CN110783013B - Solar cell electrode slurry, cell and preparation method of assembly of cell - Google Patents

Solar cell electrode slurry, cell and preparation method of assembly of cell Download PDF

Info

Publication number
CN110783013B
CN110783013B CN201911077101.8A CN201911077101A CN110783013B CN 110783013 B CN110783013 B CN 110783013B CN 201911077101 A CN201911077101 A CN 201911077101A CN 110783013 B CN110783013 B CN 110783013B
Authority
CN
China
Prior art keywords
battery
soldering flux
paste
cell
preparation
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.)
Active
Application number
CN201911077101.8A
Other languages
Chinese (zh)
Other versions
CN110783013A (en
Inventor
苗蕾
杨燕
闫兰
麻超
苑北海
郝晶晶
陈艳涛
刘凯辉
邢少辉
杨丽杰
要思思
董丛笑
聂会欣
白春晖
任辰龙
于洪浩
尚琪
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.)
Yingli Energy China Co Ltd
Original Assignee
Yingli Energy China 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 Yingli Energy China Co Ltd filed Critical Yingli Energy China Co Ltd
Priority to CN201911077101.8A priority Critical patent/CN110783013B/en
Publication of CN110783013A publication Critical patent/CN110783013A/en
Application granted granted Critical
Publication of CN110783013B publication Critical patent/CN110783013B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/02Details
    • H01L31/0224Electrodes
    • H01L31/022408Electrodes for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/022425Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
    • H01L31/022441Electrode arrangements specially adapted for back-contact solar cells
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1804Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof comprising only elements of Group IV of the Periodic System
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/547Monocrystalline silicon PV cells
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to the technical field of solar cells, and particularly discloses solar cell electrode slurry, a cell and a preparation method of a component of the cell. The electrode slurry is composed of the soldering flux and the conductive slurry in a mass ratio of 1:6-8, the electrode slurry is adopted, printing is carried out on a battery substrate according to a preset pattern, a battery piece is obtained after sintering, and the obtained battery piece is used for preparing a battery assembly. The preparation method of the assembly provided by the invention can save energy consumption, reduce cost, prolong the service life of welding equipment, improve the product quality of the battery assembly, prolong the service life of the battery assembly and improve the power generation stability of the assembly.

Description

Solar cell electrode slurry, cell and preparation method of assembly of cell
Technical Field
The invention relates to the technical field of solar cells, in particular to solar cell electrode slurry, a cell and a preparation method of a component of the cell.
Background
For the photovoltaic module to realize the power generation function, the single cells must be connected into a whole, and the common connection method is welding. However, if the welding process is not properly controlled, certain defects can be caused, and hot spots, fragments and the like can be caused during the use process. Therefore, in the production and manufacturing process of photovoltaic modules, the welding of the cell sheets becomes one of the important processes.
At present, in order to ensure the welding quality in the welding process and enable a welding strip to be welded with a battery plate quickly and perfectly, scaling powder is used as catalysis and assistance. In order to facilitate the spraying of the soldering flux on the battery piece, the soldering flux is required to be kept in a liquid state, and an alcohol solvent is added into the soldering flux. However, the alcohol solvent accounts for about 90% of the total mass of the soldering flux system, belongs to an inflammable product, has high storage requirement, great potential safety hazard and short shelf life (the alcohol solvent can expire in one week after being unsealed). In addition, the spraying amount of the soldering flux on the battery piece is not easy to control, the spraying is less easy to weld, the spraying is more likely to cause residue, a series of quality hidden dangers such as layering and residual soldering flux crystallization can be caused to the components in the later period, and the liquid soldering flux is scattered to the components of the equipment to cause corrosion, so that the service life of the equipment is influenced.
Disclosure of Invention
Aiming at the technical problems in the existing welding process, the invention provides a solar cell electrode slurry, a cell and a preparation method of a module thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
the solar cell electrode paste consists of a soldering flux and a conductive paste in a mass ratio of 1:6-8, wherein the mass content of a solvent in the soldering flux is less than 1%, the mass content of an organic acid is 20-25%, and the balance is conventional components of the soldering flux, such as base resin and the like, wherein the organic acid is conventional organic acid used for the soldering flux in the field.
Compared with the prior art, the electrode paste provided by the invention comprises the soldering flux and the conductive paste which are coated on the surface of the battery in the printing process, the boiling point is ensured to be more than 500 ℃ by regulating and controlling the contents of the alcohol solvent and the organic acid in the soldering flux, the phenomenon that the soldering flux is directly gasified in the sintering process to cause the incapability of carrying out the catalytic reaction of welding is avoided, and the problems of welding quality and easy corrosion of welding equipment caused by the residue of the soldering flux in the welding process can be effectively solved. In addition, due to the doping of the soldering flux, the penetration and fusion process of the conductive function in the cell can be accelerated in the sintering process, and is shortened from the original 2.0-2.5min to 0.8-1.2min, so that the fusion speed and the fusion effect of the conductive function in the cell are improved.
Further, the conductive paste is silver paste, aluminum paste or silver-aluminum paste. Coating electrode slurry formed by silver-aluminum slurry and soldering flux on a back electrode of a silicon chip; coating electrode slurry formed by aluminum slurry and soldering flux on other regions of the back surface of the silicon chip except for the back electrode; and coating electrode slurry formed by silver paste and soldering flux on the front surface of the silicon chip to ensure that a positive electrode and a negative electrode are manufactured on the surface of the battery.
Furthermore, the mass content of the conductive functional phase in the conductive slurry is 90-95%, so that an electrode is formed on the surface of the silicon wafer, and crystalline silicon atoms are fused into a molten electrode material in a certain proportion in the sintering process, so that good ohmic contact is formed.
Furthermore, the soldering flux is an organic acid type soldering flux (such as Kester952-S after solvent removal) so as to ensure that the boiling point of the soldering flux reaches over 500 ℃, so that the soldering flux can keep excellent activity at high temperature and ensure the soldering effect. If the boiling point of the soldering flux is lower than 500 ℃, desolvating is carried out on the soldering flux, so that the mass content of a solvent (an alcohol solvent) in the soldering flux is less than 1 percent, and the mass content of an organic acid is 20 to 25 percent. In addition, the content of the alcohol solvent in the soldering flux is reduced, so that the price of the soldering flux is reduced from 30 yuan/L to 10 yuan/L. And the alcohol solvent can be recycled, so that the energy consumption is saved, and the cost is reduced.
The invention also provides a preparation method of the battery piece, which comprises the following steps: and printing the electrode slurry on a battery substrate according to a preset pattern, and sintering to obtain the battery piece.
According to the preparation method of the cell, the electrode slurry consisting of the soldering flux and the conductive slurry is adopted to perform screen printing treatment on the coated silicon wafer, and in the sintering process, the soldering flux can accelerate the permeation and fusion process of the conductive function in the conductive slurry to the cell, so that the electrode and the silicon wafer form ohmic contact more quickly. In addition, active soldering flux is still remained on the surface of the sintered battery piece, so that the subsequent welding of the battery piece is facilitated, and potential safety hazards such as fire or explosion caused by flocculent derivatives generated after the liquid soldering flux is heated can be eliminated.
Furthermore, the sintering temperature is 400-450 ℃, the time is 0.8-1.2min, the sintering temperature is reduced from the traditional temperature of 600-450 ℃ to 400-450 ℃, the phenomenon that the soldering flux is directly gasified and loses activity in the sintering process is avoided, and the doping of the soldering flux can accelerate the permeation and fusion process of the conductive function in the conductive paste to the cell, so that good ohmic contact is ensured.
Further, the dosage of the electrode paste in the screen printing treatment process is 0.18-0.22mg/mm2And the positive electrode and the negative electrode are guaranteed to be manufactured on the surface of the battery.
The invention also provides a preparation method of the battery component, which comprises the following steps: and (3) directly welding the battery piece prepared by the preparation method, and packaging to obtain the battery assembly. The welding is performed by a welding process which is conventional in the art.
According to the preparation method of the battery pack, the battery piece is not required to be sprayed with the soldering flux, so that the problem that the soldering flux is easy to remain on the battery piece, and further quality hidden dangers such as layering and the like of the pack at the later stage are avoided effectively, meanwhile, adverse effects on the service life of equipment caused by the fact that the soldering flux is scattered are avoided, the quality of the battery pack is improved, the service life of welding equipment is prolonged, and meanwhile, the cost is saved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The solar cell electrode paste consists of a soldering flux and conductive paste in a mass ratio of 1:7, wherein the soldering flux is obtained by desolvating Kester952-S, the mass content of an alcohol solvent is 0.8%, and the mass content of organic acid is 23%. Respectively mixing the soldering flux with silver-aluminum paste PV505, aluminum paste RX8204 and silver paste PV16X in a mass ratio of 1:7 to respectively obtain electrode paste A, electrode paste B and electrode paste C.
A preparation method of a battery piece comprises the following steps: printing on a battery substrate according to a preset pattern by adopting the electrode paste, wherein the dosage of the electrode paste is 0.20mg/mm2Coating the electrode slurry A on a silicon wafer back electrode, and drying; coating the electrode slurry B on other regions of the back surface of the silicon wafer except the back electrode, and drying; and coating the electrode slurry C on the front surface of the silicon wafer, drying, and sintering at 420 ℃ for 1min to obtain the cell.
A method of making a battery assembly comprising the steps of: and (3) directly welding the battery pieces by adopting a conventional welding process, and packaging to obtain the battery component.
Example 2
The solar cell electrode paste consists of a soldering flux and conductive paste in a mass ratio of 1:6, wherein the soldering flux is obtained by desolvating Kester952-S, the mass content of an alcohol solvent is 0.6%, and the mass content of organic acid is 25%. And respectively mixing the soldering flux with silver-aluminum paste PV505, aluminum paste RX82121 and silver paste 159 in a mass ratio of 1:6 to respectively obtain electrode paste A, electrode paste B and electrode paste C.
A preparation method of a battery piece comprises the following steps: printing on a battery substrate according to a preset pattern by adopting the electrode paste, wherein the dosage of the electrode paste is 0.18mg/mm2Coating the electrode slurry A on a silicon wafer back electrode, and drying; coating the electrode slurry B on other regions of the back surface of the silicon wafer except the back electrode, and drying; and coating the electrode slurry C on the front surface of the silicon wafer, drying, and sintering at 450 ℃ for 0.8min to obtain the cell.
A method of making a battery assembly comprising the steps of: and (3) directly welding the battery pieces by adopting a conventional welding process, and packaging to obtain the battery component.
Example 3
The solar cell electrode paste consists of a soldering flux and conductive paste in a mass ratio of 1:8, wherein the soldering flux is obtained by desolvating Kester952-S, the mass content of an alcohol solvent is 0.9%, and the mass content of organic acid is 20%. Respectively mixing the soldering flux with silver-aluminum paste PV506, aluminum paste RX8204 and silver paste PV16X in a mass ratio of 1:8 to respectively obtain electrode paste A, electrode paste B and electrode paste C.
A preparation method of a battery piece comprises the following steps: printing on a battery substrate according to a preset pattern by adopting the electrode paste, wherein the dosage of the electrode paste is 0.22mg/mm2. Coating the electrode slurry A on a silicon wafer back electrode, and drying; coating the electrode slurry B on other regions of the back surface of the silicon wafer except the back electrode, and drying; and coating the electrode slurry C on the front surface of the silicon wafer, drying, and sintering at 400 ℃ for 1.2min to obtain the cell.
A method of making a battery assembly comprising the steps of: and (3) directly welding the battery pieces by adopting a conventional welding process, and packaging to obtain the battery component.
In order to better illustrate the characteristics of the electrode paste for solar cells and the method for preparing the cell sheet provided by the embodiment of the invention, the service life of equipment, the performance of a cell module, cost accounting and the like after the invention is adopted are summarized below.
After the method is adopted, the soldering flux spraying process is removed in the preparation process of the battery component, the corrosion to equipment can be reduced, the service life of the equipment component contacted with the soldering flux is prolonged by 2-4 years, the whole using system of the soldering flux of the welding equipment can be omitted, the cost can be saved by 16 ten thousand yuan per year, the waste soldering flux does not need to be recycled and subjected to pollution-free treatment by using capital, and the operation and maintenance cost can be saved by 11 ten thousand yuan per year. Meanwhile, the invention reduces the working temperature of the sintering furnace, and the monthly electricity charge can be saved by 1.2 ten thousand yuan. In addition, the possibility of spraying liquid soldering flux on the battery piece can be avoided, the occurrence rate of the problem of internal layering of the assembly caused by the soldering flux is reduced to 0, the adhesive force between the battery piece and a welding strip can be effectively improved by adopting the electrode slurry and the preparation method of the battery piece provided by the invention (the larger the adhesive force is, the longer the service life of the assembly is, the more stable the power generation effect is), about 0.2 newton per centimeter can be improved, the product quality of the battery assembly can be effectively improved, the service life of the battery assembly is prolonged, and the power generation stability of the assembly is improved.
According to the data, the solar cell electrode slurry, the cell and the preparation method of the module thereof can save energy consumption, reduce cost, effectively prolong the service life of welding equipment and improve the product quality of the cell module.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (7)

1. A solar cell electrode paste, characterized in that: the soldering flux consists of a soldering flux and conductive paste in a mass ratio of 1:6-8, wherein the mass content of an organic solvent in the soldering flux is less than 1%, and the mass content of an organic acid is 20% -25%.
2. The solar cell electrode paste of claim 1, wherein: the conductive paste is silver paste, aluminum paste or silver-aluminum paste.
3. The solar cell electrode paste of claim 1, wherein: the mass content of the conductive functional phase in the conductive slurry is 90-95%.
4. A preparation method of a battery piece is characterized by comprising the following steps: the method comprises the following steps: printing the electrode slurry according to any one of claims 1 to 3 on a battery substrate according to a preset pattern, and sintering to obtain a battery piece.
5. The method for producing a battery piece according to claim 4, characterized in that: the temperature of the sintering treatment is 400-450 ℃, and the time is 0.8-1.2 min.
6. The method for producing a battery piece according to claim 4, characterized in that: the dosage of the electrode slurry in the printing process is 0.18-0.22mg/mm2
7. A method of making a battery assembly, comprising: directly carrying out welding treatment on the battery piece prepared by the preparation method of any one of claims 4 to 6, and packaging to obtain the battery component.
CN201911077101.8A 2019-11-06 2019-11-06 Solar cell electrode slurry, cell and preparation method of assembly of cell Active CN110783013B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911077101.8A CN110783013B (en) 2019-11-06 2019-11-06 Solar cell electrode slurry, cell and preparation method of assembly of cell

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911077101.8A CN110783013B (en) 2019-11-06 2019-11-06 Solar cell electrode slurry, cell and preparation method of assembly of cell

Publications (2)

Publication Number Publication Date
CN110783013A CN110783013A (en) 2020-02-11
CN110783013B true CN110783013B (en) 2021-06-15

Family

ID=69389575

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911077101.8A Active CN110783013B (en) 2019-11-06 2019-11-06 Solar cell electrode slurry, cell and preparation method of assembly of cell

Country Status (1)

Country Link
CN (1) CN110783013B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102069324A (en) * 2010-12-29 2011-05-25 东莞永安科技有限公司 No-clean low-splashing soldering flux for lead-free solder wire and preparation method thereof
JP2019122982A (en) * 2018-01-16 2019-07-25 千住金属工業株式会社 Flux and solder paste

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101367160B (en) * 2008-09-26 2011-03-16 深圳市唯特偶新材料股份有限公司 Cleaning-free lead-free solder soldering fluid without containing halide
JP5741809B2 (en) * 2011-02-22 2015-07-01 三菱マテリアル株式会社 Bonding paste and method for bonding semiconductor element and substrate
CN103382327B (en) * 2012-05-02 2015-11-25 比亚迪股份有限公司 The manufacture method of a kind of copper ink used for solar batteries and preparation method thereof, a kind of solar cell main grid and solar module
CN108538442B (en) * 2015-05-27 2020-07-17 苏州市贝特利高分子材料股份有限公司 Preparation method of high-conductivity low-temperature silver paste
CN105583550B (en) * 2016-03-21 2018-06-15 苏州柯仕达电子材料有限公司 A kind of environment protection soldering fluid
CN105855746B (en) * 2016-05-13 2018-11-09 深圳市唯特偶新材料股份有限公司 A kind of high-tensile strength photovoltaic module scaling powder
JP6471306B2 (en) * 2016-08-16 2019-02-20 株式会社弘輝 Solder composition
CN107658042B (en) * 2017-08-16 2020-12-01 北京康普锡威科技有限公司 Novel lead-free slurry for solar cell electrode assembly
CN109530977B (en) * 2017-09-21 2021-11-19 株式会社田村制作所 Flux and solder paste
CN110322985A (en) * 2018-03-28 2019-10-11 上海逻骅投资管理合伙企业(有限合伙) A kind of electrocondution slurry and its preparation method and application
CN110328466B (en) * 2019-07-06 2021-09-21 苏州龙腾万里化工科技有限公司 Halogen-free cleaning-free soldering flux

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102069324A (en) * 2010-12-29 2011-05-25 东莞永安科技有限公司 No-clean low-splashing soldering flux for lead-free solder wire and preparation method thereof
JP2019122982A (en) * 2018-01-16 2019-07-25 千住金属工業株式会社 Flux and solder paste

Also Published As

Publication number Publication date
CN110783013A (en) 2020-02-11

Similar Documents

Publication Publication Date Title
TWI718261B (en) Electrically conductive composition and applications for said composition
CN101944555A (en) Al and B doped silicon solar cell back surface and preparation method thereof
CN112041994B (en) Crystalline silicon solar cell front conductive paste and preparation method thereof and solar cell
CN104157331B (en) Silicon solar cell electrode silver coated copper sizing agent and preparing method thereof
WO2020024254A1 (en) Glass powder, glass powder composition and preparation method for the glass powder
WO2013129578A1 (en) Conductive paste for solar cell electrodes, solar cell, and method for manufacturing solar cell
CN110112388A (en) The positive electrode and preparation method thereof of porous tungstic acid coating modification
CN102114546A (en) Method for preparing spherical silver powder
CN102623564B (en) Method for producing crystalline silicon solar cell with laser grooved positive electrode
JP2016515302A (en) Method for manufacturing electrode of solar cell and solar cell using the same
CN103367545A (en) Method for synchronously implementing local contact and local doping at back of solar cell by utilizing laser
CN110783013B (en) Solar cell electrode slurry, cell and preparation method of assembly of cell
CN110277459A (en) A kind of preparation method of P-type crystal silicon rear electrode
CN208422924U (en) A kind of passivation contact N-type solar battery, component and system
WO2020024253A1 (en) Slurry for perc cell and method for preparing said slurry
CN108428866B (en) Method for improving electrode capacity by in-situ reduction of clad metal
CN102456929B (en) Method for manufacturing lithium iron phosphate all-solid-state film cell by in-situ spray pyrolysis
CN103021510B (en) A kind of crystal silicon solar energy battery front electrode silver slurry and preparation method thereof
CN110255889B (en) Glass composition for crystalline silicon solar double-side passivated PERC cell front silver paste and preparation method thereof
CN107742711B (en) Preparation method of diboron trioxide coated ternary cathode material
CN102263161A (en) Method for manufacturing electrodes of crystalline silicon solar cell
CN102773577A (en) Welding method for solar cells and interconnectors
CN106935799A (en) The nickle cobalt lithium manganate ternary positive plate of lithium battery and preparation method of a kind of stabilization
CN112420989A (en) Pre-lithiation equipment and using method
CN205692842U (en) solar battery sheet

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant