CN101200281A - Method for realizing microstructure on pyrolytic graphite chip - Google Patents
Method for realizing microstructure on pyrolytic graphite chip Download PDFInfo
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- CN101200281A CN101200281A CNA2007101718870A CN200710171887A CN101200281A CN 101200281 A CN101200281 A CN 101200281A CN A2007101718870 A CNA2007101718870 A CN A2007101718870A CN 200710171887 A CN200710171887 A CN 200710171887A CN 101200281 A CN101200281 A CN 101200281A
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Abstract
The invention discloses a micro-structural realization method on pyrolytic graphite substrate, belonging to a micro electromechanical technical field, the method adopts pyrolytic graphite as the substrate, and then performs the leveling, cleaning, insulating and re-cleaning of the substrate; the back of the pyrolytic graphite substrate is arranged with lithography alignment marks, multi-layer structure or high aspect ratio structure is formed by overlay; the front of the pyrolytic graphite substrate is sprayed with metallic film as seed layer, positive photoresist, lithography and develop are performed, and then electroplating mold is made so as to form an electroplating structural layer, after performing the positive photoresist, lithography and developing twice, positive photoresist is removed, ultrasonic cleaning is performed, and alumina is sprayed, and then the substrate is ground and is cleaned; the alumina is sprayed with the metallic film as the seed layer, and the seed layer is spread with SU8 negative photoresist, after performing the lithography, developing and electroplating, the SU8 negative photoresist is removed and the alumina is removed, so that the high aspect ratio structure is made on the pyrolytic graphite substrate. The invention has novel substrate materials and special processing performance.
Description
Technical field
The present invention relates to a kind of method of field of micro electromechanical technology, specifically is a kind of implementation method of microstructure on pyrolytic graphite chip.
Background technology
MEMS is along with the development of semiconductor integrated circuit Micrometer-Nanometer Processing Technology and ultraprecise Machining Technology grows up, so in the past few decades, the research of making the milli machine structure on silicon chip has obtained carrying out.But, because the MEMS part category is various, and has a movable microstructure more, therefore it has all proposed new requirement in design, material, processing, the system integration, packaging and testing technology, this has formed the characteristics that MEMS oneself is different from IC on the one hand, and most typical on material and processing method is especially processing micro structure on glass substrate of non-silicon MEMS.The appearance of these non-silicon chips and processing method thereof, the fine specific demand of satisfying some devices more and more is subjected to people's attention, becomes new research focus.
Find through literature search prior art, people such as Wang Yangyuan are in " electronic letters, vol ", o. 11th in 2002, the article of delivering on the p1577-1584 " silica-based MEMS process technology and standard technology research thereof ", discuss silica-based MEMS standard technology in detail, comprised three body silicon standard technologies and the surperficial sacrifice layer standard technology of a cover; Also find in the retrieval, Zhao Xiaolin, people such as Wang Xining, in " micro-nano electronic technology ", 2005 the 1st phases, p30-32, on the article " double-layer suspension structure radio frequency little inductance make research " delivered, provided and on glass substrate, made the example of double-layer suspension micro-structural and provide corresponding technological process.But, about on pyrolytic graphite chip, carrying out the micro-structural method for processing and the moulding device yet there are no relevant report.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art and defective, a kind of implementation method of microstructure on pyrolytic graphite chip is provided, make its application possibility of diamagnetic performance in micro-structural at the pyrolytic graphite excellence, solve simultaneously and only adopt the problem of on common substrates such as silicon or glass, carrying out the making of micro-structural in the existing MEMS usually, for realizing utilizing the special and stronger diamagnetic performance of pyrolytic graphite to carry out the support that element manufacturing provides fine machining method, have the substrate material novelty, the processing device has advantages such as property.
The present invention is achieved by the following technical solutions, may further comprise the steps:
The first step adopts the positive adhesive process of tradition and negative glue of SU8 and accurate LIGA technology, adopts pyrolytic graphite as substrate, before processing substrate is cooked leveling, cleaning, insulating and preparation such as cleaning again;
Second step, do the photoetching alignment mark in the one side of pyrolytic graphite chip, be referred to as back side alignment mark, the litho machine of double-sided exposure is all used in the photoetching of every layer of structure later on, back side alignment mark is focused simultaneously, by the multilayer alignment, realizes sandwich construction or high aspect ratio structure;
In the 3rd step, pyrolytic graphite be positive at the another side of substrate after substrate is carried out back side alignment mark through preparation and the back side, and sputtered metal film is as Seed Layer, positive-glue removing on Seed Layer, photoetching, develop after, the mould of making electroplated structural layer;
The 4th step, electroplate structure sheaf on the Seed Layer in the mould of electroplated structural layer, after twice positive-glue removing, photoetching, development and plating, remove positive glue, ultrasonic cleaning, sputter aluminium oxide, then grind substrate and do cleaning;
In the 5th step, sputtered metal film is made Seed Layer on aluminium oxide, gets rid of the negative glue of SU8 again on Seed Layer, by photoetching, development and plating, goes SU8 to bear glue, and deoxidation aluminium is realized making high aspect ratio microstructures on the pyrolytic graphite.
On the pyrolytic graphite chip of the present invention, no matter adopt positive adhesive process, the negative adhesive process of SU8, perhaps both combinations, can on substrate, realize making differing heights, width, and relative positional accuracy height between structure sheaf, the micro-structural that adhesion is strong, utilize the special diamagnetic performance of pyrolytic graphite chip again, the micro-structural in conjunction with making reaches the realization of required function device.
Pyrolytic graphite is with hydrocarbon gas (methane, propane etc.) pyrolysis and the very strong novel graphite of a kind of anisotropy under depositing is called oriented graphite again on the surface of solids of heating.This graphite not only has very high purity and near the density of theoretical value, and has on unique electricity and the anisotropy on the calorifics.In the present invention, exactly because pyrolytic graphite has excellent electric conductivity, for avoiding itself and conductive structure layer that unnecessary short circuit takes place, the primary work that realizes processing micro structure thereon is will carry out insulating to it to handle, and only utilizes the diamagnetic performance of its excellence.
Owing to utilize positive glue to come processing micro structure, attainable depth-to-width ratio is limited, adds structure in order to realize that high-aspect-ratio or multilayer are built, and need carry out the multilayer alignment.For guaranteeing the accuracy of multilayer alignment, reduce the interlayer error, need available alignment mark.In the present invention, because what adopt is the litho machine with double-sided exposure, consider that simultaneously positive aligned pattern faces the possibility of being covered by Seed Layer or structure sheaf, the final back side alignment mark that adopts is assisted, mainly be by in substrate back sputter one deck Seed Layer, directly utilizing Seed Layer to make alignment mark by photoetching, etching technics, processing step is simple.Moreover for protection back side alignment mark is not damaged in follow-up series of process process, the present invention is sputter protective layer on the alignment mark overleaf, as aluminium oxide, is protected.
In the present invention, positive glue is mainly used in the mould of electroplating the Cu structure, and the mask during as etching (dry method or wet method); Negative glue SU-8 thick film based on the UV-LI6A technology, is used to make high-aspect-ratio Cu micro-structural.No matter adopt which kind of technology, all will be before whirl coating the sputtering seed layer, make to electroplate and be achieved, the material that Seed Layer generally requires Seed Layer with the electroplated metal structural material character of wanting approaching, require it to have stronger metallic conductivity again, passivation takes place in Seed Layer idle surface easily, so require the surface passivation layer of Seed Layer easily to remove, because electroplated structural layer employing Cu is an example, adoptable Seed Layer has: Ti/Cu, Cr/Cu, Cr/Au etc. among the present invention.
Compared with prior art, the substrate material of the present invention's employing is a pyrolytic graphite.This material has been widely used for aerospace, atomic energy, metallurgy, electronics, bioengineering etc.It is the more intense a kind of material of a kind of diamagnetism.Common diamagnetic substance also comprises water, protein, diamond, DNA, plastic cement, wood, bismuth etc.In these diamagnetic substances, the chances are surpasses 20 times more than of water for the diamagnetic performance of graphite.Because the magnetic susceptibility of diamagnetic substance is negative value, under the effect of external magnetic field, can produce the effect of slight resistance external magnetic field.If diamagnetic substance is used in the permanent magnet suspension structure, for the magnet that suspends diamagnetic stable effect is arranged, when levitated magnet had the trend of the skew up and down that departs from the equilbrium position, the diamagnetism of diamagnetic substance will resist this trend, makes it balance again.Utilize diamagnetic substance to realize that passive magnetic suspends, and is significant equally under the normal temperature on engineering: 1) can realize passive stable magnetic suspension fully, system is simple, and operational reliability is improved greatly; 2) owing to neither need to control the energy input, also do not need the energy of superconduction refrigeration, system effectiveness improves greatly; 3) system bulk and weight reduce.These characteristics determined pyrolytic graphite be highly suitable for and make micro-structural among the MEMS, realize waiting some phenomena such as diamagnetic suspension, can utilize this feature to realize microgravimetry, micro-acceleration gauge even little gyro simultaneously again.
The present invention adopts the positive adhesive process of tradition and negative glue of SU8 and accurate LIGA technology, considered that substrate is that non-silicon non-glass materials, substrate need problems such as insulating, multilayer overlay alignment difficulty, Seed Layer conduction and adhesion, thereby provided the implementation method of on pyrolytic graphite chip, making micro-structural.The positive general whirl coating thickness of glue AZ4620 5-10 μ m among the present invention and the general whirl coating thickness of another kind of AZ4903 10-30 μ m; The negative glue SU8-50 whirl coating thickness of the SU8 of MicroChem company is mainly below 200 μ m, the SU8-100 single whirl coating thickness that adopts among the present invention then can reach more than the 400 μ m, thereby utilize this method can realize more than three layers that micro-structural and interlayer adhesion are good, utilize the positive photoresist of different model can realize several microns thickness of single layer structure simultaneously to the twenty or thirty micron, if utilize negative photoresist, then can realize the structure of hundreds of microns of thickness in monolayer.
Description of drawings
Fig. 1 is the inventive method flow chart; wherein: A; substrate is prepared; B; make back side alignment mark and protective mulch; C; positive sputtering seed layer; positive-glue removing and photoetching for the first time; develop; D; electroplate ground floor copper (Cu) structure; E; positive-glue removing and photoetching for the second time; develop F; electroplate second layer copper (Cu) structure, G; positive glue removes photoresist; spatter the Seed Layer at quarter; H; the sputter aluminium oxide also carries out planarizing process; I; the sputtering seed layer gets rid of negative glue of SU8 and photoetching; develop J; electro-coppering for the third time (Cu) structure; K; SU8 removes photoresist; spatter the Seed Layer at quarter, L; phosphoric acid etching oxidation aluminium; clean.
Among the figure: 1, pyrolytic graphite chip; 2, silica; 3, Seed Layer (mark is used); 4, protective layer; 5, positive glue; 6, Seed Layer (electroplate and use); 7, copper (Cu); 8, aluminium oxide; 9, the negative glue of SU8.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
With the negative adhesive process of positive glue AZ P4620 and the SU8-100 processing micro structure that combines is example, Seed Layer adopts the Cr/Cu metal composite thin film, the structural material of electroplating is copper (Cu), use the double-sided exposure litho machine, in the present embodiment, the concrete parameter condition of some technologies is: (1) sputtering seed layer Cr/Cu metal composite thin film adopts the German Leybold-Heraus Z550 of company type alternating current-direct current magnetic control sputtering system, and the primary condition of sputter is: base vacuum 2 * 10
-4Pa, operating air pressure 0.6-0.8Pa, sputtering power 600W, sputter rate 10-50nm/min; (2) spatter the 2440 type sputters that carving technology adopts U.S. Comptech company, spattering the flow of carving gas Ar is 70ml/min, base vacuum 6 * 10
-4Pa, operating air pressure 2.7Pa, sputtering power 500-700W.(3) the sputter aluminium oxide also adopts 2440 type sputters of U.S. Comptech company, base vacuum 2 * 10
-4Pa, operating air pressure 2.7Pa, sputtering power 4000W.But these technological parameters do not constitute limitation of the invention.
The present embodiment implementing procedure as shown in Figure 1.A among Fig. 1, substrate is prepared, and may further comprise the steps:
(1) pyrolytic graphite chip is carried out planarizing process, employing be on the abrasive disk of 15 type grinders of LAPMASTER company, to grind its surface, and adopt pitch stencil plate and ruby micro mist (0.2 μ m) polishing material that it is carried out polishing.
(2) because pyrolytic graphite has electric conductivity, for preventing that the micro-structural that needs on-load voltage or electric current to be processed on its substrate surface and some lead-in wires and the electrode that goes between are exerted an influence, cause the unnecessary conducting of these structures and lead-in wire, need do insulation at the substrate surface of polishing handles, common adoptable insulating materials has silica and silicon nitride, and silica/insulating silicon nitride film can place plasma to strengthen the method preparation that deposition system adopts PECVD (plasma-reinforced chemical vapor deposition).Before doing insulating barrier, with acetone, alcohol, deionized water substrate is carried out ultrasonic cleaning, flushing and oven dry earlier.
(3) substrate of carrying out insulating barrier carries out ultrasonic cleaning, flushing and oven dry with acetone, alcohol, deionized water to substrate once more.So far finish the preparation of pyrolytic graphite chip.
Shown in B among Fig. 1, at substrate back sputtering seed layer Cr/Cu metal composite thin film, sputter thickness 200 /800 .Positive-glue removing and photoetching back side alignment key pattern, the exposed portion photoresist removes after developing, and without the mask layer of exposed portion as back side alignment mark, and then removes unnecessary Seed Layer by spattering carving technology, spatters and carves thickness 1000 .The photoresist that covers on the alignment mark of the back side is removed in final acetone ultrasonic cleaning; obtain back side alignment mark; in order to prevent the damage of back side alignment mark in subsequent technique, make protective layer on the alignment mark overleaf simultaneously, the material that protective layer can adopt has aluminium oxide or polyimides; usually aluminium oxide can adopt sputtering technology; polyimides then passes through whirl coating, and is heating and curing, and the present invention adopts alumina material; sputter thickness is 2 μ m, the about 1h of sputtering time.
Shown in C among Fig. 1, sputtering seed layer, Cr/Cu metal composite thin film, sputter thickness 200 /800 .On Seed Layer, adopt the RC8 type photoresist spinner positive-glue removing first time of Karsuss company then, the about 6 μ m of whirl coating thickness, rotating speed 3000r/s, time 30s, 95 ° of preceding down bakings 30 minutes, during photoetching, the mask of structure sheaf pattern is aimed at according to back side alignment mark, and photoetching is placed on thick apparent, the thin about 50s of showing of warp in the special-purpose developer solution, obtains the electroplating mold of desired structure layer pattern.
Shown in D among Fig. 1, in the electroplating mold of the structure sheaf pattern that obtains after developing for the first time among the C, grow the Cu structure of certain depth-to-width ratio by plating, the electroplate liquid type is the sulfuric acid type copper plating bath, in room temperature, strong acid and current strength is under the environment of 700mA, electroplates Cu thickness 5 μ m, and growth rate is about 0.2-0.5 μ m/min, electroplating time is about 20min, electroplates the back that finishes planarizing process is carried out on the electrodeposited coating surface.
Shown in E among Fig. 1, positive-glue removing for the second time, the about 8 μ m of whirl coating thickness, rotating speed 3000r/s, time 30s, 95 ° of preceding down bakings 30 minutes, the mask of structure sheaf pattern are equally according to the electroplating mold that obtains the desired structure layer pattern behind back side alignment mark photoetching, the about 60s that develops.
Shown in F among Fig. 1, in the electroplating mold of the structure sheaf pattern that obtains behind the second development among the E, grow the Cu structure of certain depth-to-width ratio by plating, electroplate Cu thickness 6 μ m, electroplate the back that finishes planarizing process is carried out on the electrodeposited coating surface.Owing to be to continue to electroplate on ground floor Cu structure, for guaranteeing the electrodeposited coating bond quality twice, the Cu structure after should as far as possible avoiding electroplating for the first time is exposed to for a long time and causes oxidation in the air, as producing the passivation layer of oxidation, can consider to adopt HCl to soak.In addition, substrate after photoetching, the development should be put into electroplate liquid as early as possible and electroplate, reduce the time that contacts with air, to prevent that oxidative phenomena from appearring in Seed Layer, in the electroplating process, also reduce as far as possible and take out the number of times that substrate is observed and measured, the probability of passivation may occur with reduction electrodeposited coating (Cu), thereby guarantee and the adhesion of substrate and the adhesion between electrodeposited coating.
Shown in G among Fig. 1, the acetone ultrasonic cleaning is removed photoresist, and alcohol, washed with de-ionized water then, and oven dry by spattering carving technology, are removed Seed Layer at last.
Shown in H among Fig. 1, sputter aluminium oxide, sputter thickness are 13 μ m, the about 6h of sputtering time, and carry out planarizing process, guarantee to expose the Cu structure.
Shown in I among Fig. 1, sputtering seed layer Cr/Cu metal composite thin film on aluminium oxide, about 3000 of sputter thickness get rid of the negative glue of SU8-100, the whirl coating thickness 230 μ m of present embodiment then, be placed on before the photoetching on the hot plate of the program control baking oven of convection current and carry out preceding baking, temperature is warming up to 65 ℃ from room temperature in 30min, keep 30min, is warming up to 95 ℃ through 15min again, keep 1.5h, cool off with stove then.According to back side alignment mark photolithographic structures layer pattern, the photolithographic exposure power density is 2.6mw/cm again
2, the time for exposure is 180s, the exposure meron places the special-purpose developer solution of SU8 to develop under million acoustic environments, obtains the electroplating mold of desired structure layer pattern.
Shown in J among Fig. 1, obtain in the electroplating mold of desired structure layer pattern after SU8 develops in I, grow Cu structure by plating than high-aspect-ratio, electroplate the about 230 μ m of Cu thickness, electroplate the back that finishes planarizing process is carried out on the electrodeposited coating surface.
Shown in K among Fig. 1, SU8 removes photoresist, and available oleum makes SU8 glue be subjected to the strong acid oxidation under ultrasound environments, uses washed with de-ionized water again.
Shown in L among Fig. 1, to use phosphoric acid solution (85%) constant temperature (65 ℃) water-bath heating aluminium oxide is corroded, corrosion rate is about 0.1 μ m/min, and acetone, alcohol, washed with de-ionized water then, and oven dry obtain final structure sheaf.
The present invention is given in the processing method that realizes micro-structural on the pyrolytic graphite chip, no matter adopt positive adhesive process, the negative adhesive process of SU8, perhaps both combinations can realize making differing heights, width on substrate, and relative positional accuracy height between structure sheaf, micro-structural that adhesion is strong.The positive general whirl coating thickness of glue AZ4620 5-10 μ m among the present invention and the general whirl coating thickness of another kind of AZ4903 10-30 μ m; The negative glue SU8-50 whirl coating thickness of the SU8 of MicroChem company is mainly below 200 μ m, the SU8-100 single whirl coating thickness that adopts among the present invention then can reach more than the 400 μ m, thereby utilize this method can realize more than three layers that micro-structural and interlayer adhesion are good, utilize the positive photoresist of different model can realize several microns height of single layer structure simultaneously to the twenty or thirty micron, if utilize negative photoresist, then can realize the structure of hundreds of microns of individual layer height.
Claims (5)
1. the implementation method of a microstructure on pyrolytic graphite chip is characterized in that: may further comprise the steps:
The first step adopts negative glue of positive adhesive process and SU8 and accurate LIGA technology, adopts pyrolytic graphite as substrate, before processing substrate is cooked leveling, cleaning, insulating and is cleaned preparation again;
Second step, simultaneously do photoetching back side alignment mark at pyrolytic graphite chip, this face is the back side, the litho machine of double-sided exposure is all used in the photoetching of every layer of structure later on, back side alignment mark is focused simultaneously, by the multilayer alignment, realizes sandwich construction or high aspect ratio structure;
In the 3rd step, pyrolytic graphite be positive at the substrate another side after substrate is carried out back side alignment mark through preparation and the back side, and sputtered metal film is as Seed Layer, positive-glue removing on Seed Layer, photoetching, develop after, the mould of making electroplated structural layer;
The 4th step, electroplate structure sheaf on the Seed Layer in the mould of electroplated structural layer, after twice positive-glue removing, photoetching, development and plating, remove positive glue, ultrasonic cleaning, sputter aluminium oxide, then grind substrate and do cleaning;
In the 5th step, sputtered metal film is made Seed Layer on aluminium oxide, gets rid of the negative glue of SU8 again on Seed Layer, by photoetching, development and plating, goes SU8 to bear glue, and deoxidation aluminium is realized making high aspect ratio microstructures on the pyrolytic graphite.
2. the implementation method of microstructure on pyrolytic graphite chip according to claim 1 is characterized in that, described substrate is cooked leveling, is meant: adopt Ginding process to handle its surface and polishing.
3. the implementation method of microstructure on pyrolytic graphite chip according to claim 1 is characterized in that, described substrate is cooked cleaning, is meant: before doing insulating barrier, with acetone, alcohol, deionized water substrate is carried out ultrasonic cleaning, flushing and oven dry earlier.
4. the implementation method of microstructure on pyrolytic graphite chip according to claim 1, it is characterized in that, described substrate is cooked insulating, be meant: the substrate surface in polishing carries out insulation processing, the insulating materials that adopts has silica and silicon nitride, and silica/insulating silicon nitride film places plasma to strengthen the method preparation that deposition system adopts plasma-reinforced chemical vapor deposition.
5. the implementation method of microstructure on pyrolytic graphite chip according to claim 1, it is characterized in that, described substrate is cleaned again, be meant: the substrate of carrying out insulating barrier carries out ultrasonic cleaning, flushing and oven dry with acetone, alcohol, deionized water to substrate once more, so far finishes the preparation of pyrolytic graphite chip.
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Cited By (9)
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| CN101794072B (en) * | 2010-01-15 | 2012-02-15 | 中国科学技术大学 | Method for preparing substrate with nano structure with line width below 20 nanometers |
| CN103103583A (en) * | 2013-01-14 | 2013-05-15 | 大连理工大学 | Method for manufacturing multi-layer metal mobile microstructure on metal base |
| CN103121659A (en) * | 2013-01-15 | 2013-05-29 | 西北工业大学 | Method for processing microstructure on highly oriented pyrolytic graphite by using photolithography technique |
| CN103531510A (en) * | 2013-10-24 | 2014-01-22 | 华东光电集成器件研究所 | Transfer and alignment photoetching method of P+ epitaxy pattern of semiconductor circuit |
| CN103928439A (en) * | 2014-04-11 | 2014-07-16 | 北京理工大学 | Anti-overload non-silicon MEMS thick metal suspended micro inductor |
| CN105329849A (en) * | 2015-10-16 | 2016-02-17 | 上海师范大学 | MEMS micro array structure processing method based on micro-electroplating |
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| CN101794072B (en) * | 2010-01-15 | 2012-02-15 | 中国科学技术大学 | Method for preparing substrate with nano structure with line width below 20 nanometers |
| CN103103583A (en) * | 2013-01-14 | 2013-05-15 | 大连理工大学 | Method for manufacturing multi-layer metal mobile microstructure on metal base |
| 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 |
| CN103121659A (en) * | 2013-01-15 | 2013-05-29 | 西北工业大学 | Method for processing microstructure on highly oriented pyrolytic graphite by using photolithography technique |
| CN103531510A (en) * | 2013-10-24 | 2014-01-22 | 华东光电集成器件研究所 | Transfer and alignment photoetching method of P+ epitaxy pattern of semiconductor circuit |
| CN103928439A (en) * | 2014-04-11 | 2014-07-16 | 北京理工大学 | Anti-overload non-silicon MEMS thick metal suspended micro inductor |
| CN105329849A (en) * | 2015-10-16 | 2016-02-17 | 上海师范大学 | MEMS micro array structure processing method based on micro-electroplating |
| CN106145029A (en) * | 2016-06-15 | 2016-11-23 | 合肥工业大学 | A kind of method preparing micro coaxle metal structure on the metallic substrate |
| CN106145029B (en) * | 2016-06-15 | 2017-08-25 | 合肥工业大学 | A kind of method for preparing micro coaxle metal structure on the metallic substrate |
| WO2018076432A1 (en) * | 2016-10-28 | 2018-05-03 | 中国科学院深圳先进技术研究院 | Biocompatible encapsulated magnetic robot and preparation method therefor |
| CN107452600A (en) * | 2017-08-21 | 2017-12-08 | 中国电子科技集团公司第二十研究所 | A kind of preparation method of compound anti-plate mask |
| CN107452600B (en) * | 2017-08-21 | 2020-01-14 | 中国电子科技集团公司第二十研究所 | Preparation method of composite electroplating-resistant mask |
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