CN114059118B - Method for simultaneously electrodepositing films with different component ratios on different areas of electrode surface - Google Patents
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- CN114059118B CN114059118B CN202111562919.6A CN202111562919A CN114059118B CN 114059118 B CN114059118 B CN 114059118B CN 202111562919 A CN202111562919 A CN 202111562919A CN 114059118 B CN114059118 B CN 114059118B
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000005291 magnetic effect Effects 0.000 claims abstract description 84
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 238000004070 electrodeposition Methods 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 22
- 239000000956 alloy Substances 0.000 claims description 22
- 230000005294 ferromagnetic effect Effects 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003792 electrolyte Substances 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 230000005408 paramagnetism Effects 0.000 claims description 4
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 238000000151 deposition Methods 0.000 abstract description 7
- 230000008021 deposition Effects 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 230000001360 synchronised effect Effects 0.000 abstract description 2
- 238000012546 transfer Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 239000010935 stainless steel Substances 0.000 description 12
- 229910001220 stainless steel Inorganic materials 0.000 description 12
- 239000004065 semiconductor Substances 0.000 description 10
- 229910052742 iron Inorganic materials 0.000 description 6
- 239000010409 thin film Substances 0.000 description 5
- 230000005298 paramagnetic effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910001437 manganese ion Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910013553 LiNO Inorganic materials 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000002659 electrodeposit Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/12—Process control or regulation
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/007—Electroplating using magnetic fields, e.g. magnets
Abstract
The invention provides a method for simultaneously electrodepositing films with different component ratios on different areas of the surface of an electrode, belonging to the technical field of material preparation. The invention utilizes the external magnetic field array to regulate and control the liquid phase mass transfer behavior of the local area near the surface of the deposition substrate, thereby leading the components of the deposited film in the action area of the gradient magnetic field array to be different from those in the area without the gradient magnetic field, and realizing the synchronous electrodeposition of materials with different components in different areas of the substrate. The process provided by the invention can be applied to the preparation of low-dimensional materials and electronic devices.
Description
Technical Field
The invention belongs to the technical field of electrodeposition, and particularly relates to a method for simultaneously electrodepositing films with different component ratios on different areas of the surface of an electrode.
Background
In order to meet the different performance requirements of functional materials, the electrodeposition technology can be used for preparing various complex structures besides uniform two-dimensional film materials. The structure and composition of various deposited films can be effectively constructed in the direction vertical to the substrate by means of potential regulation and control, but the precise regulation and control of the composition and structure of the deposited films in different areas (transversely) of the substrate electrode are difficult (see figure 1), and the structural material has important application and prospect in various electronic devices, such as transverse giant magnetoresistance, transverse homojunction/heterojunction, thermoelectric devices and the like.
Disclosure of Invention
The invention aims to solve the technical blank that the prior electrodeposition field can not realize the controllable preparation of the films with different component proportions in different areas on the surface of an electrode, and provides a simple and easy method for simultaneously electrodepositing the films with different component proportions in different areas on the surface of the electrode, which can accurately control the component distribution of a coating on the surface of a substrate.
In order to realize the purpose of the invention, the adopted technical scheme is as follows:
a method for simultaneously electrodepositing films with different composition ratios on different areas of the surface of an electrode comprises the following steps:
(1) Determining a gradient magnetic field applying region and a non-gradient magnetic field applying region of the electrode substrate according to requirements, specifically, dividing the surface of the electrode substrate into the gradient magnetic field applying region and the non-gradient magnetic field applying region according to the distribution of film components on the surface of the electrode substrate;
(2) Preparing a gradient magnetic field template, distributing ferromagnetic metal or alloy on the gradient magnetic field template, and constructing the ferromagnetic metal or alloy into a required pattern;
further, a ferromagnetic metal or alloy is embedded at intervals in the resin substrate, the ferromagnetic metal or alloy corresponding to the gradient magnetic field application region;
(3) And (3) magnetic field electrodeposition, namely putting a gradient magnetic field template in a main magnet, magnetizing ferromagnetic metal or alloy to generate a gradient magnetic field which is perpendicular to the electrode substrate and parallel to the current direction, and selecting a gradient magnetic field action area through the gradient magnetic field template, wherein the gradient magnetic field is generated continuously or intermittently in the electrodeposition process.
Further, an electrode substrate is used as a cathode, a gradient magnetic field template is attached to the electrode substrate, then the electrode substrate is integrally placed in an electrolytic cell, the gradient magnetic field template is controlled to be attached to the inner wall of the electrolytic cell, meanwhile, one side of the electrode substrate, which is far away from the gradient magnetic field template, is opposite to and parallel to an anode, an iron neodymium boron permanent magnet is placed on the outer wall of the electrolytic cell at one side of the gradient magnetic field template, an electrolyte is filled in the electrolytic cell, the electrolyte contains at least one element with paramagnetism, then a constant voltage is applied between the cathode and the anode, the magnetic field electrodeposition process is carried out, in the process, a gradient magnetic field formed based on ferromagnetic metal or alloy is correspondingly and vertically loaded in a target gradient magnetic field application area, and therefore different component films are electrodeposited in different areas of the surface of the electrode substrate at the same time.
Further, the element having paramagnetism in step (3) may be cobalt, iron, nickel, manganese ion, or the like.
The invention is suitable for alloy electrodeposition, at least one element in the alloy components has paramagnetism in solution, the element can be one of the components of the film, or not, when the elements for forming the film component by electrodeposition are all non-paramagnetic, paramagnetic elements which do not participate in forming the film are required to be addedElements, e.g. paramagnetic manganese ions, having a more negative equilibrium potential due to reduction of manganese ions
Are generally not reduced in aqueous solution, i.e., do not participate in the formation of thin films.
It was found that a gradient magnetic field generates a kelvin force, which, when ferromagnetic or paramagnetic ions are present in the solution, results in a magnetic field that, at B =1T,
under the action of the magnetic field, the Kelvin force is one order of magnitude larger than the driving force of natural convection, when the gradient magnetic field is vertically loaded in a local area of the substrate, the Kelvin force acts to enable the area to generate convection, and the ion transmission rate in the area is improved, so that the component proportion of the coating in the local area is different from that in the area without the gradient magnetic field. Therefore, by selecting the gradient magnetic field application area, the alloy with special composition ratio can be constructed in the specified area of the substrate.
Compared with the prior art, the invention has the following technical advantages: the invention cooperates with the arrangement of ferromagnetic metal or alloy to form an external magnetic field array, and correspondingly and vertically loads the external magnetic field array in a target area, and regulates and controls the liquid phase mass transfer behavior of a local area near the surface of the deposition substrate, so that the components of the deposited film in an action area of the gradient magnetic field array are different from those in a non-gradient magnetic field area, and the synchronous electrodeposition of materials with different components in different areas of the substrate is realized. The process provided by the invention can be applied to the preparation of low-dimensional materials and electronic devices. Meanwhile, when the method constructs the different-component structure in different areas of the cathode substrate, the method can be flexibly controlled according to the size, the distance (the minimum interval can reach micron level) and the style (parallel array, dot matrix or free graph and the like) of the gradient magnetic field template. Finally, the method of the present invention, in conjunction with a photolithographic mask, allows discrete structures such as thermoelectric devices to be fabricated in which both n-type and p-type thermoelectric materials are fabricated and then connected together, thus simplifying the process flow.
Drawings
FIG. 1 is a schematic view of a composition difference film for different regions of a substrate.
FIG. 2 is a schematic diagram of a gradient magnetic field template, an electrode assembly and deposition results.
Fig. 3 is a schematic diagram of a gradient magnetic field template in embodiment 1 of the present invention.
FIG. 4 is a schematic view of the electrolytic cell system in example 1 of the present invention.
FIG. 5 is a schematic view showing the distribution of the surface coating composition in example 1 of the present invention.
FIG. 6 is a comparison of the process of preparing a thermoelectric device according to the present invention and the conventional method, (a) is a schematic view of the structure of the thermoelectric device, (b) is a schematic view of the process of preparing a micro thermoelectric device according to the conventional electrodeposition method, and (c) is a schematic view of the process of preparing the thermoelectric device according to the present invention.
FIG. 7 is a schematic diagram of a gradient magnetic field array template and an electrolytic cell.
Detailed Description
The invention is described in further detail below with reference to examples: a method for simultaneously electrodepositing films with different composition ratios on different areas of the surface of an electrode comprises the following steps:
(1) Determining a gradient magnetic field applying region and a non-gradient magnetic field applying region of the electrode substrate according to requirements, specifically, dividing the surface of the electrode substrate into the gradient magnetic field applying region and the non-gradient magnetic field applying region according to the film component distribution on the surface of the electrode substrate;
(2) Preparing a gradient magnetic field template, distributing ferromagnetic metal or alloy on the gradient magnetic field template, and constructing the ferromagnetic metal or alloy into a required pattern;
further, a ferromagnetic metal or alloy is embedded at intervals in the resin substrate, the ferromagnetic metal or alloy corresponding to the gradient magnetic field application region (see fig. 2);
(3) And (3) magnetic field electrodeposition, namely putting a gradient magnetic field template in a main magnet, magnetizing ferromagnetic metal or alloy to generate a gradient magnetic field which is perpendicular to the electrode substrate and parallel to the current direction, and selecting a gradient magnetic field action area through the gradient magnetic field template, wherein the gradient magnetic field is generated continuously or intermittently in the electrodeposition process.
The technical solutions of the present invention are further described below with reference to specific examples, but the present invention is not limited to the following specific embodiments, and a person skilled in the art may implement the present invention in other various specific embodiments according to the disclosure of the present invention, or make simple changes or modifications based on the design structure and idea of the present invention, and fall into the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Example 1 in this example, iron pieces were specifically selected as ferromagnetic metals
A method for simultaneously electrodepositing CoBi alloy with two component ratios comprises the following steps:
(1) See fig. 3, preparation of magnetic field template: an iron sheet with the width of 5mm, the length of 10mm and the thickness of 1mm is embedded in resin with the width of 15mm, the length of 15mm and the thickness of 1.5mm, and the iron sheet is positioned in the middle of the resin.
(2) Adopting stainless steel with the length and the width of 15mm as a cathode, placing a magnetic field template on the back of the stainless steel cathode and aligning, and fixing the magnetic field template and the stainless steel cathode by using a clamp so that the gradient magnetic field template is tightly attached to the cathode;
(3) The gradient magnetic field template and the stainless steel cathode are placed in a square electrolytic cell, the back of the magnetic field template is tightly attached to the inner wall of the electrolytic cell, and an iron neodymium boron permanent magnet (N40) is placed on the outer wall of the electrolytic cell, wherein the length and width of the permanent magnet are 50mm, and the thickness of the permanent magnet is 25mm.
(4) The platinum mesh anode with length and width of 20mm and the stainless steel cathode are placed in parallel, the magnetic field direction is perpendicular to the cathode, and the distance is 15mm (figure 4). Adding electrolyte into the electrolytic cell, wherein the electrolyte composition is 5.0g/L Bi 3+ 、25g/L Co 2+ 96.0g/L citric acid.
(5) And applying constant voltage between the cathode and the anode for 2.1V for 10 minutes, taking out the stainless steel cathode after deposition is finished, cleaning the stainless steel cathode with water, and drying the stainless steel cathode by blowing to obtain a gray plating layer. The bismuth content in the plating layer of the corresponding region of the gradient magnetic field template iron sheet is 33at%, and the bismuth content in the rest region is 47at% (fig. 5).
When two-component-ratio CoBi alloys need to be electrodeposited on different areas of the surface of the stainless steel cathode simultaneously, the surface of the stainless steel cathode is divided into a gradient magnetic field application area and a non-gradient magnetic field application area according to the film component distribution on the surface of the stainless steel cathode, iron sheets on a magnetic field template correspond to the gradient magnetic field application areas one by one, and finally, electrodeposition is carried out according to the steps (3) to (5) of the embodiment, so that the two-component-ratio CoBi alloys can be electrodeposited on different areas of the surface of the stainless steel cathode simultaneously.
Example 2: preparation of thermoelectric devices
A typical thermoelectric device structure is made by connecting pairs of p-type and n-type semiconductors with a current guiding plate and then packaging, as shown in fig. 6 (a). The existing electrodeposition method can not prepare n-type and p-type semiconductors at the same time, and a step deposition method is generally adopted. As shown in fig. 6 (b), the conductive substrate is covered with a photoresist before electrodeposition, a position where an n-type (or p-type) semiconductor is deposited is etched, and a corresponding semiconductor thin film is prepared at the position. The substrate surface is then covered again completely with photoresist, and the insulating layer that is needed to deposit another electrode is removed and deposited. And removing all the insulating coatings after deposition is finished, and then connecting the n-type semiconductor and the p-type semiconductor. By adopting the gradient magnetic field method, the n-type semiconductor and the p-type semiconductor can be deposited on the substrate at the same time, the preparation process is greatly simplified, and the preparation efficiency and the preparation precision are improved, as shown in (c) of fig. 6. Specifically, as shown in fig. 7, the gradient magnetic field template is an array of iron nanowires, a photolithographic mask is used as a template for the array of iron nanowires, and the iron nanowires are prepared by electrodeposition. And corresponding the magnetic field template to the template substrate of the thermoelectric film to be deposited to realize the precise control of the gradient magnetic field region (except for the magnetic field template and the template substrate of the thermoelectric film to be deposited, referring to FIG. 4, the electrodeposition device), specifically, the electrolyte contains 0.10mol/L Bi (NO) 3 ) 3 、0.05mol/L TeCl 4 、0.05mol/L Mn(NO 3 ) 2 And 0.3mol/L LiNO 3 At a temperature of 70 ℃ and a deposition potential of-0.10V (vs. SHE). The thin film having no gradient magnetic field region contains 52at% Te and is a p-type semiconductor; the thin film with the gradient magnetic field area contains 65at% Te and is an n-type semiconductor, and the embodiment further proves that the technical scheme of the invention can simultaneously electrodeposit thin films with different composition ratios in different areas on the surface of the electrode and has higher practical value.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
Claims (1)
1. A method for simultaneously electrodepositing films with different composition ratios on different areas of the surface of an electrode is characterized in that: the method is suitable for alloy electrodeposition and comprises the following steps:
(1) Dividing the surface of the electrode substrate into a gradient magnetic field applying area and a non-gradient magnetic field applying area according to the film component distribution of the surface of the electrode substrate;
(2) Preparing a gradient magnetic field template, wherein ferromagnetic metal or alloy is distributed on the gradient magnetic field template and is constructed into a required pattern;
(3) Magnetic field electrodeposition, namely putting a gradient magnetic field template in a main magnet, magnetizing ferromagnetic metal or alloy distributed on the gradient magnetic field template to generate a gradient magnetic field which is vertical to an electrode substrate and parallel to a current direction, and continuously or intermittently generating the gradient magnetic field in the electrodeposition process;
the gradient magnetic field template in the step (2) further comprises a resin substrate, and the ferromagnetic metal or the ferromagnetic alloy is embedded in the resin substrate according to a required pattern;
and (3) taking the electrode substrate as a cathode, attaching the gradient magnetic field template on the electrode substrate, then integrally placing the electrode substrate into an electrolytic tank, controlling the gradient magnetic field template to be attached to the inner wall of the electrolytic tank, simultaneously enabling one side of the electrode substrate, which is far away from the gradient magnetic field template, to be opposite to and parallel to the anode, placing an iron neodymium boron permanent magnet on the outer wall of the electrolytic tank on one side of the gradient magnetic field template, filling an electrolyte into the electrolytic tank, wherein the electrolyte contains at least one element with paramagnetism, and then applying constant voltage between the cathode and the anode to perform the magnetic field electrodeposition process.
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Application publication date: 20220218 Assignee: Yancheng Haoxin Technology Co.,Ltd. Assignor: CHANGZHOU University Contract record no.: X2023980052004 Denomination of invention: A method for simultaneously electrodepositing thin films with different composition ratios in different areas of the electrode surface Granted publication date: 20230407 License type: Common License Record date: 20231213 |
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