk Barrel planting method and plating drum
JPH06272095A (en) * 1993-03-19 1994-09-27 Taiyo Yuden Co Ltd Barrel plating device
CN106507857B (en) * 2008-11-25 2011-07-27 中核北方核燃料元件有限公司 Cobalt block nickel plating technology
CN102719868A (en) * 2012-07-20 2012-10-10 滨中元川金属制品(昆山)有限公司 Nickel plating process of stainless steel fastener
CN202808983U (en) * 2012-07-30 2013-03-20 保定市普天奥电子科技设备有限公司 Synergia rotary barrel for barrel plating machine
CN104047044A (en) * 2014-07-04 2014-09-17 旺诠科技(昆山)有限公司 Circulation mechanism for filling electroplating liquid into electroplating barrel

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