CN104162677A - Preparing method of flat and columnar metal microparticles - Google Patents
Preparing method of flat and columnar metal microparticles Download PDFInfo
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- CN104162677A CN104162677A CN201410149411.7A CN201410149411A CN104162677A CN 104162677 A CN104162677 A CN 104162677A CN 201410149411 A CN201410149411 A CN 201410149411A CN 104162677 A CN104162677 A CN 104162677A
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Abstract
The invention discloses a preparing method of flat and columnar metal microparticles and belongs to the field of preparation of metal particles. The preparing method of the metal particles can overcome the defects that in an existing metal particle preparing method, particles are not uniform in size, irregular in shape and the like. The method is mainly characterized in that the metal particles are prepared through photoetching and electroplating technologies, firstly, particle grooves are formed in a substrate through photoetching, then, the metal particles are made to grow in the grooves through the electroplating technology, finally, the metal particles can break away from the substrate through ultrasonic vibration impact, and therefore the metal particles can be prepared. The metal particles prepared with the method are regular and uniform in shape and equal in size and can be applied to industrial product development, scientific experiment research and the like.
Description
Technical field
The present invention is a kind of preparation method of metal micro particles, is specially the preparation method of consistent, the of uniform size flat of a kind of shape or cylindrical metal microparticle, the invention belongs to metallic particles preparation field.
Background technology
The metallic particles out-of-shape that existing metallic particles preparation method makes, size disunity, is difficult to meet the demands such as industrial products exploitation, scientific research experiment.
City comes great one in the disclosed method of preparing metallic particles by electrolysis of patent publication No. CN1727098A, the method is by vibration, fine carbon to be scattered in electrolytic solution, then by electrolytic method, the metallic particles that contains fine carbon is deposited on negative electrode, finally impacts metallic particles is separated with negative electrode by excusing from death.Although the method can be prepared metallic particles in batches, it cannot accurately control the size and shape of metallic particles.
The preparation method of the disclosed zinc granule of Chinese invention patent publication number CN1255415.The method is that the zinc liquid of molten condition is directly splashed in condensation bath, and the direct cooling molten condition zinc liquid of water is housed in condensation bath, finally obtains zinc granule.The method still can not effectively be controlled the size and dimension of particle.
United States Patent (USP) 388956 has been announced a kind of method that adopts molten method processing metal grains.In the method, the liquation of molten iron is fallen towards the fixed part of a level, when solution clashes into these parts, broken due to the kinetic energy of itself, form irregular molten, these the molten top toward above-mentioned parts and outside motion, then fall into the cooling medium solution being arranged in below company headquarters of institute part, adopt and can make in this way metallic particles, but the granular size that the method is made differs, different.
Under this background, the present invention proposes a kind of metallic particles preparation method based on photoetching, electroplating technology, the method can produce there is regular shape, size evenly, can batch making, the metallic particles densification of preparation, any surface finish, flawless, etc. the metallic particles of advantage.
Summary of the invention
The object of the invention is to overcome in existing preparation method of granules, and the shortcomings such as granular size disunity, out-of-shape, realize the accurate preparation of cylindrical metal particulate.The preparation of the metal particles such as that the present invention is applicable to is cylindric, prism-shaped, the cross sectional dimensions of cylindrical metal particulate from 1 micron to 1 millimeter all can, the 0.01-3 that height can reach cross sectional dimensions is doubly.When the relative lateral dimension of height of cylindrical particle hour, metallic particles is flat.
The present invention is characterized in that adopting photoetching, electroplates and prepare metallic particles, and concrete steps are as follows:
S1, first prepare mask plate, go out the metallic particles shape of cross section that will make with computer Software on Drawing, be then transferred on quartz glass or film, in the time of exposure, use.
S2, select glass, epoxy resin board or glass mat to do substrate, adopt washed with de-ionized water clean, and dry.
S3, employing sputtering technology or evaporation process, sputter one deck plating seed layer in substrate front surface; Described plating seed layer is necessary for conductor.
S4, on the plating seed layer of substrate front surface, be coated with one deck positive photoresist, then even glue on glue evenning table, is evenly distributed on plating seed layer photoresist, and drying glue; Photoresist has dividing of positive photoresist and negative photoresist, and positive photoresist is will be exposed part photoresist to remove, and will not be exposed part photoresist and retains, and negative photoresist is contrary; Select positive photoresist or negative photoresist according to the figure of mask plate.
S5, by correct the substrate that coats photoresist being arranged on exposure machine, and align with the mask plate of making in advance, make the graphics field of mask plate just drop on the center of substrate, then expose.
S6, metallic particles figure is transferred on photoresist, then substrate is toasted, remove the developer solution and the residual moisture that while development, absorb.
S7, Pre-treatment before plating first, be placed into substrate in dilute sulfuric acid and clean, and then starts to electroplate, and using substrate as negative electrode, metal derby is made anode, is placed in plating bath respectively, and passes into DC current or pulse direct current, electroplates; There is the position of photoresist unchanged, can grow metallic particles without the position of photoresist;
S8, adopt the liquid that removes photoresist to remove on-chip photoresist, be then placed in the container that pure water is housed, adopt supersonic cleaning machine to carry out ultrasonic vibration impact to it, make metallic particles depart from plating seed layer, thereby obtain required metallic particles.
S9, substrate take out, and then liquid in containers are filtered and are obtained metallic particles, then metallic particles is dried.
In described step S4, if make the particle of flat, can adopt BP212 type photoresist, make the particle of larger depth-to-width ratio as need, can select SU8 or AZ460 series photoresist.Described larger depth-to-width ratio scope is generally 2-3.
The available chemical plating of plating adopting in described step S7 replaces.
The present invention includes following advantage:
1., shape, the size of cylindrical metal particle that can be as required, adopt in advance computer software graphing, be made into mask plate, thereby realize more accurately the controlling of metal particle size, the metallic particles shape of made is consistent, size evenly.
2., can as required, select the plating bath of heterogeneity, thereby obtain different types of metallic particles.
3., can batch making, mask plate can be arranged on exposure machine and reuse, therefore can be by the larger substrate of manufactured size, then to the exposure of substrate zones of different, to realize batch making.
Brief description of the drawings
Fig. 1: the reticle pattern that implementing process of the present invention is used
Fig. 2: the process schematic diagram one of implementing process of the present invention
Fig. 3: the process schematic diagram two of implementing process of the present invention
Fig. 4: the process schematic diagram three of implementing process of the present invention
Fig. 5: the process schematic diagram four of implementing process of the present invention
Fig. 6: the process schematic diagram five of implementing process of the present invention
Fig. 7: the process schematic diagram six of implementing process of the present invention
Fig. 8: the process schematic diagram seven of implementing process of the present invention
Fig. 9 is circular flat metallic particles schematic diagram and rectangle flat metallic particles schematic diagram
Figure 10 is in circular flat metallic particles schematic diagram and rectangle flat metallic particles schematic diagram figure: 1. substrate, 2. plating seed layer (copper), 3. positive photoresist, 4. metallic particles figure hole, 5. metallic particles, 6. container, 7. pure water, 8. supersonic cleaning machine, 9. screen pack, 10. mask plate transmission region, the 11. light tight regions of mask plate, 12. circular flat metallic particles schematic diagrames, 13. rectangle flat metallic particles schematic diagrames, 14. circular cylindrical shape metallic particles schematic diagrames, 15. rectangle cylindrical metal particle schematic diagrames
Detailed description of the invention
To make copper particle as example, but be not limited to copper particle, also can make the metallic particles of other kinds such as iron, magnesium, nickel, chromium.Below in conjunction with diagram, the specific embodiment of the present invention is described further:
(1) as shown in Figure 1, the metallic particles figure cross sectional shape of first using computer drawing software (L-EDIT) to draw out will to make, is then transferred on quartz glass by quartz plate-making company.
(2) as shown in Figure 2, select glass as substrate (1), by deionized water, glass cleaning is clean, and dry.The size and number of the metallic particles that the size of the substrate of glass of selecting here can be made is as required selected suitable size.
(3) as shown in Figure 3, adopt sputtering technology, it is 300W at power that sputtering unit is set, normal temperature, gas flow is 65ml/min, sputter 8min, at glass front sputter one deck plating seed layer copper (2), the plating seed layer of selecting is here generally copper, because copper is little at adhesive force on glass, when excusing from death wave impact, easily come off from substrate, be convenient to take out particle, but be not limited to copper.Power, gas flow and the sputtering time of sputtering unit can difference as required be adjusted.
(4) as shown in Figure 4, at the upper one deck SU8 positive photoresist that is coated with of plating seed layer copper (2) of preparation, then first low speed (40r/min) rotation 9s on glue evenning table, then (800r/min) rotates 60s at a high speed, positive photoresist (3) is evenly distributed on plating seed layer (2), it is 65 DEG C that drying glue platform temperature is set, and dries 35min.Glue evenning table rotating speed, time and bake out temperature, the time of selecting are here adjusted according to the difference of the thickness of the difference of substrate sizes and photoresist.The different spin coating multilevel resists of metallic particles thickness that can be as required.
(5) as shown in Figure 5, adopt mask plate shown in Fig. 1 to be arranged on exposure machine, align and expose with substrate, the time for exposure is 400s, then in NaOH developer solution (NaOH: water=6g:1L), first static 30min, after rock 1min, then in deionized water fixing solution, rock 2min, expose the Seed Layer that is exposed position, form metallic particles figure hole (4), and solidify.The time for exposure of selecting is here carried out suitable prolongation and shortening according to the thickness difference of photoresist, generally taking SU8 photoresist as example, and the photoresist exposure 300-400s of 300um thickness, development 30min.The photoresist exposure 580-620s of 500um thickness, development 50min.According to the difference of the kind of photoresist and thickness, can select exposure and the developing time parameter of being correlated with.
(6) as shown in Figure 6, adopt electroplating technology, first Pre-treatment before plating, is placed into substrate in dilute sulfuric acid, rock 20s, then start to electroplate, using substrate as the negative electrode of electroplating, copper billet is made anode, be placed in plating bath respectively, and pass into DC current, electroplate.Generate metallic particles (5), the plating bath composition of selecting is here copper sulphate 180g/L, H
2sO
450g/L and glucose 30g/L.Illustrated metallic particles is cuboid, but is not limited to cuboid, also can be the regular shapes such as triangular prism, pentagon post, octagonal post, rhombus column, cylinder, also can make the particle of the flat in various cross sections.
(7) as shown in Figure 7, substrate is placed on to the beaker that acetone soln is housed, rocks to remove remaining photoresist.And then put into the container that pure water is housed, and adopt supersonic cleaning machine to carry out ultrasonic vibration impact to it, make metallic particles depart from plating seed layer copper (2).Here ultrasonic wave adopts medium (20kHZ, 4kW/L) intensity.Also can be in step (three) before spin coating one deck BP212 photoresist in glass front, in the time of ultrasonic impact, more easily make like this metallic particles depart from plating seed layer copper (2).
(8) as shown in Figure 8, substrate is taken out, then liquid in containers is filtered and obtained metallic particles, then metallic particles is dried, can obtain required metallic particles.Fig. 9 is circular flat metallic particles schematic diagram (12) and rectangle flat metallic particles schematic diagram (13), Figure 10 is circular flat metallic particles schematic diagram (14) and rectangle flat metallic particles schematic diagram (15), and described Fig. 9 and Figure 10 are metallic particles enlarged diagram.
Attached: as need electronickelling can adopt electroplating bath components as follows:
| Composition | Content |
| Sodium chloride | 6-10g/L |
| Boric acid | 30-35g/L |
| Sodium sulphate | 50-70g/L |
| Nickelous sulfate | 120-140g/L |
| Current density | 30-40A/dm 2 |
| Temperature | 30-35℃ |
As need electrodeposited chromium can adopt electroplating bath components as follows:
| Composition | Content |
| Chromic anhybride | 80-120g/L |
| Sulfuric acid (pure) | 0.8-1.2g/L |
| Boric acid | 8-12g/L |
| Current density | 0.8-1.5A/dm 2 |
| Temperature | 58-62℃ |
Claims (3)
1. the preparation method of flat and cylindrical metal microparticle, is characterized in that: adopt photoetching, electroplate and prepare metallic particles, concrete steps are as follows:
S1, first prepare mask plate, go out the metallic particles shape of cross section that will make with computer Software on Drawing, be then transferred on quartz glass or film, in the time of exposure, use;
S2, select glass, epoxy resin board or glass mat to do substrate, adopt washed with de-ionized water clean, and dry;
S3, employing sputtering technology or evaporation process, sputter one deck plating seed layer in substrate front surface; Described plating seed layer is necessary for conductor;
S4, on the plating seed layer of substrate front surface, be coated with one deck positive photoresist, then even glue on glue evenning table, is evenly distributed on plating seed layer photoresist, and drying glue; Photoresist has dividing of positive photoresist and negative photoresist, and positive photoresist is will be exposed part photoresist to remove, and will not be exposed part photoresist and retains, and negative photoresist is contrary; Select positive photoresist or negative photoresist according to the figure of mask plate;
S5, by correct the substrate that coats photoresist being arranged on exposure machine, and align with the mask plate of making in advance, make the graphics field of mask plate just drop on the center of substrate, then expose;
S6, metallic particles figure is transferred on photoresist, then substrate is toasted, remove the developer solution and the residual moisture that while development, absorb;
S7, Pre-treatment before plating first, be placed into substrate in dilute sulfuric acid and clean, and then starts to electroplate, and using substrate as negative electrode, metal derby is made anode, is placed in plating bath respectively, and passes into DC current or pulse direct current, electroplates; There is the position of photoresist unchanged, can grow metallic particles without the position of photoresist;
S8, adopt the liquid that removes photoresist to remove on-chip photoresist, be then placed in the container that pure water is housed, adopt supersonic cleaning machine to carry out ultrasonic vibration impact to it, make metallic particles depart from plating seed layer, thereby obtain required metallic particles;
S9, substrate take out, and then liquid in containers are filtered and are obtained metallic particles, then metallic particles is dried.
2. the preparation method of flat according to claim 1 and cylindrical metal microparticle, is characterized in that: in described step S4, when making the particle of flat, adopt BP212 type photoresist; Need to make the particle of larger depth-to-width ratio, select SU8 or AZ460 series photoresist; Described larger depth-to-width ratio scope is 2-3.
3. the preparation method of flat according to claim 1 and cylindrical metal microparticle, is characterized in that: the plating adopting in described step S7 chemical plating replaces.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6312351A (en) * | 1986-04-08 | 1988-01-19 | ケルンフオルシユングスツエントルム・カ−ルスル−エ・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング | Catalyst supporter and manufacture thereof |
| US20070111366A1 (en) * | 2005-04-26 | 2007-05-17 | Odom Teri W | Mesoscale pyramids, arrays and methods of preparation |
| CN1986011A (en) * | 2006-12-08 | 2007-06-27 | 中国科学院上海微系统与信息技术研究所 | Miniature needle array for medicine transmission and its making process |
| CN103018800A (en) * | 2011-09-23 | 2013-04-03 | 中国科学院微电子研究所 | Surface-plasma-enhanced symmetric structure and preparation method thereof |
| CN103197793A (en) * | 2013-02-06 | 2013-07-10 | 南昌欧菲光科技有限公司 | Micro-structural conductive pattern forming method and system |
| CN103257178A (en) * | 2013-04-25 | 2013-08-21 | 南通大学 | One-dimensional nanometer electrode material, and preparation method and application thereof |
-
2014
- 2014-04-12 CN CN201410149411.7A patent/CN104162677B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6312351A (en) * | 1986-04-08 | 1988-01-19 | ケルンフオルシユングスツエントルム・カ−ルスル−エ・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング | Catalyst supporter and manufacture thereof |
| US20070111366A1 (en) * | 2005-04-26 | 2007-05-17 | Odom Teri W | Mesoscale pyramids, arrays and methods of preparation |
| CN1986011A (en) * | 2006-12-08 | 2007-06-27 | 中国科学院上海微系统与信息技术研究所 | Miniature needle array for medicine transmission and its making process |
| CN103018800A (en) * | 2011-09-23 | 2013-04-03 | 中国科学院微电子研究所 | Surface-plasma-enhanced symmetric structure and preparation method thereof |
| CN103197793A (en) * | 2013-02-06 | 2013-07-10 | 南昌欧菲光科技有限公司 | Micro-structural conductive pattern forming method and system |
| CN103257178A (en) * | 2013-04-25 | 2013-08-21 | 南通大学 | One-dimensional nanometer electrode material, and preparation method and application thereof |
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Effective date of registration: 20210401 Address after: 313000 No.1-2 Quanxing Road, Shuanglin Town, Nanxun District, Huzhou City, Zhejiang Province Patentee after: Huzhou Nanxun Shuangxin Construction Development Co.,Ltd. Address before: 100124 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee before: Beijing University of Technology |
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Denomination of invention: Preparation methods of flat and columnar metal microparticles Effective date of registration: 20230322 Granted publication date: 20160817 Pledgee: Zhejiang Nanxun Rural Commercial Bank branch Shuanglin Limited by Share Ltd. Pledgor: Huzhou Nanxun Shuangxin Construction Development Co.,Ltd. Registration number: Y2023330000579 |
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