CN103232023A - Silicon microstructure processing method based on femtosecond laser treatment and wet etching - Google Patents
Silicon microstructure processing method based on femtosecond laser treatment and wet etching Download PDFInfo
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- CN103232023A CN103232023A CN2013101410352A CN201310141035A CN103232023A CN 103232023 A CN103232023 A CN 103232023A CN 2013101410352 A CN2013101410352 A CN 2013101410352A CN 201310141035 A CN201310141035 A CN 201310141035A CN 103232023 A CN103232023 A CN 103232023A
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Abstract
The invention discloses a silicon microstructure processing method based on femtosecond laser treatment and wet etching. The method comprises the steps of scanning a monocrystal silicon substrate by using a femtosecond laser at an oxygen-containing gas atmosphere; inducing silicon to generate refractive index change in a scanning region; and then, etching by using a hydrofluoric acid wet process to remove a refractive index change region to form a silicon microstructure. The method disclosed by the invention is simple in process; compared with the prior art, the method has the advantage that a distribution drawing of the microstructure does not need to be defined by using a mask plate; compared with the ordinary wet etching and dry etching, the method has the advantages that the corrosion selectivity is good, the etching region is completely determined by a femtosecond laser processing region, and no sidewise underetching exists; and a silicon slot with high depth-to-width ratio and large depth can be obtained during deep silicon slot processing. The method disclosed by the invention can be applied to a micro-electro-mechanical system.
Description
Technical field
The invention belongs to micromechanics electronic system (MEMS) and semiconductor integrated circuit technical field, relate to a kind of processing method of silicon microstructure, especially a kind of dark silicon groove processing method based on femtosecond laser processing and wet etching.
Background technology
In the processing of semiconductor devices and micromechanics electronic system, the main wet etching that adopts processes micro-nano structure with being dry-etched on the silicon at present.Wet etching and dry etching generally need adopt mask definition etch areas.The solution that wet etching utilization energy and silicon carry out chemical reaction carries out etching to silicon, adopts alkali (KOH, NaOH etc.) or acid (HF and HNO usually
3Mixed solution etc.) solution.Dry etching is that the effect that utilizes plasma to pass through chemistry or physics realizes etching to silicon.Anisotropic dry etching is the topmost method of dark silicon groove of processing high-aspect-ratio at present.
Has important use in isolation channel, micro-fluidic chip and the MEMS device of the dark silicon groove of high-aspect-ratio in semiconductor devices.For example in body silicon MEMS device, the electricity of micro-structural and circuit part is isolated and be interconnected is a kind of very important technology.Because bulk silicon technological and traditional cmos process are incompatible, the silicon isolation channel that forms high-aspect-ratio becomes the technological problems that needs to be resolved hurrily.Generally require this isolation channel degree of depth to reach 20～100 μ m, depth-to-width ratio is greater than 25:1.Usually adopt the method for deep reaction ion etching (DRIE) to process dark silicon groove.The DRIE processing method adopts photoetching technique to define the groove figure earlier, utilizes inductively coupled plasma (ICP) lithographic technique to carry out etching and passivation repeatedly then, up to processing enough dark silicon of high aspect ratio groove.The depth-to-width ratio of present this method etch silicon groove has reached 40:1.Yet this method technology is more numerous and diverse.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of silicon microstructure processing method based on femtosecond laser processing and wet etching is provided, it adopts the mode of femtosecond laser irradiation to define etch areas, and the method for recycling wet etching etches silicon microstructure.This method not only operation is more simple, and does not need mask to define etch areas.
The objective of the invention is to solve by the following technical programs:
This silicon microstructure processing method based on femtosecond laser processing and wet etching is to utilize femtosecond laser scanning monocrystalline silicon substrate in the oxygen-containing gas atmosphere, induce silicon to produce variations in refractive index at scanning area, remove the variations in refractive index district by the hydrofluoric acid wet etching again and form silicon microstructure.
Further, above method is specifically carried out according to following steps:
(1) selects monocrystalline silicon substrate for use, in acetone, alcohol and deionized water, clean successively;
(2) in the oxygen-containing gas atmosphere, utilize femtosecond laser in the distribution pattern of silicon scanning definition micro-structural, make the scanning area refraction index changing;
(3) silicon chip after the femtosecond laser processing is carried out the auxiliary corrosion of ultrasonic wave in hydrofluoric acid, remove the variations in refractive index zone, form silicon microstructure;
(4) silicon chip after the hydrofluoric acid corrosion is cleaned in deionized water.
Further, above-mentioned monocrystalline silicon substrate be＜100,＜111,＜110〉crystal orientation silicon chip.
Further, in the above step (2), described oxygen-containing gas is selected air.
In the above-mentioned steps (2), utilize femtosecond laser scanning monocrystalline silicon substrate within it portion form oxygen containing variations in refractive index zone, surface laser is removed the degree of depth less than 5 microns.
In the above-mentioned steps (2), the variations in refractive index regional depth that the femtosecond laser irradiation produces and width are by femtosecond laser energy, focused condition and the sweep speed control of irradiation; The degree of depth in variations in refractive index zone is more than 200 microns.
Compared with prior art, the present invention has following beneficial effect:
The silicon microstructure processing method technology that the present invention is based on femtosecond laser processing and wet etching is simple, and compared with prior art, it does not need to use the distribution pattern of mask plate definition micro-structural; Hydrofluoric acid only carries out chemical reaction with the variations in refractive index zone, and with respect to common wet method and dry etching, it is selectively good to corrode, and etch areas is determined by the femtosecond laser processing region fully, do not have the side direction undercutting; In the processing of dark silicon groove, can obtain depth-to-width ratio height, silicon groove that the degree of depth is big.The present invention is lower with respect to the needed laser energy of method of the direct etch silicon groove of femtosecond laser in the prior art.Method of the present invention can be applicable to the micromechanics electronic system.
Description of drawings
Fig. 1 is the processing unit (plant) figure that this processing method adopts;
Fig. 2 is etch silicon micro-structural schematic flow sheet of the present invention;
Fig. 3 is side SEM (SEM) image of femtosecond laser scanning back silicon in the inventive method process and SEM image and the elements are contained result who etches silicon flute profile looks;
The shape appearance figure of the silicon groove that Fig. 4 finally processes for embodiment 2;
The shape appearance figure of the silicon groove that Fig. 5 finally processes for embodiment 3.
Wherein, 1 is monocrystalline silicon substrate; 2 is microcobjective; 3 is femtosecond laser; 4 induce for femtosecond laser and to produce the variations in refractive index zone; 5 is HF solution; 6 is deionized water; 7 is computer; 8 is the three-D electric translation stage; 9 is CCD.
The specific embodiment
The silicon microstructure processing method that the present invention is based on femtosecond laser processing and wet etching is to utilize femtosecond laser scanning monocrystalline silicon substrate in the oxygen-containing gas atmosphere, induce silicon generation variations in refractive index rather than directly remove silicon materials at scanning area, remove the variations in refractive index district by the hydrofluoric acid wet etching again and form silicon microstructure.The present invention is applicable to the monocrystalline silicon substrate in various crystal orientation, the present invention is preferred＜and 100 〉,＜111,＜110〉crystal orientation silicon chip.
The concrete steps of this method are carried out according to following steps:
(1) selects monocrystalline silicon substrate for use, in acetone, alcohol and deionized water, clean successively;
(2) in air or other oxygen-containing gas atmosphere, utilize femtosecond laser in the distribution pattern of silicon chip scanning definition micro-structural, scanning area generation refraction index changing, and be not directly removed or the only a small amount of removal in surface; In this step, utilize femtosecond laser scanning monocrystalline silicon substrate within it portion form oxygen containing variations in refractive index zone, surface laser is removed the degree of depth below 5 microns.And the variations in refractive index regional depth that the femtosecond laser irradiation produces and width are by femtosecond laser energy, focused condition and the sweep speed control of irradiation; The degree of depth in variations in refractive index zone is more than 200 microns.
(3) silicon chip after the femtosecond laser processing is carried out the auxiliary corrosion of ultrasonic wave in hydrofluoric acid.The time of the auxiliary corrosion of ultrasonic wave is relevant with the variations in refractive index zone that step (2) femtosecond laser induces.Typical case's time is 20-40min, but is not limited thereto scope.Temperature is at 20 ℃ but be not limited thereto temperature when corrosion in hydrofluoric acid.The concentration of hydrofluoric acid is about 20%, but is not limited only to this concentration.
(4) silicon chip after the hydrofluoric acid solution corrosion is cleaned in deionized water.
After finishing above step, the method that also can adopt wet etching is further improved the silicon microstructure of etching.
Below in conjunction with drawings and Examples the present invention is done and to describe in further detail:
Fig. 1 is for realizing a kind of processing unit (plant) schematic diagram of the present invention, it is made up of microcobjective 2, three-D electric translation stage 8, computer 7, femtosecond laser 3., monocrystalline silicon substrate 1 is placed on the three-D electric translation stage 8, computer 7 and three-D electric translation stage 8 and the CCD that is arranged on microcobjective 2 tops are connected, and femtosecond laser 3 is radiated on the monocrystalline silicon substrate 1 after microcobjective 2 focuses on.
Utilize device shown in Figure 1, provide several embodiments of the present invention below in conjunction with accompanying drawing:
Present embodiment is example to process dark silicon groove, and is specific as follows:
Original material: the n type single crystal silicon sheet of single-sided polishing,＜100〉crystal orientation, thickness 500 μ m.
The detailed embodiment of preparation process of the dark silicon groove of high-aspect-ratio is described below:
(1) utilizes acetone, alcohol and deionized water that monocrystalline silicon substrate 1 is carried out the auxiliary cleaning of ultrasonic wave successively, after the cleaning it is dried up, see Fig. 2 (a).
(2) femtosecond laser 3 pulse widths are 50fs, and power setting is 30mW.Select 10 *, the microcobjective 2 of numerical aperture 0.3, femtosecond laser 3 is focused on the monocrystalline silicon substrate 1 by microcobjective 2, three-D electric translation stage 8 sweep speeds are 2 μ m/s.Utilize femtosecond laser 3 to scan the distribution pattern of groove at silicon chip, see Fig. 2 (b).Femtosecond laser 3 is induced at scanning area and is produced variations in refractive index zone 4, and femtosecond laser 3 is at the about 5 μ m of the irradiation area surface removal degree of depth, the dark 270 μ m in variations in refractive index zone, and its sem photograph is shown in Fig. 3 (a).
(3) monocrystalline silicon piece after the laser scanning is carried out the auxiliary corrosion of ultrasonic wave in 20%HF solution 5, etching time 20min sees Fig. 2 (c).Femtosecond laser 3 induces the variations in refractive index zone of generation to be corroded, and forms the silicon groove, sees Fig. 2 (d).After finishing, corrosion utilize the silicon chip after 6 pairs of HF solution of deionized water 5 corrode to carry out ultrasonic cleaning.
Fig. 3 (a) is the pattern of the silicon groove that finally processes.As can be seen from the figure, the degree of depth of groove is 270 μ m, and depth-to-width ratio is 36:1, can satisfy the demand of isolation channel.Fig. 3 (b) is that the elemental composition of machine silicon groove is measured, and around the silicon groove of final processing element silicon is only arranged, and does not have the pollution of other element.
Original material: the n type single crystal silicon sheet of single-sided polishing,＜100〉crystal orientation, thickness 500 μ m.
(1) respective process of the cleaning reference example 1 of monocrystalline silicon substrate 1.
(2) respective process of the process reference example 1 of femtosecond laser 3 scanning monocrystalline silicon substrates 1, parameter is: femtosecond laser 3 pulse widths are 50fs, power setting is 30mW; Select 50 *, the microcobjective 2 of numerical aperture 0.5; Three-D electric translation stage 8 sweep speeds are 2 μ m/s.
(3) respective process of the corrosion reference example 1 of femtosecond laser 3 scanning back silicon chips.
(4) respective process of the cleaning reference example 1 of corrosion back silicon chip.
The pattern of the silicon groove that Fig. 4 finally processes for embodiment 2.As can be seen from the figure, the degree of depth of groove is 100 μ m, and depth-to-width ratio is 8.5:1.
Original material: the n type single crystal silicon sheet of single-sided polishing,＜100〉crystal orientation, thickness 500 μ m.
(1) respective process of the cleaning reference example 1 of monocrystalline silicon substrate 1.
(2) respective process of the process reference example 1 of femtosecond laser 3 scanning monocrystalline silicon substrates 1, parameter is: femtosecond laser 3 pulse widths are 50fs, power setting is 40mW; Select 10 *, the microcobjective 2 of numerical aperture 0.3; Three-D electric translation stage 8 sweep speeds are 2 μ m/s.
(3) respective process of the corrosion reference example 1 of femtosecond laser 3 scanning back silicon chips.
(4) respective process of the cleaning reference example 1 of corrosion back silicon chip.
The pattern of the silicon groove that Fig. 5 finally processes for embodiment 3.As can be seen from the figure, the degree of depth of groove is 285 μ m, and depth-to-width ratio is 44:1.
Claims (6)
1. handle based on femtosecond laser and the silicon microstructure processing method of wet etching for one kind, it is characterized in that: in the oxygen-containing gas atmosphere, utilize femtosecond laser scanning monocrystalline silicon substrate, induce silicon to produce variations in refractive index at scanning area, remove the variations in refractive index district by the hydrofluoric acid wet etching again and form micro-structural at silicon face.
2. according to claim 1ly handle and the silicon microstructure processing method of wet etching based on femtosecond laser, it is characterized in that this method is specifically carried out according to following steps:
(1) selects monocrystalline silicon substrate for use, in acetone, alcohol and deionized water, clean successively;
(2) in the oxygen-containing gas atmosphere, utilize femtosecond laser in the distribution pattern of silicon scanning definition micro-structural, make the refraction index changing of scanning area silicon;
(3) silicon chip after the femtosecond laser processing is carried out the auxiliary corrosion of ultrasonic wave in hydrofluoric acid, remove the variations in refractive index zone, form micro-structural at silicon face;
(4) silicon chip after the hydrofluoric acid corrosion is cleaned in deionized water.
3. according to claim 1 and 2ly to handle and the silicon microstructure processing method of wet etching based on femtosecond laser, it is characterized in that, described monocrystalline silicon substrate is＜100 〉,＜111,＜110〉crystal orientation silicon chip.
4. the silicon microstructure processing method based on femtosecond laser processing and wet etching according to claim 2 is characterized in that, in the step (2), described oxygen-containing gas is selected air.
5. according to claim 2ly handle and the silicon microstructure processing method of wet etching based on femtosecond laser, it is characterized in that, in the step (2), utilize femtosecond laser scanning monocrystalline silicon substrate within it portion form oxygen containing variations in refractive index zone, surface laser is removed the degree of depth less than 5 microns.
6. according to claim 2ly handle and the silicon microstructure processing method of wet etching based on femtosecond laser, it is characterized in that, in the step (2), the variations in refractive index regional depth that the femtosecond laser irradiation produces and width are by femtosecond laser energy, focused condition and the sweep speed control of irradiation; The degree of depth in variations in refractive index zone is more than 200 microns.
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| CN106735947A (en) * | 2016-11-30 | 2017-05-31 | 北京理工大学 | A kind of method of efficiently controllable processing bulk silicon micro-nano structure |
| CN106744662A (en) * | 2017-01-12 | 2017-05-31 | 北京理工大学 | A kind of method that utilization dynamic control prepares silicon nanowire structure |
| CN109037026A (en) * | 2017-06-09 | 2018-12-18 | 中国科学院上海高等研究院 | Epitaxial layer shifts monocrystalline silicon seed crystal array substrate and preparation method thereof |
| CN109592685A (en) * | 2018-12-07 | 2019-04-09 | 西南交通大学 | A kind of laser ablation and electrochemical anodic oxidation combine the method for preparing porous silicon |
| CN110534880A (en) * | 2019-09-04 | 2019-12-03 | 暨南大学 | Single nanoparticle light scattering electricity regulation antenna and the method for preparation, electricity regulation |
| CN110735186A (en) * | 2018-07-18 | 2020-01-31 | 李俊豪 | Method for manufacturing biomedical chip |
| CN113247859A (en) * | 2021-05-13 | 2021-08-13 | 北京理工大学 | Method for preparing crack type nano gap structure based on femtosecond laser |
| CN115535959A (en) * | 2022-11-23 | 2022-12-30 | 山东大学 | Wet etching auxiliary femtosecond laser processing method for monocrystalline silicon microstructure array |
| CN117285002A (en) * | 2023-11-23 | 2023-12-26 | 华东理工大学 | Method for rapidly manufacturing silicon micro-channel by laser induction and wet etching |
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| CN106735947A (en) * | 2016-11-30 | 2017-05-31 | 北京理工大学 | A kind of method of efficiently controllable processing bulk silicon micro-nano structure |
| CN106744662A (en) * | 2017-01-12 | 2017-05-31 | 北京理工大学 | A kind of method that utilization dynamic control prepares silicon nanowire structure |
| CN109037026A (en) * | 2017-06-09 | 2018-12-18 | 中国科学院上海高等研究院 | Epitaxial layer shifts monocrystalline silicon seed crystal array substrate and preparation method thereof |
| CN110735186A (en) * | 2018-07-18 | 2020-01-31 | 李俊豪 | Method for manufacturing biomedical chip |
| CN109592685B (en) * | 2018-12-07 | 2020-05-19 | 西南交通大学 | Method for preparing porous silicon by combining laser etching and electrochemical anodic oxidation |
| CN109592685A (en) * | 2018-12-07 | 2019-04-09 | 西南交通大学 | A kind of laser ablation and electrochemical anodic oxidation combine the method for preparing porous silicon |
| CN110534880A (en) * | 2019-09-04 | 2019-12-03 | 暨南大学 | Single nanoparticle light scattering electricity regulation antenna and the method for preparation, electricity regulation |
| CN110534880B (en) * | 2019-09-04 | 2020-06-26 | 暨南大学 | Single nanoparticle light scattering electric control antenna and preparation and electric control methods thereof |
| CN113247859A (en) * | 2021-05-13 | 2021-08-13 | 北京理工大学 | Method for preparing crack type nano gap structure based on femtosecond laser |
| CN115535959A (en) * | 2022-11-23 | 2022-12-30 | 山东大学 | Wet etching auxiliary femtosecond laser processing method for monocrystalline silicon microstructure array |
| CN115535959B (en) * | 2022-11-23 | 2023-04-11 | 山东大学 | Wet etching auxiliary femtosecond laser processing method for monocrystalline silicon microstructure array |
| CN117285002A (en) * | 2023-11-23 | 2023-12-26 | 华东理工大学 | Method for rapidly manufacturing silicon micro-channel by laser induction and wet etching |
| CN117285002B (en) * | 2023-11-23 | 2024-02-23 | 华东理工大学 | Method for rapidly manufacturing silicon micro-channel by laser induction and wet etching |
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