CN102530841B - Processing method of high depth-width ratio microstructure of optical glass - Google Patents
Processing method of high depth-width ratio microstructure of optical glass Download PDFInfo
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- CN102530841B CN102530841B CN201210014024.3A CN201210014024A CN102530841B CN 102530841 B CN102530841 B CN 102530841B CN 201210014024 A CN201210014024 A CN 201210014024A CN 102530841 B CN102530841 B CN 102530841B
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Abstract
The invention discloses a processing method of a high depth-width ratio microstructure of optical glass, which is characterized in that the method adopts a high-precision optical glass as a research object, on the basis of a machining method for manufacturing different creasing shapes and creasing array patterns with pressing head microhardness testers of different shapes, combines with a wet method corrosion process, and carries out corrosions with different time intervals on a sample by using BOE solution (a mixture of HF and NH4F solution), thereby manufacturing high-precision optical glass structures of different shapes and different high depth-width ratio structures.
Description
Technical field
The present invention relates to a kind of optical glass micro-structural processing and lithographic technique.
Background technology
Development along with large scale integrated circuit manufacturing technology, micromachine has completed the development from unit to system, and be successfully applied to optical field and formed novel focus-MOEMS MOEMS (Micro-Optic-Electro-Mechanical-System), and aspect a lot of, obtained application.Because MOEMS need to carry out various optical detections, so just need to be applied to a large amount of transparent materials, optical glass is first when its choosing.Optical glass has obtained extensive application in MEMS (MEMS), MOEMS and biochip at present, except silicon materials are had demand, the various novel MEMS devices of doing basic material with optical glass arise at the historic moment, there is following problem for the processing of optical glass micro-structural in existing high aspect ratio technology: existing technology majority is directly to process high aspect ratio structure with dry etching, be used for the anisotropic structures such as machine silicon crystal, and for this isotropic material of optical glass, be difficult to control its machined parameters; In addition, this dry etching processing method cost is higher, is not suitable for large-scale production processing; And existing wet etching technique carrys out etching optical glass processing micro structure, on this isotropic material, be difficult to process the micro-structural with higher depth-to-width ratio, this just needs exploitation to be specifically designed to the high-aspect-ratio process technology of optical glass.
Summary of the invention
The object of the invention is by studying different pressure heads for the impact of optical glass micro-structural shape and holographic characteristic, find the relation between mechanical impression method and etch technological condition, a kind of optical glass high aspect ratio microstructures processing method that adopts machinery and the combination of traditional chemical etching phase is provided.
For achieving the above object, the present invention takes following technical scheme to be achieved:
A high aspect ratio microstructures processing method for optical glass, is characterized in that, comprises the steps:
(1) get optical glass sheet as sample, in its one side, with microhardness testers, make regularly arranged two-dimentional impression, four diagonal of each impression have four linear cracks of radiation, and this radiation crack is exactly for making the microstructure of high-aspect-ratio;
(2) with paraffin, glass sheet sample periphery is wrapped up, the place that only leaves impression is not wrapped;
(3) preparation BOE solution, i.e. HF and NH
4the mixed solution of F is stand-by, wherein NH
4the volumetric concentration ratio of F and HF is 6: 1;
(4) glass sheet sample that is enclosed with paraffin is carried out to ultrasonic cleaning, be placed in the culture dish that fills BOE solution after dry, make BOE solution flood glass sheet sample, and culture dish is put into 25 ℃ of waters bath with thermostatic control corrode after at least 10 minutes and take out;
(5) repeating step (4) is until obtain the micro-structural in required depth-to-width ratio crack.
In said method, described ultrasonic cleaning is three times, uses for the first time 25 ℃ of water-bath ultrasonic cleaning of deionized water 5 minutes; Use for the second time the water-bath ultrasonic cleaning 5 minutes of 25 ℃, acetone; Use for the third time 25 ℃ of water-bath ultrasonic cleaning of absolute ethyl alcohol 5 minutes.Described dry employing nitrogen dries up.
Advantage of the present invention is:
1, combine machining and chemical etching method and make high-precision optical glass high aspect ratio microstructures, method is quick, workable.
2, can choose according to the difference of processing method, be choosing of micro-impression indenter shape, the different spread geometries of impression are made different impression arrays, produce different crackle arrays, and the crackle array that these are had to high aspect ratio structure is applied to its micro-manufacture field being applicable to.
3, wet etching method is applied in the middle of the making of high aspect ratio microstructures of isotropism optical glass surface, compared with dry etching method in the past, greatly reduce processing cost like this, in conjunction with machining, there is the further controllability of the present invention that strengthened again.
The present invention be suitable in K9 substrate of glass processing more carefully, the microchannel microstructure of dark (hundreds of micron), owing to thering is good micro-processing characteristics and less expensive price, gain great popularity.But the invention is not restricted to K9 glass, also can be used for making the micron of brittle optical material etc. and the micro-structural of nanoscale, these micro-structurals can be widely used in the occasions such as microwave technology, sensor, optical element.
Accompanying drawing explanation
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Fig. 1 is the impression schematic diagram of the inventive method.Wherein: (a) figure is the positive rectangular pyramid shape of Vickers impression array schematic diagram (two row); (b) figure is Knoop indentation array schematic diagram.
Fig. 2 amplifies the impression photo that the power with 4.903N of 1000 times is produced under light microscope.
Fig. 3 is the glass sample (four impressions are exposed) that is enclosed with paraffin.
Fig. 4 is that the impression dynamics of Fig. 2 is 4.903N, and the laser co-focusing of the impression that guarantor's lotus time is 10s crackle after corrosion in 40 minutes is measured photo.
Fig. 5 is that Fig. 4 corrodes the schematic three dimensional views that rear impression records with laser co-focusing.
Fig. 6 be Fig. 1 array impression through 30 minutes corrosion after shape.
The specific embodiment
Adopt microhardness testers to use different pressure heads on high-precision optical glass, to produce different minute yardstick crackle, obtain not same microstructure of depth-to-width ratio.Can of square cone pressure head, Knoop indenter, positive Rhizoma Sparganii cone pressure head, wedge shape pressure head, double cone body pressure head, bicylindrical body pressure head etc., make the array structure of difform impression and impression, make based on this high-precision optical glass surface high aspect ratio microstructures.As shown in Fig. 1 (a), can produce two row impressions with the positive rectangular pyramid pressure head of Vickers, the radioactive crackle of periphery has also formed the fine cracks of certain rule.In like manner can make a row impression with Knoop indenter, the shape of impression is shown in Fig. 1 (b), all edge cracks form one group of very regular arrangement, after next step corrosion, just can become a fracture swarm with high aspect ratio structure, can be used in micro-structures such as making MEMS grating, mems switch.
Adopt the BOE solution effects on surface of variable concentrations to have the glass sample of impression to carry out the corrosion of certain hour, because optical glass is non-single crystal silicon material, so its corrosion is isotropic etch, in corrosion downwards, the width of its crackle also can change.The corrosion of the cushioning liquid of process finite concentration ratio like this, also makes the crackle of impression periphery amplify when just can make impression corrosion, so just can produce the high aspect ratio microstructures suiting the requirements.
In the present embodiment, take K9 optical glass as base material, and glass size is φ 12mm, and thickness is 6mm.
Experimental facilities: HVS-1000 type digital display microhardness testers partly form (as shown in Figure 3) by testing machine main body, workbench, elevating screw, loading system, soft key display operating panel, high magnification optical measuring system etc.By soft key, input, can regulate measurement light source strong and weak, preset trial force retaining time, Vickers and exert coomb's test Coomb method and switch.On LCD display on soft key panel, can show test method, test force, impression length, hardness number, test force retention time, measure number of times etc., and can key in the testing time.Specific embodiments is as follows:
(1) the K9 sheet glass of getting φ 12 * 6mm is as sample, at it, simultaneously use microhardness testers (Vickers) to make the positive rectangular pyramid impression of four arranged in squares of different loads, four diagonal of each impression have four linear cracks of radiation, and this radiation crack is exactly the structure that is used for making high-aspect-ratio that will use in this example.The impression that the power of employing 4.903N is made as shown in Figure 2.Different loads is as shown in table 1.
Table 1
| Load (GF) | 10 | 300 | 500 | 1000 |
| Power (N) | 0.0981 | 2.942 | 4.903 | 9.807 |
| Protect the lotus time (S) | 10 | 10 | 10 | 10 |
| Fracture width (μ m) | 0.34 | 0.76 | 0.82 | 1.10 |
| The penetration of fracture (μ m) | 0.67 | 19.25 | 22.23 | 28.7 |
(2) with paraffin, glass sheet sample periphery is wrapped up, the place that only leaves impression is not wrapped, and as shown in Figure 3, the object of doing is like this in order to guarantee that measurement datum is not destroyed.
(3) preparation BOE solution (HF and NH
4the mixed solution of F): the NH of 90g
4f is dissolved in 130ml water, and formation mass concentration is 40%NH
4f solution, gets 180ml standby;
Get again 15ml mass concentration and be 40% HF acid and add water 17ml to be diluted to mass concentration be 18.75% HF acid solution, join 180ml NH
4in F solution, mix, obtain BOE solution.NH now
4the volumetric concentration ratio of F and HF is 6: 1.
(4) sheet glass cleans: first sample is placed on to the water-bath with 25 ℃ in the glass beaker that fills deionized water and adds ultrasonic cleaning 5 minutes, put it into again the water-bath with 25 ℃ in the plastic beaker that fills acetone and add ultrasonic cleaning 5 minutes, put it into again the water-bath with 25 ℃ in the glass beaker that fills absolute ethyl alcohol and add ultrasonic cleaning 5 minutes, after taking-up, with nitrogen, dry up.
(5) sample is placed in the plastic culture dish of the BOE solution that fills the 3rd step preparation (making BOE solution flood mother glass sheet), and culture dish is put into water bath with thermostatic control (25 ℃) corrodes, after 10 minutes, take out.
(6) with confocal laser scanning microscope, record the width d in crack
1with degree of depth h
1, its ratio is ω
1=h
1/ d
1, now just can obtain the micro-structural of isotropism glass material surface depth-to-width ratio.
(7) can also repeat (4), (5) step and obtain the ω that depth-to-width ratio further improves
2=h
2/ d
2, ω
3=h
3/ d
3..., ω
n=h
n/ d
n.
For example, wherein impression dynamics is 4.903N, the impression that guarantor's lotus time is 10s, and corroding the fracture width that after 40 minutes, taking-up oven dry records with laser confocal microscope is d
4=2.372 μ m, h
4=24.718 μ m, depth-to-width ratio is now ω
4=10.420, measurement result as shown in Figure 4.Fig. 5 is the schematic three dimensional views of this impression.
Can in processing, process various array structures (Fig. 1).In the diversified while of assurance, also expanded its using value like this, Fig. 6 is the figure that the array of the positive rectangular pyramid impression of Fig. 1 is observed after corrosion in 30 minutes under laser confocal microscope.The figure of this many tissues that obtain has higher depth-to-width ratio, can well be applied in the processing of microsensor, micro-optical device, such array high-aspect-ratio crackle can have the micro element of array high aspect ratio structure for processing low-light grid etc., its using value is embodied.
Claims (2)
1. a high aspect ratio microstructures processing method for optical glass, is characterized in that, comprises the steps:
(1) get optical glass sheet as sample, in its one side, with microhardness testers, make regularly arranged two-dimentional impression, four diagonal of each impression have four linear cracks of radiation, and this radiation crack is exactly for making the microstructure of high-aspect-ratio;
(2) with paraffin, glass sheet sample periphery is wrapped up, the place that only leaves impression is not wrapped;
(3) preparation BOE solution, i.e. HF and NH
4the mixed solution of F is stand-by, wherein NH
4the volumetric concentration ratio of F and HF is 6:1;
(4) glass sheet sample that is enclosed with paraffin is carried out to ultrasonic cleaning, be placed in the culture dish that fills BOE solution after dry, make BOE solution flood glass sheet sample, and culture dish is put into 25 ℃ of waters bath with thermostatic control corrode after at least 10 minutes and take out;
(5) repeating step (4) is until obtain the micro-structural in required depth-to-width ratio crack.
2. the high aspect ratio microstructures processing method of optical glass as claimed in claim 1, is characterized in that, described ultrasonic cleaning is three times, uses for the first time 25 ℃ of water-bath ultrasonic cleaning of deionized water 5 minutes; Use for the second time the water-bath ultrasonic cleaning 5 minutes of 25 ℃, acetone; Use for the third time 25 ℃ of water-bath ultrasonic cleaning of absolute ethyl alcohol 5 minutes.
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Citations (4)
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| CN1506297A (en) * | 2002-12-12 | 2004-06-23 | 财团法人工业技术研究院 | Manufacture of microstructure with great depth/width ratio |
| CN1572738A (en) * | 2003-06-05 | 2005-02-02 | 三星钻石工业股份有限公司 | Lining method for fragile material base plate and apparatus therefor |
| CN101037185A (en) * | 2007-01-12 | 2007-09-19 | 中国科学院上海微系统与信息技术研究所 | Method for making nano-groove on quartz glass |
| CN102183602A (en) * | 2011-01-27 | 2011-09-14 | 电子科技大学 | Micro gas chromatographic column with high depth-to-width ratio and wet corrosion manufacturing method thereof |
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| JP4510405B2 (en) * | 2003-06-17 | 2010-07-21 | 西山ステンレスケミカル株式会社 | Method for forming recess on glass plate surface and method for manufacturing microlens array |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1506297A (en) * | 2002-12-12 | 2004-06-23 | 财团法人工业技术研究院 | Manufacture of microstructure with great depth/width ratio |
| CN1572738A (en) * | 2003-06-05 | 2005-02-02 | 三星钻石工业股份有限公司 | Lining method for fragile material base plate and apparatus therefor |
| CN101037185A (en) * | 2007-01-12 | 2007-09-19 | 中国科学院上海微系统与信息技术研究所 | Method for making nano-groove on quartz glass |
| CN102183602A (en) * | 2011-01-27 | 2011-09-14 | 电子科技大学 | Micro gas chromatographic column with high depth-to-width ratio and wet corrosion manufacturing method thereof |
Non-Patent Citations (2)
| Title |
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| 玻璃微流控芯片廉价快速制作方法的研究;陈强等;《化学学报》;20070915;第65卷(第17期);第1864页1.2节及第1865页第2.2节第三段第4-6行 * |
| 陈强等.玻璃微流控芯片廉价快速制作方法的研究.《化学学报》.2007,第65卷(第17期),第1864页1.2节及第1865页第2.2节第三段第4-6行. |
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