CN1274582C - Method and device for processing complex three dimensional microstructure on the surface of silicon - Google Patents
Method and device for processing complex three dimensional microstructure on the surface of silicon Download PDFInfo
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- CN1274582C CN1274582C CN 200410037771 CN200410037771A CN1274582C CN 1274582 C CN1274582 C CN 1274582C CN 200410037771 CN200410037771 CN 200410037771 CN 200410037771 A CN200410037771 A CN 200410037771A CN 1274582 C CN1274582 C CN 1274582C
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Abstract
The present invention relates to a method and a device for processing a complex three-dimensional microstructure on the surface of silicon. A template is fixed on a rack to be immersed in an electrochemistry etching solution, and is regarded as a working electrode. An auxiliary electrode and a reference electrode are additionally arranged in a container. An electrochemistry system is started up, the template is gradually moved to a silicon sheet to be etched, and the template is away from the surface of the silicon sheet after etching. An etching agent only can be diffused for a very short distance due to the fact that the life of the etching agent is shortened, and therefore, an etching agent layer formed on the surface of the template is very thin. The self complex three-dimensional figure of the template, which is processed at the silicon sheet, is kept by a very high resolution. The batch copy processing of various complex three-dimensional microstructures (such as a hemispherical surface, a conic surface, etc.) can be carried out for silicon materials. The processing of silicon is carried out by the system under proper conditions, the processing speed can be achieved depth of 10 mu m/s, and the resolution is achieved over 0.1 mu m.
Description
Technical field
The present invention relates to a kind of micro-processing method that adopts electrochemical method, especially adopt electro-etching method to remove the method for material on the object, adopt confined etchant layer technique (celt) to carry out the processing method and the device thereof of complicate three dimension microstructure at silicon face.
Background technology
Silicon materials perhaps be human up to now solve one of the most deep material.On earth, the mineral reserve of silicon are very abundant, and content is only second to oxygen.Because silicon has fabulous electronics and mechanical property, is to make components and parts such as integrated circuit, sensor, actuator on a large scale, and first-selection and a large amount of material that uses of making the micro electronmechanical and MOEMS of integrated these elements.
Micro-processing technology is the unify key technology of MOEMS of micro-electro-mechanical systems.Existing micro-processing technology can be divided into two types substantially, and a class is the pointwise process technology, as the processing of high energy beams such as laser beam, electron beam and ion beam, fine electric spark processing and scanning probe microscopy (SPM) processing (containing STM, SECM, AFM etc.).In the processing 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 micro-structural, carries out wet method or dry etching later on again as photoetching.Wet etching promptly carries out chemistry or electrochemical corrosion with chemical reagent solution to silicon; Dry etching is meant and with high energy particle or reacting gas silicon is bombarded corrosion under high vacuum condition, as plasma and reactive ion etching technology etc.In this class technical method, can process a collection of (or an array) micro-structural each time.
Existing silicon batch processing method, no matter be that wet etching or dry etching only are applicable to that (this simple 3-D solid structure exactly should be called 2.5 dimensions to the vertical substantially stereochemical structure in making side, to be different from real complex three-dimensional structure), and be difficult to accomplish vertical utterly.Main method in machining 3 D stereochemical structure on the silicon materials is to utilize silicon materials to have anisotropic etching characteristic in alkaline corrosion liquid at present, but because of the crystal face angle of silicon crystal is a fixed value, want the 3-D solid structure of processed complex, as the sphere and the conical surface, still need to adopt the multistep lithographic method, be so-called alignment process, its resolution ratio is very limited.Photoetching process is original just quite complicated, the alignment process that this multistep etching is formed thereby more complicated, and also for ultra microstructure, the fine registration in each step is difficulty particularly.
The ultra microstructure of complex three-dimensional has very application prospects in the micro-system field, as binary optical device, low-light lens array and complicated microactrator etc.But up to now, also do not have a kind ofly both possessed that cost is lower, technology is simple, structure resolution ratio advantages of higher, can realize silicon is carried out the method for complex three-dimensional ultra microstructure batch machining again.
Summary of the invention
The present invention aims to provide a kind of shortcoming that above-mentioned process technology exists that overcomes, and is mainly used at silicon face and carries out the batch processing method of complicate three dimension microstructure and the chemical solution of device and use thereof.
Processing method of the present invention is:
1). the template that will have complementary structure structure to be processed is fixed on the fixed mount;
2). electrochemical etching solution is injected the container that is placed with silicon chip to be processed;
3). mobile fixed mount makes template immerse electrochemical etching solution;
4). as working electrode, in container, establish auxiliary electrode and reference electrode with template in addition, start electro-chemical systems;
5). template is progressively shifted to silicon chip, begin workpiece to be machined is carried out etching;
6). drive unit constantly with template to being moved by silicon chip keeping etching constantly to carry out, finish to etching, template is left silicon chip surface.
The said electrochemical etching solution of the present invention contains two parts: etching agent and scavenger (or claiming agent for capturing).Etching agent is selected from and contains Br
1-, Br
2, SO
4 2-, Cl
1-, PO
3 3-, Cr
2O
7 2-, CrO
4 2-, Cr
3-, CrO
2 1-, OH
1-, isopropyl alcohol or F
1-Among at least a, its concentration range is 0.05～0.2M; Scavenger (or claim agent for capturing) is selected from the amino acids that contains sulfydryl, at least a in phenol or the inorganic arsenious acid, and its concentration range is 0.005～0.1M.
The etching agent of in situ preparation can be itself directly chemical etching silicon etching agent, possess at least a among the etching agent of accelerating the etching speed of other etching agent chemical etching silicon in the solution.
Cleaning reaction to etching agent also can be photochemistry decomposition reaction, the Thermochemical Decomposition reaction of etching agent self, or the chemical reaction of etching agent self and silicon is at least a.
Because using, the present invention contains Br
1-, Br
2, SO
4 2-, Cl
1-, PO
3 3-, Cr
2O
7 2-, CrO
4 2-, Cr
3-, CrO
2 1-, OH
1-, isopropyl alcohol or F
1-Among at least a, its concentration range is the etching agent of 0.001～2M and can is the particular electrical chemical etching solution that one or more the scavenger (or claiming agent for capturing) of combination in the amino acids that contains sulfydryl, phenol, the inorganic arsenious acid is formed; Etching agent can the certain electric electrochemical conditions issue the electrochemical reaction that looks closes and generate can the etching workpiece etch species (lewis' acid); Scavenger can make the etch species agent lost of life with the etch species generation fast chemical reaction of template surface.Because the etching agent lost of life and can only spread very short distance,, kept the complex three-dimensional solid figure of template itself to be machined on the silicon chip with high resolution ratio so the etching agent layer that forms at template surface as thin as a wafer.The present invention can carry out the batch duplicating processing of various complicate three dimension microstructures (as hemisphere face, the conical surface etc.) to silicon materials;
The core of confined etchant layer technique (celt) is the composition (prescription) of employed chemical solution system, the compositing formula of the chemical solution system that the present invention is used has satisfied following requirement: 1. certain component can produce the product (etch species) that processed material is had corrosive effect by electrochemical reaction in the solution, and corrosion reaction is enough fast; 2. etch species must be an isotropic to the corrosiveness of processed material; 3. corrosion process can not produce indissoluble or insoluble material; 4. remover can consume etch species fast, and etch species is strapped in the distance of the surface micron of electrode or sub-micron; 5. whole chemical solution system must be stable.
The three-dimensional little of semiconductor, especially silicon is processed with and important economic value.But be used for the research of chemical solution system of confined etchant layer technique (celt) of silicon and preparation and be unusual difficulty, its reason mainly contains: 1. the silicon that generally uses is monocrystalline silicon, the reagent of many corrosion all has anisotropy, and is promptly inequality along the corrosion rate of each crystal face, causes the distortion of processing; 2. silicon is contaminated easily, if contain metal ion in the solution, then is penetrated into silicon inside easily, causes the variation of silicon character, changes the speed of processing even processing is stopped; 3. most of slaines of silicon are all water insoluble, can form precipitation at silicon face after promptly many etching agent processing, stop further the carrying out of processing.
Under suitable condition, the processing of carrying out silicon with this system can reach the speed of about 10 micrometer depth of per minute, and resolution ratio reaches more than 0.1 micron.
Compare as can be seen with the process technology of existing various silicon, use electrochemistry process technology that electrochemical etching solution of the present invention carries out on silicon, to have unique advantage during the processed complex three-dimensional structure.
Description of drawings
Fig. 1 is that device of the present invention is formed schematic diagram.
Fig. 2 is the silicon face micro-image of the present invention machining 3 D pattern embodiment 2 on silicon.
Fig. 3 is the silicon face micro-image of the present invention machining 3 D pattern embodiment 3 on silicon.
Fig. 4 is the silicon face micro-image of the present invention machining 3 D pattern embodiment (embodiment 4) on p-type Si＜100〉monocrystalline silicon piece.
Fig. 5 is the silicon face micro-image of the present invention machining 3 D pattern embodiment (embodiment 5) on p-type Si＜100〉monocrystalline silicon piece.
The specific embodiment
Following examples will the present invention is further illustrated in conjunction with the accompanying drawings.
Embodiment 1
Fig. 1 provides the device for carrying out said example of processing method of the present invention and forms schematic diagram.Machining tool adopts the template 5 that has high-resolution complex three-dimensional solid figure, template 5 is fixed in the bottom of metal fixed mount 4, metal frame 4 can adopt two sections cylinders that diameter is different, its top connects the little driving governor 2 of Z axle (vertical 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, auxiliary electrode 8, reference electrode 9, etching solution 10, electrolytic cell 11 etc., in fact, template 5 also can be considered the part of electro-chemical systems, and template 5 is received potentiostat 1 by metal fixed mount 4 becomes working electrode.Auxiliary electrode 8 inserts in the etching solution 10 with reference electrode 9, and etching solution 10 is packed in the electrolytic cell 11.Electrolytic cell 11 is located on the little driving governor 7 of XY axle (trunnion axis) of drive unit.Machined material 6 places electrolytic cell 11.
Embodiment 2
Fig. 2 is the example of the present invention's machining 3 D pattern on silicon, carries out the silicon face micro-image after three-dimensional little processing.Processing conditions: adopt 0.1mol dm
-3HF solution contains 10mmol dm
-3HBr and 0.5mol dm
-3H
2SO
4Chemical system; Etching agent is at template electrode surface electrolysis Br
-The Br that produces
2Agent for capturing is for adding the H of etching solution
3AsO
3Adopt the constant potential method that the electrode potential of template electrode is remained 0.9V (with respect to the current potential of saturated calomel electrode) in whole etching process.The dentation template is made by silicon, and through splash-proofing sputtering metal titanium, platinum and conductive diamond film successively, template surface is coated by the inactive, conductive material conductive diamond film.Template is fixed on the bottom of metal fixed mount 4 shown in Figure 1 by conductive adhesive.Start drive unit and template is shifted to be fixed on the electrolytic cell bottom and be in n-type Si＜100〉monocrystalline silicon piece open-circuit condition under, after both distances reach certain value, start electro-chemical systems, generation etching agent Br
2, the processing of beginning etching, constantly moving die plate constantly carries out etching, and etching finished after the kind in 10 minutes, cut off electro-chemical systems, mentioned the template electrode.
Embodiment 3
Fig. 3 is the example of the present invention's machining 3 D pattern on silicon, carries out the silicon face micro-image after three-dimensional little processing.Processing conditions: adopt 0.2mol dm
-3K
2CrO
4With 0.01mol dm
-3Close CH
3COO NH
4With 12% isopropyl alcohol (2mol dm
-3) electrochemical etching solution; The etch species of in situ preparation is the OH that produces at the carbon fiber electrode surface reduction
-, agent for capturing is the CH in the electrochemical etching solution
3COONH
4Adopt the constant current method, keep the reduction current of 1.2mA on carbon fiber electrode (diameter is 7～8 microns) surface; Carbon fiber electrode is fixed on the bottom of metal fixed mount 4 shown in Figure 1.Starting drive unit shifts to carbon fiber electrode and is fixed on the electrolytic cell bottom and is in n-type Si＜110〉monocrystalline silicon piece under the open-circuit condition, after both distances reach certain value, the processing of beginning etching, constantly moving die plate constantly carries out etching, etching finished after the kind in 10 minutes, cut off electro-chemical systems, mention the template electrode.Cr wherein
3-, CrO
2 1-Be product.
Embodiment 4
Fig. 4 is the example of the present invention's machining 3 D pattern on p-type Si＜100〉monocrystalline silicon piece, carries out the silicon face micro-image after three-dimensional little processing.Processing conditions: adopt 1mol dm
-3HF solution contains 0.02mol dm
-3HBr and 0.5mol dm
-3H
2SO
4Chemical system; The etch species of in situ preparation is at template electrode surface electrolysis Br
-The Br that produces
2Agent for capturing is for adding the 100mmol dm of electrochemical etching solution
-3H
3AsO
3Adopt the constant current method that the anode current of template electrode is remained 12.5mA/cm in whole etching process
2
Embodiment 5
Fig. 5 is the example of the present invention's machining 3 D pattern on p-type Si＜100〉monocrystalline silicon piece, carries out the silicon face micro-image after three-dimensional little processing.Processing conditions: adopt 1mol dm
-3HF solution contains 0.05mol dm
-3HBr and 0.5mol dm
-3H
2SO
4Chemical system; The etch species of in situ preparation is at template electrode surface electrolysis Br
-The Br that produces
2Agent for capturing is for adding the 100mmol dm of electrochemical etching solution
-3H
3AsO
3Adopt the constant current method that the anode current of template electrode is remained 15mA/cm in whole etching process
2
Embodiment 6～107
Its processing step is similar to the above embodiments, and its difference is the composition and the content of etching solution and scavenger, and concrete composition and content and etching effect thereof see following table for details.
| Etching solution | Scavenger (or claiming agent for capturing) | Etching effect | ||
| Hydrobromic acid (or ammonium bromide, or 4 bromide, or tetraethyl bromination | Sulfuric acid (or hydrochloric acid, or phosphoric acid) (mol dm -3) | Hydrofluoric acid (or ammonium fluoride) (mol dm -3) | Arsenious acid (or NAC, or phenol) (mol dm -3) | |
| 0.005 | 1 | 2 | 0.01 | + |
| 0.005 | 1 | 1 | 0.01 | + |
| 0.005 | 1 | 0.1 | 0.01 | + |
| 0.005 | 0.1 | 2 | 0.01 | + |
| 0.005 | 0.1 | 1 | 0.01 | + |
| 0.005 | 0.1 | 0.1 | 0.01 | + |
| 0.005 | 1 | 1 | 0.05 | + |
| 0.005 | 1 | 1 | 0.01 | + |
| 0.005 | 1 | 1 | 0.02 | + |
| 0.005 | 1 | 1 | 0.03 | + |
| 0.005 | 1 | 1 | 0.04 | + |
| 0.005 | 1 | 1 | 0.05 | + |
| 0.005 | 1 | 1 | 0.1 | + |
| 0.005 | 1 | 5 | 0.08 | - |
| 0.005 | 1 | 4 | 0.08 | - |
| 0.005 | 1 | 3 | 0.08 | - |
| 0.01 | 1 | 2 | 0.01 | + |
| 0.01 | 1 | 1 | 0.01 | + |
| 0.01 | 1 | 0.1 | 0.01 | + |
| 0.01 | 0.1 | 2 | 0.01 | + |
| 0.01 | 0.1 | 1 | 0.01 | + |
| 0.01 | 0.1 | 0.1 | 0.01 | + |
| 0.01 | 1 | 1 | 0.05 | + |
| 0.01 | 1 | 1 | 0.01 | + |
| 0.01 | 1 | 1 | 0.02 | + |
| 0.01 | 1 | 1 | 0.03 | + |
| 0.01 | 1 | 1 | 0.04 | + |
| 0.01 | 1 | 1 | 0.05 | + |
| 0.01 | 1 | 1 | 0.1 | + |
| 0.01 | 1 | 5 | 0.08 | - |
| 0.01 | 1 | 4 | 0.08 | - |
| 0.05 | 1 | 2 | 0.01 | + |
| 0.05 | 1 | 1 | 0.01 | + |
| 0.05 | 1 | 0.1 | 0.01 | + |
| 0.05 | 0.1 | 2 | 0.01 | + |
| 0.05 | 0.1 | 1 | 0.01 | + |
| 0.05 | 0.1 | 0.1 | 0.01 | + |
| 0.05 | 1 | 1 | 0.05 | + |
| 0.05 | 1 | 1 | 0.01 | + |
| 0.05 | 1 | 1 | 0.02 | + |
| 0.05 | 1 | 1 | 0.03 | + |
| 0.05 | 1 | 1 | 0.04 | + |
| 0.05 | 1 | 1 | 0.05 | + |
| 0.05 | 1 | 1 | 0.1 | + |
| 0.05 | 1 | 5 | 0.08 | - |
| 0.05 | 1 | 4 | 0.08 | - |
| 0.05 | 1 | 3 | 0.08 | - |
| 0.1 | 1 | 2 | 0.01 | + |
| 0.1 | 1 | 1 | 0.01 | + |
| 0.1 | 1 | 0.1 | 0.01 | + |
| 0.1 | 0.1 | 2 | 0.01 | + |
| 0.1 | 0.1 | 1 | 0.01 | + |
| 0.1 | 0.1 | 0.1 | 0.01 | + |
| 0.1 | 1 | 1 | 0.05 | + |
| 0.1 | 1 | 1 | 0.01 | + |
| 0.1 | 1 | 1 | 0.02 | + |
| 0.1 | 1 | 1 | 0.03 | + |
| 0.1 | 1 | 1 | 0.04 | + |
| 0.1 | 1 | 1 | 0.05 | + |
| 0.1 | 1 | 1 | 0.1 | + |
| 0.1 | 1 | 3 | 0.08 | - |
| Potassium chromate | Isopropyl alcohol | Ammonium acetate | ||
| 0.05 | 6 | 0.01 | - | |
| 0.05 | 8 | 0.01 | + | |
| 0.05 | 10 | 0.01 | + | |
| 0.05 | 15 | 0.01 | + | |
| 0.05 | 30 | 0.01 | + | |
| 0.1 | 6 | 0.01 | - | |
| 0.1 | 10 | 0.01 | + | |
| 0.1 | 30 | 0.01 | + | |
| 0.1 | 10 | 0.02 | + | |
| 0.1 | 10 | 0.03 | + | |
| 0.2 | 10 | 0.04 | + | |
| 0.2 | 10 | 0.05 | + | |
| 0.2 | 10 | 0.06 | + | |
| 0.2 | 10 | 0.01 | + | |
| 0.5 | 10 | 0.01 | + | |
| Potassium chromate | Isopropyl alcohol | Hydrochloric acid | ||
| 0.05 | 6 | 0.01 | - | |
| 0.05 | 8 | 0.01 | + | |
| 0.05 | 10 | 0.01 | + | |
| 0.05 | 15 | 0.01 | + | |
| 0.05 | 30 | 0.01 | + | |
| 0.1 | 6 | 0.01 | - | |
| 0.1 | 10 | 0.01 | + |
| 0.1 | 30 | 0.01 | + | |
| 0.1 | 10 | 0.02 | + | |
| 0.1 | 10 | 0.03 | + | |
| 0.2 | 10 | 0.04 | + | |
| 0.2 | 10 | 0.05 | + | |
| 0.2 | 10 | 0.06 | + | |
| Potassium bichromate (mol dm -3) | Isopropyl alcohol (content %) | Hydrochloric acid (mol dm -3) | ||
| 0.05 | 6 | 0.01 | - | |
| 0.05 | 8 | 0.01 | + | |
| 0.05 | 10 | 0.01 | + | |
| 0.05 | 15 | 0.01 | + | |
| 0.05 | 30 | 0.01 | + | |
| 0.1 | 6 | 0.01 | - | |
| 0.1 | 10 | 0.01 | + | |
| 0.1 | 30 | 0.01 | + | |
| 0.1 | 10 | 0.02 | + | |
| 0.1 | 10 | 0.03 | + | |
| 0.2 | 10 | 0.04 | + | |
| 0.2 | 10 | 0.05 | + | |
| 0.2 | 10 | 0.06 | + |
Annotate
*: "+" expression can etch three-dimensional ultra microstructure figure; "-" expression fails to etch three-dimensional ultra microstructure figure.
Claims (3)
1, silicon face complicate three dimension microstructure processing method is characterized in that the steps include:
1). the template that will have complementary structure structure to be processed is fixed on the fixed mount;
2). electrochemical etching solution is injected the container that is placed with silicon chip to be processed, and described electrochemical etching solution contains two parts: etching agent and scavenger, etching agent are selected from and contain SO
4 2-, Cl
1-, PO
3 3-, Cr
2O
7 2-, CrO
4 2-, Cr
3-, CrO
2 1-, OH
1-, isopropyl alcohol or F
1-In at least a, its concentration range is 0.05～0.2M; Scavenger is selected from least a in the amino acids that contains sulfydryl or the phenol, and its concentration range is 0.005～0.1M;
3). mobile fixed mount makes template immerse electrochemical etching solution;
4). as working electrode, in container, establish auxiliary electrode and reference electrode with template in addition, start electro-chemical systems;
5). template is progressively shifted to silicon chip, begin workpiece to be machined is carried out etching;
6). drive unit constantly with template to being moved by silicon chip keeping etching constantly to carry out, finish to etching, template is left silicon chip surface.
2, the processing method of silicon face complicate three dimension microstructure as claimed in claim 1, it is characterized in that etching agent is itself directly etching agent of chemical etching silicon, possess at least a in the etching agent of accelerating the etching speed of other etching agent chemical etching silicon in the solution.
3, the processing method of silicon face complicate three dimension microstructure as claimed in claim 1, it is characterized in that the cleaning reaction to etching agent is photochemistry decomposition reaction, the Thermochemical Decomposition reaction of etching agent self, or the chemical reaction of etching agent self and silicon is at least a.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274742B (en) * | 2007-03-28 | 2010-07-28 | 中国科学院微电子研究所 | Bulk silicon corrosion corollary equipment resistant to water flow impact |
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|---|---|---|---|---|
| CN101880907B (en) * | 2010-07-07 | 2012-04-25 | 厦门大学 | Electrochemical levelling and polishing processing method with nanometer precision and device thereof |
| CN102092676A (en) * | 2011-01-20 | 2011-06-15 | 浙江大学 | Method and system for preparing high-aspect ratio three-dimensional microstructures in batch |
| CN109292731A (en) * | 2018-09-11 | 2019-02-01 | 西南交通大学 | Micro-nano processing method based on electrochemistry friction induction |
| CN113651289B (en) * | 2021-07-07 | 2024-06-04 | 北京大学 | Preparation method of sucker structure forming die and preparation method of sucker structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101274742B (en) * | 2007-03-28 | 2010-07-28 | 中国科学院微电子研究所 | Bulk silicon corrosion corollary equipment resistant to water flow impact |
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