CN106637355B - Electrophoretic deposition set and its method that film is prepared using electrophoretic deposition - Google Patents

Electrophoretic deposition set and its method that film is prepared using electrophoretic deposition Download PDF

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CN106637355B
CN106637355B CN201611055848.XA CN201611055848A CN106637355B CN 106637355 B CN106637355 B CN 106637355B CN 201611055848 A CN201611055848 A CN 201611055848A CN 106637355 B CN106637355 B CN 106637355B
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anode
cathode
electrophoretic deposition
fixed plate
insulation board
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CN106637355A (en
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陈涛
关维
申雪飞
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Beijing University of Technology
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Beijing University of Technology
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00Electrophoretic coating characterised by the process
    • C25D13/22Servicing or operating apparatus or multistep processes

Abstract

A kind of method that the present invention provides electrophoretic deposition set and its prepares film, device includes: electrophoresis tank;Insulation board is placed on the open end of electrophoresis tank, there is through-hole thereon, fluted or raised on through-hole wall;Anode fixed plate is placed in groove or protrusion;Anode, one end are connected to anode fixed plate, and the other end protrudes into electrophoresis tank;Multiple cathodes, outer encirclement anode, one end are connected to insulation board, and the other end protrudes into electrophoresis tank, and the relative angle of anode and multiple cathodes is adjusted by rotary anode fixed plate.Method includes: that insulation board is erected on electrophoresis tank;The cathode parallel with anode is set by rotary anode fixed plate;It is passed through setting voltage between the anode and cathode, carries out electrophoretic deposition;It repeats the above steps, the deposition on different cathodes is realized by rotary anode fixed plate.Device and method uses multiple cathode electrodes, improves electrophoretic deposition efficiency, is rotated by anode fixed plate, the convenient accurate relative angle for adjusting anode and cathode.

Description

Electrophoretic deposition set and its method that film is prepared using electrophoretic deposition
Technical field
The present invention relates to electrophoretic deposition technique fields, more particularly, to a kind of electrophoretic deposition set and its use electrophoresis The method that sedimentation prepares film.
Background technique
Electrophoretic deposition is the effect in stable suspension through DC electric field, driving charged particle to its belt electrode The opposite electrode movement of property, is deposited into the process of film in electrode surface.
Electrophoretic deposition method has significant advantage compared with spin-coating method, print process etc. in terms of degree of purity and uniformity, and prepares week Phase is short, and equipment is simple, low in cost, and process repeatability is high, can manufacture.Therefore, the method for electrophoretic deposition production and It is widely used in experiment.
Conventional electrophoretic precipitation equipment after the completion of deposition, is needed frequent using single a pair of electrodes, i.e. an anode and a cathode It takes out and replaces electrode, and the problem for making deposition efficiency low.
In addition, being related to the state modulators such as voltage, pole plate spacing, the pole plate depth of parallelism in electrophoresis process, these parameters are final The film performance of deposition can be had an impact.And in an experiment to probe into the influence that these parameters deposit film, utilize tradition Electrophoretic deposition set generally require cumbersome step.
Summary of the invention
In view of the above problems, the object of the present invention is to provide a kind of raising electrophoretic deposition efficiency, cathode and anode angle tune The method for saving easily and accurately electrophoretic deposition set and its film being prepared using electrophoretic deposition.
According to an aspect of the present invention, a kind of electrophoretic deposition set, including electrophoresis tank are provided, wherein further include: insulation The open end of the electrophoresis tank is arranged in plate, and through-hole is provided on the insulation board, is arranged on the inner wall of the through-hole fluted Or protrusion;Anode fixed plate is placed in the groove or protrusion;Anode, one end are connected in anode fixed plate, the other end It protrudes into electrophoresis tank;Multiple cathodes, outer to surround the anode, one end is connected on insulation board, and the other end protrudes into electrophoresis tank, In, the relative angle of the anode and multiple cathodes is adjusted by rotary anode fixed plate.
According to another aspect of the present invention, a kind of above-mentioned electrophoretic deposition set of utilization is provided to prepare using electrophoretic deposition The method of film, comprising: electrophoresis liquid is placed in electrophoresis tank;Insulation board is erected on electrophoresis tank, by multiple cathodes with it is described Insulation board connection, the anode is connect with the anode fixed plate, anode fixing frame plate is located in the through-hole of insulation board;It is logical It crosses rotary anode fixed plate and sets the cathode parallel with the anode;Setting voltage, institute are passed through between above-mentioned anode and cathode It states electrophoresis liquid electrophoretic deposition setting time and obtains film;It repeats the above steps, is realized by rotary anode fixed plate in different yin Deposition on extremely.
Electrophoretic deposition set of the present invention and its method for preparing film are produced using multiple cathode electrodes, significantly The efficiency for improving electrophoretic deposition can easily and accurately adjust the opposite of anode and cathode by the rotation of anode fixed plate Angle.
Detailed description of the invention
By reference to following specific embodiments and in conjunction with attached drawing, other objects and results of the present invention be will be more apparent And it should be readily appreciated that.In the accompanying drawings:
Fig. 1 is the schematic diagram of electrophoretic deposition set of the present invention;
Fig. 2 is the schematic diagram of the anode and cathode relative position of electrophoretic deposition set.
In the accompanying drawings, identical appended drawing reference indicates similar or corresponding feature or function.
Specific embodiment
In the following description, for purposes of illustration, it in order to provide the comprehensive understanding to one or more embodiments, explains Many details are stated.It may be evident, however, that these embodiments can also be realized without these specific details.
Each embodiment according to the present invention is described in detail below with reference to accompanying drawings.
Fig. 1 is the schematic diagram of electrophoretic deposition set of the present invention, as shown in Figure 1, the electrophoretic deposition set 100 includes:
Electrophoresis tank 110, the container of open at one end, for holding electrophoresis liquid;
Insulation board 120 is arranged in the open end of the electrophoresis tank 110, through-hole 121, institute is provided on the insulation board 120 It states and fluted or raised (not shown) is set on the inner wall of through-hole 121, it is preferable that it is provided with scale on the through-hole 121, it is described Scale indicates angle;
Anode fixed plate 130 (Fig. 2 shows) is placed in the groove or protrusion;
One anode 140, one end are connected in anode fixed plate 130, and the other end protrudes into electrophoresis tank 110;
Multiple cathodes 150, outer to surround the anode 140, one end is connected on insulation board 120, and the other end protrudes into electrophoresis tank In 110,
Wherein, the relative angle of the anode and multiple cathodes 150 is adjusted by rotary anode fixed plate 140.
Preferably, pointer 131 is provided in the anode fixed plate 130, the direction of the pointer 131 and anode 140 are solid The direction being scheduled in the anode fixed plate 130 is identical, and the scale of through-hole 121 is directed at by pointer 131, determines anode fixed plate 130 angle.
The method that film is prepared using electrophoretic deposition using above-mentioned electrophoretic deposition set 100, comprising:
Electrophoresis liquid is placed in electrophoresis tank 110;
Insulation board 120 is erected on electrophoresis tank 110, multiple cathodes 150 are connect with the insulation board 120, it will be described Anode 140 is connect with the anode fixed plate 130, and anode fixed plate 130 is erected in the through-hole 121 of insulation board 120;
The cathode 150 parallel with the anode 140 is set by rotary anode fixed plate 130;
Setting voltage is passed through between above-mentioned anode 140 and cathode 150, the electrophoresis liquid electrophoretic deposition setting time obtains Film;
It repeats the above steps, the deposition on different cathodes 150 is realized by rotary anode fixed plate 130.
It, can be simultaneously when the cathode 150 parallel with the anode 140 has multiple in the above-mentioned method for preparing film Setting voltage is applied to multiple cathodes, while being deposited on multiple cathodes.
In a preferred embodiment of invention, as shown in Figure 1, multiple through slots 122 are provided on the insulation board 120, It opens up direction to intersect with the through-hole 121, for setting up the multiple cathode 150, by the cathode 150 along the through slot 122 slidings, adjust the relative distance of the cathode 150 and anode 140, for example, the size of 150 one end of the cathode is greater than described The size of through slot 122, the other end is less than the through slot 122, and cathode 150 is inserted into electrophoresis tank 110 by through slot 122, is greater than One end of 122 size of through slot is erected on the through slot 122, for another example, is arranged on the inner wall of the through slot 122 fluted or convex It rises, for placing the cathode 150, cathode 150 can slide in the groove or in protrusion, and cathode 150 is in through slot 122 On modes of emplacement can using any of the above-described kind of mode and use above two mode.
Preferably, scale is provided on the through slot 122, the scale indicates the cathode 150 being placed on the slot and institute The relative distance between the parallel anode 140 of cathode 150 is stated, for example, the scale on through-hole 121 is directed at the through slot 122 Center, when the pointer 131 in anode fixed plate 130 is directed toward the scale, with the unidirectional anode of pointer and the through slot Cathode 150 on 122 other vertical through slots is parallel, as shown in Fig. 2, the A in anode fixed plate 130 indicates anode, insulation is solid B1~B8 on fixed board indicates that 8 cathodes, rotation A are overlapped one end with 0 scale, i.e., A is parallel with B3, B7, when rotation A makes it One end is overlapped with 45 scales, i.e., A is parallel with B4, B8, and the cathode that B4 or B8 are represented at this time is moved along through slot, can change anode with The relative distance of corresponding cathode, when electrophoretic deposition, DC power anode is connected to the end A, cathode be connected to Bx parallel with it (x=1~ 8) hold, finally can on the cathode of the end Bx deposition film (for example, can be deposited on the corresponding cathode of B4 or B8, can also be same When deposited on two cathodes), deposition terminates, and A is rotated to another scale, and flat with the end By (y=1~8, y ≠ x) cathode Row, power cathode reconfiguration to the end By, can on the cathode electrode of the end By deposition film, to can realize on B1~B8 cathode electrode The deposition one by one of film.When rotation A is overlapped one end with 15 scales, the cathode that anode is connect with B3 is in 75 degree of angles, realizes sun The adjusting of the relative angle of pole and cathode.
The method that film is prepared using electrophoretic deposition using above-mentioned electrophoretic deposition set 100, comprising:
By moving cathode 150 along through slot 122, the relative distance of cathode 150 and anode 140 is adjusted;
By rotating anode fixed plate 130, the relative angle of anode 140 and cathode 150 is adjusted.
Above-mentioned electrophoretic deposition set 100 and its method for preparing film slide adjustment yin by cathode 150 on through slot 122 The relative distance of pole 150 and anode 140 is rotated opposite between adjustment anode 140 and cathode 150 by anode fixed plate 122 Angle, so that it is more convenient accurate apart from adjustment and angular adjustment, improve the efficiency and reliability of actual production and Experimental Research.
The depth of electrophoresis liquid is inserted into order to adjust anode 140 and cathode 150, it is preferable that electrophoretic deposition set 100 also wraps Include: lifting unit 160 is connect with the insulation board 120, opposite with the electrophoresis tank 110 for adjusting the insulation board 120 Distance is inserted into the depth of electrophoresis liquid in electrophoresis tank 110, the lifting unit 160 so as to adjust the cathode 150 and anode 140 It can be the electric up-downs structure such as mechanical arm and piston structure (pneumatically or hydraulically), screw rod auxiliary structure.
Preferably, the lifting unit 160 further includes the platform 161 for placing electrophoresis tank 110.
In order to facilitate the replacement of anode 140 and cathode 150, it is preferable that the anode 140 and cathode 150 pass through conductive base Plate 170 is connected to insulation board, it is further preferred that the electrically-conductive backing plate 170 is brass conductive substrate.
It further include preparation electrophoresis liquid using the method that electrophoretic deposition set 100 of the present invention prepares carbon nano-tube film, The preparation electrophoresis liquid includes:
Distilled water is added in carbon nanotube powder and containing the nonionic surfactant of aromatic group, carry out stirring in water bath and Ultrasound obtains dispersion liquid;
Above-mentioned dispersion liquid and magnesium nitrate hexahydrate is taken to be added in isopropanol, sonic oscillation obtains needed for carbon nano-tube film deposition Electrophoresis liquid.
In one particular embodiment of the present invention, using above-mentioned electrophoretic deposition set 100 and its method for preparing film The specific steps for preparing carbon nano-tube film include:
Step 1, the multi-walled carbon nanotube prepared using the method for chemical vapor deposition, 10~20nm of outer diameter, internal diameter 5~ 10nm, 10~30um of length, specific surface area > 180m2/ g, by purifying, being dried to obtain purity > 95wt% multi-walled carbon nanotube Powder;
Step 2, above-mentioned carbon nanotube powder 0.1g is weighed, 100ml distilled water is added, adds 0.1g containing aromatic group Nonionic surfactant, stirring in water bath, ultrasound 1h obtain the stable carbon nano-tube point that concentration is 1mg/ml at 50 c Dispersion liquid, and measuring the absorbance of dispersion liquid at this time on spectrophotometer is 3.667, shows that the degree of scatter of dispersion liquid is good;
Step 3, above-mentioned dispersion liquid 1.6ml is taken, 98.4ml isopropanol is added, adds 8.1mg magnesium nitrate hexahydrate, ultrasound vibration 10min is swung, electrophoresis liquid needed for obtaining carbon nano-tube film deposition;
Step 4, in electrophoresis experiment, cathode is that p-type list throws silicon wafer, and anode is graphite flake, and size is 10 × 20mm2, adjust The position for saving A and B4 makes two electrode runs parallels, and relative distance is 2cm;
Step 5, under room temperature, D.C. regulated power supply is provided with electrophoresis apparatus, the voltage adjusted between anodic-cathodic is The connected silicon chip extracting of cathode electrode B4 is obtained carbon nano-tube film after dry by 110V, electrophoretic deposition 6min, with a thickness of 144.9nm。
In an embodiment of the present invention, anode 140 can be laminated structure, be also possible to polyhedral structure, pass through rotation Anode fixed plate 130 can make multiple faces of anode 140 and multiple cathodes 150 parallel simultaneously, can carry out simultaneously multiple Electrophoretic deposition is carried out on cathode 150.
Although content disclosed above shows exemplary embodiment of the present invention, it should be noted that without departing substantially from power Under the premise of benefit requires the range limited, it may be many modifications and modify.According to the side of inventive embodiments described herein Function, step and/or the movement of method claim are not required to the execution of any particular order.In addition, although element of the invention can It is unless explicitly limited individual element it is also contemplated that having multiple elements to be described or be required in the form of individual.

Claims (10)

1. a kind of electrophoretic deposition set, including electrophoresis tank, which is characterized in that further include:
The open end of the electrophoresis tank is arranged in insulation board, and through-hole is provided on the insulation board, is set on the inner wall of the through-hole It is equipped with groove or protrusion;
Anode fixed plate is placed in the groove or protrusion;
Anode, one end are connected in anode fixed plate, and the other end protrudes into electrophoresis tank;
Multiple cathodes, outer to surround the anode, one end is connected on insulation board, and the other end protrudes into electrophoresis tank,
Wherein, the relative angle of the anode and multiple cathodes is adjusted by rotary anode fixed plate, it is parallel in anode every time Deposition film on one or more cathodes gradually completes the film deposition of all cathodes.
2. electrophoretic deposition set according to claim 1, which is characterized in that multiple through slots are provided on the insulation board, It opens up direction to intersect with the through-hole, for setting up the multiple cathode, be slided by the cathode along the through slot, adjusted The relative distance of the cathode and anode.
3. electrophoretic deposition set according to claim 2, which is characterized in that the cathode is placed on the mode of the through slot Including one or both of following two mode: a kind of mode, the size of one end of the cathode are greater than the ruler of the through slot Very little, the size of the other end of the cathode is less than the size of the through slot, and the other end of the cathode passes through the through slot, described One end-rack of cathode is on the through slot;The second way is provided on the inner wall of the through slot and sets up groove or protrusion, institute Cathode is stated to be placed in the groove or protrusion.
4. electrophoretic deposition set according to claim 2, which is characterized in that one or more of the through-hole and through slot On be provided with scale, scale on the through-hole indicates angle, and the scale on the through slot indicates the cathode being placed on the slot Relative distance between the anode of the cathode parallel.
5. electrophoretic deposition set according to claim 1, which is characterized in that further include:
Lifting unit is connect with the insulation board, for adjusting the relative distance of the insulation board Yu the electrophoresis tank, to adjust The depth of electrophoresis liquid in the whole cathode and anode insertion electrophoresis tank.
6. electrophoretic deposition set according to claim 1, which is characterized in that one or more of described anode and cathode Anode fixed plate or insulation board are connected to by electrically-conductive backing plate.
7. a kind of method for using electrophoretic deposition to prepare film using electrophoretic deposition set described in claim 1, feature exist In, comprising:
Electrophoresis liquid is placed in electrophoresis tank;
Insulation board is erected on electrophoresis tank, multiple cathodes are connect with the insulation board, the anode and the anode are consolidated Fixed board connection, anode fixing frame plate is located in the through-hole of insulation board;
The cathode parallel with the anode is set by rotary anode fixed plate;
Setting voltage is passed through between above-mentioned anode and cathode, the electrophoresis liquid electrophoretic deposition setting time obtains film;
It repeats the above steps, the deposition film on the parallel one or more cathodes of anode, passes through rotary anode fixed plate every time It realizes the deposition on different cathodes, gradually completes the film deposition of all cathodes.
8. the method according to claim 7 for preparing film, which is characterized in that further include:
Adjust the relative distance of anode and the cathode parallel with the anode.
9. the method according to claim 7 for preparing film, which is characterized in that further include preparation electrophoresis liquid, the preparation Electrophoresis liquid includes:
Distilled water and the nonionic surfactant containing aromatic group is added in carbon nanotube powder, carries out stirring in water bath and ultrasound, Obtain dispersion liquid;
Above-mentioned dispersion liquid and magnesium nitrate hexahydrate is taken to be added in isopropanol, electricity needed for sonic oscillation obtains carbon nano-tube film deposition Swimming liquid.
10. the method according to claim 7 for preparing film, which is characterized in that further include:
Apply setting voltage when the cathode parallel with the anode has multiple, while to multiple cathodes, while in multiple cathodes Upper carry out electrophoretic deposition.
CN201611055848.XA 2016-11-25 2016-11-25 Electrophoretic deposition set and its method that film is prepared using electrophoretic deposition Active CN106637355B (en)

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CN110592632B (en) * 2019-10-29 2024-04-05 中国兵器工业第二一三研究所 Electrolytic reaction device suitable for porous metal composite flyer electrodeposition
CN112442721A (en) * 2020-11-13 2021-03-05 西安昆仑工业(集团)有限责任公司 Electrophoresis painting process for heat-insulation bridge-cut-off aluminum profile

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US3200057A (en) * 1960-12-27 1965-08-10 Ford Motor Co Electrophoretic coating process
US5279511A (en) * 1992-10-21 1994-01-18 Copytele, Inc. Method of filling an electrophoretic display
CN101017754A (en) * 2006-02-09 2007-08-15 东元电机股份有限公司 A method for making carbon nano-pipe electronic emission source with circular sequence electrophoresis sediment
TWI550139B (en) * 2011-04-04 2016-09-21 諾菲勒斯系統公司 Electroplating apparatus for tailored uniformity profile
CN102230207A (en) * 2011-06-21 2011-11-02 华映光电股份有限公司 Electrophoretic deposition apparatus and electrophoretic deposition method
CN205603710U (en) * 2016-05-19 2016-09-28 山东建筑大学 Hanging electroplating experimental apparatus is pressed from both sides to simple and easy multi -disc

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