CN100590062C - Method for making three-dimension electric casting micro structure - Google Patents
Method for making three-dimension electric casting micro structure Download PDFInfo
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- CN100590062C CN100590062C CN200710012854A CN200710012854A CN100590062C CN 100590062 C CN100590062 C CN 100590062C CN 200710012854 A CN200710012854 A CN 200710012854A CN 200710012854 A CN200710012854 A CN 200710012854A CN 100590062 C CN100590062 C CN 100590062C
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Abstract
The present invention relates to micro electroformed metal devices, belongs to the field of micro manufacture technology, and is especially process of making 3D electroformed micro structure. The making process includes the steps of pre-treatment of the substrate, making micro electroforming mold for the connecting layer, micro electroforming, preparing copper crystal seed layer, making the nickelstructure layer, post-treatment and eliminating the sacrificial layer. The process can make micro cantilever structure with firm binding and small interlayer stress, and the micro cantilever structure is applied as the key device of micro sensor and micro driver.
Description
Technical field
The invention belongs to the micro-fabrication technology field, relate to the little electroforming metal device of metallic substrates class.
Background technology
Along with the development of device microminaturization and micro electro mechanical system (MEMS) technology, three-dimensional cantilever micro-structural has been widely used in microsensor and microdrive field at present as the core component of micro sensing/driver.Its processing and fabricating method more and more receives scientific research personnel's concern.The making of existing three-dimensional cantilever micro-structural is main on silicon or substrate of glass to be realized by methods such as photoetching, little electroforming, rolls up supplementary issue in July, 2005 252-254 page or leaf as 2005 the 5th phase 658-660 pages or leaves of magazine " Xiamen University's journal " and magazine " Chinese mechanical engineering " the 16th.The technological process of document 1 is: the silica of on silicon substrate, growing earlier, and photoetching sacrifice layer (material is photoresist BP212), sputter Cu is as crystal seed layer.Resist coating AZP4620 photoetching again forms the thick type photoresist pattern that the electroforming structure sheaf is used.Carry out little electroforming of nickel then, remove photoresist, remove crystal seed layer, remove sacrifice layer, discharge the cantilever beam micro-structural at last.Have only several microns with the sacrifice layer part of the cantilever beam structures of the method processing and the thickness of the little electroforming part of nickel.And 2 in document has provided on glass substrate the decline processing and fabricating scheme of overload cut-out of brush sheet of making, and does not have the actual micro switch that processes.At present in microsensor and microdrive field, in the cantilever micro-structural that the occasion urgent need metallic substrates that motion requires and structural strength is had relatively high expectations or claimed structure conducts electricity is arranged.
Summary of the invention
The problem to be solved in the present invention is on the basis of little electroforming metal mould preparation method, makes full use of sacrificial layer technology, proposes to make on metal substrate the method for three-dimensional cantilever micro-structural, for example, and nickel metal, 5CrNiMo steel alloy etc.The micro-structural of making based on this method has layer and combines with layer that firm, little electroformed layer internal stress is little, the micro-structural verticality of side wall is good, surface smoothness is high, can be used as the core devices of the high microsensor/microdrive of motion requirement and requirement of strength.
The technical solution used in the present invention is a kind of preparation method of three-dimension electric casting micro structure, comprises the preparation of substrate pre-treatment, the making of the little electroforming pattern of articulamentum, little electroforming, copper crystal seed layer, the making of nickel structure sheaf, little electroforming post processing, sacrifice layer removal operation.It is characterized in that: adopt sacrificial layer technology, on metallic substrates, little electroforming of the ultraviolet photolithographic by 2 SU-8 photoresists, the preparation of copper crystal seed layer and 2 nickel realizes the making of three micro-cantilever micro-structurals; In the production process of the little electroforming pattern of articulamentum, select the SU-8 photoresist as sacrificial layer material; In little electroforming process, to carry out surface activation process before the ni substrate electroforming, the prescription of activation corrosion liquid is 10～20% nitric acid, 80～90% glacial acetic acids (volume ratio); In the preparation section of copper crystal seed layer, the corrosive liquid of copper adopts is 2.5% HNO3 solution, for removing the positive photoresist on copper surface, adopts the method for uv-exposure simultaneously; Remove in the operation at sacrifice layer, the method that adopts the concentrated sulfuric acid to boil, the concrete steps of its preparation method are as follows:
(1) substrate pre-treatment: the substrate pre-treatment is divided into machining pre-treatment and two parts of surface clean, the machining pre-treatment comprises successively: milling, grinding, correct grinding, line cutting and polishing, surface clean adopts the Solvent degreasing method, and organic solvent adopts acetone and ethanol;
(2) making of the little electroforming pattern of articulamentum: the little electroforming pattern of articulamentum also claims the sacrifice layer of cantilever micro-structural, sacrificial layer material adopts the SU-8 photoresist, in the production process of the little electroforming pattern of articulamentum, adopt the adhesion layer of homemade photoresist as the SU-8 photoresist, SU-8 photoresist and adhesion layer adopt the alignment process in the photoetching technique, the microstructure graph that obtains after developing, direct pattern as little electroforming;
(3) little electroforming: little electroforming of nickel is exactly the electro-deposition that realizes nickel in the free space of little electroforming pattern, in little electroforming process, to carry out surface activation process before the ni substrate electroforming, the prescription of activation corrosion liquid is 10～20% nitric acid, 80～90% glacial acetic acids (volume ratio), etching time is 10～20 seconds, and electroforming solution adopts unstressed casting nickel prescription;
(4) preparation copper crystal seed layer: the preparation section of copper crystal seed layer comprises the sputter of copper and the photoetching of copper, and the sputtering equipment of copper is the radio-frequency sputtering platform; The lithography step of copper is: evenly be coated with homemade positive photoresist with sol evenning machine, and 3500 rev/mins of rotating speeds, baking is 45 minutes on 60 ℃ of hot plates, utilize exposure machine to carry out uv-exposure the 1st time, 30 seconds time for exposure, put into 0.5% NaOH developer solution and develop, the back baking is 1 hour on 60 ℃ of hot plates; Put into 2.5% HNO
3Corrosion copper is about 2 minutes in the solution; With sol evenning machine the water on copper surface is dried, whole substrate surface is carried out uv-exposure the 2nd time, 2 minutes time for exposure, then substrate to be put into 0.5% NaOH and removed the photoresist on copper surface, water is rinsed well;
(5) making of nickel structure sheaf: the making of nickel structure sheaf comprises the making and the little electroforming of nickel of little electroforming pattern, in the production process of little electroforming pattern, adopts the ultraviolet photolithographic technology of SU-8 photoresist; The little electroforming of nickel is exactly the electro-deposition that realizes nickel in the free space of little electroforming pattern;
(6) little electroforming post processing: little electroforming post processing comprises correct grinding, the polishing of vacuum annealing and micro element.To remove internal stress is that the vacuum annealing of purpose is exactly that the micro-structural that has the SU-8 photoresist is put into vacuum annealing furnace, is warmed up to 350～400 ℃ after reaching the specified vacuum degree, keeps cooling off naturally after 100～120 minutes.Micro-structural after the annealing also will be through correct grinding and polishing;
(7) sacrifice layer is removed: the method that the removal of sacrifice layer adopts the concentrated sulfuric acid to boil.It is 95%～98% the concentrated sulfuric acid that micro-structural to be removed photoresist is put into concentration, the concentrated sulfuric acid is placed on the electric furnace boils, and the time is 5～10 minutes, treats that SU-8 photoresist on the micro-structural all after the dissolving, rinses well with deionized water.
The invention has the beneficial effects as follows: overcome traditional on silicon substrate the flimsy shortcoming of substrate during preparation cantilever micro-structural, improved the intensity of structure.At user's specific requirement, can prepare thickness and reach hundreds of microns, structural strength height, cantilever micro-structural that little electroformed layer internal stress is little; Can provide the metallic substrates micro-cantilever core devices that layer combines firmly with interlayer, verticality of side wall is good, surface smoothness is high, structural strength is high for microsensor/microdrive field.
Description of drawings
Fig. 1 is the structure diagram of cantilever beam.
Fig. 2 is the making schematic flow sheet of three-dimensional cantilever micro-structural.
Fig. 3 is the 1st photo-mask process, and Fig. 4 is a developing procedure, and Fig. 5 is the 1st little electroforming process, and Fig. 6 is a preparation copper crystal seed layer operation, and Fig. 7 is the 2nd photo-mask process, and Fig. 8 is the 2nd little electroforming process, and Fig. 9 is that sacrifice layer is removed operation.Wherein: 1-ni substrate, 2-adhesion layer, 3-SU-8 photoresist, 4-mask blank, 5-free space, 6-electroformed nickel metal, 7-copper crystal seed layer, UV-ultraviolet light.
The specific embodiment
Below in conjunction with accompanying drawing, describe the concrete embodiment of the present invention in detail.For example: (53mm * 63mm * (bracketed part 1 is of a size of 15mm * 100um * 300um to the high purity nickel substrate after correct grinding, polishing 2mm) to go up electroforming one " cantilever beam " shape, cantilever 1 is of a size of 100um * 100um * 50um with the articulamentum 2 of substrate 3, see accompanying drawing 1) three-dimensional microstructures, it is as follows by the concrete steps of flow chart 2 that it makes this structure:
1, substrate pre-treatment base material is selected highly purified nickel metal, the nickel substrate pre-treatment is divided into machining pre-treatment and two parts of surface clean, the machining pre-treatment comprises successively: milling, grinding, correct grinding, line cutting and polishing, surface clean adopts the Solvent degreasing method, and organic solvent adopts acetone and ethanol.
2. the little electroforming pattern of the making articulamentum of the little electroforming pattern of the articulamentum sacrifice layer that also is the cantilever micro-structural, sacrificial layer material adopts the SU-8 photoresist, sees accompanying drawing 3.In order to improve the adhesion of SU-8 photoresist 3 and ni substrate 1, adopt the adhesion layer 2 of homemade photoresist in the test as SU-8 photoresist 3.Little electroforming pattern is made by the photoetching process of SU-8 photoresist 3 and is formed.The microstructure graph that obtains after developing can be seen accompanying drawing 4 directly as the pattern of little electroforming.
3. little electroforming of little electroformed nickel is exactly the 5 li electro-deposition that realize nickel of free space at the little electroforming pattern shown in the accompanying drawing 4, sees accompanying drawing 5.In little electroforming process, to carry out surface activation process before the ni substrate electroforming, the prescription of activation corrosion liquid is 10～20% nitric acid, 80～90% glacial acetic acids (volume ratio), and the time is 10～20 seconds, and electroforming solution adopts unstressed casting nickel prescription.
4. the preparation section of the preparation copper crystal seed layer of copper crystal seed layer comprises the sputter of copper and the photoetching of copper.The sputtering equipment of copper is the radio-frequency sputtering platform, and process conditions are: 400～500 watts of radio-frequency powers, time: 6～8 minutes.The lithography step of copper is: evenly be coated with homemade positive photoresist with sol evenning machine, and 3500 rev/mins of rotating speeds, baking is 45 minutes on 60 ℃ of hot plates, utilize exposure machine to carry out uv-exposure the 1st time, 30 seconds time for exposure, put into 0.5% NaOH developer solution and develop, the back baking is 1 hour on 60 ℃ of hot plates; Put into 2.5% HNO
3Corrosion copper is about 2 minutes in the solution; With sol evenning machine the water on copper surface is dried, whole substrate surface is carried out uv-exposure the 2nd time, 2 minutes time for exposure, then substrate to be put into 0.5% NaOH and removed the photoresist on copper surface, water is rinsed well, sees accompanying drawing 6.
5. the making of the making nickel structure sheaf of nickel structure sheaf comprises the making and the little electroforming of nickel of little electroforming pattern.In the production process of little electroforming pattern, adopt the ultraviolet photolithographic technology of SU-8 photoresist, see accompanying drawing 7; The little electroforming of nickel is exactly the 5 li electro-deposition that realize nickel of free space at the little electroforming pattern shown in the accompanying drawing 7, sees accompanying drawing 8.
6. the little electroforming post processing of little electroforming post processing comprises correct grinding, the polishing of vacuum annealing and micro element.To remove internal stress is that the vacuum annealing of purpose is exactly that the micro-structural that has the SU-8 photoresist is put into vacuum annealing furnace, is warmed up to 350～400 ℃ after reaching the specified vacuum degree, keeps cooling off naturally after 100～120 minutes.Micro-structural after the annealing also will be through correct grinding and polishing.
7.SU-8 the method that the removal of the removal sacrifice layer of photoetching glue victim layer adopts the concentrated sulfuric acid to boil.It is 95%～98% the concentrated sulfuric acid that micro-structural to be removed photoresist is put into concentration, the concentrated sulfuric acid is placed on the electric furnace boils, and the time is 5～10 minutes, treats that SU-8 photoresist on the micro-structural all after the dissolving, rinses well with deionized water, sees accompanying drawing 9.
Claims (1)
1, a kind of preparation method of three-dimension electric casting micro structure, comprise the preparation of substrate pre-treatment, the making of the little electroforming pattern of articulamentum, little electroforming, copper crystal seed layer, the making of nickel structure sheaf, little electroforming post processing, sacrifice layer removal operation, it is characterized in that: adopt sacrificial layer technology, on metallic substrates, little electroforming of the ultraviolet photolithographic by 2 SU-8 photoresists, the preparation of copper crystal seed layer and 2 nickel realizes the making of three micro-cantilever micro-structurals; In the production process of the little electroforming pattern of articulamentum, select the SU-8 photoresist as sacrificial layer material; In little electroforming process, to carry out surface activation process before the ni substrate electroforming, the prescription of activation corrosion liquid is 10～20% nitric acid, 80～90% glacial acetic acids (volume ratio); In the preparation section of copper crystal seed layer, the corrosive liquid of copper adopts is 2.5% HNO
3Solution for removing the positive photoresist on copper surface, adopts the method for uv-exposure simultaneously; Remove in the operation at sacrifice layer, the method that adopts the concentrated sulfuric acid to boil, the concrete steps of its preparation method are as follows:
(1) substrate pre-treatment: the substrate pre-treatment is divided into machining pre-treatment and two parts of surface clean, the machining pre-treatment comprises successively: milling, grinding, correct grinding, line cutting and polishing, surface clean adopts the Solvent degreasing method, and organic solvent adopts acetone and ethanol;
(2) making of the little electroforming pattern of articulamentum: the little electroforming pattern of articulamentum also claims the sacrifice layer of cantilever micro-structural, sacrificial layer material adopts the SU-8 photoresist, in the production process of the little electroforming pattern of articulamentum, adopt the adhesion layer of homemade photoresist as the SU-8 photoresist, SU-8 photoresist and adhesion layer adopt the alignment process in the photoetching technique, the microstructure graph that obtains after developing, direct pattern as little electroforming;
(3) little electroforming: little electroforming of nickel is exactly the electro-deposition that realizes nickel in the free space of little electroforming pattern, in little electroforming process, to carry out surface activation process before the ni substrate electroforming, the prescription of activation corrosion liquid is 10～20% nitric acid, 80～90% glacial acetic acids (volume ratio), etching time is 10～20 seconds, and electroforming solution adopts unstressed casting nickel prescription;
(4) preparation copper crystal seed layer: the preparation section of copper crystal seed layer comprises the sputter of copper and the photoetching of copper, and the sputtering equipment of copper is the radio-frequency sputtering platform; The lithography step of copper is: evenly be coated with homemade positive photoresist with sol evenning machine, and 3500 rev/mins of rotating speeds, baking is 45 minutes on 60 ℃ of hot plates, utilize exposure machine to carry out uv-exposure the 1st time, 30 seconds time for exposure, put into 0.5% NaOH developer solution and develop, the back baking is 1 hour on 60 ℃ of hot plates; Put into 2.5% HN0
3Corrosion copper is about 2 minutes in the solution; With sol evenning machine the water on copper surface is dried, whole substrate surface is carried out uv-exposure the 2nd time, 2 minutes time for exposure, then substrate to be put into 0.5% NaOH and removed the photoresist on copper surface, water is rinsed well;
(5) making of nickel structure sheaf: the making of nickel structure sheaf comprises the making and the little electroforming of nickel of little electroforming pattern, in the production process of little electroforming pattern, adopts the ultraviolet photolithographic technology of SU-8 photoresist; The little electroforming of nickel is exactly the electro-deposition that realizes nickel in the free space of little electroforming pattern;
(6) little electroforming post processing: little electroforming post processing comprises correct grinding, the polishing of vacuum annealing and micro element, to remove internal stress is that the vacuum annealing of purpose is exactly that the micro-structural that has the SU-8 photoresist is put into vacuum annealing furnace, be warmed up to 350～400 ℃ after reaching the specified vacuum degree, keep cooling naturally after 100～120 minutes, the micro-structural after the annealing also will be through correct grinding and polishing;
(7) sacrifice layer is removed: the method that the removal of sacrifice layer adopts the concentrated sulfuric acid to boil, it is 95%～98% the concentrated sulfuric acid that micro-structural to be removed photoresist is put into concentration, the concentrated sulfuric acid is placed on the electric furnace boils, time is 5～10 minutes, after treating the whole dissolvings of SU-8 photoresist on the micro-structural, rinse well with deionized water.
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| CN101814866B (en) * | 2010-04-16 | 2012-08-01 | 大连理工大学 | Method for manufacturing electrothermal drive microstructure |
| CN102494833A (en) * | 2011-12-16 | 2012-06-13 | 淮阴工学院 | Mini-type pressure sensor based on SU-8 polymer |
| CN102995098B (en) * | 2012-12-04 | 2015-07-01 | 哈尔滨飞机工业集团有限责任公司 | Electric cutting process for electroforming nickel-coated piece |
| CN103103583B (en) * | 2013-01-14 | 2016-03-02 | 大连理工大学 | A kind of metal base makes the method for multiple layer metal movable microstructure |
| CN105603468B (en) * | 2015-12-21 | 2018-08-21 | 大连理工大学 | The method that highly dense fine nickel cylindrical-array is prepared in metal nickel substrate |
| CN105908222A (en) * | 2016-05-03 | 2016-08-31 | 岭南师范学院 | Preparation method of precise chip metal mold with low cost and high utilization rate |
| CN107177866B (en) * | 2017-04-28 | 2019-03-05 | 大连理工大学 | The method of micro- radio frequency T shape power splitter is prepared in metallic substrates |
| CN111001982B (en) * | 2019-11-25 | 2022-03-29 | 大连理工大学 | Metal copper micro-channel heat sink with comb-tooth structure and manufacturing method |
| CN111791026A (en) * | 2020-06-15 | 2020-10-20 | 深圳市精铸模具有限公司 | Micro-thin metal device manufactured by electroforming and precision machining process |
| CN111659000A (en) * | 2020-06-30 | 2020-09-15 | 华东师范大学 | Hollow metal microneedle, hollow metal microneedle array and preparation method thereof |
| CN113173552B (en) * | 2021-04-09 | 2023-06-23 | 深圳清华大学研究院 | Large-scale super-slip element with conductivity, processing technology thereof and large-scale super-slip system |
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