CN103077870B - Processing method of silicon micro-channel plate substrate provided with reinforcing ring - Google Patents
Processing method of silicon micro-channel plate substrate provided with reinforcing ring Download PDFInfo
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- CN103077870B CN103077870B CN201210590676.1A CN201210590676A CN103077870B CN 103077870 B CN103077870 B CN 103077870B CN 201210590676 A CN201210590676 A CN 201210590676A CN 103077870 B CN103077870 B CN 103077870B
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Abstract
The invention discloses a processing method of a silicon micro-channel plate substrate provided with a reinforcing ring, which belongs to the technical field of manufacturing of photoelectric imaging devices. In the prior art, a back face thinning procedure has the defects of low efficiency and damage to a micro-channel while a polishing procedure has the defects that a micro-channel blockage phenomenon exists and a manufactured silicon micro-channel plate substrate is not provided with any reinforcing ring. The method consists of the following procedures of: performing electrochemical corrosion to manufacture a micro-channel array; thinning the back face of a silicon chip to penetrate the micro-channel; performing circle cutting to form a silicon micro-channel plate substrate reinforcing ring; and polishing on a front face and a back face of the silicon micro-channel plate substrate. A silicon micro-channel plate made of the silicon micro-channel plate substrate provided with the reinforcing ring processed with the method has the advantages that: the micro-channel is through, the inside of the channel is clean and free from pollution, a surface is flat and smooth, the channel is 320 Mu m in length, the section shape of the channel is approximately square, side lengths are only 8 Mu m, the slenderness ratio is up to 40, and the mechanical strength of the silicon micro-channel plate is enhanced effectively through the edge solid reinforcing ring.
Description
Technical field
The present invention relates to a kind of silicon micro-channel board substrate processing method with reinforcing ring, belong to photoelectronic imaging device fabrication techniques field.
Background technology
MCP(microchannel plate, Microchannel Plates) there is the advantages such as high-gain, low noise, high-resolution, low-power consumption, long-life and self-saturation effect, be widely used in the fields such as low-light image tube, fast phtotmultiplier tube, cathode ray tube, camera tube, storage tube and electronics, ion, ultra-violet radiation and X-ray detector.Compared with common MCP, Si-MCP has lot of advantages, comprise that material purity is high, substrate and dynode material can be selected arbitrarily, be easy to make small-bore micro channel array, MCP resolution are high, MCP overall performance improves and and integrated circuit technology between have better compatible etc.Adopt silicon materials to make MCP, need to produce surfacing, smooth circular distribution silicon microchannel array, require that microchannel is penetrating, cleanliness without any pollution in structural integrity, passage, there is big L/D ratio.
The C. P. Beetz of nano science company of the U.S. in 1999 proposes a kind of new Si base MCP preparation technology, see Silicon Etching Process For Making MicrochannelPlates. US Patent, 5997713 [P], 1999-12-07, this technique adopts electrochemistry and photoelectrochemical etching method to prepare big L/D ratio micro channel array, adopt low-pressure chemical vapor deposition (LPCVD) technology to prepare dynode film, manufactured MCP is Si-MCP.But the method, after electrochemical corrosion forms passage, completes the thinning formation first through passage in back by grinding and polishing, plasma etching or chemical corrosion.Not only speed is too low for direct grinding and polishing wherein, consuming time oversize, in grinding and polishing process, understands blocking channel and is difficult to cleaning; And plasma etch apparatus is expensive, cost is high, process length consuming time, etching rear surface out-of-flatness, also needing polishing, understands blocking channel equally, though through repeatedly cleaning, still there is a large amount of polishing dirt, as shown in Figure 1 in microchannel; Its etching-stop time of chemical corrosion is wayward, and when passage is penetrating, meeting etching channels inwall, destroys structure.Si-MCP periphery made by the method is without reinforcing ring, and the micro channel array periphery namely formed does not have solid edge, bad mechanical strength, very easily broken, is unfavorable for following process process, particularly follow-up tubulature.
Summary of the invention
In order to improve the thinning efficiency of silicon micro-channel board substrate silicon chip back side, guarantee that microchannel is not destroyed in thinning process, the blocking of microchannel is avoided in the glossing at front side of silicon wafer, the back side, made silicon micro-channel board substrate has reinforcing ring, and we propose a kind of silicon micro-channel board substrate processing method with reinforcing ring.
The method of the present invention adopts electrochemical etching method to make micro channel array, it is characterized in that:
Make in micro channel array operation in electrochemical corrosion, adhere to shading endless belt 2 at silicon chip 1 back side simultaneously, shading endless belt 2 is concentric with microchannel corrosion starting point array border circular areas 3, as shown in Figure 2, the ring inner region of shading endless belt 2 is exactly microchannel corrosion starting point array border circular areas 3, ring strip region between shading endless belt 2 and contact-making surface electrode 4 is circle of contact corrosion area 5, corrodes irregular distribution microchannel 7, as shown in Figure 3 while corrosion array microchannel 6 at circle of contact corrosion area 5;
In the operation that make microchannel penetrating thinning by silicon chip back side, first adopt the SiO that dry-oxygen oxidation technique is formed on microchannel smooth internal walls surface
2layer, as the protective layer of microchannel interior walls, then carries out silicon chip 1 backside chemical corrosion thinning, until whole microchannels is penetrating, as shown in Figure 3;
Formed in silicon micro-channel board substrate reinforcing ring operation at the circle of contact, first remove the irregular distribution microchannel 7 inwall SiO in circle of contact corrosion area 5
2layer, then corrode this microchannel, make it to communicate with each other, finally make silicon chip distribution micro channel array part be separated with silicon chips periphery part, complete circle of contact operation, around the disc-shaped silicon micro-channel board substrate 8 obtained, have a circle reinforcing ring 9, as shown in Figure 4;
In silicon microchannel plate front side of matrix, polished backside operation, first disc-shaped silicon micro-channel board substrate 8 is oxidized, forms SiO in array microchannel 6 inner wall surface
2layer, under vacuum paraffin is filled in the front side of silicon wafer of array microchannel 6, back side port 10 again, then polished silicon slice front, the back side, finally removes the polishing dirt in array microchannel 6 and paraffin, completes silicon micro-channel board substrate 8 front, polished backside.
Its technique effect of the present invention is, owing to adopting the thinning silicon chip back side of chemical corrosion, improve compared to direct grinding and polishing efficiency, and chemical corrosion is very low relative to plasma etching cost, meanwhile, owing to adopting oxidation technology to form SiO in microchannel smooth internal walls in advance
2layer, so, can not because of chemical corrosion until penetrating rear destruction microchannel, microchannel.There is a circle reinforcing ring around the disc-shaped silicon micro-channel board substrate obtained, the Si-MCP mechanical strength completed through subsequent technique is improved, not easily broken, be beneficial to following process process, particularly follow-up tubulature.Owing to taking the measure of filling paraffin in front side of silicon wafer, polished backside operation, and be easy to remove, therefore, eliminate microchannel clogging, as shown in Figure 5.
Accompanying drawing explanation
Fig. 1 is that prior art polishing process does not take preventive measures the local displaing micro picture of the polished dirt clogging in the part microchannel occurred in silicon micro-channel board substrate.Fig. 2 is that the present invention makes silicon chip back side schematic layout pattern in micro channel array operation in electrochemical corrosion.Fig. 3 is that the present invention makes the penetrating situation schematic diagram in microchannel by silicon chip back side is thinning.Fig. 4 is the silicon micro-channel board substrate form schematic diagram formed after the circle of contact of the present invention, and this figure is simultaneously as Figure of abstract.Fig. 5 is that the microchannel after polishing process of the present invention takes preventive measures in silicon micro-channel board substrate does not have polished dirt stopping state local displaing micro picture.
Embodiment
The specific embodiment of the present invention is as follows:
1, micro channel array is made by electrochemical corrosion
(1) on silicon chip 1, SiO is formed by oxidation
2mask, adopts RIE(reactive ion etching) technique etching removes the SiO at silicon chip 1 back side
2layer;
(2) adopt phosphorus to be diffused in silicon chip 1 and form ohmic contact layer;
(3) adopt photoetching process, RIE technique at definition photochemical corrosion region, silicon chip 1 front, figure, namely at the microchannel corrosion starting point array of silicon chip central area setting circular distribution;
(4) form induction hole array with 30 wt% KOH solution corrosion of silicon 1 under 80 DEG C of conditions, described induction hole is microchannel corrosion starting point;
(5) the region attachment contact-making surface electrode 4 beyond the corrosion starting point array of microchannel, silicon chip 1 back side, contact-making surface electrode 4 adopts aluminium foil or Copper Foil to make, as shown in Figure 2, adhere to shading endless belt 2 at silicon chip 1 back side simultaneously, shading endless belt 2 is concentric with microchannel corrosion starting point array border circular areas 3, the ring inner region of shading endless belt 2 is exactly microchannel corrosion starting point array border circular areas 3, ring strip region between shading endless belt 2 and contact-making surface electrode 4 is circle of contact corrosion area 5, and the width of shading endless belt 2 is more than or equal to the width of the silicon micro-channel board substrate reinforcing ring 9 that needs make; Adopt three-electrode cell to carry out electrochemical corrosion, described three electrodes comprise work electrode, auxiliary electrode, reference electrode, with wavelength be the LED array of 850 nm as light source, irradiate silicon chip 1 back side and excite and produce hole needed for corrosion reaction, with H
2o, C
2h
5the mixed liquor of OH, HF, anion surfactant is as corrosive liquid, corrosion is started from silicon chip 1 front, along the axial array microchannel 6 forming draw ratio and be greater than 40 of silicon chip 1 in microchannel corrosion starting point array border circular areas 3, erode away irregular distribution microchannel 7 at circle of contact corrosion area 5, as shown in Figure 3 simultaneously.
2, penetrating by the thinning microchannel that makes of silicon chip back side
(1) RCA method cleaning silicon chip 1 in mega sonic wave cleaning machine is adopted;
(2) microchannel interior walls owing to obtaining through photochemical corrosion is porous silicon form, inner wall surface is coarse, need to do smoothing processing, its technique is: be oxidized silicon chip 1 at 900 ~ 1100 DEG C of temperature, oxidation technology is the one of dry oxygen, wet oxygen, steam, Oxidation Process By Hydrogen Oxygen Synthesis, oxidization time 30 ~ 90 minutes, porous silicon oxide layer is removed with hydrofluoric acid solution afterwards in mega sonic wave cleaning machine, acquisition smooth internal walls surface, this is because hydrofluoric acid solution not easily dissolves silicon, but it is possible to dissolved oxygen SiClx;
(3) at 900 ~ 1100 DEG C of temperature, again carry out oxidation processes to silicon chip 1, oxidation technology is dry-oxygen oxidation, oxidization time 30 ~ 90 minutes, at the SiO that smooth internal walls surface in microchannel is formed
2layer, as the protective layer of microchannel interior walls, the corrosive liquid avoiding next step to use damages microchannel interior walls, and this step also forms SiO at silicon chip 1 front, the back side certainly
2layer;
(4) adopt 20 ~ 35 wt% TMAH solution (Tetramethylammonium hydroxide) corrosion of silicon 1 back side at 70 ~ 85 DEG C of temperature, remove silicon chip 1 back side SiO
2layer also continues thinning silicon chip, until whole microchannels is penetrating, as shown in Figure 3.
3, the circle of contact forms silicon micro-channel board substrate reinforcing ring
Holder silicon chip 1, removes the irregular distribution microchannel 7 inwall SiO be distributed in circle of contact corrosion area 5 with hydrofluoric acid solution
2layer, adopt 20 ~ 35 wt% TMAH solution at 70 ~ 85 DEG C of temperature, corrode irregular distribution microchannel 7 in circle of contact corrosion area 5 again, make it to communicate with each other, silicon chip distribution micro channel array part is finally made to be separated with silicon chips periphery part, complete circle of contact operation, a circle reinforcing ring 9 is had, as shown in Figure 4 around the disc-shaped silicon micro-channel board substrate 8 obtained.
4, silicon microchannel plate front side of matrix, polished backside
(1) in mega sonic wave cleaning machine, adopt RCA forensic chemistry to clean disc-shaped silicon micro-channel board substrate 8;
(2) at 900 ~ 1100 DEG C of temperature, disc-shaped silicon micro-channel board substrate 8 is oxidized, forms SiO in array microchannel 6 inner wall surface
2layer, mode of oxidizing is the one of dry oxygen, wet oxygen, steam, Oxidation Process By Hydrogen Oxygen Synthesis, oxidization time 30 ~ 90 minutes;
(3) under vacuum paraffin is filled in the front side of silicon wafer of array microchannel 6, back side port 10;
(4) cmp method polished silicon slice front, the back side is adopted, polishing fluid particle size range 20 ~ 100 nm, pH value 9 ~ 11;
(5) hydrofluoric acid solution, rear employing carbon tetrachloride or trichloroethylene is first adopted to soak silicon micro-channel board substrate (8), remove the polishing fluid in array microchannel 6 and paraffin, complete silicon micro-channel board substrate 8 front, polished backside, owing to forming SiO in array microchannel 6 inner wall surface in advance
2layer, and SiO
2easily be removed, polishing fluid and paraffin are also just easy to be removed thereupon.
In mega sonic wave cleaning machine, finally adopt the silicon micro-channel board substrate 8 after RCA forensic chemistry cleaning polishing, in order to techniques such as follow-up oxidation, chemical meteorology deposition, plated electrodes, final products are exactly silicon microchannel plate, and microchannel is penetrating, channel interior cleanliness without any pollution, surfacing is smooth, passage reaches 320 μm, channel cross-sectional shape approximating square, the length of side only 8 μm, draw ratio reaches 40, the mechanical strength of edge entity reinforcing ring efficient hardening silicon microchannel plate.
Claims (2)
1. one kind has the silicon micro-channel board substrate processing method of reinforcing ring, electrochemical etching method is adopted to make micro channel array, last procedure is: in silicon microchannel plate front side of matrix, polished backside operation, first disc-shaped silicon micro-channel board substrate (8) is oxidized, forms SiO in array microchannel (6) inner wall surface
2layer, under vacuum paraffin is filled in the front side of silicon wafer of array microchannel (6), back side port (10) again, then polished silicon slice front, the back side, finally remove the polishing dirt in array microchannel (6) and paraffin, complete silicon micro-channel board substrate (8) front, polished backside; It is characterized in that:
Make in micro channel array operation in electrochemical corrosion, adhere to shading endless belt (2) at silicon chip (1) back side simultaneously, shading endless belt (2) is concentric with microchannel corrosion starting point array border circular areas (3), the ring inner region of shading endless belt (2) is exactly microchannel corrosion starting point array border circular areas (3), ring strip region between shading endless belt (2) and contact-making surface electrode (4) is circle of contact corrosion area (5), while corrosion array microchannel (6), corrode irregular distribution microchannel (7) at circle of contact corrosion area (5);
In the operation that make microchannel penetrating thinning by silicon chip back side, first adopt the SiO that dry-oxygen oxidation technique is formed on microchannel smooth internal walls surface
2layer, as the protective layer of microchannel interior walls, then carries out silicon chip (1) backside chemical corrosion thinning, until whole microchannels is penetrating;
Formed in silicon micro-channel board substrate reinforcing ring operation at the circle of contact, first remove irregular distribution microchannel (7) the inwall SiO in circle of contact corrosion area (5)
2layer, corrode this microchannel again, make it to communicate with each other, finally make silicon chip distribution micro channel array part be separated with silicon chips periphery part, complete circle of contact operation, around the disc-shaped silicon micro-channel board substrate (8) obtained, have a circle reinforcing ring (9).
2. the silicon micro-channel board substrate processing method with reinforcing ring according to claim 1, it is characterized in that, the described circle of contact forms silicon micro-channel board substrate reinforcing ring operation: holder silicon chip (1), removes irregular distribution microchannel (7) the inwall SiO be distributed in circle of contact corrosion area (5) with hydrofluoric acid solution
2layer, adopt 20 ~ 35wt%TMAH solution at 70 ~ 85 DEG C of temperature, corrode irregular distribution microchannel (7) in circle of contact corrosion area (5) again, make it to communicate with each other, finally make silicon chip distribution micro channel array part be separated with silicon chips periphery part, complete circle of contact operation.
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CN104326439B (en) * | 2014-08-22 | 2016-09-21 | 华东师范大学 | A kind of method improving silicon microchannel plate surface topography |
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5997713A (en) * | 1997-05-08 | 1999-12-07 | Nanosciences Corporation | Silicon etching process for making microchannel plates |
CN101054158A (en) * | 2007-03-09 | 2007-10-17 | 华东师范大学 | Self-separation manufacturing method for silicon micro-channel structure |
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Publication number | Priority date | Publication date | Assignee | Title |
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US5997713A (en) * | 1997-05-08 | 1999-12-07 | Nanosciences Corporation | Silicon etching process for making microchannel plates |
CN101054158A (en) * | 2007-03-09 | 2007-10-17 | 华东师范大学 | Self-separation manufacturing method for silicon micro-channel structure |
Non-Patent Citations (1)
Title |
---|
《硅微通道板的研究进展》;黄永刚 等;《应用光学》;20110930;第32卷(第5期);第960~965页 * |
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