CN115011937A - Surface oxidation method - Google Patents

Surface oxidation method Download PDF

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Publication number
CN115011937A
CN115011937A CN202110247606.5A CN202110247606A CN115011937A CN 115011937 A CN115011937 A CN 115011937A CN 202110247606 A CN202110247606 A CN 202110247606A CN 115011937 A CN115011937 A CN 115011937A
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CN
China
Prior art keywords
oxidation
product
cavity
chamber
inert gas
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CN202110247606.5A
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Chinese (zh)
Inventor
高佳
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Dongguan Fenggu Nanotechnology Co ltd
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Dongguan Fenggu Nanotechnology Co ltd
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Priority to CN202110247606.5A priority Critical patent/CN115011937A/en
Publication of CN115011937A publication Critical patent/CN115011937A/en
Pending legal-status Critical Current

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    • 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
    • C23C14/351Sputtering by application of a magnetic field, e.g. magnetron sputtering using a magnetic field in close vicinity to the substrate
    • 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
    • C23C14/58After-treatment
    • C23C14/5846Reactive treatment
    • C23C14/5853Oxidation
    • 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/08Solid 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
    • C23C8/10Oxidising
    • C23C8/12Oxidising using elemental oxygen or ozone
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention relates to a surface oxidation method, which comprises the following steps: s1, roughly cleaning the surface of the product, and drying the roughly cleaned product; s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree in the vacuum cavity ranges from 5pa to 0.05 pa; s3, introducing inert gas into the sputtering chamber, wherein the inert gas introduction speed range is 10-5000sccm, and introducing active gas and inert gas into the oxidation chamber, wherein the gas introduction speed range is 10-5000 sccm; in the invention, a graphite electrode is used as an oxidation target source, inert gas and active gas are ionized to generate oxygen ions and oxygen compounds, and the product is sputtered and then oxidized on the premise of high-speed rotation; the surface of the product after sputtering coating is oxidized step by step, so that the oxidation rate of the coated product reaches 99.9 percent.

Description

Surface oxidation method
Technical Field
The invention relates to the technical field of products, in particular to a surface oxidation method.
Background
In the traditional oxidation treatment process, synchronous oxidation is often adopted, namely oxidation is completed in the same chamber while sputtering, the sputtering efficiency is low due to objective factors such as temperature and the like, the oxidation quality is influenced, and the oxidation effect of a product is directly influenced, so that the technical defects can be solved only by carrying out sputtering and oxidation step by step.
Disclosure of Invention
In view of the above, the present invention is directed to a surface oxidation method to solve the problems of the prior art.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method of surface oxidation comprising the steps of:
s1, roughly cleaning the surface of the product, and drying the roughly cleaned product;
s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree in the vacuum cavity ranges from 5pa to 0.05 pa;
s3, introducing inert gas into the sputtering chamber, introducing the inert gas at a speed range of 10-5000sccm, introducing active gas and the inert gas into the oxidation chamber at a speed range of 10-5000sccm, introducing constant-temperature cooling water into the graphite electrode, rotating the cage provided with the substrate at a high speed, rotating the cylindrical target material with the magnetic field facing the substrate, and connecting the negative high voltage of the power supply to the graphite electrode through the insulating electrode;
s4, respectively electrifying the target in the sputtering chamber and the graphite target in the oxidation chamber, wherein the electrifying voltage range is 200-;
s5, rotating the sputtered product from the sputtering chamber to an oxidation chamber to complete oxidation, wherein the rotating speed range is 5-200 q/min;
s6, taking out the product with forceps and placing into a storage box.
Preferably, the rough cleaning of the product surface in step S1 is to place the product into an NMP solution for degumming to remove colloidal objects on the product surface.
Preferably, in step S2, a rotating rack is disposed in the vacuum chamber, and the rotating rack drives the product to rotate from the sputtering chamber to the oxidation chamber.
Preferably, the inert gas in step S3 is any one of helium, neon, argon, krypton, xenon, and radon.
Preferably, the active gas in step S5 is oxygen.
Compared with the prior art, the surface oxidation method has the following advantages:
the graphite electrode is used as an oxidation target source, inert gas and active gas are ionized to generate oxygen ions and oxygen compounds, and the product is sputtered and then oxidized on the premise of high-speed rotation; the surface of the product is subjected to post-oxidation treatment step by step, so that the oxidation rate of the surface of the product sputtered by the sputtering chamber in the oxidation process can reach 99.9%.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments of the present invention will be briefly described below. Wherein the drawings are only for purposes of illustrating some embodiments of the invention and are not to be construed as limiting the invention to all embodiments thereof.
FIG. 1 is a diagram of a cleaning apparatus for cleaning products according to a fourth embodiment of the present invention;
FIG. 2 is a diagram showing the distribution of substances during the cleaning process of the product of the present invention;
FIG. 3 is a schematic view of a circuit board cleaning system of the present invention;
fig. 4 is a schematic view of an ion distribution region in the cleaning system of the present invention.
Reference numerals are as follows:
1. a main body; 2. a cavity; 3. a vacuum pump set; 4. a separator plate; 5. a flexible joint; 6. a rotating frame; 7. a graphite electrode; 8. an inert gas box; 9. an electromagnetic valve; 10. a vacuum degree detector; 11. a high voltage power supply; 12. and a reactive gas box.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Referring to FIGS. 1-4:
the first embodiment is as follows:
a method of surface oxidation comprising the steps of:
s1, roughly cleaning the surface of the product, and drying the roughly cleaned product by blowing;
s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree range in the vacuum cavity is 0.05 pa;
s3, introducing inert gas into the sputtering chamber, wherein the inert gas introduction speed range is 10sccm, introducing active gas and inert gas into the oxidation chamber, wherein the gas introduction speed range is 10sccm, introducing constant-temperature cooling water into the graphite electrode, rotating the cage provided with the substrate at high speed, rotating the cylindrical target material, and connecting the negative high voltage of the power supply to the graphite electrode by the magnetic field facing the substrate through the insulated electrode;
s4, respectively electrifying the target in the sputtering chamber and the graphite target in the oxidation chamber, wherein the electrifying voltage range is 5000 v;
s5, rotating the sputtered product from the sputtering chamber to the oxidation chamber to complete oxidation, wherein the rotating speed range is 200 q/min;
s6, taking out the product with forceps and placing into a storage box.
The second embodiment:
on the basis of the first embodiment, the surface oxidation method of the first embodiment is further optimized:
a method of surface oxidation comprising the steps of:
s1, roughly cleaning the surface of the product, and drying the roughly cleaned product by blowing;
s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree range in the vacuum cavity is 0.1 pa;
s3, introducing inert gas into the sputtering chamber, introducing the inert gas at a speed range of 200sccm, introducing active gas and the inert gas into the oxidation chamber at a speed range of 200sccm, introducing constant-temperature cooling water into the graphite electrode, rotating the cage provided with the substrate at a high speed, rotating the cylindrical target material at the same time, and connecting the negative high voltage of the power supply to the graphite electrode by the magnetic field facing the substrate through the insulated electrode;
s4, respectively electrifying the target in the sputtering chamber and the graphite target in the oxidation chamber, wherein the electrifying voltage range is 2500 v;
s5, rotating the sputtered product from the sputtering chamber to the oxidation chamber to complete oxidation, wherein the rotating speed range is 150 q/min;
s6, taking out the product with tweezers, and placing the product in a storage box.
Example three:
on the basis of the first embodiment, the surface oxidation method of the first embodiment is further optimized:
a method of surface oxidation comprising the steps of:
s1, roughly cleaning the surface of the product, and drying the roughly cleaned product;
s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree range in the vacuum cavity is 1 pa;
s3, introducing inert gas into the sputtering chamber, wherein the inert gas introduction speed range is 2000sccm, introducing active gas and inert gas into the oxidation chamber, wherein the gas introduction speed range is 2000sccm, introducing constant-temperature cooling water into the graphite electrode, rotating the cage provided with the substrate at a high speed, rotating the cylindrical target material at the same time, and connecting the negative high voltage of the power supply to the graphite electrode by the magnetic field facing the substrate through the insulated electrode;
s4, respectively electrifying the target in the sputtering chamber and the graphite target in the oxidation chamber, wherein the electrifying voltage range is 1000 v;
s5, rotating the sputtered product from the sputtering chamber to the oxidation chamber to complete oxidation, wherein the rotating speed range is 100 q/min;
s6, taking out the product with tweezers, and placing the product in a storage box.
Example four:
on the basis of the first embodiment, the surface oxidation method of the first embodiment is further optimized:
a method of surface oxidation comprising the steps of:
s1, roughly cleaning the surface of the product, and drying the roughly cleaned product;
s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree range in the vacuum cavity is 5 pa;
s3, introducing inert gas into the sputtering chamber, wherein the inert gas is introduced at a speed range of 5000sccm, introducing active gas and inert gas into the oxidation chamber, wherein the gas is introduced at a speed range of 5000sccm, introducing constant-temperature cooling water into the graphite electrode, rotating the cage provided with the substrate at a high speed, rotating the cylindrical target material, and connecting the negative high voltage of the power supply to the graphite electrode by the magnetic field facing the substrate through the insulated electrode;
s4, respectively electrifying the target in the sputtering chamber and the graphite target in the oxidation chamber, wherein the electrifying voltage range is 200 v;
s5, rotating the sputtered product from the sputtering chamber to an oxidation chamber to complete oxidation, wherein the rotating speed range is 50 q/min;
s6, taking out the product with tweezers, and placing the product in a storage box.
The vacuum cavity is divided into a sputtering cavity and an oxidation cavity by the isolation plate 4, the rotating frame and the isolation plate 4 are sealed by the flexible joint 5, a part to be cleaned is placed on the rotating frame 6, and the cavity 2 of the main machine body 1 is vacuumized by the vacuum pump unit 3 to enable the cavity 2 to be a vacuum cavity 2; the vacuum degree detector 10 detects the vacuum degree in the cavity 2, the graphite electrode 7 can be cleaned under different vacuum degrees according to different parts, the graphite electrode 7 is electrically connected with a high-voltage power supply 11, an electric field is formed in the cavity 2, then inert gas and active gas are introduced into the cavity 2 through the inert gas box 8 and the active gas box 12, the electromagnetic valve 9 controls the ventilation speed of the inert gas and the active gas, the cavity 2 is isolated by the isolation plate 4, two sides of the isolation plate 4 are respectively in the inert gas atmosphere and the active gas atmosphere, the inert gas can be helium, neon, argon and the like in the inert gas atmosphere, the selection can be carried out according to production requirements, the graphite electrode emits a large amount of electrons under the action of the electric field to fly to a grounding anode and together with the argon in the vacuum, Oxygen collides to generate ionization to generate plasma, the plasma bombards and cleans residues on the surface of a product, in the active gas atmosphere, positive ions are accelerated to collide with a graphite electrode to generate a sputtering reaction, the graphite electrode and the active gas generate an oxidation reaction, sputtered substances react with oxygen and oxygen ions in the vacuum to generate oxygen compounds and then bombard the surface of the product, negative ions are accelerated to collide with the product and C, CC which is not oxidized, CO2 and CO generated by the reaction bombard the surface of the product, and all the substances exist in the form of gas or electrons finally, so that no residue exists on the product, and the purpose of high-efficiency oxidation is achieved.
The results of testing the surface dyne values and the film layer oxidation rates of the products after cleaning in examples 1-4 are shown in table 1:
TABLE 1
Dyne value Film layer Oxidation Rate (%)
Example one 54 96.4
Example two 56 97.8
EXAMPLE III 60 99.9
Example four 60 99.9
The surface cleanliness dyne value of the product treated by the oxidation method of the embodiment can reach 60, the oxidation rate of the film layer can reach 99.9%, and the effect of oxidizing the surface of the product is effectively improved.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected by one skilled in the art without departing from the spirit and scope of the invention, as defined in the appended claims.

Claims (4)

1. A method of surface oxidation, comprising the steps of:
s1, roughly cleaning the surface of the product, and drying the roughly cleaned product by blowing;
s2, placing the roughly cleaned product into a vacuum cavity, wherein an isolation plate is arranged in the vacuum cavity, the isolation plate divides the vacuum cavity into a sputtering cavity and an oxidation cavity, and vacuumizing the vacuum cavity, wherein the vacuum degree in the vacuum cavity ranges from 5pa to 0.05 pa;
s3, introducing inert gas into the sputtering chamber, introducing the inert gas at a speed range of 10-5000sccm, introducing active gas and the inert gas into the oxidation chamber at a speed range of 10-5000sccm, introducing constant-temperature cooling water into the graphite electrode, rotating the cage provided with the substrate at a high speed, rotating the cylindrical target material with the magnetic field facing the substrate, and connecting the negative high voltage of the power supply to the graphite electrode through the insulating electrode;
s4, respectively electrifying the target in the sputtering chamber and the graphite target in the oxidation chamber, wherein the electrifying voltage range is 200-5000 v;
s5, rotating the sputtered product from the sputtering chamber to the oxidation chamber to complete oxidation, wherein the rotating speed range is 5-200 q/min;
s6, taking out the product with tweezers, and placing the product in a storage box.
2. The method of claim 1, wherein a rotating rack is disposed in the vacuum chamber in step S2, and the rotating rack rotates the product from the sputtering chamber to the oxidation chamber.
3. A surface oxidation method as claimed in claim 1, wherein the inert gas in step S3 is any one of helium, neon, argon, krypton, xenon, and radon gas.
4. A surface oxidation method according to claim 1, wherein the reactive gas in step S5 is oxygen.
CN202110247606.5A 2021-03-06 2021-03-06 Surface oxidation method Pending CN115011937A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110247606.5A CN115011937A (en) 2021-03-06 2021-03-06 Surface oxidation method

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Application Number Priority Date Filing Date Title
CN202110247606.5A CN115011937A (en) 2021-03-06 2021-03-06 Surface oxidation method

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CN115011937A true CN115011937A (en) 2022-09-06

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105803408A (en) * 2014-12-29 2016-07-27 天津三环乐喜新材料有限公司 Neodymium-iron-boron permanent magnet surface protection method
CN107841712A (en) * 2017-11-01 2018-03-27 浙江水晶光电科技股份有限公司 Preparation method, high index of refraction hydrogenated silicon film by utilizing, optical filtering lamination and the optical filter of high index of refraction hydrogenated silicon film by utilizing

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105803408A (en) * 2014-12-29 2016-07-27 天津三环乐喜新材料有限公司 Neodymium-iron-boron permanent magnet surface protection method
CN107841712A (en) * 2017-11-01 2018-03-27 浙江水晶光电科技股份有限公司 Preparation method, high index of refraction hydrogenated silicon film by utilizing, optical filtering lamination and the optical filter of high index of refraction hydrogenated silicon film by utilizing

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