CN102789128B - Method for preparing patterned ZnO nanorod array - Google Patents
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- CN102789128B CN102789128B CN201210300106.4A CN201210300106A CN102789128B CN 102789128 B CN102789128 B CN 102789128B CN 201210300106 A CN201210300106 A CN 201210300106A CN 102789128 B CN102789128 B CN 102789128B
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Abstract
The invention discloses a method for preparing a patterned ZnO nanorod array and belongs to the field of nano material patterning growth. Three techniques including an all-optical-path medium holophote, an airflow preventing organic glass shade and a low-density multi-cup method development are adopted on the basis of a three-light-beam laser interference template method for preparing the patterned ZnO nanorod array, the problem of template deformity caused by multi-time exposure in double-light-beam laser interference rotation is avoided while adverse influences caused by airflow fluctuation and development fatigue are lowered, porous template contrast and structural stability are greatly improved, an improved template is subjected to confining hydrothermal growth, and the obtained patterned ZnO nanorod array is controllable and stable. The method for preparing the patterned ZnO nanorod array is simple, efficient, low in cost and easy to popularize and establish a firm foundation for development of the patterned ZnO nanorod array towards device application.
Description
Technical field
The invention belongs to nano material patterned growth field, be specifically related to template synthesis patterning ZnO nano-rod array.
Background technology
Due to special material and architectural characteristic, ZnO nano-rod array become in ZnO nano material system research the most extensively, one of the most deep material, be the nano material with huge applications and through engineering approaches prospect of generally acknowledging.Except the power photoelectric characteristic of self, it also has advantages of prepared by high-specific surface area, low-cost large-area.Therefore, ZnO nano-rod array has obtained successfully using on many nano functional devices, as nano generator, power electric transducer, light emitting diode, field emission cold-cathode, ultraviolet detector, solar cell, electrochromic film and biology sensor etc.
Yet, the performance of above nano functional device with realize market-oriented industrialized standard and also have certain gap, many devices also just rest on the original reason test stage.Tracing it to its cause, is conventional growth technique, and as liquid phase epitaxial method and chemical vapour deposition technique, the ZnO nano-rod array making also exists many defects, such as c-axis orientation is not good, spacing is overstocked, thickness is uneven and different in size etc.These defects can cause the problems such as electrode loose contact, electric current obstruction, electric leakage or inverse current are large, military service poor stability in device is built.In addition, classic method can not realize the truly accuracy controlling of appearance and size, thereby cannot meet the requirement of different components design.
Patterned growth technology can effectively address the above problem.So-called patterned growth technology, is by the template by regularly arranged, and confinement growth and accuracy controlling are carried out in the nucleation site of ZnO nano-rod array and size pattern, thereby make nanometer rods length consistent, even thickness, C axle vertical-growth, thus solve the bad problem of device performance.
At present, comparatively common ZnO nano-rod array patterned growth technology mainly comprises following four kinds:
1. photoetching ([1] Chun Cheng, Ming Lei, Lin Feng, Tai Lun Wong, K. M. Ho; Kwok Kwong Fung, Michael M. T. Loy, Dapeng Yu, and Ning Wang, ACSnano; VOL. 3, NO. 1,53-58,2009; [2] H. S. Song, W. J. Zhang, C. Cheng, Y. B. Tang, L. B. Luo, X. Chen, C. Y. Luan, X. M. Meng, J. A. Zapien, N. Wang, C. S. Lee, I. Bello, and S. T. Lee, Crystal Growth & Design, Vol. 11, No. 1,2011): the Ning Wang[1 of Hong Kong University of Science and Thchnology in 2009] group makes photoresist nano-dot matrix in Si substrate, then by CVD method using its high temperature cabonization and as the grow ZnO nano-rod array of patterning of forming core point; The Li Shu of City University of Hong Kong soup [2] group in 2011, by photoetching and etching, first forms Si micron bar array, subsequently continued growth ZnO nano-rod array on micron bar sidewall.
The self assembly of 2.PS ball ([3] Xudong Wang, Christopher J. Summers, and Zhong Lin Wang, Nano Lett., Vol. 4, and No. 3,2004; [4] D. F. Liu, Y. J. Xiang, X. C. Wu, Z. X. Zhang, L. F. Liu, L. Song, X. W. Zhao, S. D. Luo, W. J. Ma, J. Shen, W. Y. Zhou, G. Wang, C. Y. Wang, and S. S. Xie, Nano Lett., Vol. 6, No. 10,2006): the king of Georgia Institute of Technology middle forest [3] group in 2004, fills in film formed regular sphere gap PS ball is self-service, Au particle is entered in sputter, uses subsequently legal some catalytic growth of ZnO nanometer stick array of CVD; Within 2006, dark [4] group of CAS Institute of Physics solution think of of the Chinese Academy of Sciences improves template by the method for etching and annealing, thereby realizes the single growth of nanometer rods single-point.
3. electron beam exposure ([5] Sheng Xu; Yaguang Wei; Melanie Kirkham, Jin Liu, Wenjie Mai; Dragomir Davidovic; Robert L. Snyder, and Zhong Lin Wang, J. Am. Chem. Soc. 2008; 130,14958-14959; [6] Robert Erdelyi, Takahiro Nagata, David J. Rogers, Ferechteh H. Teherani, Zsolt E. Horvath, Zoltan Labadi, Zsofia Baji, Yutaka Wakayama, and Janos Volk, Cryst. Growth Des. 2011,11,2515-2519): the king of Georgia Institute of Technology middle forest [5] group in 2008 has made the square PMMA hole template of approximately 200 μ m with EBL pointwise punching, and thus hydrothermal growth the single ZnO nano-rod array of single hole; Hungary's technology physics in 2011 and the Janos Volk[6 of material science research institute] group investigated the impact of different crystal seed layer preparation technologies on subsequent pattern ZnO nano-rod array pattern in conjunction with EBL.
4. laser interference ([7] Dong Sik Kim, Ran Ji, Hong Jin Fan; Frank Bertram, Roland Scholz, Armin Dadgar; Kornelius Nielsch, Alois Krost, Jrgen Christen; Ulrich G sele; and Margit Zacharias, Small 2007,3; No. 1,76-80; [8] Ki Seok Kim, Hyun Jeong, Mun Seok Jeong, and Gun Young Jung, Adv. Funct. Mater. 2010,20,3055-3063; [9] Yaguang Wei, Wenzhuo Wu, Rui Guo, Dajun Yuan, Suman Das, and Zhong Lin Wang, Nano Lett. 2010,10,3414-3419): the German Max Planck microstructure Dong Sik Kim[7 of physics Institute in 2007] utilize double light beam laser interference technique to make the hole template of square arrangement, Au particle is entered in sputter, uses afterwards CVD legal system for regularly arranged ZnO nano-rod array; Gwangju, Korea technical college Gun Young Jung[8 in 2010] group utilizes double light beam laser interference technique on Si, the SiO2 of even glue crystal seed layer, FTO, to make the hole template that square arrangement and hexagonal are arranged being prefabricated with, then by hydro-thermal method, vertical growth, evenly distributed ZnO nano-rod array have been obtained, nanometer rods diameter 200-300nm, size of foundation base reaches 2 inches of wafer levels; Within 2010, the king of Georgia Institute of Technology middle forest [9] group utilizes double light beam laser interference technique in the Si substrate of GaN and prefabricated magnetron sputtering crystal seed layer, to make square arrangement hole template equally, and obtain patterning ZnO nano-rod array by hydrothermal growth, nanometer rods diameter 500-600nm, size of foundation base also reaches 2 inches of wafer levels.
Generally speaking, photoetching technique is due to the existence of diffraction effect, and by hole/dot matrix template of photoetching technique making, diameter is difficult to reach the following level of incident wavelength, so the most cluster shape distribution of gained ZnO nano-rod array, and controllability is not ideal.PS ball self-assembling method is had relatively high expectations to substrate surface flatness and hydrophilic hydrophobic property, PS ball large area continuous uniform distribution difficulty is larger, because adopt the metallic particles such as Au to carry out high growth temperature as catalyzer, not only can introduce a large amount of defects, but also substrate is had to resistant to elevated temperatures requirement again.EBL(electron beam exposure) although machining precision is high, process velocity is slow, cost is high, so be also unsuitable for making large area pattern ZnO nano-rod array.Laser interference patterning techniques has with low cost, pattern hole hole dia and the advantage such as density is adjustable by contrast, from but realize the first-selection that large area high-sequential is arranged ZnO nano-rod array.
Yet, in laser interference template synthesis patterning ZnO nano-rod array process, there is the multinomial unfavorable factor that affects the controlled and stable output of array.Make a concrete analysis of as follows:
First, double light beam laser is interfered, need be rotated multiexposure, multiple exposure, could generate hole template (square arrangement and hexagonal are arranged).Rotation multiexposure, multiple exposure has following deficiency: 1, because Lloyd mirror double light beam laser interferes the energy Gaussian distributed of exposure area (strong from the region energy close to spot center, a little less than the region energy away from spot center, Fig. 1 a), be in the sample area (the A district in Fig. 1 b) of non-rotary central, rotation front and back position will change, under the identical time shutter, corresponding exposure dose also will change, and this can cause hole template to present oval aperture; 2, be in the sample area (the B district in Fig. 1 b) of rotation center, rotation front and back are because of invariant position, before and after the exposure dose that obtains be (as Fig. 1 c-d) equating, but due to after photoresist successively exposes, sensitivity meeting constantly declines, this exposure dose absorption difference can cause rotating after multiexposure, multiple exposure, under the identical time shutter, (Fig. 1 e-f, along with exposure frequency increases to occur equally oval hole template, absorptivity declines, and corresponding live width constantly reduces).This non-circular hole template cannot confinement growth cross section be orthohexagonal patterning ZnO nano-rod array.
2012, inventor proposes and has set up two-sided Lloyd mirror three beam lasers and interfered template technology, can generate fast large area hexagonal arrangement circular opening template (the template deformity problem of having avoided double light beam laser to interfere rotation multiexposure, multiple exposure to cause) by single exposure, then utilize this template to carry out confinement hydrothermal growth to ZnO nano-rod array, thereby realized the accuracy controlling of ZnO nanorod on position, thickness, length and density.This technology possess system architecture simple, with low cost, without mask and turntable, the advantage such as process velocity is fast and ability of regulation and control is strong.The improvement that the present invention does based on technique just.
Secondly, in two-sided Lloyd mirror three beam lasers are interfered, (Fig. 2 a) affect hexagonal arrangement hole template and be whether circular principal element and be the reflectivity of the square reflector that two sides is 120 degree angles.Under this interference pattern, the incident light of direct irradiation on sample and the reflected light of two sides mirror interfere between two in rhombus exposure area, in three directions of-60/0/60 degree, produce wire interference fringe (need to respectively expose once three angles under two-beam interference pattern) simultaneously, thereby single exposure just can generate hexagonal, arrange hole template.If adopting reflectivity is the ultraviolet enhancing aluminium reflector of 90% left and right, the catoptrical light intensity of two bundles will be less than direct incident light, and be responsible for (being upper and lower both sides, hole) that horizontal direction interferes this two bundles reflected light just, the result that intensity loss is brought is the decline of this direction interference energy, corresponding in structure is reducing of live width, and final hole becomes ellipse (Fig. 2 b).
Again, interference fringe is fixed in the ideal situation, and photoresist records and can obtain circular opening template that contrast is very high after this energy distribution (Fig. 3 a).But, extraneous low-frequency vibration and airflow fluctuation can cause certain impact to optical element, making to expand hot spot occurs occurring relative displacement between shake or optical element, thus, interference fringe will cannot be completely fixed thereupon shaking, cause interference energy distribution contrast obviously to decline (Fig. 3 b), its contrast of the template obtaining under this state will be low (Fig. 3 c).Low contrast hole template bottom has cull particle, sidewall has slope, with this template growth patterning ZnO nano-rod array, can come up against a series of problems (Fig. 3 d), as nanometer rods merging growth (Fig. 3 e), thickness uneven (Fig. 3 f), fracture of root (Fig. 3 g) and blocking-up growth etc.
Finally, relate to two development effect problems: 1, commercialization developer solution normally designs for micron order thickness photoresist, solute concentration is higher, and the photoresist thickness adopting while carrying out laser interference only has 100-500nm, if directly thin photoresist is developed with high concentration developer solution, easily there is development (former structure of expecting to retain also can be removed) 2, while carrying out the manual development of batch, the same cup of Reusability developer solution can make developer solution solute concentration decline gradually (developing tired), easily there is owing to develop (former structure of expecting to remove also can be retained) in the sample of post-production.Above-mentioned two problems all can cause hole template contrast to decline to a great extent, and technique is controlled simultaneously becomes undesirable with stability.
As can be seen here, if will realize the stable and controlled preparation of patterning ZnO nano-rod array, circular opening and high-contrast template are most important, and process controllability and stability are indispensable.
Summary of the invention
The object of the invention is in order to improve process controllability and stability, proposed a kind of controlled and stable method of preparing patterning ZnO nano-rod array.
The technical solution adopted in the present invention is to adopt a kind of method of preparing patterning ZnO nano-rod array, can realize the controlled and stable output of patterning ZnO nano-rod array, it is characterized in that: the method concrete steps are as follows:
(1) build the three beam laser interference systems based on two-sided Lloyd mirror, full light path working medium completely reflecting mirror, except laser instrument, optical table hides with transparent organic glass shade;
(2) growth is carried out to ultrasonic cleaning spin coating negativity ultraviolet photoresist with substrate;
(3) substrate with photoresist is carried out to three beam lasers and interfere single exposure, the many agar diffusion methods of rear employing low concentration develop and obtain high-contrast hexagonal arrangement circular opening template;
(4) by put into growth-promoting media with the growth substrate of described template, carry out patterning ZnO nano-rod array confinement hydrothermal growth, rear taking-up, cleaning oven dry, can obtain patterning ZnO nano-rod array.
Further, the structure of described step (1) three beam laser interference system is to adopt: a branch of 325nm laser of He-Cd laser instrument, through two sides medium completely reflecting mirror, enter spatial filter and carry out filtering processing, expand subsequently 100cm and form the large spot that diameter is 12cm; Sample stage is placed with certain incident angle, and the another mutual angle of two sides medium completely reflecting mirror is 120 degree and all perpendicular to sample stage, sample stage is aimed at the center of large spot with the intersection point of two-face mirror; Lay electronic shutter, for accurately controlling the time shutter.
Further, the substrate of described medium completely reflecting mirror adopting quartz glass, is divided into two kinds of models, a kind of is diameter 25.4mm circular reflector, for the laser reflection before spatial filter, another kind is 50*100mm square reflector, for carrying out two-sided Lloyd mirror three beam lasers, interferes; In incident angle, be within the scope of 5-45 degree, described catoptron is more than 99.0% to the average reflectance of 325nm laser, can realize the loss of full light path least energy, can promote to greatest extent again the contrast that interference energy distributes.
Further, in described step (1), transparent organic glass shade is to adopt lightweight organic glass to make anti-air-flow air shade, and design sliding door, in order to regulate light path and to change sample, this shade has not only been avoided the pollution of koniology to optical element, and has reduced the equipment such as laser instrument heating radiator, clarifier blower fan and cause the impact of airflow fluctuation to optical element.
Further, the concrete operation of the many agar diffusion methods of low concentration is in described step (3): by original content developer solution 1:1 deionized water dilution process by volume, substrate is successively put into three beakers that fill above-mentioned dilute development liquid, manually develop, development time is respectively 1min, photoresist adsorption bubble during for anti-development, substrate need tilt to put into dilute development liquid.
Further, described substrate is Si or p-GaN.
Further, the pin hole that the saturating object lens of height that described spatial filter is 2cm by focal length and diameter are 5um forms.
The present invention is simply effective, with low cost, be easy to promote, and for patterning ZnO nano-rod array moves towards device application, established solid foundation, has important science and commercial value.
Accompanying drawing explanation
Fig. 1 a) one side Lloyd mirror double light beam laser interferes, exposure area energy distribution simulation drawing; B) rotation multiexposure, multiple exposure (0/90 degree ,-60/0/60 degree) schematic flow sheet; C) energy distribution simulation drawing after the double exposure of B area 0/90 degree; D) energy distribution simulation drawing after three exposures of B region-60/0/60 degree; E) corresponding templates structure FESEM figure (front elevation) after the double exposure of B area 0/90 degree; F) corresponding templates structure FESEM figure (front elevation) after three exposures of B region-60/0/60 degree.
Fig. 2 a) two-sided Lloyd mirror three beam lasers interferes exposure desk photo; B) use the FESEM figure (front elevation) of the ultraviolet enhancing aluminium reflector rear pattern plate structure that reflectivity is 90%.
Fig. 3 is high-contrast circular opening template section FESEM figure (45 degree side view) a); B) because of interference fringe shake, energy distribution changes schematic diagram by high-contrast to low contrast; C) low contrast hole template section FESEM figure (45 side view); D1-d4) with low contrast template growth ZnO nano-rod array, FAQs gathers schematic diagram; E) nanometer rods merging growth FESEM figure (45 degree side view); F) the uneven FESEM figure of nanometer rods thickness (front elevation); G) nanometer rods fracture of root FESEM figure (front elevation).
Fig. 4 a) repeats 9 times by same template method technique on 0.7*0.7cm p-GaN, gained high-contrast circular shuttering glory photo; B) high-contrast circular opening template low power and high power FESEM figure (front elevation); C) the patterning ZnO nano-rod array low power obtaining with this template confinement hydrothermal growth and high power FESEM figure (front elevation).
Embodiment
Below in conjunction with example, technical scheme of the present invention is elaborated, obviously, described example is only a part very little in the present invention, rather than whole examples.Example based in the present invention, those skilled in the art, not making the every other example obtaining under creative work prerequisite, belong to the scope of protection of the invention.
1: three beam laser interferometric method of example is prepared hexagonal and is arranged circular opening template
(1) three beam laser interference system builds: a branch of 325nm laser of He-Cd laser instrument, through the circular medium completely reflecting mirror of two sides diameter 25.4mm, enter spatial filter (pin hole that the saturating object lens of height that are 2cm by focal length and diameter are 5um forms) and carry out filtering processing, expand subsequently 100cm and form the large spot that diameter is 12cm; Sample stage is placed with 18.5 degree incident angles, and the mutual angle of the square medium completely reflecting mirror of two sides 5*10cm is 120 degree and all perpendicular to sample stage, sample stage is aimed at the center of large spot with the intersection point of two-face mirror; Lay electronic shutter, for accurately controlling the time shutter; Except laser instrument, related optical element is hidden (Fig. 4) by organic glass shade.
(2) substrate cleans and photoresist spin coating: 1*1cm Si substrate is after acetone, Piranha solution (concentrated sulphuric acid and hydrogen peroxide volume ratio 3:1) and deionized water ultrasonic cleaning, and nitrogen dries up; I line negativity ultraviolet photoresist, after the dilution of 1:1 mass ratio, carries out 500rpm*6s+4000rpm*30s spin coating, obtains thickness 300nm; To spin coating, there is the substrate of photoresist to carry out the soft baking of 85 degree hot plate 1min.
(3) substrate exposure and development: have the substrate of photoresist to be respectively fixed to rhombus exposure area above-mentioned spin coating and expose (substrate is positioned on the horizontal diagonal line in rhombus exposure area, and substrate center is apart from spot center 2cm), the time shutter is 40s; Substrate after exposure is carried out to 95 degree hot plates and firmly dry 1min; With (the original content developer solution: deionized water volume ratio 1:1 dilution) carry out the many agar diffusion methods of low concentration and develop of developer solution after three glasss of dilutions, the substrate 1min that respectively develops in each cup, the 20s of deionized water photographic fixing afterwards, nitrogen dries up, and can obtain high-contrast hexagonal and arrange circular opening template.
2: three beam laser interferometric methods of example are prepared p-GaN base patterning ZnO nano-rod array
(1) three beam laser interference system builds: a branch of 325nm laser of He-Cd laser instrument, through the circular medium completely reflecting mirror of two sides diameter 25.4mm, enter spatial filter (pin hole that the saturating object lens of height that are 2cm by focal length and diameter are 5um forms) and carry out filtering processing, expand subsequently 100cm and form the large spot that diameter is 12cm; Sample stage is placed with 26.8 degree incident angles, and the mutual angle of the square medium completely reflecting mirror of two sides 5*10cm is 120 degree and all perpendicular to sample stage, sample stage is aimed at the center of large spot with the intersection point of two-face mirror; Lay electronic shutter, for accurately controlling the time shutter; Except laser instrument, related optical element is hidden by organic glass shade.
(2) substrate cleans and photoresist spin coating: 0.7*0.7cm p-GaN substrate is after acetone, isopropyl alcohol and deionized water ultrasonic cleaning, and nitrogen dries up; I line negativity ultraviolet photoresist, after the dilution of 1:1 mass ratio, carries out 500rpm*6s+4000rpm*30s spin coating, obtains thickness 300nm; To spin coating, there is the substrate of photoresist to carry out the soft baking of 85 degree hot plate 1min.
(3) substrate exposure and development: have the substrate of photoresist to be respectively fixed to rhombus exposure area above-mentioned spin coating and expose (substrate is positioned on the horizontal diagonal line in rhombus exposure area, and substrate center is apart from spot center 2cm), the time shutter is 50s; Substrate after exposure is carried out to 95 degree hot plates and firmly dry 1min; With (the original content developer solution: deionized water volume ratio 1:1 dilution) carry out the many agar diffusion methods of low concentration and develop of developer solution after three glasss of dilutions, the substrate 1min that respectively develops in each cup, the 20s of deionized water photographic fixing afterwards, nitrogen dries up, and can obtain high-contrast hexagonal and arrange circular opening template.
(4) the template hydro-thermal method confinement of patterning ZnO nano-rod array growth: will arrange the p-GaN face down of circular opening template with hexagonal, swim on the zinc nitrate and hexamethylene tetramine aqueous solution liquid level of 0.05mol/L, temperature of reaction 95 degree, reaction time 3h.
(5) removal of the cleaning of array and photoresist template: hydro-thermal reaction finishes, by a large amount of deionized water rinsings of substrate, then in supporting glue-dispenser, soak 20s in order to remove photoresist template, use again rinsed with deionized water, then put into isopropyl alcohol and soak 1min, finally take out and dry, can obtain the patterning ZnO nano-rod array based on p-GaN.
The present invention interferes on the basis of single exposure template synthesis patterning ZnO nano-rod array at three beam lasers, (all optical elements are unified to be hidden with organic glass shade to adopt full light path medium completely reflecting mirror (all catoptrons all adopt medium completely reflecting mirror), anti-air-flow organic glass shade, specifically adopt lightweight organic glass to make anti-air-flow air shade, and design sliding door, in order to regulate light path and to change sample) and the many agar diffusion methods developments of low concentration (dilute by a certain percentage original-pack developer solution, obtain suitable low concentration developer solution; While manually developing, first the developer solution having diluted is poured in a plurality of beakers, then substrate develops a period of time successively in each beaker) three technology, not only avoided double light beam laser to rotate the template deformity that multiexposure, multiple exposure causes in interfering, and reduced airflow fluctuation and developed the tired adverse effect of bringing, significantly improved contrast and the structural stability of circular opening template, made patterning ZnO nano-rod array be able to stable and controlled output.
Claims (5)
1. a method of preparing patterning ZnO nano-rod array, can realize the controlled and stable output of patterning ZnO nano-rod array, it is characterized in that: the method concrete steps are as follows:
(1) build the three beam laser interference systems based on two-sided Lloyd mirror, full light path working medium completely reflecting mirror, except laser instrument, optical table hides with transparent organic glass shade;
(2) growth is carried out to ultrasonic cleaning spin coating negativity ultraviolet photoresist with substrate;
(3) substrate with photoresist is carried out to three beam lasers and interfere single exposure, the many agar diffusion methods of rear employing low concentration develop and obtain high-contrast hexagonal arrangement circular opening template;
(4) by put into growth-promoting media with the growth substrate of described template, carry out patterning ZnO nano-rod array confinement hydrothermal growth, rear taking-up, cleaning oven dry, can obtain patterning ZnO nano-rod array;
Building of described step (1) three beam laser interference system is to adopt: a branch of 325nm laser of He-Cd laser instrument, through the circular medium completely reflecting mirror of two sides diameter 25.4mm, enter spatial filter and carry out filtering processing, expand subsequently 100cm and form the large spot that diameter is 12cm; Sample stage is placed with certain incident angle, the another mutual angle of the square medium completely reflecting mirror of two sides 50*100mm is 120 degree and all perpendicular to sample stage, for carrying out two-sided Lloyd mirror three beam lasers of described three beam laser interference systems, interfere, sample stage is aimed at the center of large spot with the intersection point of the another square medium completely reflecting mirror of two sides 50*100mm, lay electronic shutter, for accurately controlling the time shutter; Described circular medium completely reflecting mirror and the substrate of square medium completely reflecting mirror adopting quartz glass; In incident angle, be within the scope of 5-45 degree, described square reflector is more than 99.0% to the average reflectance of 325nm laser, can realize the loss of full light path least energy, can promote to greatest extent again the contrast that interference energy distributes.
2. the method for claim 1, it is characterized in that: in described step (1), transparent organic glass shade is to adopt lightweight organic glass to make anti-air-flow air shade, and design sliding door, in order to regulate light path and to change sample, this shade has not only been avoided the pollution of koniology to optical element, and reduced laser instrument heating radiator, clarifier blower fan causes the impact of airflow fluctuation to optical element.
3. the method for claim 1, it is characterized in that: the concrete operation of the many agar diffusion methods of low concentration is in described step (3): by original content developer solution 1:1 deionized water dilution process by volume, three beakers that fill above-mentioned dilute development liquid are successively put in substrate, manually develop, development time is respectively 1min, photoresist adsorption bubble during for anti-development, substrate tilts to put into dilute development liquid.
4. the method for claim 1, is characterized in that: described substrate is Si or p-GaN.
5. the method for claim 1, is characterized in that: the pin hole that the saturating object lens of height that described spatial filter is 2cm by focal length and diameter are 5 μ m forms.
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