CN116590711A - Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof - Google Patents

Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof Download PDF

Info

Publication number
CN116590711A
CN116590711A CN202310555181.3A CN202310555181A CN116590711A CN 116590711 A CN116590711 A CN 116590711A CN 202310555181 A CN202310555181 A CN 202310555181A CN 116590711 A CN116590711 A CN 116590711A
Authority
CN
China
Prior art keywords
palladium
chemical mechanical
copper
polishing
mechanical polishing
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
Application number
CN202310555181.3A
Other languages
Chinese (zh)
Inventor
张驰
石磊
施元军
殷岚勇
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.)
Suzhou Jingsheng Micro Nano Semiconductor Technology Co ltd
Original Assignee
Suzhou Jingsheng Micro Nano Semiconductor Technology 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 Suzhou Jingsheng Micro Nano Semiconductor Technology Co ltd filed Critical Suzhou Jingsheng Micro Nano Semiconductor Technology Co ltd
Priority to CN202310555181.3A priority Critical patent/CN116590711A/en
Publication of CN116590711A publication Critical patent/CN116590711A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • 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
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F3/00Brightening metals by chemical means
    • C23F3/04Heavy metals

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

The application provides a polishing solution for palladium and copper chemical mechanical polishing, a preparation method and a use method thereof. The polishing solution for the chemical mechanical polishing of palladium and copper comprises the following components in percentage by weight: 0.5 to 10 percent of nano diamond, 5 to 10 percent of complexing agent, 0.03 to 0.05 percent of corrosion inhibitor, 0.02 to 1 percent of pH regulator and 83 to 95 percent of deionized water. The polishing solution can be used for removing redundant materials on the surface of a workpiece and flattening the workpiece in a global nanoscale manner aiming at palladium-copper coplanar materials with the same thickness, so that the phenomenon that metal crosslinking loses the flatness of the workpiece due to multilayer superposition effect is avoided, and the subsequent photoetching process is facilitated.

Description

Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof
Technical Field
The application belongs to the technical field of polishing solutions, and particularly relates to a polishing solution for chemical mechanical polishing of palladium and copper, a preparation method and a use method thereof.
Background
Chemical mechanical polishing (Chemical Mechanical Polishing, CMP) is a means of achieving global planarization in integrated circuit fabrication, while the polishing slurry is a mixture used during the workpiece surface planarization process that includes abrasive materials and chemical additives. Currently, the chemical mechanical polishing slurry used for electroplating palladium materials has a composition similar to metallic copper, i.e., a silica slurry. The silicon dioxide polishing solution mainly comprises grinding particles, a metal corrosion inhibitor, a complexing agent, an oxidant and the like. In recent years, the surface of a substrate is often plated with a palladium material as a functional material, and also plated with a copper material as an auxiliary material. After the substrate is ground, a flat surface with palladium and copper coexisting is formed on the front surface of the workpiece, wherein the Roughness (Roughness) is measured to be 0.08-0.1 mu m by a 3D microscope, and the surface Roughness is 0.041 mu m after the substrate is ground.
However, the above processing results cannot meet the process requirements. It has the following problems: first, the object of the chemical mechanical polishing is palladium copper coplanar material with the same thickness, and the effect of the chemical mechanical polishing treatment on palladium and copper is greatly different. The chemical property of palladium is inactive, the palladium can be kept stable in air and a humid environment at normal temperature, weak acid corrosion resistance is realized, and even the removal of oxides of palladium is required to be performed at high temperature, so that an oxidant with oxidation corrosion effect on copper in a polishing solution cannot corrode palladium, and the problem that the removal rate of the two is large is caused, for example, when copper has a removal amount of 6 mu m, copper and palladium form a height difference of 1.45 mu m, and the surface of a substrate is uneven. Secondly, as the removal increases, the difference in height between palladium and copper increases. In addition, palladium is higher than copper in height and has no supporting function of copper, radian can be formed due to mechanical action in the chemical mechanical polishing process, and the requirements of product morphology and usability cannot be met. In summary, the above factors ultimately lead to failure of the workpiece to achieve global nanoscale planarization, and subsequent photolithography processes are also not performed.
Therefore, there is a need in the art to develop a chemical mechanical polishing solution for palladium copper coplanar materials, so as to solve the above-mentioned problems and meet the use requirements.
Disclosure of Invention
Aiming at the defects of the prior art, the application aims to provide a polishing solution for palladium and copper chemical mechanical polishing, and a preparation method and a use method thereof. The polishing solution can be used for removing redundant materials on the surface of a workpiece and flattening the workpiece in a global nanoscale manner aiming at palladium-copper coplanar materials with the same thickness, so that the phenomenon that metal crosslinking loses the flatness of the workpiece due to multilayer superposition effect is avoided, and the subsequent photoetching process is facilitated.
In order to achieve the aim of the application, the application adopts the following technical scheme:
in a first aspect, the present application provides a polishing solution for palladium and copper chemical mechanical polishing, which comprises the following components in percentage by weight:
according to the application, through improving the composition of the polishing solution, no oxidizing agent is added, the added nano-grade diamond grinding particles have the advantages of high hardness and low friction coefficient, the surface roughness of palladium and copper polished by adopting the chemical mechanical polishing solution with the specific composition is low, the two materials of palladium and copper can be taken into account, the removal amount of the two materials is ensured to be consistent, and the effect of global nano-grade planarization can be achieved.
In addition, the application ensures that the removal amount of palladium and copper is basically balanced by regulating and controlling the content of various components, and the removal amount is not generated when the content is too low, otherwise, the surface of the wafer is embossed to generate steps.
In the present application, the weight percentage of the nanodiamond is 0.5 to 10%, for example, may be 0.5%, 1%, 2%, 5%, 8%, 10%, etc.
In the present application, the complexing agent may be 5-10% by weight, for example, 5%, 6%, 7%, 8%, 9%, 10% by weight, etc.
In the present application, the weight percentage of the corrosion inhibitor is 0.03 to 0.05%, for example, may be 0.03%, 0.035%, 0.04%, 0.045%, 0.05%, etc.
In the present application, the weight percentage of the pH adjuster is 0.02 to 1%, for example, may be 0.02%, 0.05%, 0.08%, 0.1%, 0.5%, 0.8%, 1%, etc.
In the present application, the deionized water may be 83-95% by weight, for example, 83%, 85%, 88%, 90%, 92%, 95% by weight, etc.
Preferably, the polishing solution for palladium and copper chemical mechanical polishing consists of the following components in percentage by weight:
the particle size distribution of the nanodiamond is preferably 10 to 100nm, preferably 20 to 80nm, and may be, for example, 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm, 80nm, 90nm, 100nm, etc.
Preferably, the average particle size of the nanodiamond is 60nm, preferably 50nm.
Preferably, the complexing agent comprises any one or a combination of at least two of ethylenediamine tetraacetic acid, ethylenediamine, malonic acid or oxalic acid.
Preferably, the corrosion inhibitor comprises any one or a combination of at least two of benzene propane triazole, 5-phenyl tetrazole or hydrophobic phenyl tetrazole.
Preferably, the pH adjuster comprises any one or a combination of at least two of sodium chloride solution, ammonium acetate or potassium nitrate.
Preferably, the mass ratio of the nano diamond to the complexing agent is (0.5-1): 1, for example, 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, etc.
In the application, the removal amount of palladium and copper is balanced by adjusting the mass ratio of the nano diamond to the complexing agent, if the mass ratio is too low, the removal amount is not available, otherwise, the height difference between the palladium and the copper is caused to generate a step.
In a second aspect, the present application provides a method for preparing the polishing liquid for palladium and copper chemical mechanical polishing according to the first aspect, the method comprising the steps of:
and (3) mixing the complexing agent, the corrosion inhibitor and deionized water for the first time to obtain a first mixed solution, then mixing the first mixed solution and the nano diamond for the second time to obtain a second mixed solution, adding a pH regulator, and then adjusting the pH value of the system to obtain the polishing solution for the chemical mechanical polishing of palladium and copper.
Preferably, the pH of the conditioning system is 6.95.
In a third aspect, the present application provides a method for using the polishing liquid for palladium and copper chemical mechanical polishing according to the first aspect, the method comprising: the polishing solution for the chemical mechanical polishing of palladium and copper is subjected to chemical mechanical polishing.
Preferably, the chemical mechanical polishing is performed at a pressure of 2psi for 30 minutes at a rotational speed of 70rpm.
Preferably, the polishing solution for palladium and copper chemical mechanical polishing is used in an amount of 3mL/min.
Compared with the prior art, the application has the following beneficial effects:
the application provides a polishing solution for chemical mechanical polishing of palladium and copper, which has the advantages of large hardness and low friction coefficient by improving the composition of the polishing solution and not adding an oxidant, and the added nano-scale diamond grinding particles have the advantages of low surface roughness of palladium and copper after being polished by adopting the chemical mechanical polishing solution with the specific composition, can give consideration to both materials of palladium and copper, ensure the consistent removal quantity of the two materials and achieve the effect of global nano-scale planarization.
In addition, the application ensures that the removal amount of palladium and copper is basically balanced by regulating and controlling the content of various components, and the removal amount is not generated when the content is too low, otherwise, the surface of the wafer is embossed.
Drawings
FIG. 1 is a graph showing the effect of a substrate polished by the polishing liquid provided in application example 1;
fig. 2 is an effect diagram of a substrate polished by the polishing liquid provided in comparative application example 1.
Detailed Description
The technical scheme of the application is further described below by combining the attached drawings and the specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the application and are not to be construed as a specific limitation thereof.
Example 1
The embodiment provides a polishing solution for palladium and copper chemical mechanical polishing, which comprises the following components in percentage by weight:
the particle size distribution of the nano diamond is 10-100 nm, the average particle diameter is 60nm, and the mass ratio of the nano diamond to the ethylenediamine tetraacetic acid complexing agent is 0.5:1.
The embodiment also provides a preparation method of the polishing solution, which comprises the following steps:
preparing a primary mixed solution with the volume of 500mL by using an ethylenediamine tetraacetic acid complexing agent, a benzotriazole corrosion inhibitor and deionized water with the resistivity of 6MΩ & cm, then secondarily mixing the primary mixed solution with nano diamond to obtain a secondary mixed solution, adding a sodium chloride solution, and then adjusting the pH value of the system to 6.95 to obtain the polishing solution for palladium and copper chemical mechanical polishing.
Example 2
The embodiment provides a polishing solution for palladium and copper chemical mechanical polishing, which comprises the following components in percentage by weight:
the particle size distribution of the nano diamond is 10-100 nm, the average particle diameter is 60nm, and the mass ratio of the nano diamond to the ethylenediamine tetraacetic acid complexing agent is 0.5:1.
The embodiment also provides a preparation method of the polishing solution, which comprises the following steps:
preparing a primary mixed solution with the volume of 500mL by using an ethylenediamine tetraacetic acid complexing agent, a benzotriazole corrosion inhibitor and deionized water with the resistivity of 6MΩ & cm, then secondarily mixing the primary mixed solution with nano diamond to obtain a secondary mixed solution, adding a sodium chloride solution, and then adjusting the pH value of the system to 6.95 to obtain the polishing solution for palladium and copper chemical mechanical polishing.
Example 3
The embodiment provides a polishing solution for palladium and copper chemical mechanical polishing, which comprises the following components in percentage by weight:
the particle size distribution of the nano diamond is 10-100 nm, the average particle diameter is 60nm, and the mass ratio of the nano diamond to the ethylenediamine tetraacetic acid complexing agent is 0.5:1.
The embodiment also provides a preparation method of the polishing solution, which comprises the following steps:
preparing a primary mixed solution with the volume of 500mL by using an ethylenediamine tetraacetic acid complexing agent, a benzotriazole corrosion inhibitor and deionized water with the resistivity of 6MΩ & cm, then secondarily mixing the primary mixed solution with nano diamond to obtain a secondary mixed solution, adding a sodium chloride solution, and then adjusting the pH value of the system to 6.95 to obtain the polishing solution for palladium and copper chemical mechanical polishing.
Example 4
The embodiment provides a polishing solution for palladium and copper chemical mechanical polishing, which comprises the following components in percentage by weight:
the particle size distribution of the nano diamond is 10-100 nm, the average particle diameter is 60nm, and the mass ratio of the nano diamond to the ethylenediamine tetraacetic acid complexing agent is 0.5:1.
The embodiment also provides a preparation method of the polishing solution, which comprises the following steps:
preparing a primary mixed solution with the volume of 500mL by using an ethylenediamine tetraacetic acid complexing agent, a benzotriazole corrosion inhibitor and deionized water with the resistivity of 6MΩ & cm, then secondarily mixing the primary mixed solution with nano diamond to obtain a secondary mixed solution, adding a sodium chloride solution, and then adjusting the pH value of the system to 6.95 to obtain the polishing solution for palladium and copper chemical mechanical polishing.
Example 5
The embodiment provides a polishing solution for palladium and copper chemical mechanical polishing, which comprises the following components in percentage by weight:
the particle size distribution of the nano diamond is 10-100 nm, the average particle diameter is 60nm, and the mass ratio of the nano diamond to the ethylenediamine tetraacetic acid complexing agent is 1:1.
The embodiment also provides a preparation method of the polishing solution, which comprises the following steps:
preparing a primary mixed solution with the volume of 500mL by using an ethylenediamine tetraacetic acid complexing agent, a benzotriazole corrosion inhibitor and deionized water with the resistivity of 6MΩ & cm, then secondarily mixing the primary mixed solution with nano diamond to obtain a secondary mixed solution, adding a sodium chloride solution, and then adjusting the pH value of the system to 6.95 to obtain the polishing solution for palladium and copper chemical mechanical polishing.
Example 6
This example differs from example 1 in that the mass ratio of nanodiamond to complexing agent is 0.05:1, all other things being equal to example 1.
Example 7
This example differs from example 1 in that the mass ratio of nanodiamond to complexing agent is 1:0.5, all other things being equal to example 1.
Comparative example 1
This comparative example differs from example 1 in that nanodiamond was replaced with an equal amount of alumina, all other things being equal to example 1.
Comparative example 2
The comparative example differs from example 1 in that the weight percent of nanodiamond in the slurry was 0.1%, and the deionized water content was adjusted adaptively so that the total weight percent was 100%, all other things being equal to example 1.
Comparative example 3
The comparative example differs from example 1 in that the weight percentage of nanodiamond in the polishing liquid was 15%, and the content of deionized water was adjusted adaptively so that the total weight percentage of the total system was 100%, and the other was the same as example 1.
Comparative example 4
This comparative example provides a silica polishing solution comprising the following components:
application examples 1 to 7 and comparative application examples 1 to 4
The polishing solutions provided in examples 1 to 7 and comparative examples 1 to 4 were used for polishing palladium-copper wafers as follows:
the palladium-copper wafer with the size of 4 inches was polished with the above-mentioned slurry at a polishing pressure of 2psi, a polishing disk rotation speed of 70rpm, a slurry flow rate of 3mL/min, and a polishing time of 30min.
Test conditions
The palladium-copper wafers provided in application examples 1 to 7 and comparative application examples 1 to 4 were tested as follows:
(1) Surface roughness: measurement using a 3D microscope;
(2) Thickness: measuring by using a step instrument;
(3) Polishing rate: i.e., the difference in thickness between before and after polishing divided by the polishing time.
The test results are shown in table 1:
TABLE 1
As can be seen from Table 1, FIG. 1 and FIG. 2, the surface roughness of palladium and copper polished by the chemical mechanical polishing solution with specific composition is low, and the two materials of palladium and copper can be taken into account, so that the removal amounts of the two materials are consistent, and the effect of global nanoscale planarization can be achieved.
Compared with application example 1, application examples 6-7 are the conditions that the mass ratio of the nano diamond to the complexing agent is out of a limit range, if the mass ratio is too low, the removal amount is not available, otherwise, the height difference between palladium and copper is caused to generate steps, and the surface roughness is higher.
Compared with the case of replacing nano diamond in application example 1, the polishing rate is slower and the roughness is higher; comparative application examples 2 to 3 are cases where the weight percentage of nanodiamond is out of a defined range; comparative application example 4 provides a silica polishing solution containing an oxidizing agent, which does not achieve the technical effect of the present application.
The applicant states that the process of the application is illustrated by the above examples, but the application is not limited to, i.e. does not mean that the application must be carried out in dependence on the above process steps. It should be apparent to those skilled in the art that any modification of the present application, equivalent substitution of selected raw materials, addition of auxiliary components, selection of specific modes, etc. fall within the scope of the present application and the scope of disclosure.

Claims (10)

1. The polishing solution for the chemical mechanical polishing of palladium and copper is characterized by comprising the following components in percentage by weight:
2. the polishing liquid for palladium and copper chemical mechanical polishing according to claim 1, wherein the polishing liquid for palladium and copper chemical mechanical polishing is composed of the following components in percentage by weight:
3. polishing liquid for palladium and copper chemical mechanical polishing according to claim 1 or 2, characterized in that the particle size distribution of the nanodiamond is 10 to 100nm, preferably 20 to 80nm;
preferably, the average particle size of the nanodiamond is 60nm, preferably 50nm;
preferably, the complexing agent comprises any one or a combination of at least two of ethylenediamine tetraacetic acid, ethylenediamine, malonic acid or oxalic acid.
4. The polishing liquid for chemical mechanical polishing of palladium and copper according to any one of claims 1 to 3, wherein the corrosion inhibitor comprises any one of or a combination of at least two of benzotriazol, 5-phenyltetrazol, or mercaptophenyltetrazol;
preferably, the pH adjuster comprises any one or a combination of at least two of sodium chloride solution, ammonium acetate or potassium nitrate.
5. The polishing liquid for chemical mechanical polishing of palladium and copper according to any one of claims 1 to 4, wherein the mass ratio of the nanodiamond to the complexing agent is (0.5 to 1): 1.
6. A method of preparing the polishing liquid for palladium and copper chemical mechanical polishing according to any one of claims 1 to 5, characterized by comprising the steps of:
and (3) mixing the complexing agent, the corrosion inhibitor and deionized water for the first time to obtain a first mixed solution, then mixing the first mixed solution and the nano diamond for the second time to obtain a second mixed solution, adding a pH regulator, and then adjusting the pH value of the system to obtain the polishing solution for the chemical mechanical polishing of palladium and copper.
7. The method of claim 6, wherein the pH of the conditioning system is 6.95.
8. A method of using the polishing liquid for palladium and copper chemical mechanical polishing according to any one of claims 1 to 5, comprising: the polishing solution for the chemical mechanical polishing of palladium and copper is subjected to chemical mechanical polishing.
9. The method of claim 8, wherein the chemical mechanical polishing is performed at a pressure of 2psi, a time of 30 minutes, and a rotational speed of 70rpm.
10. The method of use according to claim 8 or 9, wherein the polishing liquid for use in the chemical mechanical polishing of palladium and copper is used in an amount of 3mL/min.
CN202310555181.3A 2023-05-17 2023-05-17 Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof Pending CN116590711A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310555181.3A CN116590711A (en) 2023-05-17 2023-05-17 Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310555181.3A CN116590711A (en) 2023-05-17 2023-05-17 Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof

Publications (1)

Publication Number Publication Date
CN116590711A true CN116590711A (en) 2023-08-15

Family

ID=87607575

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310555181.3A Pending CN116590711A (en) 2023-05-17 2023-05-17 Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof

Country Status (1)

Country Link
CN (1) CN116590711A (en)

Similar Documents

Publication Publication Date Title
CN102516875B (en) Polishing solution based on polishing process of metal Co and application thereof
Zhang et al. Two-step chemical mechanical polishing of sapphire substrate
EP1190005A1 (en) Magnetic polishing fluids
EP1272579B1 (en) Method for polishing a memory or rigid disk with an amino acid-containing composition
KR20010029433A (en) Polishing composition and polishing process
WO2005014753A1 (en) Non-polymeric organic particles for chemical mechanical planarization
KR20070105301A (en) Aqueous slurry containing metallate-modified silica particles
TWI736623B (en) Chemical mechanical polishing slurry composition
CN1955249B (en) Chemical mechanical polishing material for tantalum barrier layer
WO2005093805A1 (en) Composition for polishing semiconductor
CN111040640A (en) Composite abrasive chemical mechanical polishing slurry for silicon wafer substrate and preparation method thereof
KR20180089307A (en) Chemical mechanical polishing method for tungsten
CN103382368A (en) Chemical machinery planarization slurry
CN101665664B (en) Quaternary ammonium salt cationic surfactant and application of chemical mechanical polishing solution
CN107936848B (en) Polishing solution for polishing silicon substrate and preparation method thereof
JP3653133B2 (en) Polishing composition, magnetic disk substrate polishing method, and manufacturing method
WO2006122492A1 (en) Polishing slurry
KR20020010910A (en) Magnetic polishing fluids
WO2014112418A1 (en) Polishing solution for metal and polishing method
CN116590711A (en) Polishing solution for palladium and copper chemical mechanical polishing and preparation method and application method thereof
JP4346712B2 (en) Wafer edge polishing method
JP2017063173A (en) Method for polishing semiconductor substrate
JP6379764B2 (en) Polishing liquid and polishing method
WO2011077973A1 (en) Polishing agent for copper polishing and polishing method using the same
JP2006012969A (en) Silica sol for polish, and its manufacturing method

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