CN115404458A - Stainless steel surface treatment process for improving durability of driving shaft - Google Patents
Stainless steel surface treatment process for improving durability of driving shaft Download PDFInfo
- Publication number
- CN115404458A CN115404458A CN202211029159.7A CN202211029159A CN115404458A CN 115404458 A CN115404458 A CN 115404458A CN 202211029159 A CN202211029159 A CN 202211029159A CN 115404458 A CN115404458 A CN 115404458A
- Authority
- CN
- China
- Prior art keywords
- shaft
- vacuum
- voltage
- heating
- mbar
- 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.)
- Pending
Links
Classifications
-
- 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
-
- 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
- C23C—COATING 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
-
- 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
- C23C—COATING 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention relates to a stainless steel surface treatment process for improving the durability of a driving shaft. A sealed drive shaft that is in a high-pressure water environment for a long time, cannot rust, and has a long service life is in demand in various industries. The invention firstly carries out nitriding process and then DLC coating process on stainless steel, wherein the DLC coating process is to put a workpiece treated by the nitriding process into a vacuum chamber, heat the workpiece to 200-300 ℃ and ensure that the vacuum degree is lower than 1 x 10 ‑5 mbar, introducing methane gas at a flow rate to make vacuum degree reach 5 × 10 ‑3 mbar, applying a voltage of-850V to-750V to the shaft, after stable operation for 2-2.5 hours, closing the voltage applied to the shaft, closing heating, and taking out the shaft after the temperature in the vacuum chamber is reduced to obtain a final product. The invention adopts a nitriding process and a DLC processThe combination of (2) improves the surrounding hardness to more than 2000, and simultaneously reduces the friction coefficient from 0.2 to about 0.05, thereby effectively improving the service life and the durability of the shaft.
Description
Technical Field
The invention relates to a treatment process for the surface of a driving shaft and a stainless steel shaft, in particular to a stainless steel surface treatment process for improving the durability of the driving shaft.
Background
A sealed drive shaft that is in a high-pressure water environment for a long time, cannot rust, and has a long service life is in demand in various industries. In the vacuum coating industry, a sealed driving shaft which can bear a certain torque, has low rotating speed, does not rust, is wear-resistant and self-lubricating is needed.
The common treatment mode in the market at present is nickel or chromium electroplating after nitridation, which can increase the service life of the shaft to a certain extent and has certain self-lubricating property, but cannot meet the actual requirements on the service life, hardness and self-lubricating property of the sealed shaft in the market.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the stainless steel surface treatment process for improving the durability of the driving shaft, and the surface hardness and the surface self-lubricating property of the driving shaft are effectively improved by combining the stainless steel nitriding process and the DLC process.
Therefore, the invention adopts the following technical scheme: a stainless steel surface treatment process for improving the durability of a driving shaft is characterized in that a stainless steel driving shaft is subjected to a nitriding process and then subjected to a DLC (diamond-like carbon) coating process, wherein the DLC coating process is to place a workpiece treated by the nitriding process into a vacuum chamber, heat the workpiece to 200-300 ℃ and enable the vacuum degree to be lower than 1 x 10 - 5 mbar, introducing methane gas at a flow rate to make vacuum degree reach 5 × 10 -3 mbar, applying a voltage of-850V to-750V to the shaft, after stable operation for 2-2.5 hours, closing the voltage applied to the shaft, closing heating, and taking out the shaft after the temperature in the vacuum chamber is reduced to obtain a final product.
Preferably, the nitriding process is to install the driving shaft on a tool, put the tool in a vacuum furnace, heat the vacuum furnace to 500-600 ℃, and simultaneously vacuumize to ensure that the vacuum degree is lower than 1 x 10 -5 mbar, then in a vacuum furnace, introducing a proper amount of high-purity nitrogen to make the pressure reach 1X 10 -1 mbar, applying a voltage of-850V to-750V to the shaft, closing the voltage applied to the shaft after stable operation is carried out for 2-2.5 hours, closing heating, and taking out the shaft after the temperature in the furnace is reduced; the surface of the shaft is then subjected to a polishing treatment.
Preferably, in the DLC coating process, the workpiece is placed in a vacuum chamber, heated to 250 ℃, then-800V voltage is applied to the shaft, after stable operation is carried out for 2 hours, the voltage applied to the shaft is closed, heating is closed, and the shaft is taken out after the temperature in the vacuum chamber is lower than 50 ℃.
Preferably, in the nitriding process, the driving shaft is installed on a tool and then heated to 550 ℃ in a vacuum furnace.
Preferably, in the nitriding process, after nitrogen is introduced, a voltage of-800V is applied to the shaft, and after the nitriding process is stably operated for 2 hours, the voltage applied to the shaft is closed.
Preferably, in the nitriding process, the shaft is taken out after the temperature in the furnace is reduced to below 50 ℃ after the heating is turned off.
The invention can make the surface hardness of the shaft reach Hv0.1 to 900-1200 by the nitridation process, which is improved by 3 times compared with the original state of stainless steel about 400, and then the invention can improve the surrounding hardness to over 2000 by the DLC process, and simultaneously reduce the friction coefficient from 0.2 to about 0.05, thereby effectively improving the service life and durability of the shaft.
Detailed Description
The invention is described in further detail below with reference to specific examples.
Example 1: the shaft was mounted on a tooling, placed in a vacuum oven, which was first heated to 550 ℃. Simultaneously, vacuumizing to make the vacuum degree lower than 1 × 10 -5 mbar, then in a vacuum furnace, introducing a proper amount of high-purity nitrogen to make the pressure reach 1X 10 - 1 mbar, applying a voltage of-800V to the shaft, turning off the voltage applied to the shaft after stable operation for 2 hours, turning off heating, taking out the shaft after the temperature in the furnace is reduced to below 50 ℃, and polishing the surface of the shaft.
Cleaning the polished shaft, then performing a DLC (Diamond like carbon) coating process, putting the workpiece into a vacuum chamber, heating to 250 ℃, wherein the background vacuum degree is lower than 1 x 10-5mbar, introducing methane gas with a certain flow rate to ensure that the vacuum degree reaches 5 x 10-3mbar, then applying a voltage of-800V on the shaft, stably operating for 2 hours, closing the voltage applied on the shaft, closing the heating, and taking out the shaft after the temperature in the vacuum chamber is lower than 50 ℃ to obtain a final product.
Through the nitriding process, the surface hardness of the shaft can reach Hv0.1 to 1200, which is improved by 3 times compared with the original state of the stainless steel by about 400, and then through the DLC process, the surrounding hardness is improved to over 2400, and the friction coefficient is reduced from 0.2 to 0.04.
Example 2:
the shaft was mounted on a tooling, placed in a vacuum oven, which was first heated to 550 ℃. Simultaneously, vacuumizing to a vacuum degree of less than 1 × 10 -5 mbar, then introducing appropriate amount of high-purity nitrogen gas in a vacuum furnace to make the gas pressure reach 1 × 10 -1 mbar, applying a voltage of-800V to the shaft, stopping applying the voltage to the shaft after stable operation for 2 hours, stopping heating, taking out the shaft after the temperature in the furnace is reduced to below 50 ℃, and then polishing the surface of the shaft.
Cleaning the polished shaft, then carrying out a DLC (Diamond like carbon) coating process, putting the workpiece into a vacuum chamber, heating to 200 ℃, wherein the background vacuum degree is lower than 1 x 10-5mbar, introducing methane gas with a certain flow rate to ensure that the vacuum degree reaches 5 x 10-3mbar, then applying a voltage of-850V on the shaft, stably operating for 2 hours, closing the voltage applied on the shaft, closing the heating, and taking out the shaft after the temperature in the vacuum chamber is lower than 50 ℃, thus obtaining the final product.
Through the nitriding process, the surface hardness of the shaft can reach Hv0.1 to 1200, which is improved by 3 times compared with the original state of the stainless steel by about 400, and then through the DLC process, the surrounding hardness is improved to more than 2300, and the friction coefficient is reduced from 0.2 to 0.05.
Example 3:
the shaft was mounted on a tooling, placed in a vacuum oven, which was first heated to 550 ℃. Simultaneously, vacuumizing to make the vacuum degree lower than 1 × 10 -5 mbar, then introducing appropriate amount of high-purity nitrogen gas in a vacuum furnace to make the gas pressure reach 1 × 10 -1 mbar, applying a voltage of-800V to the shaft, turning off the voltage applied to the shaft after stable operation for 2 hours, turning off heating, taking out the shaft after the temperature in the furnace is reduced to below 50 ℃, and polishing the surface of the shaft.
Cleaning the polished shaft, then performing a DLC (Diamond like carbon) coating process, putting the workpiece into a vacuum chamber, heating to 300 ℃, wherein the background vacuum degree is lower than 1 x 10-5mbar, introducing methane gas with a certain flow rate to ensure that the vacuum degree reaches 5 x 10-3mbar, then applying a voltage of-750V on the shaft, stably operating for 2.5 hours, closing the voltage applied on the shaft, closing the heating, and taking out the shaft after the temperature in the vacuum chamber is lower than 50 ℃ to obtain a final product.
Through the nitriding process, the surface hardness of the shaft can reach Hv0.1 to 1200, which is improved by 3 times compared with the original state of the stainless steel by about 400, and then through the DLC process, the surrounding hardness is improved to over 2200, and the friction coefficient is reduced from 0.2 to 0.05.
Example 4:
the shaft was mounted on a tooling and placed in a vacuum oven which was first heated to 500 ℃. Simultaneously, vacuumizing to make the vacuum degree lower than 1 × 10 -5 mbar, then introducing appropriate amount of high-purity nitrogen gas in a vacuum furnace to make the gas pressure reach 1 × 10 -1 mbar, applying a voltage of-750V to the shaft, stopping applying the voltage to the shaft after stable operation for 2.5 hours, stopping heating, taking out the shaft after the temperature in the furnace is reduced to below 50 ℃, and then polishing the surface of the shaft.
Cleaning the polished shaft, then performing a DLC film coating process, putting the workpiece into a vacuum chamber, heating to 300 ℃, wherein the background vacuum degree is lower than 1 x 10-5mbar, introducing methane gas with a certain flow rate to ensure that the vacuum degree reaches 5 x 10-3mbar, then applying a voltage of-750V on the shaft, after stable operation is performed for 2.5 hours, closing the voltage applied on the shaft, closing heating, and taking out the shaft after the temperature in the vacuum chamber is lower than 50 ℃, thus obtaining the final product.
Through the nitriding process, the surface hardness of the shaft can reach Hv0.1 to 1000, which is improved by nearly 3 times compared with the original state of the stainless steel by about 400, and then through the DLC process, the surrounding hardness is improved to more than 2000, and the friction coefficient is reduced from 0.2 to 0.05.
The invention combines the stainless steel nitriding process and the DLC process. The surface hardness and the surface self-lubricating property of the workpiece can be effectively improved. The service life and the durability of the shaft are obviously prolonged.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (6)
1. A stainless steel surface treatment process for improving the durability of a driving shaft is characterized in that a stainless steel driving shaft is subjected to a nitriding process and then subjected to a DLC (diamond-like carbon) coating process, wherein the DLC coating process is to place a workpiece treated by the nitriding process into a vacuum chamber, heat the workpiece to 200-300 ℃ and enable the vacuum degree to be lower than 1 x 10 -5 mbar, introducing methane gas at a flow rate to make vacuum degree reach 5 × 10 -3 mbar, applying a voltage of-850V to-750V to the shaft, after stable operation for 2-2.5 hours, closing the voltage applied to the shaft, closing heating, and taking out the shaft after the temperature in the vacuum chamber is reduced to obtain a final product.
2. The process of claim 1, wherein the nitriding process comprises installing the drive shaft on a tool, placing the tool in a vacuum furnace, heating the furnace to a temperature of 500-600 ℃, and simultaneously evacuating to a vacuum level of less than 1 x 10 - 5 mbar, then introducing appropriate amount of high-purity nitrogen gas in a vacuum furnace to make the gas pressure reach 1 × 10 -1 mbar, applying a voltage of-850V to-750V to the shaft, closing the voltage applied to the shaft after stable operation is carried out for 2-2.5 hours, closing heating, and taking out the shaft after the temperature in the furnace is reduced; the surface of the shaft is then subjected to a polishing treatment.
3. The process of claim 1, wherein the DLC coating process comprises placing the workpiece in a vacuum chamber, heating to 250 deg.C, applying-800V voltage to the shaft, stopping the voltage applied to the shaft after stable operation for 2 hr, and taking out the shaft after the temperature in the vacuum chamber is below 50 deg.C.
4. The process of claim 2, wherein the nitriding process is carried out by heating the drive shaft to 550 ℃ in a vacuum furnace after the drive shaft is mounted on the tool.
5. The process according to claim 2, wherein the nitriding process comprises introducing nitrogen gas, applying a voltage of-800V to the shaft, and stopping the voltage applied to the shaft after the nitriding process is stably operated for 2 hours.
6. The process according to claim 2, wherein the shaft is removed after the temperature in the furnace is reduced to below 50 ℃ after the heating is turned off in the nitriding process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211029159.7A CN115404458A (en) | 2022-08-26 | 2022-08-26 | Stainless steel surface treatment process for improving durability of driving shaft |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211029159.7A CN115404458A (en) | 2022-08-26 | 2022-08-26 | Stainless steel surface treatment process for improving durability of driving shaft |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115404458A true CN115404458A (en) | 2022-11-29 |
Family
ID=84161852
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211029159.7A Pending CN115404458A (en) | 2022-08-26 | 2022-08-26 | Stainless steel surface treatment process for improving durability of driving shaft |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115404458A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090040756A (en) * | 2007-10-22 | 2009-04-27 | 한국생산기술연구원 | Method for coating dlc(diamond like carbon) film with nitriding hardening on the vane of air compressor by low temperature pecvd |
| JP2011026660A (en) * | 2009-07-24 | 2011-02-10 | Jtekt Corp | Sliding member and method for producing the same |
| KR20140022526A (en) * | 2012-08-13 | 2014-02-25 | 한국생산기술연구원 | Nitriding product and method for nitriding by plasma |
| CN106011738A (en) * | 2016-06-16 | 2016-10-12 | 常州普威特涂层有限公司 | Surface plating composite coating process for die |
| CN108754406A (en) * | 2018-06-25 | 2018-11-06 | 宁波中材钰翔新材料科技有限公司 | A kind of die surface compounding method |
| RU2712661C1 (en) * | 2018-12-29 | 2020-01-30 | федеральное государственное бюджетное образовательное учреждение высшего образования "Национальный исследовательский университет "МЭИ" (ФГБОУ ВО "НИУ "МЭИ") | Method for formation of tribological coating |
| CN113061845A (en) * | 2021-03-19 | 2021-07-02 | 安徽纯源镀膜科技有限公司 | Preparation process of ultra-black high-performance Ti-DLC coating |
-
2022
- 2022-08-26 CN CN202211029159.7A patent/CN115404458A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090040756A (en) * | 2007-10-22 | 2009-04-27 | 한국생산기술연구원 | Method for coating dlc(diamond like carbon) film with nitriding hardening on the vane of air compressor by low temperature pecvd |
| JP2011026660A (en) * | 2009-07-24 | 2011-02-10 | Jtekt Corp | Sliding member and method for producing the same |
| KR20140022526A (en) * | 2012-08-13 | 2014-02-25 | 한국생산기술연구원 | Nitriding product and method for nitriding by plasma |
| CN106011738A (en) * | 2016-06-16 | 2016-10-12 | 常州普威特涂层有限公司 | Surface plating composite coating process for die |
| CN108754406A (en) * | 2018-06-25 | 2018-11-06 | 宁波中材钰翔新材料科技有限公司 | A kind of die surface compounding method |
| RU2712661C1 (en) * | 2018-12-29 | 2020-01-30 | федеральное государственное бюджетное образовательное учреждение высшего образования "Национальный исследовательский университет "МЭИ" (ФГБОУ ВО "НИУ "МЭИ") | Method for formation of tribological coating |
| CN113061845A (en) * | 2021-03-19 | 2021-07-02 | 安徽纯源镀膜科技有限公司 | Preparation process of ultra-black high-performance Ti-DLC coating |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111962014B (en) | Stainless steel reinforced heat treatment process and heat treatment nitriding furnace | |
| US5792519A (en) | Method for the plasma assisted high vacuum physical vapor coating of parts with wear resistant coatings and equipment for carrying out the method | |
| CN105937018A (en) | Low temperature ion nitriding method for austenitic stainless steel | |
| CN108866472A (en) | A kind of metallic material surface treating method | |
| CN115404458A (en) | Stainless steel surface treatment process for improving durability of driving shaft | |
| CN101724808A (en) | Surface carburization processing method for steel bearing ring of high-carbon chromium bearing | |
| CN117187517B (en) | High-pressure valve production heat treatment method and equipment | |
| CN109778109A (en) | A method of it is off quality to solve carbo-nitriding | |
| KR101414257B1 (en) | pressure nitriding furnace | |
| CN109972077B (en) | Nitriding process for carburizing Ferrium steel | |
| JP2011026660A (en) | Sliding member and method for producing the same | |
| CN106637063A (en) | Ion nitriding surface modification method for improving heat fatigue of H13 hot-working die | |
| CN111519129A (en) | Rotation-driven surface soft nitriding chemical heat treatment strengthening method | |
| CN114262863B (en) | Green high-efficiency multi-ion co-permeation surface modification method with high wear resistance and corrosion resistance | |
| CN205420524U (en) | Titanium closes surface treatment device of compound nitridation of low pressure vacuum carburization | |
| CN113462858B (en) | Method for performing vacuum stress relief annealing by using ion nitriding furnace | |
| JP5674180B2 (en) | Method for surface modification of stainless steel materials | |
| CN1253587C (en) | Heat treating technology of 30CrMnSi steel for higher toughness and antiwear nature | |
| CN111876563A (en) | Rolling process of carbon-chromium bearing steel | |
| CN111850456A (en) | Titanium alloy segmented vacuum rapid nitriding method and device | |
| CN116426864B (en) | Carburizing and magnetron sputtering composite treatment process for large-shaft driving lead screw of glass rotary tube | |
| JP4911451B2 (en) | Method for surface modification of metal material containing iron as main component | |
| CN113846284B (en) | Ion nitriding process for 25Cr2Ni3Mo material | |
| KR100602879B1 (en) | Member of air motor | |
| CN109207698A (en) | A kind of production technology for high-strength stainless steel fastening modifier treatment |
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 |