CN105862112A - Clamp used for electrochemical deposition, electrochemical deposition apparatus and electrochemical deposition method thereof - Google Patents
Clamp used for electrochemical deposition, electrochemical deposition apparatus and electrochemical deposition method thereof Download PDFInfo
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- CN105862112A CN105862112A CN201510029460.1A CN201510029460A CN105862112A CN 105862112 A CN105862112 A CN 105862112A CN 201510029460 A CN201510029460 A CN 201510029460A CN 105862112 A CN105862112 A CN 105862112A
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Abstract
The invention relates to a clamp used for electrochemical deposition, an electrochemical deposition apparatus and an electrochemical deposition method thereof. The clamp comprises a clamping plate (1) used for clamping a growth substrate, a flat (2) used for bearing a counter electrode, a support member (3) and a pedestal (4) used for arranging a reference electrode; the clamping plate (1) and the pedestal (4) are fixed together through a pillar (5), the flat (2) is arranged between the clamping plate and the pedestal in an adjustable mode along a first direction (y) through the pillar (5), the clamp, the flat and the pedestal are mutually parallel, and the support member is arranged between the clamping plate and the flat. The electrochemical deposition apparatus comprises an electrolytic bath (6), the above clamp and an electrochemical work station (7), and the electrolytic bath is used for placing the clamp. The uniformity of the materials prepared by the electrochemical deposition apparatus can be greatly increased.
Description
Technical field
The invention belongs to field of electrochemical deposition, in particular it relates to a kind of fixture for electrochemical deposition
And electrochemical depositer and electrochemical deposition method.
Background technology
Electrochemical deposition is one of important method preparing metal and metal oxide nanostructure array.Electricity
Depositing system device comprises fixture, constant temperature water bath apparatus, electrochemical workstation, connecting line, other auxiliary
Device etc..Experiment carries out electrodeposited material with three electrodes or two electrode forms and prepares in production.
Carrying out in large area electrodeposition process, tradition electric deposition device system is deposited the most urgently to be resolved hurrily
Technical problem.On the one hand, conventional brace upper end is exposed in air (as shown in Figure 1), lower end electrode
(working electrode 71, to electrode 72, reference electrode 73) immerses electrolyte, and print 10 vertically puts into electricity
Solve liquid.Due to print 10 vertically place, the heater of constant temperature water bath apparatus is usually located at below water-bath,
Therefore the Gradient distribution of temperature and concentration of electrolyte causes the material of preparation to there is longitudinal inhomogeneities.Another
Aspect, when preparing little area print, the constant temperature water bath apparatus for heating in water bath electrolyzer 6 is usually glass
From transparent side surfaces, glass beaker or crystallizing dish, may determine that reference electrode immerses the electrolyte degree of depth.And carrying out
Time prepared by large area print, usual water bath device is stainless steel, therefore cannot observe reference from side
Electrode immersion depth.The vapor barrier sight line produced due to water-bath, is also difficult to from top judge immersion depth.
The uncertain accuracy making deposition process of reference electrode position cannot ensure.Therefore, it is necessary to explore new
Metal and metal-oxide electro-deposition method and technology, effectively to solve in the actual application of electro-deposition techniques
Key issue.
Summary of the invention
It is an object of the invention to overcome the drawbacks described above existing for existing electrochemical depositer, it is provided that one
Plant the new fixture for electrochemical deposition and electrochemical depositer and electrochemical deposition method.
The invention provides a kind of fixture for electrochemical deposition, this fixture includes for clamping growth base
The clamping plate at the end, for carrying to the flat board of electrode, for disposing support member and the base of reference electrode, folder
Plate and base are fixed together by pillar, and flat board is adjustably mounted at along a first direction by pillar
Between clamping plate and base, and clamping plate, flat board and base are parallel to each other, described support member be arranged on clamping plate and
Between flat board.
Preferably, described clamping plate include cover plate and base plate, are provided with at least two circle silicon between cover plate and base plate
Adhesive tape, and it is provided with a circle for fixing the fixing groove of working electrode between two circle silica gel strips.
It is further preferred that be provided with two circle silica gel strips on described cover plate, described base plate is provided with a circle
Silica gel strip and a circle are for fixing the fixing groove of working electrode.
It is highly preferred that be provided with print draw-in groove on described cover plate, being used on described base plate fixes work electricity
Between the fixing groove of pole silica gel strip and the print draw-in groove outward flange on described cover plate on described base plate.
Preferably, the thickness of described base plate is not more than 2cm, more preferably no more than 1.5cm, the most excellent
Choosing is not more than 3mm.
Preferably, described pillar be provided with nut and arrange along a first direction multiple anti-skidding for inserting
The hole of location bar, described flat board is stable on described pillar by nut and anti-skidding location bar.
Preferably, described support member includes arranging and position adjustable first in the first direction along third direction
Support bar, and be optionally adjustably disposed on the first support bar and with described along third direction
It is provided with on the second support bar that first support bar is vertical, described first support bar and described second support bar
For inserting the through hole of reference electrode.
It is highly preferred that described pillar be provided with nut and arrange along a first direction multiple anti-for inserting
The hole of sliding location bar, described first support bar is stable on described pillar by nut and anti-skidding location bar.
Preferably, the material of described fixture is polyether-ether-ketone, politef, polyimides, polyphenylene sulfide
Ether or Polyetherimide.
Present invention also offers a kind of electrochemical depositer, this device includes that electrolyzer, the present invention provide
Above-mentioned fixture and electrochemical workstation, described electrolyzer is used for placing described fixture, described electrochemistry work
Working electrode, reference electrode and to electrode contact, described working electrode, described reference electrode it is furnished with as station
Electrode is installed in described fixture with described and be connected with the joint of electrochemical workstation by wire.
Present invention also offers the method using above-mentioned electrochemical depositer to carry out electrochemical deposition, the party
Method includes: be immersed in described electrolyzer by connecting working electrode, reference electrode and the fixture to electrode
In electrolyte, then carry out electrochemical deposition.
In the described electrochemical depositer that the present invention provides, installment work electrode, reference electrode and right
The fixture of electrode can carry out electrochemical deposition to be totally submerged in the way of electrolyte, such that it is able to accurately
Control the contact area of reference electrode and electrolyte, it is ensured that apply the accuracy of current potential;And, described folder
Tool can level, vertically or at other angles place in the electrolytic solution, it is to avoid at preparation large area material
Time, the discontinuity of materials that thermograde and electrolyte concentration gradient cause;Additionally, to electrode and ginseng
More adjustable than the position of electrode, thus enhance the motility of electrochemical depositer.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Fig. 1 is the structural representation of traditional electrochemical depositer;
Fig. 2 is the structural representation of the fixture that the present invention provides;
Fig. 3 is the structural representation of the cover plate in the clamping plate of the fixture that the present invention provides;
Fig. 4 is the structural representation of the base plate in the clamping plate of the fixture that the present invention provides;
Fig. 5 is the structural representation of the electrochemical depositer that the present invention provides;
Fig. 6 is the photo of nano structure of zinc oxide material prepared by embodiment;
Fig. 7 is the luminescence generated by light collection of illustrative plates of nano structure of zinc oxide material prepared by embodiment;
Fig. 8 is the optical quality uniformity test figure of nano structure of zinc oxide material prepared by embodiment.
Detailed description of the invention
Below in conjunction with accompanying drawing, the detailed description of the invention of the present invention is described in detail.It should be appreciated that
Detailed description of the invention described herein is merely to illustrate and explains the present invention, is not limited to this
Bright.
The invention provides a kind of fixture for electrochemical deposition, as in figure 2 it is shown, this fixture includes using
In the clamping plate 1 of clamping growth substrate, for carrying the flat board 2 to electrode, for disposing reference electrode
Support member 3 and base 4, clamping plate 1 and base 4 are fixed together by pillar 5, and flat board 2 is by propping up
Post 5 y along a first direction is adjustably mounted between clamping plate 1 and base 4, and clamping plate 1, flat board
2 and base 4 be parallel to each other, described support member 3 is arranged between clamping plate 1 and flat board 2.
In the described fixture that the present invention provides, can be along to the position of the flat board 2 of electrode for carrying
First direction y regulates, such that it is able to regulation is to the distance between electrode and growth substrate.And, clamping plate
1, flat board 2 and base 4 are parallel to each other, and control growth substrate by adjusting the placed angle of fixture
Placed angle so that growth substrate can with level, vertically and other angles are placed in the electrolytic solution.
In the described fixture that the present invention provides, it is preferably two-layer knot for clamping the clamping plate 1 of growth substrate
Structure, i.e. includes cover plate 11 and base plate 12, and growth substrate is clamped between cover plate 11 and base plate 12.
In a preferred embodiment, described cover plate 11 or base plate 12 are arranged print draw-in groove 15 (such as figure
Shown in 3), growth substrate is embedded in described print draw-in groove 15.
Under normal circumstances, working electrode contacts with growth substrate.In the described fixture that the present invention provides,
Working electrode is preferably mounted between cover plate 11 and base plate 12.It is further preferred that in order to prevent electrolysis
Liquid and the conductive contact being connected working electrode, arrange at least two circle silica gel between cover plate 11 and base plate 12
Bar 13, and it is provided with a circle for fixing the fixing groove 14 of working electrode between two circle silica gel strips 13,
So by installment work electrode in fixing groove 14, it is possible to achieve make working electrode and growth substrate four
Enclose contact Monday to conduct electricity.It is further preferred that as shown in Figures 3 and 4, described cover plate 11 sets
It is equipped with two circle silica gel strips 13, described base plate 12 is provided with a circle silica gel strip 13 and a circle for regular worker
Make the fixing groove 14 of electrode, and the face that arranges of the silica gel strip on cover plate 11 and the silica gel strip on base plate 12
It is opposed facing with the face that arranges of fixing groove 14, that is, when cover plate 11 and base plate 12 are combined
Time, the face that the arranges phase of the face that arranges of the silica gel strip on cover plate 11 and the silica gel strip on base plate 12 and fixing groove
Contact mutually.
Most preferably, as it is shown on figure 3, arrange print draw-in groove 15 on described cover plate 11, when cover plate 11
The fixing groove 14 for fixing working electrode when being combined with base plate 12, on described base plate 12
Between silica gel strip 13 and print draw-in groove 15 outward flange on described cover plate 11 on described base plate 12.
In the described fixture that the present invention provides, the middle part of described base plate 12 is provided with opening so that institute
State cover plate 11 and after described growth substrate is clamped in wherein by described base plate 12, with right in growth substrate
The surface that electrode is relative may be used for deposited material.Described cover plate 11 can be arranged or be not provided with opening,
If arranging opening, it is more beneficial for observing.Further, when described cover plate 11 is not provided with opening, institute
The inner ring stating cover plate 11 can arrange silica gel strip;When described cover plate 11 arranges opening, described
The inner ring of cover plate 11 needs to arrange silica gel strip, to prevent liquid connecing from described cover plate 11 and growth substrate
Contacting surface is penetrated into.
In the described fixture that the present invention provides, in order to avoid a large amount of during carrying out electrochemical deposition
Air stays the surface of growth substrate, and the thickness of described base plate 12 is preferably no greater than 2cm, the most not
More than 1.5cm, most preferably no greater than 3mm.When arranging sample draw-in groove on described base plate 12 and raw
When long substrate is embedded in this sample draw-in groove, the thickness of described base plate 12 refers to the base plate at this sample draw-in groove
Thickness.
In the described fixture that the present invention provides, for make described flat board 2 can clamping plate 1 and base 4 it
Between y adjusting position along a first direction, the set-up mode that this area can be used conventional realizes.In one
In embodiment, as in figure 2 it is shown, arrange nut 51 and y arrangement along a first direction on pillar 5
Multiple holes for inserting anti-skidding location bar 52, so can pass through nut 51 and anti-skidding location bar 52
By stable for flat board 2 on described pillar 5, and adjust anti-skidding location bar 52 by y along a first direction
Can realize adjusting the distance of flat board 2 and clamping plate 1 with the position of nut 51.
In the described fixture that the present invention provides, for disposing the support member 3 of reference electrode to be preferably arranged to
The installation position making reference electrode is adjustable, can y, second direction x and the 3rd along a first direction
Direction z is the most adjustable.In a preferred embodiment, the tectonic sieving of described support member 3 is: bag
Include and arrange and adjustable first support bar 31 of its position y in the first direction along third direction z, and
Optionally be adjustably disposed on the first support bar 31 along third direction z and with described first
On the second support bar 32 that strut 31 is vertical, described first support bar 31 and described second support bar 32
It is provided with the through hole for inserting reference electrode.It is preferable to carry out according to above-mentioned, it is possible to achieve reference electrode edge
First direction y, second direction x and third direction z and adjust position.In one embodiment, will
The mode that second support bar 32 is adjustably disposed on the first support bar 31 along third direction z is permissible
For: the second support bar 32 is inserted on described first support bar 31 along third direction z arrangement any
On through hole, so can realize the second support bar 32 edge by adjusting the on position of the second support bar 32
Third direction z and adjust position.
It is further preferred that by arranging nut 51 and and y arrangement along a first direction on pillar 5
Multiple holes for inserting anti-skidding location bar 52, so can pass through nut 51 and anti-skidding location bar 52
By stable on described pillar 5 for described support member 3, particularly described first support bar 31 is stablized
On described pillar 5, and adjust anti-skidding location bar 52 and the position of nut 51 by y along a first direction
Put and can realize adjusting the position on described support member 3 y in a first direction.
In the present invention, the material of described fixture can be there is insulation, high temperature resistant, chemical-resistant resistance is rotten
The macromolecular material of the physical and chemical performances such as erosion.In the preferred case, the material of described fixture be selected from but
It is not limited to polyether-ether-ketone, politef, polyimides, polyphenylene sulfide and Polyetherimide.Described folder
The material of tool refers to the material of material of main part of fixture, be primarily referred to as clamping plate 1, flat board 2, support member 3,
Base 4 and the material of pillar 5.
In the present invention, the nut used in described fixture and screw etc. the most all configure waterproof gasket.
Present invention also offers a kind of electrochemical depositer, as it is shown in figure 5, this device includes electrolyzer
6, the present invention provide above-mentioned fixture and electrochemical workstation 7, described electrolyzer 6 is used for placing described folder
Tool, described electrochemical workstation 7 is furnished with working electrode 71, reference electrode 72 and the joint to electrode 73.
When implementing electrochemical deposition, by described working electrode 71, described reference electrode 72 and described to electrode
73 relevant positions being installed in described fixture are also connected with the joint of electrochemical workstation by wire, tool
Body ground, makes working electrode 71 be arranged between cover plate 11 and base plate 12, is preferably mounted on base plate 12
Fixing groove 14 on;Reference electrode 72 is made to be arranged on support member 3;Make to be arranged on flat to electrode 73
The upper surface of plate 2.
In one embodiment, when chemical deposition process needs heating, described electrochemical depositer
The most also include heater 8 (such as constant temperature water bath apparatus), for the electrolyte in electrolyzer 6 is carried out
Heating.
Present invention also offers employing electrochemical depositer of the present invention and carry out electrochemical deposition
Method, the method includes: will connect working electrode (WE), reference electrode (RE) and to electrode
(CE) fixture is immersed in the electrolyte of described electrolyzer, then carries out electrochemical deposition.In necessity
When, use heater 8 (such as water bath with thermostatic control heater) that electrolyte is heated.
Specifically, electrochemical depositer of the present invention is used to carry out the operating process of electrochemical deposition
May comprise steps of:
(1) assemble the fixture that the present invention provides, and install working electrode, reference electrode and to electrode;
(2) fill the electrolyzer of electrolyte to put into water bath with thermostatic control heater and be heated to suitable temperature;
(3) growth substrate is arranged in the clamping plate of fixture, and is fully contacted with working electrode;
(4) preheating in electrolyte is put into by being provided with working electrode, reference electrode and the fixture to electrode;
(5) three electrodes of connection (i.e. working electrode, to electrode and reference electrode) drawn are led
Line respectively with the working electrode of electrochemical workstation, electrode and reference electrode joint are connected;
(6) suitable sedimentation potential and sedimentation time are set, come into effect electrochemical deposition;
(7) after electrochemical deposition is implemented to terminate, take out fixture, rinse well with deionized water, take out
Deposition has the growth substrate deionized water of target product to rinse well and dry up with nitrogen.
Compared with prior art, it is an advantage of the current invention that:
A (), when preparing large area material, can accurately control the contact surface of reference electrode and electrolyte
Long-pending, it is ensured that experiment applies the accuracy of current potential;
In (b) electrochemical deposition process can by growth substrate with level, vertically or other angles are placed,
Avoiding when preparing large area material, the material that thermograde and electrolyte concentration gradient cause is uneven
Property;
C () is adjustable with the distance of growth substrate to electrode;
D () reference electrode position is adjustable in three dimensions, greatly enhance Novel electric precipitation equipment system
The motility of system;
E electrode is contacted by () with growth substrate surrounding, it is ensured that the uniformity of electric field in electrodeposition process.
Therefore, provided by the present invention metal and metal oxygen can be improved by immersion electrochemical depositer
The uniformity of compound nano structural material, and there is great motility.
It is described further with the comparative example present invention by the following examples.
The electrolyte used in following example and comparative example is: zinc nitrate and the aqueous solution of ammonium nitrate, and
Nitric acid zinc concentration is 5mmol/L, and the concentration of ammonium nitrate is 6mmol/L.
(FTO serves as a contrast the tin ash substrate that growth substrate is fluorine doped used in following example and comparative example
The end), purchased from MB Group Plc, model is A8.
Embodiment
Use the fixture shown in Fig. 2, make the growth substrate level being clamped in fixture put in electrolyte
Row electrochemical deposition, the condition of electrochemical deposition is: current potential is-1.41V, and the time is 1800s, temperature
It is 76 DEG C, obtains nano structure of zinc oxide materials A 1.As shown in Figure 6, it is photic for the photo of this material
Luminous collection of illustrative plates as it is shown in fig. 7, its optical quality uniformity test figure as shown in Figure 8.
Comparative example
The Conventional electrochemical precipitation equipment shown in Fig. 1 is used to carry out electrochemical deposition, the bar of electrochemical deposition
The same above example of part, obtains nano structure of zinc oxide material D1.
Optical property by the nano structure of zinc oxide material prepared by luminescence generated by light test evaluation.Photic
The He-Cd laser that excitation source used by luminous test uses wavelength to be 325nm, test environment is room
Temperature.As it is shown in fig. 7, lack with visual field by calculating the print nearly band-edge emission intensity near 380nm
The ratio falling into state emissive porwer determines the optical quality of prepared nano structural material.Test as shown in Figure 8
The luminescence generated by light collection of illustrative plates of 9 various locations in print, obtains corresponding nearly band-edge emission intensity and defect
State emissive porwer ratio X 1 X9.The optical quality inhomogeneities of print is defined as follows:
Optical quality inhomogeneities=(Xmax-Xmin)/2X
Maximum during wherein Xmax is 9 test points, Xmin is minima in 9 test points, and X is 9
The arithmetic mean of instantaneous value of individual test point numerical value.
According to above-mentioned test and result of calculation, use zinc-oxide nano prepared by Conventional electrochemical precipitation equipment
The optical quality inhomogeneities of structural material is 55.7%, and uses the electrochemical depositer system of the present invention
The optical quality inhomogeneities of standby nano structure of zinc oxide material reduces 57.8%, reaches 23.5%.
Visible, the uniformity of material prepared by the electrochemical depositer of the employing present invention is greatly improved.Separately
Outward, in deposition process, stay surface without a large amount of bubbles, further ensure the uniformity of prepared material.
The preferred embodiment of the present invention is described in detail above in association with accompanying drawing, but, the present invention does not limit
Detail in above-mentioned embodiment, in the technology concept of the present invention, can be to the present invention
Technical scheme carry out multiple simple variant, these simple variant belong to protection scope of the present invention.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as its
Without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (11)
1. the fixture for electrochemical deposition, it is characterised in that this fixture includes for clamping life
The clamping plate (1) of long substrate, for carrying to the flat board (2) of electrode, for disposing the support of reference electrode
Part (3) and base (4), clamping plate (1) and base (4) are fixed together by pillar (5), flat
Plate (2) is adjustably mounted at clamping plate (1) and base by pillar (5) (y) along a first direction
(4) between, and clamping plate (1), flat board (2) and base (4) are parallel to each other, described support member (3)
It is arranged between clamping plate (1) and flat board (2).
Fixture the most according to claim 1, wherein, described clamping plate (1) include cover plate (11)
With base plate (12), between cover plate (11) and base plate (12), it is provided with at least two circle silica gel strips, and
It is provided with a circle for fixing the fixing groove of working electrode between two circle silica gel strips.
Fixture the most according to claim 2, wherein, described cover plate is provided with two circles on (11)
Silica gel strip (13), described base plate (12) is provided with a circle silica gel strip (13) and a circle is used for fixing
The fixing groove (14) of working electrode.
Fixture the most according to claim 3, wherein, described cover plate is provided with print on (11)
Draw-in groove (15), being used on described base plate (12) is fixed the fixing groove (14) of working electrode and is positioned at institute
State the silica gel strip (13) on base plate (12) and the outside of the print draw-in groove (15) on described cover plate (11)
Between edge.
Fixture the most according to claim 1, wherein, the thickness of described base plate (12) is not more than
2cm, preferably no greater than 1.5cm, the most no more than 3mm.
Fixture the most according to claim 1, wherein, described pillar (5) is provided with nut (51)
Multiple holes for inserting anti-skidding location bar (52) that (y) is arranged along a first direction, described flat
Plate (2) is stable on described pillar (5) by nut (51) and anti-skidding location bar (52).
Fixture the most according to claim 1, wherein, described support member (3) includes along third party
Arrange and adjustable first support bar in (y) position (31) in a second direction to (z), and optionally
Along third direction (z) be adjustably disposed in the first support bar (31) upper and with described first
The second support bar (32) that strut (31) is vertical, described first support bar (31) and described second
The through hole for inserting reference electrode it is provided with on strut (32).
Fixture the most according to claim 7, wherein, described pillar (5) is provided with nut (51)
Multiple holes for inserting anti-skidding location bar (52) that (y) is arranged along a first direction, described
One support bar (31) is stable in described pillar (5) by nut (51) and anti-skidding location bar (52)
On.
Fixture the most according to claim 1, wherein, the material of described fixture be polyether-ether-ketone,
Politef, polyimides, polyphenylene sulfide or Polyetherimide.
10. an electrochemical depositer, this device includes appointing in electrolyzer (6), claim 1-9
Anticipating a described fixture and electrochemical workstation (7), described electrolyzer (6) is used for placing described folder
Tool, described electrochemical workstation (7) is furnished with working electrode (71), reference electrode (72) and to electrode
(73) joint, described working electrode, described reference electrode and described electrode is installed in described fixture
In and be connected with the joint of electrochemical workstation by wire.
11. use the method that the electrochemical depositer described in claim 10 carries out electrochemical deposition,
The method includes: be immersed in described electrolysis by connecting working electrode, reference electrode and the fixture to electrode
In the electrolyte in pond, then carry out electrochemical deposition.
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CN201410837107 | 2014-12-29 | ||
CN2014108371071 | 2014-12-29 |
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CN201520042082.6U Active CN204570074U (en) | 2014-12-29 | 2015-01-21 | For fixture and the electrochemical depositer of electrochemical deposition |
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CN108842177A (en) * | 2018-07-10 | 2018-11-20 | 深圳拓扑精膜科技有限公司 | A kind of electrochemical deposition bracket being used to prepare nano material |
CN109239168A (en) * | 2018-09-12 | 2019-01-18 | 太原科技大学 | A kind of electrochemical depositer |
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CN105862112B (en) * | 2014-12-29 | 2018-06-15 | 神华(北京)光伏科技研发有限公司 | For the fixture and electrochemical depositer and electrochemical deposition method of electrochemical deposition |
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CN108842177A (en) * | 2018-07-10 | 2018-11-20 | 深圳拓扑精膜科技有限公司 | A kind of electrochemical deposition bracket being used to prepare nano material |
CN108842177B (en) * | 2018-07-10 | 2023-12-26 | 深圳拓扑精膜科技有限公司 | Electrochemical deposition bracket for preparing nano material |
CN109239168A (en) * | 2018-09-12 | 2019-01-18 | 太原科技大学 | A kind of electrochemical depositer |
CN109239168B (en) * | 2018-09-12 | 2020-06-16 | 太原科技大学 | Electrochemical deposition device |
CN112981506A (en) * | 2021-02-09 | 2021-06-18 | 苏州晶洲装备科技有限公司 | Electrochemical deposition equipment |
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CN105862112B (en) | 2018-06-15 |
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