CN117790050A - Double-sided ITO transparent conductive film and preparation method thereof - Google Patents
Double-sided ITO transparent conductive film and preparation method thereof Download PDFInfo
- Publication number
- CN117790050A CN117790050A CN202410004805.7A CN202410004805A CN117790050A CN 117790050 A CN117790050 A CN 117790050A CN 202410004805 A CN202410004805 A CN 202410004805A CN 117790050 A CN117790050 A CN 117790050A
- Authority
- CN
- China
- Prior art keywords
- ions
- ito
- argon
- oxygen
- optical low
- 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
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 230000003287 optical effect Effects 0.000 claims abstract description 45
- 238000002834 transmittance Methods 0.000 claims abstract description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 111
- -1 argon ions Chemical class 0.000 claims description 71
- 229910052786 argon Inorganic materials 0.000 claims description 69
- 239000001301 oxygen Substances 0.000 claims description 62
- 229910052760 oxygen Inorganic materials 0.000 claims description 62
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 36
- 229910052710 silicon Inorganic materials 0.000 claims description 24
- 239000010703 silicon Substances 0.000 claims description 24
- 238000004544 sputter deposition Methods 0.000 claims description 21
- 230000005684 electric field Effects 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 15
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 15
- 239000013077 target material Substances 0.000 claims description 15
- 150000002500 ions Chemical class 0.000 claims description 14
- 229910052709 silver Inorganic materials 0.000 claims description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000004332 silver Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- 239000005329 float glass Substances 0.000 claims description 6
- 238000007747 plating Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 230000000149 penetrating effect Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 32
- 239000004973 liquid crystal related substance Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention belongs to the technical field of transparent conductive films, and particularly discloses a double-sided ITO transparent conductive film and a preparation method thereof. Compared with the prior art, the invention has the advantages that two ITO conductive layers are arranged, and the Ag conductive layers are arranged outside the two ITO conductive layers, so that the resistance of the whole conductive film is lower and more uniform, and the reaction is more sensitive; in addition, the first optical low-refraction layer and the second optical low-refraction layer with the transmittance of more than 96% are arranged on two sides of the Ag conductive layer, the transmittance of the light source penetrating material is high after the front and back surfaces are etched with circuits in the visible light, the display is clearer, the transmittance of the prepared double-sided ITO transparent conductive film is more than 95%, and the sheet resistance is less than 4.0 ohm/sq.
Description
Technical Field
The invention relates to the technical field of transparent conductive films, in particular to a double-sided ITO transparent conductive film and a preparation method thereof.
Background
A Liquid Crystal Display (LCD) is a flat panel display used in various electronic devices. Generally, LCDs include two sheets of polarizing material with a liquid crystal solution between them. Each sheet of polarizing material typically comprises a glass or transparent plastic substrate; liquid Crystals (LC) are used as optical switches. The substrate is typically fabricated with transparent electrodes, typically made of Indium Tin Oxide (ITO) or other conductive metal layers, into which electrical "drive" signals are coupled. The electric field caused by the drive signal can cause a phase change or a state change in the LC material, depending on which phase or state the LC exhibits different reflective properties.
The transparent conductive film should not only have good conductivity, but also have good visible light transmittance and infrared light wave reflection performance. Since the Sn-doped indium oxide thin film (ITO) has high light transmittance (85%) and low resistance in the visible light region and also has good etching properties, it is widely used for electrode films of flat Liquid Crystal Displays (LCDs), electroluminescent displays (ELDs), plasma Displays (PDs), solar cells, energy-saving infrared reflective films, and the like. Dielectric/metal/dielectric (D/M/D) multilayer films have been widely used as an important low emissivity film (hot mirror) in the last 80 th century. However, its research report as a transparent conductive film is less fashionable. From literature searches, it was found that M.Bender and W.Seelig et al in 1998, in Thin Solid Films 326 (1998) 67-71, written "Dependence of film composition and thicknesses on optical and electrical properties ofITO-metal-ITO multilayers (relationship between the photoelectric properties of ITO-metal-ITO multilayers and their film thickness and composition)", which proposed replacing a single ITO Thin film with an ITO/Ag/ITO (I/M/I) multilayers, attempted to obtain better conductivity and lower cost. However, the ITO film is not ideal as a dielectric film, the refractive index (n-2.0) and the resistivity (2-3 orders of magnitude higher than Ag and Cu) of the ITO film are poor in reflection reduction and leakage current, and the I/M/I photoelectric performance of the sandwich structure does not reach the expected value.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a double-sided ITO transparent conductive film and a preparation method thereof.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
the first object of the present invention is to provide a double-sided ITO transparent conductive film, which comprises a first ITO conductive layer, a first optical low-refraction layer, an Ag conductive layer, a second optical low-refraction layer and a second ITO conductive layer from bottom to top.
Further, the first optical low-refraction layer and the second optical low-refraction layer are silicon oxide plating layers, and the thicknesses of the first optical low-refraction layer and the second optical low-refraction layer are 10-15 nanometers.
Further, the transmittance of the first optical low-refraction layer and the second optical low-refraction layer is more than 96%.
Further, the thickness of the first ITO conductive layer and the second ITO conductive layer is 30-40 nanometers.
Further, the thickness of the Ag conductive layer is 10-13 nanometers.
A second object of the present invention is to provide a method for producing a transparent conductive film of double-sided ITO, comprising the steps of:
s1, filling a proper amount of argon and oxygen into an ITO rotary target of a magnetron sputtering device in a high vacuum state of 10 < -7 > Torr, wherein the flow rate of the filled argon is 150sccm, and the flow rate of the filled oxygen is 20sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike an ITO target material, sputtering ITO ions, and combining the ITO ions and the oxygen ions in an electric field to sputter at a speed in the upper end face of a float glass substrate to form a first ITO conductive layer; filling a proper amount of argon and oxygen into a silicon rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 500sccm, and the flow rate of the filled oxygen is 200sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike a silicon target material, sputtering silicon ions, combining the silicon ions and the oxygen ions to generate silicon oxide, and sputtering the silicon oxide on the upper end face of the first ITO conductive layer in an electric field to form a first optical low-refraction layer; filling argon with the flow of 500sccm into a silver rotary target of a magnetron sputtering device; applying high-voltage direct current of 20A and 460V to ionize argon into argon ions, and accelerating to strike a pure silver target material to sputter silver ions; silver ions are sputtered at an accelerated speed in an electric field to form an Ag conductive layer on the upper end face of the first optical low-refraction layer; filling a proper amount of argon and oxygen into a silicon rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 500sccm, and the flow rate of the filled oxygen is 200sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike a silicon target material, sputtering silicon ions, combining the silicon ions and the oxygen ions to generate silicon oxide, and sputtering the silicon oxide on the upper end face of the Ag conductive layer in an electric field to form a second optical low-refraction layer; filling a proper amount of argon and oxygen into an ITO rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 150sccm, and the flow rate of the filled oxygen is 20sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike an ITO target material, sputtering ITO ions, combining the ITO ions and the oxygen ions in an electric field, and sputtering the ITO ions and the oxygen ions at an accelerating speed in the upper end face of the second optical low-refraction layer to form a second ITO conductive layer;
s2, baking at high temperature
Putting the plated conductive film into a roll-to-roll baking furnace with the set temperature of 150 ℃ and baking at a high temperature for 60 minutes to crystallize the plated first ITO conductive layer and the plated second ITO conductive layer after the high temperature so as to achieve stable properties; and (5) removing the transparent conductive film from the float glass substrate to obtain the double-sided ITO transparent conductive film.
Compared with the prior art, the invention has the advantages that two ITO conductive layers are arranged, and the Ag conductive layers are arranged outside the two ITO conductive layers, so that the resistance of the whole conductive film is lower and more uniform, and the reaction is more sensitive; in addition, the first optical low-refraction layer and the second optical low-refraction layer with the transmittance of more than 96% are arranged on two sides of the Ag conductive layer, the transmittance of the light source penetrating material is high after the front and back surfaces are etched with circuits in the visible light, the display is clearer, the transmittance of the prepared double-sided ITO transparent conductive film is more than 95%, and the sheet resistance is less than 4.0 ohm/sq.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
The present invention will be further described in detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. The specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
As shown in fig. 1, the present embodiment exemplarily provides a double-sided ITO transparent conductive film, which includes, from bottom to top, a first ITO conductive layer 1, a first optical low-refractive layer 2, an Ag conductive layer 3, a second optical low-refractive layer 4, and a second ITO conductive layer 5. Wherein: the first optical low-refraction layer 2 and the second optical low-refraction layer 4 are silicon oxide plating layers, and the thicknesses of the first optical low-refraction layer 2 and the second optical low-refraction layer 4 are 13 nanometers. The transmittance of the first optical low-refraction layer 2 and the second optical low-refraction layer 4 is more than 96 percent. The thicknesses of the first ITO conductive layer 1 and the second ITO conductive layer 5 are 40 nanometers. The thickness of the Ag conductive layer 3 was 11 nm.
The preparation method of the double-sided ITO transparent conductive film comprises the following steps:
s1, filling a proper amount of argon and oxygen into an ITO rotary target of a magnetron sputtering device in a high vacuum state of 10 < -7 > Torr, wherein the flow rate of the filled argon is 150sccm, and the flow rate of the filled oxygen is 20sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike an ITO target material, sputtering ITO ions, and combining the ITO ions and the oxygen ions in an electric field to sputter at a speed in the upper end face of the float glass substrate 6 to form a first ITO conductive layer 1; filling a proper amount of argon and oxygen into a silicon rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 500sccm, and the flow rate of the filled oxygen is 200sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike a silicon target material, sputtering silicon ions, combining the silicon ions and the oxygen ions to generate silicon oxide, and sputtering the silicon oxide on the upper end face of the first ITO conductive layer 1 in an electric field to form a first optical low-refraction layer 2; filling argon with the flow of 500sccm into a silver rotary target of a magnetron sputtering device; applying high-voltage direct current of 20A and 460V to ionize argon into argon ions, and accelerating to strike a pure silver target material to sputter silver ions; silver ions are sputtered at an accelerated speed in an electric field to form an Ag conductive layer 3 on the upper end face of the first optical low-refraction layer 2; filling a proper amount of argon and oxygen into a silicon rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 500sccm, and the flow rate of the filled oxygen is 200sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike a silicon target material, sputtering silicon ions, combining the silicon ions and the oxygen ions to generate silicon oxide, and sputtering the silicon oxide on the upper end face of the Ag conductive layer 3 in an electric field to form a second optical low-refraction layer 4; filling a proper amount of argon and oxygen into an ITO rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 150sccm, and the flow rate of the filled oxygen is 20sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike an ITO target material, sputtering ITO ions, combining the ITO ions and the oxygen ions in an electric field, and accelerating sputtering on the upper end face of the second optical low-refraction layer 4 to form a second ITO conductive layer 5;
s2, baking at high temperature
Putting the plated conductive film into a roll-to-roll baking furnace with the set temperature of 150 ℃ and baking at a high temperature for 60 minutes to crystallize the plated first ITO conductive layer and the plated second ITO conductive layer after the high temperature so as to achieve stable properties; and (5) removing the transparent conductive film from the float glass substrate to obtain the double-sided ITO transparent conductive film.
Further, the above-prepared double-sided ITO transparent conductive film was subjected to optical detection, impedance and linearity detection, and physical property detection by conventional methods in the art, and the performance parameters thereof are specifically shown in tables 1 and 2.
TABLE 1
TABLE 2
As can be seen from table 1, the prepared double-sided ITO transparent conductive film has a first optical low-refractive layer and a second optical low-refractive layer with a transmittance of more than 96% on both sides of the Ag conductive layer, and the transmittance of the light source passing through the material after etching the circuit on both sides is high and the display is clearer, so that the LCD display using the double-sided ITO copper conductive film has better display effect.
As can be seen from table 2, the square resistances of the front and back sides of the prepared double-sided ITO transparent conductive film are uniform, and after the circuit is etched, a certain voltage is applied to the circuit, and the current becomes more stable.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.
Claims (6)
1. The double-sided ITO transparent conductive film is characterized by sequentially comprising a first ITO conductive layer, a first optical low-refraction layer, an Ag conductive layer, a second optical low-refraction layer and a second ITO conductive layer from bottom to top.
2. The double-sided ITO transparent conductive film according to claim 1, characterized in that: the first optical low-refraction layer and the second optical low-refraction layer are silicon oxide plating layers, and the thicknesses of the first optical low-refraction layer and the second optical low-refraction layer are 10-15 nanometers.
3. The double-sided ITO transparent conductive film according to claim 1, characterized in that: the transmittance of the first optical low-refraction layer and the second optical low-refraction layer is more than 96 percent.
4. The double-sided ITO transparent conductive film according to claim 1, characterized in that: the thickness of the first ITO conductive layer and the second ITO conductive layer is 30-40 nanometers.
5. The double-sided ITO transparent conductive film according to claim 1, characterized in that: the thickness of the Ag conductive layer is 10-13 nanometers.
6. A method for producing the double-sided ITO transparent conductive film according to any one of claims 1 to 5, comprising the steps of:
s1, filling a proper amount of argon and oxygen into an ITO rotary target of a magnetron sputtering device in a high vacuum state of 10 < -7 > Torr, wherein the flow rate of the filled argon is 150sccm, and the flow rate of the filled oxygen is 20sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike an ITO target material, sputtering ITO ions, and combining the ITO ions and the oxygen ions in an electric field to sputter at a speed in the upper end face of a float glass substrate to form a first ITO conductive layer; filling a proper amount of argon and oxygen into a silicon rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 500sccm, and the flow rate of the filled oxygen is 200sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike a silicon target material, sputtering silicon ions, combining the silicon ions and the oxygen ions to generate silicon oxide, and sputtering the silicon oxide on the upper end face of the first ITO conductive layer in an electric field to form a first optical low-refraction layer; filling argon with the flow of 500sccm into a silver rotary target of a magnetron sputtering device; applying high-voltage direct current of 20A and 460V to ionize argon into argon ions, and accelerating to strike a pure silver target material to sputter silver ions; silver ions are sputtered at an accelerated speed in an electric field to form an Ag conductive layer on the upper end face of the first optical low-refraction layer; filling a proper amount of argon and oxygen into a silicon rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 500sccm, and the flow rate of the filled oxygen is 200sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike a silicon target material, sputtering silicon ions, combining the silicon ions and the oxygen ions to generate silicon oxide, and sputtering the silicon oxide on the upper end face of the Ag conductive layer in an electric field to form a second optical low-refraction layer; filling a proper amount of argon and oxygen into an ITO rotary target of the magnetron sputtering equipment, wherein the flow rate of the filled argon is 150sccm, and the flow rate of the filled oxygen is 20sccm; applying high-voltage direct current of 20A and 460V to ionize argon and oxygen into argon ions and oxygen ions, enabling the argon ions to accelerate to strike an ITO target material, sputtering ITO ions, combining the ITO ions and the oxygen ions in an electric field, and sputtering the ITO ions and the oxygen ions at an accelerating speed in the upper end face of the second optical low-refraction layer to form a second ITO conductive layer;
s2, baking at high temperature
Putting the plated conductive film into a roll-to-roll baking furnace with the set temperature of 150 ℃ and baking at a high temperature for 60 minutes to crystallize the plated first ITO conductive layer and the plated second ITO conductive layer after the high temperature so as to achieve stable properties; and (5) removing the transparent conductive film from the float glass substrate to obtain the double-sided ITO transparent conductive film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410004805.7A CN117790050A (en) | 2024-01-03 | 2024-01-03 | Double-sided ITO transparent conductive film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410004805.7A CN117790050A (en) | 2024-01-03 | 2024-01-03 | Double-sided ITO transparent conductive film and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117790050A true CN117790050A (en) | 2024-03-29 |
Family
ID=90383491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410004805.7A Pending CN117790050A (en) | 2024-01-03 | 2024-01-03 | Double-sided ITO transparent conductive film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117790050A (en) |
-
2024
- 2024-01-03 CN CN202410004805.7A patent/CN117790050A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP3031224B2 (en) | Transparent conductive film | |
| US20110102722A1 (en) | Indium tin oxide sputtering target and transparent conductive film fabricated using the same | |
| JP4168689B2 (en) | Thin film laminate | |
| CN105489270B (en) | A kind of sandwich transparent conductive film and preparation method thereof | |
| CN117790050A (en) | Double-sided ITO transparent conductive film and preparation method thereof | |
| CN114231903B (en) | Niobium oxide/silver nanowire double-layer structure flexible transparent conductive film and preparation method thereof | |
| CN205486019U (en) | Touch screen circuit board | |
| CN201713564U (en) | Izao transparent conductive film | |
| CN218647648U (en) | Double-sided ITO copper conductive film | |
| WO2009093580A1 (en) | Process for producing liquid crystal display device | |
| CN209297774U (en) | A kind of two-sided shadow ITO conductive film that disappears of touch screen double-sided coating | |
| JP3654841B2 (en) | Transparent conductive film and method for producing the same | |
| CN217690518U (en) | Two-sided blackened copper conducting film | |
| JPH10208554A (en) | Transparent conductive film and liquid crystal element using the same | |
| CN209297772U (en) | A kind of room temperature coating single side single side disappears shadow super thick ITO conductive film | |
| CN113990555B (en) | ITO conductive film for touch sensor, preparation method thereof and touch screen application | |
| CN111273496B (en) | Array substrate and preparation method thereof | |
| US11930649B2 (en) | Transparent top electrode composite film for organic optoelectronic devices and its preparation method | |
| CN108517500A (en) | A kind of preparation method of ST/Ag/ST structures multi-layer transparent electroconductive film | |
| CN217386689U (en) | Low-reflection ITO film | |
| CN114927261A (en) | Double-sided blackened copper conductive film and preparation method thereof | |
| CN115074666B (en) | Preparation method of multilayer composite ITO film | |
| CN217426385U (en) | Low-resistance high-transmittance ITO conductive film | |
| JPH0468315A (en) | Transparent conductive film and production thereof | |
| JPH04340522A (en) | Transparent conductive film |
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 |