CN100406618C - Process and its device for processing complecated three dimensional structure of metal surface - Google Patents
Process and its device for processing complecated three dimensional structure of metal surface Download PDFInfo
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- CN100406618C CN100406618C CNB03101271XA CN03101271A CN100406618C CN 100406618 C CN100406618 C CN 100406618C CN B03101271X A CNB03101271X A CN B03101271XA CN 03101271 A CN03101271 A CN 03101271A CN 100406618 C CN100406618 C CN 100406618C
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Abstract
The present invention relates to a method for machining complex three-dimensional microstructures on metal surfaces by an etching agent layer constraining technology. The method comprises the procedures: a machining tool with a microstructure is fixed on a fixing frame; etching solution is injected in a container; the machining tool enters the solution; an electrochemical system is started, and etching agents are generated on the surface of the machining tool; an etching agent layer is compressed to the thickness of a nanometer level or a micronanometer level by scavenging agents; a driving device is started for etching a work piece, and the surface of the work piece is concavely disengaged from the etching agent layer until etching is completed. A machining device is provided with the machining tool, the fixing frame, the driving device, a computer and the electrochemical system. Mass copying machining can be carried out to various complex three-dimensional microstructures. Mass microstructures are etched by one step, and the procedures of glue spreading, exposure, development and glue elimination in photoetching are saved. The present invention has the advantages of reduced cost, improved machining precision, improved surface evenness and distance sensitivity in machining, and can accurately control machining quality by accurately controlling the feeding distance of templates.
Description
(1) technical field
The present invention relates to a kind of micro-processing method that adopts electrochemical method, especially adopt confined etchant layer technique (celt) to carry out the working method and the device thereof of complicate three dimension microstructure in the metallic surface.
(2) background technology
Micro-processing technology is the unify key of Micro-Opto-Electro-Mechanical Systems technology of micro-electro-mechanical systems.Existing micro-processing technology has two classes, and a class is the pointwise processing technology, as the processing of high energy beams such as laser beam, electron beam and ionic fluid, fine electric spark processing and Scanning Probe Microscopy (SPM) processing (containing STM, SECM, AFM etc.).In the working method of this type, Jia Gong scope is a point each time, and therefore, working (machining) efficiency is very low, is unfavorable for batch machining.Another kind of is the batch machining technology of microstructure, as IC technology, LIGA technology, confined etchant layer technique (celt), micro-contact printing technology, EFAB technology, plasma etching technology and reactive ion etching technology etc.In this class technological method, can process a collection of (or an array) microstructure each time.If according to processing environment and medium Micrometer-Nanometer Processing Technology is classified, a class is a wet processes, and another kind of is dry process, and the kind of method is the same.
With IC technology metallic substance is carried out etching and only be applicable to that (this simple 3-D solid structure should be called 2.5 dimensions to the vertical substantially three-dimensional arrangement in making side, to be different from real complex three-dimensional structure), and be difficult to accomplish absolute vertical again, this is because the corrosion of most metallic substance in corrosive fluid is isotropic, produce the side direction undercutting thus, thereby cause the extending transversely of micropore or little raceway groove.Also just therefore, conventional photoetching process can not process the very big microstructure of depth-to-width ratio in the metallic surface.Want the 3-D solid structure of processed complex,, just need to adopt the multistep etching as the sphere and the conical surface, promptly so-called alignment process, its resolving power is very limited.Photoetching process is original just quite complicated, and the alignment process that this multistep etching is formed is just more complicated.And for ultrastructure, each step fine registration is more difficult.
Micro-contact printing method (microcontact printing is called for short μ CP) is the Whitesides of Harvard University professor study group (Kumar A, Whitesides G M, Appl.Phys.Lett.1993,63:2002; Kumar A, Biebuyck H A, Whitesides G M, Langmuir, 1994,10:1498.) a kind of micro-processing method for promoting mainly out.This method utilizes silicon rubber to mould the high resolution of casting processing, is template with the silicon chip with microstructure, is molded to the surfacial pattern of this microstructure at silastic surface, and this just becomes the elasticity " seal " of back micro-contact printing processing usefulness.With little example that is processed as of golden film, " seal " dipped in alkyl sulfhydryl " ink ", " to impress " on golden film surface then, micrographics has just printed to gold surface by this " ink ".Alkyl sulfhydryl " ink " forms the self assembly molecule individual layer in gold surface, this self assembly molecule individual layer at some chemical etching liquid (as KCN+KOH+O
2) in, play the effect of photoresist material, promptly chemical etching liquid there is barriering effect.Through after the chemical etching, just obtain the fine structure the same with former microstructure in gold surface.This technology is the same with conventional photoetching technique, only is applicable to the three-dimensional arrangement of making lateral vertical, 3-D solid structure that can't processed complex, and be difficult to make the bigger microstructure of depth-to-width ratio.
Photoetching is combined with the electrochemistry anode dissolution, also can process metallic substance.(advantage 142:3801-805.) is the neutral salt ionogen that can use corrodibility little to this method, as Na for Datta M, J.Elctrochem.Soc.1995
2SO
4, NaCl, NaNO
3Deng, environmental pollution is little, and suitable material is wide, and etching speed is very fast.But there is following shortcoming: 1) can not process complicated three-dimensional structure (as various curved surfaces), can only straight up and down carry out etching processing (2.5 dimension) to material; 2) microtexture of metal has determined the ununiformity of its anode dissolution, and in general, the anode dissolution face is quite coarse, so the difficult slick etched surface of microcosmic that obtains; 3) anode dissolution of metal generally is isotropic, though the etching distribution of current can obtain to a certain degree control by changing some external conditions, can occur in the side direction undercutting under the mask inevitably, and this will influence working accuracy; 4) only limit to electro-conductive material is processed.
Way (the Romankiw L T that LIGA---combines synchrotron radiation X-ray photoetching and galvanic deposit to make microstructure, Electrochimica Acta, 1997,42:2985.), be called LIGA technology (abbreviation of Lithografie Galvanoformung Abformung is the combination process of photoetching, electroforming and casting).It is that the investigator of Karlsruhe, Germany Nuclear Institute invented in late 1980s.This method can obtain the very microstructure of high aspect ratio, and the sidewall collimation of the microstructure that makes by lithography is fine.But there is following shortcoming in LIGA technology: the 1) expensive synchrotron radiation X-gamma ray source of its needs, and this makes applying of it be subjected to bigger restriction; 2) the same with conventional photoetching process, it also is difficult to the processed complex 3-D solid structure, as sphere, conical surface or the like.
EFAB (abbreviation of Electrochemical Fabrication), be the information science institute AdamCohen of American South University of California professor (the Cohen A of study group, et al, 12th IEEE International Microelectro-mechanical SystemsConference, 1999, Technical Digest, IEEE.Cohen A et al, Solid Freeform Fabrication Symposium1998, Proceedings, The University of Texas at Austin.) found out in 1999.It is a kind of technology that adopts electrochemical method to make 3-dimensional multi-layered microstructure.The ultimate principle of EFAB is: the figure that will process with 3D CAD software earlier resolves into a series of X-Y schemes that are made into Lithographic template that are applicable to, can make a series of masks thus then, next in electrolyzer with required metal and sacrifice layer metal according to mask patterns from level to level respectively galvanic deposit come out, at last the sacrifice layer dissolving metal is just obtained the figure of the material of wanting later on.Use the EFAB technology, if the processed complex 3-D solid structure as hemisphere and cone, just needs to make a lot of templates, this and similar with the principle (alignment) of conventional photoetching process processed complex 3-D solid structure, complex process.
The people such as Schuster of Germany Fritz-Haber institute were at " Science " magazine (Schuster R in 2000, Kircher V, Allongue P, Ert G, Science.2000 has reported that using ultrashort potential pulse carries out the micro-machined method of metal on 289:98.).Its ultimate principle is: in electrolyte solution, the charging time constant that workpiece to be machined (as anode) is gone up electrostatic double layer increases along with the increase of solution resistance between tool-electrode (as negative electrode) and the workpiece to be machined, because the near more part of workpiece surface the Distance tool electrode, solution resistance between the two is more little, and the electrostatic double layer charging is fast more.When between piece pole and tool-electrode, adding a ultrashort potential pulse, in this pulsating sphere, have only the electrostatic double layer of the workpiece to be machined (anode) under the tool-electrode to dash electricity to the current potential that is enough to take place anode dissolution, then owing to distance, resistance is big in other place, and charging is slow, and anode dissolution does not take place or meltage atomic, this has just produced the selective dissolution of workpiece surface (etching) under the tool-electrode, by moving of tool-electrode, can process simple three-dimensional structure.The shortcoming of this method is: it is quite difficult 1) will producing the ultrashort strong pulse of picosecond; 2) on big plane during the batch machining complicate three dimension microstructure, because distribution of current is difficult to control, so resolving power is very low.Up to the present, also there is not the complex three-dimensional ultra micro metal construction working method that a kind of cost is lower, technology simple, batch machining resolving power is high.
(3) summary of the invention
The present invention aims to provide a kind of above-mentioned shortcoming that overcomes, and is mainly used in the working method and the device thereof that carry out complicate three dimension microstructure in the metallic surface.
Technological method for processing of the present invention is:
1). the machining tool that will have microstructure is fixed on the anchor;
2). etching solution is injected container;
3) mobile anchor makes machining tool enter etching solution;
4). start electro-chemical systems, produce etching agent on the machining tool surface;
5) utilize the scavenging agent in the etching solution that the etching agent lamination is reduced to nano level or micron order thickness;
6). the drive unit of relative distance between start-up control machining tool and the workpiece to be machined, the machining tool that will have the etching agent layer of micron or nanometer grade thickness progressively moves to workpiece to be machined, when the protruding point of the etching agent layer enveloping surface on the machining tool touches workpiece to be machined, promptly begin workpiece to be machined is carried out etching, depression breaks away from the etching agent layer thereby etching makes the workpiece to be machined surface, and etching just stops;
7) drive unit constantly moves machining tool keeping the etching agent layer to contact with workpiece to be machined all the time to workpiece to be machined, thereby etching is constantly carried out, and finishes to etching, and machining tool leaves the workpiece to be machined surface.
The said metallic surface of the present invention complicate three dimension microstructure processing unit (plant) is provided with machining tool, anchor, drive unit, information processing computer, electro-chemical systems, machining tool is fixed in the bottom of anchor, the top of anchor connects the little driving governor of Z-axis of drive unit, and the little driving governor of Z-axis connects the information processing computer.Electro-chemical systems is provided with potentiostat, supporting electrode, reference electrode, container, the etching solution of packing in the container, machining tool and anchor are connected to potentiostat as the working electrode of potentiostat, one termination potentiostat of supporting electrode and reference electrode, the other end inserts in the interior etching solution of container, and container is located on the little driving governor of transverse axis of drive unit.
Wherein, machining tool can adopt the template that has high resolving power complex three-dimensional solid figure.
Workpiece to be machined is a metallic substance, and drive unit is used to control relative distance between above-mentioned template and the workpiece.Be loaded on above-mentioned template of etching solution submergence and workpiece in the container (container can adopt electrolyzer etc.), and can produce etching agent under given conditions, relevant electro-chemical systems generates the etching agent of energy etching workpiece in order to the relevant electrochemical reaction of etching solution generation that causes template surface, contain scavenging agent (or claiming trapping agent) in the etching solution, fast chemical reaction can take place with the etching agent of template surface and make the etching agent lost of life in it in etching solution.Because the etching agent lost of life and can only spread very short range,, be referred to as to retrain the etching agent layer so the etching agent layer that forms at template surface as thin as a wafer.The enveloping surface of this constraint etching agent layer has kept the complex three-dimensional solid figure of template with high resolving power.
Said template, its surface have the microstructure complementary microstructure with required processing; Also can be that (roughness Ra＜5nm), its complementary microstructure also is the plane of dead smooth for the plane (limit of microstructure) of dead smooth.
Template can adopt inactive, conductive material or for non-conducting material covers with conducting film, in etching solution and under the electropotential that produces etching agent, and chemistry do not take place this inactive, conductive material or galvanic corrosion.Said inactive, conductive material is a kind of of platinum or gold.
The material of workpiece to be machined can be metals such as copper, nickel, aluminium, titanium and cadmium.
Said anchor can be made by stainless material, and the part that immerses etching solution is protected by anti-corrosion coating insulation.
Machining tool (for example template) with microstructure mechanically or with conductive resin is fixed on the anchor.Anchor (together with machining tool, for example template) is installed in one by on the computer-controlled drive unit.
Drive unit is provided with the feed system or the driving governor that can carry out the nano level stepping in X, Y, three directions of Z, with relative distance and position between control machining tool and the workpiece.
The XY that said electrolyzer is installed in drive unit is on the horizontal table of driving governor, and its position is in the below of anchor.
Said etching solution contains Fe
+ 2, Cl
-1, NO
3 -1, NO
2 -1, SO
3 -2, SO
4 -2, PO
3 -3, OH
-Or F
-1Among one or more, its concentration range is 0.01-1M.Etching solution is installed in the electrolyzer.
Workpiece to be machined is flatly placed the bottom of electrolyzer.
Electrochemical system contains potentiostat, working electrode, supporting electrode and reference electrode, plays the effect of CONTROLLED POTENTIAL or control current.When template or machining tool are used as working electrode in the system, can cause etching solution at template surface that relevant electrochemical reaction takes place and generate can the etching workpiece etching agent.
Template is connected to electro-chemical systems as working electrode by conductive stainless steel anchor.
The producing method of said etching agent can be expressed as:
R→O+ne (1)
Here, template or machining tool are as anode.R is one or more in the etching solution ingredients listed, and O is an etching agent, and n is an electronic number, and e is an electronics.
The producing method of said etching agent also can produce by photoelectrochemistry:
R(+hv)→O+ne (2)
Said scavenging agent (or claiming trapping agent) can be SnCl
2, one or more the combination among Resorcinol, KHB and the NaOH.Its cleaning reaction to etching agent O of scavenging agent (or claiming trapping agent) can be expressed as:
O+S→R+Y (3)
Here, S is a scavenging agent, is also referred to as trapping agent, and Y is a reaction product, and S, R and Y all do not have corrasion.
Also can finish the cleaning reaction of etching agent O by the decomposition of O self reaction of deactivating:
O→Y (4)
Here, Y is a reaction product.
Said constraint etching agent layer is owing to exist the scavenging(action) of scavenging agent (or claiming trapping agent) to etching agent, the lost of life of etching agent and can only spread very short range, so can only be at template surface formation etching agent layer as thin as a wafer, be referred to as to retrain the etching agent layer, general thickness is nano level or micron order, and concrete thickness depends on the velocity constant of cleaning reaction.The enveloping surface of this constraint etching agent layer has kept the complex three-dimensional solid figure of template with high resolving power.
Innovative point of the present invention and advantage are: 1) can carry out the batch duplicating processing of various complicate three dimension microstructures (as hemisphere face, the conical surface etc.); 2) step is finished the etching processing of microstructure in batches, the complicated technology that has saved the gluing in the photoetching process, exposure, development and removed photoresist at last, do not need to come the processed complex three-dimensional microstructures, greatly reduce cost, improved working accuracy and surface finish with the multistep alignment process; 3) course of processing has distance sensitive, can accurately control amount of finish by the feeding distance of accurate control template, rather than rely on to estimate that etching time and etching speed control amount of finish.If control amount of finish with control etching time and etching speed, must control all factors that influence etching reaction speed.But control amount of finish with controlled distances, you belong to one-parameter control as long as the control template feeding distance is just much of that.Present piezoelectric ceramics can accurately control to nano level with the single step displacement, therefore can obtain finish size and the precision that we need; 4) less demanding to the original surface planeness of machined material, the surface accuracy that finally depends on template or machining tool of finished surface, but template need not contact with machined material; 5) can select for use different " etching-constraint " systems to process different materials, comprise metal and non-metallic material, conductor and non-conductive material; 6) there is not high energy beam processing can damage the machined surface adjacent domain like that or the danger of modification.
Many characteristics of the confined etchant layer technique (celt) of comparison of aforementioned, as can be seen, confined etchant layer technique (celt) has unique advantage when the processed complex three-dimensional structure.
(4) description of drawings
Fig. 1 forms synoptic diagram for processing unit (plant) embodiment of the present invention.
Fig. 2 is the driving device structure synoptic diagram of processing unit (plant) of the present invention.
Fig. 3 is a machining process synoptic diagram of the present invention.
(5) embodiment
Following examples will be in conjunction with Fig. 1, and 2 the present invention is further illustrated.
Fig. 1 provides processing unit (plant) embodiment of the present invention and forms synoptic diagram.Machining tool adopts the template 5 that has high resolving power complex three-dimensional solid figure, template 5 is fixed in the bottom of metal anchor 4, metal frame 4 can adopt two sections right cylinders that diameter is different, its top connects the little driving governor 2 of Z axle (Z-axis) of drive unit, the little driving governor 2 link information process computers 3 of Z axle.Electro-chemical systems is provided with potentiostat 1, supporting electrode 8, reference electrode 9, etching solution 10, electrolyzer 11 etc., in fact, template 5 also can be considered the integral part of electro-chemical systems, and template 5 is received potentiostat 1 by metal anchor 4 becomes working electrode.Supporting electrode 8 inserts in the etching solution 10 with reference electrode 9, and etching solution 10 is packed in the electrolyzer 11.Electrolyzer 11 is located on the little driving governor 7 of XY axle (transverse axis) of drive unit.Machined material 6 places electrolyzer 11.Referring to Fig. 2, drive unit comprises little driving governor of Z axle and the little driving governor of XY axle, in Fig. 2, the big stroke motion worktable 21 of the Z axle of the little driving governor of Z axle is connected with the microposition worktable 22 that is used for the feeding of template Z axle, the two ends of socle girder 23 connect microposition worktable 22 and template anchor 4 respectively, and template 5 is fixed in the lower end of anchor 4.The XY planar motion worktable 71 of the little driving governor of XY axle is located on the base 72.
Ultimate principle of the present invention is: in electrolytic solution, having the template of complicate three dimension microstructure (or little machining tool) surface generation etching agent O by electrochemical reaction or photochemical reaction, for example:
1. electrochemical means (template or machining tool are anode): see formula (1).
2. photoelectrochemistry mode: see formula (2), R is the ortho states of going back of etching agent O in the formula.
Can reduce etching agent O and make it lose the active chemical reagent of etching (being called trapping agent) owing in electrolytic solution, having added, just make the life-span of etching agent O shorten greatly by such homogeneous phase catching reaction, thereby can't must be far away to external diffusion, so the thickness of etching agent layer restrained (or claiming compression) in the very little scope of being close to template or machining tool place (micron or nano level) by template.Also can deactivate and react the thickness that retrains etching agent O diffusion layer by decomposition, as:
1. homogeneous phase catching reaction: see formula (3).
2. decompose or the reaction of deactivating: see formula (4).S is also referred to as trapping agent for the constraint agent in the formula.Y is a reaction product.For above-mentioned two classes reaction, the thickness μ of constraint etching agent layer is about:
μ＝(D/K
s)
1/2 (5)
Wherein D is the spread coefficient of etching agent in liquid phase, K
SPseudo first order reaction rate constant for the constraint reaction.
We can be with the above-mentioned etching processing (as shown in Figure 3) that has micron or the template of nanometer grade thickness etching agent layer or 5 couples of matrix M of machining tool.Allow template or machining tool progressively approach substrate material surface, the etching agent layer on template or machining tool touches body material, just begin matrix is carried out etching, shown in Fig. 3 b (etching is preceding shown in Fig. 3 a):
O+M→R+P (6)
Here, M is a body material, and R is the ortho states of going back of etching agent O, and P is other reaction product.
Along with matrix constantly is etched, in order to guarantee that retraining the etching agent layer can continue to touch matrix and etching matrix, precise driving device needs constantly template to be moved to matrix.(shown in Fig. 3 c).
At last, when the complete etching of microstructure finishes, (shown in Fig. 3 d), template is left matrix surface, (shown in Fig. 3 e).
Add man-hour with machining tool, this method can process the complicate three dimension microstructure of arbitrary shape, adds man-hour with template, and this method can process and template complementary complicate three dimension microstructure, and working accuracy is at nano level.
Claims (3)
1. the working method of metallic surface complicate three dimension microstructure is characterized in that the complete processing step is:
1). the machining tool that will have microstructure is fixed on the anchor;
2). according to the difference of institute's processing metallic, different etching solutions is injected container; The metal of being processed is nickel, aluminium and titanium;
3). mobile anchor makes machining tool enter this etching solution;
4). start electro-chemical systems, according to different etching solutions, produce different etching agents on the machining tool surface, the producing method of said etching agent is expressed as: R → O ten ne; R is the ortho states of going back of O, and O is an etching agent, and n is an electronic number, and e is an electronics;
Said etching solution contains Fe
+ 2, Cl
-1, NO
3 -1, NO
2 -1, SO
3 -2, SO
4 -2, PO
3 -3, OH
-Or F
-1Among one or more, its concentration range is 0.01～1M;
5) add different scavenging agents in the different etching solution, utilize the scavenging agent in the solution that the etching agent lamination is reduced to nano level or micron order thickness; Scavenging agent is expressed as the cleaning reaction of etching agent O: O+S → R+Y, and wherein, S is scavenging agent or trapping agent, and Y is a reaction product, and S, R and Y all do not have corrasion; Said scavenging agent or trapping agent are at least a among Resorcinol, KHB and the NaOH;
6). the drive unit of relative distance between start-up control machining tool and the workpiece to be machined, the machining tool that will have the etching agent layer of micron or nanometer grade thickness progressively moves to workpiece to be machined, when the protruding point of the etching agent layer enveloping surface on the machining tool touches workpiece to be machined, promptly begin workpiece to be machined is carried out etching, make workpiece surface break away from the etching agent layer thereby etching is removed the part material on workpiece to be machined surface, etching promptly stops;
7) drive unit constantly moves machining tool keeping the etching agent layer to contact with workpiece to be machined all the time to workpiece to be machined, thereby etching is constantly carried out, and finishes to etching, and machining tool leaves the workpiece to be machined surface.
2. metallic surface as claimed in claim 1 complicate three dimension microstructure processing unit (plant), it is characterized in that being provided with machining tool, anchor, drive unit, information processing computer, electro-chemical systems, machining tool is fixed in the bottom of anchor, the top of anchor connects the little driving governor of Z-axis of drive unit, and the little driving governor of Z-axis connects the information processing computer; Electro-chemical systems is provided with potentiostat, supporting electrode, reference electrode, container, the etching solution of packing in the container, machining tool and anchor are connected to potentiostat as the working electrode of potentiostat, one termination potentiostat of supporting electrode and reference electrode, the other end inserts in the interior etching solution of container, and container is located on the little driving governor of transverse axis of drive unit; Said machining tool adopts the template that has high resolving power complex three-dimensional solid figure; Said template surface has the microstructure complementary microstructure with required processing; Or be the plane of dead smooth, its roughness Ra＜5nm, its complementary microstructure also is the plane of dead smooth, its roughness Ra＜5nm;
Said template adopts inactive, conductive material or for non-conducting material covers with the inactive, conductive material film, and in etching solution and under the electropotential that produces etching agent, this inactive, conductive material does not take place chemical or galvanic corrosion; Said inactive, conductive material is platinum or gold.
3. metallic surface as claimed in claim 2 complicate three dimension microstructure processing unit (plant), it is characterized in that said drive unit is provided with feed system or the driving governor that carries out the nano level stepping in X, Y, three directions of Z, with relative distance and position between control machining tool and the workpiece.
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| CN1314577C (en) * | 2004-12-28 | 2007-05-09 | 上海纳晶科技有限公司 | Electrochemical deep etching method and apparatus thereof |
| CN100564241C (en) * | 2007-01-30 | 2009-12-02 | 厦门大学 | GaAs micro/nono optical element preparation method |
| CN101880907B (en) * | 2010-07-07 | 2012-04-25 | 厦门大学 | Electrochemical levelling and polishing processing method with nanometer precision and device thereof |
| CN102658404B (en) * | 2012-05-11 | 2014-04-16 | 南昌航空大学 | Precision combined electrochemical machining method |
| CN102766892B (en) * | 2012-08-10 | 2015-04-29 | 中国科学院重庆绿色智能技术研究院 | Micro-nano processing method and device |
| CN103145092B (en) * | 2013-02-28 | 2015-08-12 | 中国科学院半导体研究所 | Nanolithographic seal and utilize it to carry out the method for nanolithographic |
| CN103342334B (en) * | 2013-05-10 | 2016-01-20 | 厦门大学 | A kind of method of electrochemical etching processing of polymer materials surface |
| CN103325674B (en) * | 2013-05-23 | 2015-09-09 | 厦门大学 | A kind of constraint lithography method of complex three-dimensional multi-stage micro-nano structure |
| CN103322938B (en) * | 2013-06-15 | 2016-08-24 | 厦门大学 | A kind of optical element fixed point etching and observation device |
| CN103924287B (en) * | 2014-05-04 | 2016-09-28 | 大连理工大学 | Electroluminescent chemically polishing method |
| CN104018211B (en) * | 2014-06-17 | 2016-08-24 | 厦门大学 | A kind of electrochemical etching processing method of nano-precision |
| CN106191983B (en) * | 2016-08-12 | 2018-06-29 | 厦门大学 | A kind of micro fluidic device and its application process for electrochemical etching processing |
| CN107385504B (en) * | 2017-06-30 | 2019-03-19 | 哈尔滨工业大学 | The Constraints etching system of array electrode |
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