CN110093641A - A kind of micro-structure is without magnetic property method and system - Google Patents

A kind of micro-structure is without magnetic property method and system Download PDF

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CN110093641A
CN110093641A CN201910326158.0A CN201910326158A CN110093641A CN 110093641 A CN110093641 A CN 110093641A CN 201910326158 A CN201910326158 A CN 201910326158A CN 110093641 A CN110093641 A CN 110093641A
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micro
ultra
anode
fine linear
conductive substrates
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张新民
孔泽宇
明平美
郑兴帅
闫亮
王伟
李新潮
侯亚楠
李云涛
秦歌
杨文娟
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Henan University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D17/00Constructional parts, or assemblies thereof, of cells for electrolytic coating
    • C25D17/10Electrodes, e.g. composition, counter electrode
    • C25D17/12Shape or form
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/02Electroplating of selected surface areas
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/04Electroplating with moving electrodes

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Abstract

The invention patent discloses a kind of micro-structure without magnetic property method and system, the system includes that power supply, X-Y-Z triaxial movement platform, holding frame, the conductive substrates being placed on the X-Y platform of X-Y-Z triaxial movement platform, the glass capillary being fixed on the Z axis of X-Y-Z triaxial movement platform by holding frame, the accurate micro-shifting moving cell for the surface be fixed on holding frame and be located at glass capillary and lower part are coaxially placed in glass capillary, and the ultra-fine linear anode that upper end is located at the top of glass capillary and is fixedly connected with accurate micro-shifting moving cell.Based on the system, electro-deposition goes out first layer metal layer in meniscus limitation range first in conductive substrates, then using first layer metal layer as substrate, continue electro-deposition second layer metal layer ... in meniscus limitation range on it and so persistently carry out, until reaching processing request.The configuration of the present invention is simple, operation is easy, at low cost, can obtain the metal micro structure of better quality.

Description

A kind of micro-structure is without magnetic property method and system
Technical field
The present invention relates to a kind of electro-deposition method and systems more particularly to a kind of micro-structure without magnetic property method and to be System.
Background technique
Minute manufacturing technology is the basic manufacturing industry of relationship national economy, is super large-scale integration, micro-electro-mechanical systems The core technology of system, modern precision optical system etc..Metal micro structure is one of main object of minute manufacturing.Electrochemistry micro-nano The features such as processing technology is low with its technological temperature, and machinable material range is wide, without heat/power cause defect, in field of micro-Na manufacture There is extremely important status.By process principle point, it is (former based on anodic solution that electrochemistry micro-nano technology can be divided into electrochemical micromachining Reason) and electro-deposition micro Process (being based on negative electrode electro-deposition principle) two types.Electro-deposition micro Process is a kind of layer-by-layer accumulation mode Micro-processing technology, including magnetic property micro Process and no magnetic property micro Process.In comparison, no magnetic property is micro- adds Work in terms of manufacturing complicated shape micro-nano structure advantageously.Commonly have without magnetic property micro-processing method: local growth Electro-deposition, jet stream electro-deposition and crescent electrolyte constrain three-dimensional electro-deposition forming.
Local growth electro-deposition induce electrochemical reaction using the local electric field that tip orients, in conductive substrates at Shape 3-dimensional metal micro-structure.Local grows smallest cross-sectional size achieved by electro-deposition and forming accuracy mainly by anode end portions Geometry and size determine.But since the anode and cathode of this technique all needs to immerse in the electrolytic solution, anode (electrochemicaUy inert anode) is extremely sensitive to the movement of electrolyte, and stray electrical current is not easy to control, and confinement is poor, so it is extremely difficult Deposition prepares very fine three-dimensional structure, and (too thin anode can be formed by external force because electrodeposition process can not be resisted And vibrate or deform), deposition velocity is also limited (electrolyte is generally static, and mass transfer is limited, it is difficult to implement high speed deposition).Jet stream electricity Deposition is impacted the electrolyte containing metal ion in the form of high-speed jet in cathode substrate to carry out regioselectivity The processing technology of electro-deposition.Though it can be carried out high speed electro-deposition, stream is formed after depositing cathode plane or sedimentary by jet stream The easily-deformable of field, ambiguity and complexity, it is extremely difficult to form the micro-structure of high-precision great surface quality, and due to by surface tension Limitation, the prior art is hardly formed the high-speed jet of nanoscale beam diameter, so the three-dimensional that it can not prepare nanoscale is micro- Structure.It is curved to be sustainedly and stably formed in the micro-nano-scale of pole clearance that crescent electrolyte, which constrains three-dimensional electro-deposition forming, Month shape electrolyte group is electrochemistry micro reaction pool and the processing method for carrying out local chemical/electrodeposition.It has good confinement, Also it is able to achieve the forming of complex micro structure body.But meniscus electrolyte inside is because by a variety of microscopic heat conductions (viscosity, surface tension Deng) effect, mass transfer in liquid phase is limited, and deposition velocity is low and side reaction product cannot transport out of meniscus as early as possible, easily causes " useless Object " bulk deposition, so the technology is difficult to obtain the high metal micro structure of ingredient purity with higher speed.Therefore, of the invention Purpose be to be difficult to take into account high deposition velocity, high confinement, great surface quality for existing no magnetic property micro-processing method With the deficiency of high ingredient quality, propose the new micro-structure of one kind without magnetic property method and system.
Summary of the invention
In view of the above-mentioned problems, high heavy the purpose of the present invention is being difficult to take into account for existing no magnetic property micro-processing method Product speed, high confinement, great surface quality and high ingredient quality deficiency, propose a kind of micro-structure without magnetic property method and System.
The technical scheme is that a kind of micro-structure is without magnetic property system, including power supply, conductive substrates, capillary Glass tube, the electrolyte being placed in glass capillary, ultra-fine linear anode, holding frame and X-Y-Z triaxial movement platform, it is special Sign is: it further includes accurate micro-shifting moving cell;The lower part of the ultra-fine linear anode is coaxially placed in capillary glass In glass pipe;The upper end of the ultra-fine linear anode is located at the top of glass capillary and fixes with accurate micro-shifting moving cell and connects It connects;The accurate micro-shifting moving cell is fixed on the surface on holding frame and being located at glass capillary;The capillary glass Pipe is fixed on the Z axis of X-Y-Z triaxial movement platform by holding frame;The ultra-fine linear anode is dynamic single in accurate micro-shifting It can make under the driving of member mobile relative to the adjustable reciprocating linear of speed of holding frame.
The internal diameter of the glass capillary be 200 μm ~ 300 μm, lower end be conical outlet, exit inside diameter be 60 μm ~ 100μm。
The diameter of the ultra-fine linear anode is 10 μm ~ 50 μm, and lower end is plane.
The conductive substrates are placed on the X-Y platform of X-Y-Z triaxial movement platform.
The ultra-fine linear anode is connected with the anode of power supply, and the conductive substrates are connected with the cathode of power supply It connects.
The material of the ultra-fine linear anode is electrochemicaUy inert conductive material, such as platinum, titanium.
A kind of micro-structure without magnetic property method, it the following steps are included:
S1: the height relative to conductive substrates is exported by the lower end that the Z axis of X-Y-Z triaxial movement platform adjusts glass capillary h2For 2mm ~ 3mm;
S2: adjusting relative position of the ultra-fine linear anode in glass capillary by accurate micro-shifting moving cell, makes ultra-fine straight The micro- plane in the lower end of Linear anode to glass capillary lower end surface distance be 3mm;
S3: the anode of ultra-fine linear anode and power supply is connected, and the cathode of conductive substrates and power supply is connected;
S4: ultra-fine linear anode is for linear motion downwards under the control of accurate micro-shifting moving cell and passes through electrolyte until super Distance h of the micro- plane in lower end of thin linear anode to the upper surface of conductive substrates1It is 1 μm ~ 10 μm, it is in the process, ultra-fine The micro- plane in lower end of linear anode can be because surface tension and viscous effect, which stick, microlayer model when passing through electrolyte;
S5: it is h that microlayer model, which contacts with conductive substrates and forms height,1Liquid bridge, at this point, ultra-fine linear anode, liquid bridge, conduction Substrate, power supply together form electrochemical reaction cell, then, in conductive substrates constantly there is the metallic atom heap being restored Product is got up;
The 1st layer of metal layer, work of the ultra-fine linear anode in accurate micro-shifting moving cell are formd after S6:2 ~ 10s, in conductive substrates With lower quick return and it is docked to initial position set by S2 step, at this point, ultra-fine linear anode and power supply disconnect power loss, Electrodeposition process stops;
S7: ultra-fine linear anode is for linear motion downwards under the control of accurate micro-shifting moving cell and passes through electrolyte until super Distance h of the micro- plane in lower end of thin linear anode to the upper surface of the 1st layer of metal layer1It is 1 μm ~ 10 μm, in the process, surpasses The micro- plane in lower end of thin linear anode can be because surface tension and viscous effect, which stick, microlayer model when passing through electrolyte;
S8: it is h that microlayer model, which contacts with the 1st layer of metal layer and forms height,1Liquid bridge, at this point, ultra-fine linear anode, liquid bridge, 1st layer of metal layer, power supply together form electrochemical reaction cell, then, constantly have on the 1st layer of metal layer and to be restored Metallic atom heap comes;
After S9:2 ~ 10s, the 2nd layer of metal layer is formd on the 1st layer of metal layer, ultra-fine linear anode is in accurate micro-shifting moving cell Under the action of quickly return to and be docked to initial position set by S2 step, at this point, ultra-fine linear anode and power supply disconnect Power loss, electrodeposition process stop;
S10: the step of repeating S7, S8 and S9, until the deposited metal layer of this position reaches required height in conductive substrates Degree;
S11: adjusting the position of conductive substrates by the X-Y platform of X-Y-Z triaxial movement platform, repeat S4, S5, S6, S7, S8, The step of S9 and S10, until the electrodeposit metals micro-structure in conductive substrates reaches necessary requirement.
Compared with prior art, the invention has the following advantages that
1, machining accuracy is high, and deposition velocity is fast, and sedimentary surface quality is good.Ultra-fine linear anode is logical in layer-by-layer electrodeposition process It crosses the microlayer model that the micro- plane in its lower end is sticked and constantly provides fresh electrolyte to cathode crystallizing field, confinement is high, mass transfer in liquid phase ring Border is good, and implementable application larger current density (current density is high, and enforceable deposition velocity is with regard to big) avoids a variety of side reactions from producing The generation of object;
2, micro-meter scale, nano-scale structures can high quality depositions.By the micro- plane in lower end for changing ultra-fine linear anode Size, correspondingly can control and adjust the size for sticking microlayer model, and combine and promote the Parameter Conditions such as speed, processing gap Combination adjustment, make it easy to obtain different scale microstructure features.
Detailed description of the invention
Fig. 1 is a kind of overall structure diagram of the micro-structure without magnetic property system of the present invention.
Fig. 2 be the method for the present invention be used for planar substrates when micro-structure without magnetic property flow diagram.
Fig. 3 is the schematic diagram in Fig. 2 implementation steps in the 1st layer of metal layer of electro-deposition in conductive substrates.
Fig. 4 is the schematic diagram for continuing to deposit the 2nd layer of metal layer in Fig. 2 implementation steps on the 1st layer of metal layer.
Fig. 5 be the method for the present invention be used for curved substrate when micro-structure without magnetic property flow diagram.
Figure label and title: 1, ultra-fine linear anode;2, glass capillary;3, electrolyte;4, conductive substrates;5, electric Source;6;Microlayer model, 7, X-Y-Z triaxial movement platform;8, accurate micro-shifting moving cell;9, holding frame;10, liquid bridge;11, the 1st layer of gold Belong to layer;12, the 2nd layer of metal layer.
Specific embodiment
The implementation of the invention patent is further described with reference to the accompanying drawing.
Fig. 1 show a kind of micro-structure without magnetic property system, it includes power supply 5, conductive substrates 4, glass capillary 2, it is placed in electrolyte 3 in glass capillary 2, ultra-fine linear anode 1, holding frame 9, tri- axis of X-Y-Z that material is metal platinum Motion platform 7 and accurate micro-shifting moving cell 8;Glass capillary 2 is fixed on the Z of X-Y-Z triaxial movement platform 7 by holding frame 9 On axis;The lower part of ultra-fine linear anode 1 is coaxially placed in glass capillary 2, and upper end is located at glass capillary 2 Top is simultaneously fixedly connected with accurate micro-shifting moving cell 8;Accurate micro-shifting moving cell 8 is fixed on holding frame 9 and is located at capillary glass The surface of pipe 2 drives ultra-fine linear anode 1 to make mobile relative to the adjustable reciprocating linear of speed of holding frame 9;Conductive base Bottom 4 is placed on the X-Y platform of X-Y-Z triaxial movement platform 7;Ultra-fine linear anode 1 is connected with the anode of power supply 5, conductive Substrate 4 is connected with the cathode of power supply 5.
The internal diameter of glass capillary 2 is 200 μm, and lower end is conical outlet, and exit inside diameter is 60 μm.
The diameter of ultra-fine linear anode 1 is 10 μm, and lower end is plane.
Fig. 2 show micro-structure of the method for the present invention for planar substrates when without magnetic property flow diagram, it is wrapped Include following steps:
S1: it is exported by the lower end that the Z axis of X-Y-Z triaxial movement platform 7 adjusts glass capillary 2 relative to conductive substrates 4 Height h2For 2mm;
S2: relative position of the ultra-fine linear anode 1 in glass capillary 2 is adjusted by accurate micro-shifting moving cell 8, is made ultra-fine The micro- plane in lower end of linear anode 1 to the lower end surface of glass capillary 2 distance be 3mm;
S3: the anode of ultra-fine linear anode 1 and power supply 5 is connected, the cathode of conductive substrates 4 and power supply 5 is connected;
S4: ultra-fine linear anode 1 is for linear motion downwards under the control of accurate micro-shifting moving cell 8 and passes through electrolyte 3 directly The extremely distance h of upper surface of the micro- plane in lower end of ultra-fine linear anode 1 to conductive substrates 41It is 5 μm, it is in the process, ultra-fine The micro- plane in lower end of linear anode 1 can be because surface tension and viscous effect, which stick, microlayer model 6 when passing through electrolyte 3;
S5: it is h that microlayer model 6, which contacts with conductive substrates 4 and forms height,1Liquid bridge 10, at this point, ultra-fine linear anode 1, liquid bridge 10, conductive substrates 4, power supply 5 together form electrochemical reaction cell, then, constantly have in conductive substrates 4 and are restored Metallic atom heap comes;
After S6:5s, the 1st layer of metal layer 11 is formd in conductive substrates 4, as shown in figure 3, ultra-fine linear anode 1 is accurate micro- Initial position set by S2 step is quickly returned and is docked under the action of mobile unit 8, at this point, ultra-fine linear anode 1 Power loss is disconnected with power supply 5, electrodeposition process stops;
S7: ultra-fine linear anode 1 is for linear motion downwards under the control of accurate micro-shifting moving cell 8 and passes through electrolyte 3 directly The extremely distance h of upper surface of the micro- plane in lower end of ultra-fine linear anode 1 to the 1st layer of metal layer 111It is 5 μm, in the process, The micro- plane in lower end of ultra-fine linear anode 1 can be because surface tension and viscous effect, which stick, micro- liquid when passing through electrolyte 3 Drop 6;
S8: it is h that microlayer model 6, which contacts with the 1st layer of metal layer 11 and forms height,1Liquid bridge 10, at this point, ultra-fine linear anode 1, Liquid bridge 10, the 1st layer of metal layer 11, power supply 5 together form electrochemical reaction cell, then, constantly have on the 1st layer of metal layer 11 The metallic atom heap being restored comes;
After S9:5s, the 2nd layer of metal layer 12 is formd on the 1st layer of metal layer 11, as shown in figure 4, ultra-fine linear anode 1 is in essence Initial position set by S2 step is quickly returned and is docked under the action of close micro-shifting moving cell 8, at this point, ultra-fine linear sun Pole 1 and power supply 5 disconnect power loss, and electrodeposition process stops;
S10: the step of repeating S7, S8 and S9, until the deposited metal layer of this position reaches required height in conductive substrates 4 Degree;
S11: adjusting the position of conductive substrates 4 by the X-Y platform of X-Y-Z triaxial movement platform 7, repeat S4, S5, S6, S7, The step of S8, S9 and S10, until the electrodeposit metals micro-structure in conductive substrates 4 reaches necessary requirement.
Fig. 5 show micro-structure of the method for the present invention for curved substrate when without magnetic property flow diagram, passes through It enables electric deposition device tilt, makes ultra-fine linear anode 1 perpendicular to deposition plane, electro-deposition when using similar to planar substrates Step.Due to the capillarity of electrolyte 3 and glass capillary 2, electrolyte 3 will stay on the tip outlet of glass capillary 2 Place, and not flowed out from glass capillary 2.

Claims (7)

1. a kind of micro-structure is without magnetic property system, including power supply (5), conductive substrates (4), glass capillary (2), it is placed in hair Electrolyte (3), ultra-fine linear anode (1), holding frame (9) and X-Y-Z triaxial movement platform (7) in thin glass tube (2), Be characterized in that: it further includes accurate micro-shifting moving cell (8);It coaxially sets the lower part of the ultra-fine linear anode (1) In glass capillary (2);The upper end of the ultra-fine linear anode (1) be located at the top of glass capillary (2) and with essence Close micro-shifting moving cell (8) is fixedly connected;The accurate micro-shifting moving cell (8) is fixed on holding frame (9) and is located at capillary glass The surface of glass pipe (2);The glass capillary (2) is fixed on the Z of X-Y-Z triaxial movement platform (7) by holding frame (9) On axis;The ultra-fine linear anode (1) can be made under the driving of accurate micro-shifting moving cell (8) relative to holding frame (9) The adjustable reciprocating linear of speed is mobile.
2. a kind of micro-structure according to claim 1 is without magnetic property system, it is characterised in that: the capillary glass The internal diameter for managing (2) is 200 μm ~ 300 μm, and lower end is conical outlet, and exit inside diameter is 60 μm ~ 100 μm.
3. a kind of micro-structure according to claim 1 is without magnetic property system, it is characterised in that: the ultra-fine straight line The diameter of shape anode (1) is 10 μm ~ 50 μm, and lower end is plane.
4. a kind of micro-structure according to claim 1 is without magnetic property system, it is characterised in that: the conductive substrates (4) it is placed on the X-Y platform of X-Y-Z triaxial movement platform (7).
5. a kind of micro-structure according to claim 1 is without magnetic property system, it is characterised in that: the ultra-fine straight line Shape anode (1) is connected with the anode of power supply (5), and the conductive substrates (4) are connected with the cathode of power supply (5).
6. a kind of micro-structure according to claim 1 is without magnetic property system, it is characterised in that: the ultra-fine straight line The material of shape anode (1) is electrochemicaUy inert conductive material, such as platinum, titanium.
7. a kind of micro-structure is without magnetic property method, it is characterised in that: it the following steps are included:
S1: it is exported by the lower end of Z axis adjustment glass capillary (2) of X-Y-Z triaxial movement platform (7) relative to conductive substrates (4) height h2For 2mm ~ 3mm;
S2: adjusting relative position of the ultra-fine linear anode (1) in glass capillary (2) by accurate micro-shifting moving cell (8), Make the micro- plane in lower end of ultra-fine linear anode (1) to glass capillary (2) lower end surface distance be 3mm;
S3: the anode of ultra-fine linear anode (1) and power supply (5) is connected, and the cathode of conductive substrates (4) and power supply (5) is connected;
S4: ultra-fine linear anode (1) is for linear motion downwards under the control of accurate micro-shifting moving cell (8) and passes through electrolyte (3) until the distance h of upper surface of the micro- plane in lower end of ultra-fine linear anode (1) to conductive substrates (4)1It is 1 μm ~ 10 μm, In the process, the micro- plane in lower end of ultra-fine linear anode (1) can be because of surface tension and viscosity when passing through electrolyte (3) Effect, which is sticked, microlayer model (6);
S5: it is h that microlayer model (6), which contacts with conductive substrates (4) and forms height,1Liquid bridge (10), at this point, ultra-fine linear anode (1), liquid bridge (10), conductive substrates (4), power supply (5) together form electrochemical reaction cell, then, in conductive substrates (4) constantly Ground has the metallic atom heap being restored;
After S6:2 ~ 10s, the 1st layer of metal layer (11) is formd in conductive substrates (4), ultra-fine linear anode (1) is in accurate micro-shifting Initial position set by S2 step is quickly returned and is docked under the action of moving cell (8), at this point, ultra-fine linear anode (1) power loss is disconnected with power supply (5), electrodeposition process stops;
S7: ultra-fine linear anode (1) is for linear motion downwards under the control of accurate micro-shifting moving cell (8) and passes through electrolyte (3) until the distance h of upper surface of the micro- plane in lower end of ultra-fine linear anode (1) to the 1st layer of metal layer (11)1It is 1 μm ~ 10 μm, in the process, the micro- plane in lower end of ultra-fine linear anode (1) when passing through electrolyte (3) can because surface tension and Viscous effect, which sticks, microlayer model (6);
S8: it is h that microlayer model (6), which contacts with the 1st layer of metal layer (11) and forms height,1Liquid bridge (10), at this point, ultra-fine linear Anode (1), liquid bridge (10), the 1st layer of metal layer (11), power supply (5) together form electrochemical reaction cell, then, the 1st layer of metal Constantly there is the metallic atom heap being restored on layer (11);
After S9:2 ~ 10s, the 2nd layer of metal layer (12) is formd on the 1st layer of metal layer (11), ultra-fine linear anode (1) is in precision Initial position set by S2 step is quickly returned and is docked under the action of micro-shifting moving cell (8), at this point, ultra-fine linear sun Pole (1) and power supply (5) disconnect power loss, and electrodeposition process stops;
S10: the step of repeating S7, S8 and S9, until required by the deposited metal layer of this position reaches on conductive substrates (4) Highly;
S11: by the position of the X-Y platform of X-Y-Z triaxial movement platform (7) adjustment conductive substrates (4), repeat S4, S5, S6, The step of S7, S8, S9 and S10, until the electrodeposit metals micro-structure on conductive substrates (4) reaches necessary requirement.
CN201910326158.0A 2019-04-23 2019-04-23 A kind of micro-structure is without magnetic property method and system Pending CN110093641A (en)

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CN110565130A (en) * 2019-09-11 2019-12-13 张家港博发纳米材料科技有限公司 Laser-enhanced three-dimensional micro-area electrodeposition method and corresponding device
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Application publication date: 20190806