CN110526205A - A kind of method of plasma etching auxiliary laser processing silicon carbide - Google Patents
A kind of method of plasma etching auxiliary laser processing silicon carbide Download PDFInfo
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- CN110526205A CN110526205A CN201910793890.9A CN201910793890A CN110526205A CN 110526205 A CN110526205 A CN 110526205A CN 201910793890 A CN201910793890 A CN 201910793890A CN 110526205 A CN110526205 A CN 110526205A
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- silicon carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00388—Etch mask forming
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00531—Dry etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00539—Wet etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00841—Cleaning during or after manufacture
- B81C1/00849—Cleaning during or after manufacture during manufacture
Abstract
A kind of method of plasma etching auxiliary laser processing silicon carbide, the irradiation ablation of material is acted on first with femtosecond laser, realize that the roughing of silicon carbide quickly removes, then with the impurity of hydrofluoric acid and nitric acid mixed solution removal finished surface, plasma etching retrofit is carried out again, obtains expected micro-nano structure；The present invention realizes the high-effect high-quality material removal etching of silicon carbide, have it is high in machining efficiency, it is at low cost, the advantages that machined surface quality.
Description
Technical field
The invention belongs to MEMS (MEMS) technical field of micro and nano fabrication, and in particular to a kind of plasma etching is auxiliary
The method for helping laser processing silicon carbide.
Background technique
High-temperature-resistance pressure sensor has broad application prospects in defence and military field, such as in various engine cavity bodies
The heat-resisting cavity and surface each section such as pressure measurement, jet engine, rocket, guided missile, satellite pressure measurement, especially in force
In device system, high-temp pressure sensor be dynamical system it is indispensable.And used at present is mostly on silicon substrate or insulator
The MEMS pressure sensor of silicon (SOI) substrate, in the high-temperature severe environment pressure measurement more than 600 DEG C, frequently with pressure guiding pipe
Or indirect measurement is realized to the mode of sensor installation water-cooled jacket.As the Typical Representative of third generation wide bandgap semiconductor, carbonization
The forbidden bandwidth of silicon is nearly 3 times of silicon, has the advantages such as high-melting-point, high rigidity, acid-alkali-corrosive-resisting, has high-temperature severe environment
The great potential of lower pressure measurement, was widely studied in recent years.And the above-mentioned material advantage of ARTSemiconductor silicon carbide is also used as to it
MEMS sensor base material brings great challenge, is mainly reflected in lithography difficulty.For a long time, by means of from silicon
The etching technics that base MEMS transplanting comes realizes the plasma etching of silicon carbide by the optimization of machined parameters substantially, however
Lower etch rate limits the further development of silicon carbide-based pyrostat always, then, and has researched and proposed and makes
Silicon carbide is processed with modes such as picosecond lasers, and processing result and surface quality are all to be improved.Therefore, it is directed at present
The high-effect high-quality material removal process of silicon carbide is still in the exploratory stage.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of plasma etching auxiliary to swash
Light process silicon carbide method, realize silicon carbide high-effect high-quality material removal, have it is high in machining efficiency, it is at low cost, add
The advantages that work surface quality is preferable.
In order to achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of method of plasma etching auxiliary laser processing silicon carbide burns the irradiation of material first with femtosecond laser
Erosion effect, realizes that the roughing of silicon carbide quickly removes, and then removes the miscellaneous of finished surface with hydrofluoric acid and nitric acid mixed solution
Matter, then plasma etching retrofit is carried out, obtain expected micro-nano structure.
A kind of method of plasma etching auxiliary laser processing silicon carbide, comprising the following steps:
Step 1, it cleans: silicon carbide whisker disk is successively impregnated in acetone and ethanol solution, be cleaned by ultrasonic 20-30
Minute；
Step 2, Gold Films Irradiated by Femtosecond Laser is processed: the silicon carbide whisker disk that step 1 was cleaned is placed in femtosecond laser processing
On workbench, according to the good machining path of program setting, machined parameters are adjusted, laser is focused on the surface of the material and starts to scan
Processing；
Step 3, corrode: the silicon carbide whisker disk laser machined by step 2 is immersed to the mixing of hydrofluoric acid and nitric acid
In solution, first it is cleaned by ultrasonic 15-20 minutes, then stands 24 hours；
Step 4, it cleans: the silicon carbide whisker disk that step 3 was corroded successively is impregnated in acetone and ethanol solution,
Ultrasonic cleaning 15-30 minutes, deionized water are dried after rinsing；
Step 5, the sic wafer on piece pattern mask cleaned according to micro-nano technology technique in step 4；
Step 6, plasma etching is carried out to the processed silicon carbide whisker disk of step 5, obtains expected micro-nano structure.
The silicon carbide whisker disk is any one crystal form including 3C, 4H or 6H.
The silicon carbide whisker disk is any crystal orientation.
The processing structure that Gold Films Irradiated by Femtosecond Laser is processed in the step 2 is any one planform that program is realized,
Including circular shape and rectangular shape etc.: for circular shape structure, successively being processed using helical-like path；For rectangle shape
Shape successively removes material using bow vee path V；For other shapes, then uses corresponding program or write new machining path
Program.
The machined parameters that Gold Films Irradiated by Femtosecond Laser is processed in the step 2 include femtosecond laser power, scanning speed, scanning
Line interval and the scanning number of plies etc..
Hydrofluoric acid and nitric acid volumetric concentration be in 40%~70% range in the step 3, and according to volume ratio 1:1
Arbitrary proportion within the scope of~1:5 is mixed to get mixed solution.
The step 6 plasma etching refers to the phase that material removal is realized using plasma bombardment material surface
Close dry etching, including sense coupling (ICP) and reactive ion etching (RIE).
The beneficial effects of the present invention are: the present invention processes femtosecond laser in conjunction with plasma etching, swashed using femtosecond
The high efficiency advantage of light processing quickly removes most of material, then carries out plasma quarter to sample using traditional micro-nano technique
Erosion finishing can modify laser processing gained sample surfaces and perfect；It realizes using silicon carbide as the high rigidity of representative, it is corrosion-resistant
Property material efficient removal, substantially increase the efficiency of silicon carbide-based sensor micro-nano technology, reduce manufacturing cost, push
The research and application of all kinds of silicon carbide-based pyrostats.
Detailed description of the invention
Fig. 1 is the flow chart of the method for the present invention.
Fig. 2 is the part pattern in print hole after the embodiment of the present invention 1 is processed, and figure (a) is to observe under scanning electron microscope
The shape appearance figure arrived；Figure (b) is the shape appearance figure observed under laser confocal microscope.
Fig. 3 is the pattern in print hole after the embodiment of the present invention 2 is processed.
Specific embodiment
The present invention will be described in further detail with reference to the accompanying drawings and embodiments.It should be appreciated that described herein
The specific embodiments are only for explaining the present invention, is not intended to limit the present invention.
Embodiment 1, in the present embodiment, used laser is titanium: sapphire laser, processing is square hole, side
800 μm long, hole depth is different, depends primarily on working power and the scanning number of plies.
Referring to Fig.1, a kind of method of plasma etching auxiliary laser processing silicon carbide, comprising the following steps:
Step 1, it cleans: a piece of 4 cun of N-types conduction 4H-SiC wafer is taken, with a thickness of 340 μm, relative to<1120>crystal orientation
4.0 ° ± 0.5 ° of off-axis, the small-sized print that scribing is cut into 1.5cm × 1cm is spare, by one of print successively in acetone and
It impregnates, is cleaned by ultrasonic 20 minutes in ethanol solution, remove surface impurity pollutant and dry；
Step 2, Gold Films Irradiated by Femtosecond Laser processes square hole: with the quadrangle of normal transparent tape-stripping print, being fixed in dry
On net frosted glass plate, prevent print from moving in laser irradiation process；The frosted glass slide glass of print will be pasted with
It is placed on femtosecond laser processing articles holding table；Titanium: sapphire femto-second laser central wavelength is 800nm, and pulse width is less than
120fs, setting program are that " bow font " path processes square hole, start to process after having debugged processing program；The power of femtosecond laser
Adjustable range is 30mw~80mw, and for scan line spacings from 2 μm~4 μm, scanning speed is 2000 μm/s, 3000 μm/s, 4000 μm/
S, the scanning number of plies are 2~5 layers；
Step 3, corrode: the silicon carbide print laser machined by step 2 is immersed in the mixing of hydrofluoric acid and nitric acid
In solution, first ultrasound 15 minutes, then stand 24 hours；The mixed solution be by volumetric concentration be 68% hydrofluoric acid and
The nitric acid that volumetric concentration is 45% is made after mixing according to the ratio of 1:1；
Step 4, it cleans: after the silicon carbide print that step 3 was corroded takes out, successively using acetone and soaked in absolute ethyl alcohol,
Ultrasonic cleaning 15 minutes, deionized water are dried after rinsing, removal residual acid solution and impurity；
Step 5, the sic wafer on piece pattern mask cleaned according to micro-nano technology technique in step 4；
Step 6: sense coupling (ICP) being carried out to the processed silicon carbide print of step 5, etch thicknesses
It is 40 μm；Sample surface pattern after being processed with optical microscopy, scanning electron microscope and confocal laser scanning microscope,
Working depth and surface roughness are measured, Fig. 2 is the part pattern in print hole after the embodiment of the present invention 1 is processed, and figure (a) is scanning
The shape appearance figure that observed under electron microscope arrives；Figure (b) is the shape appearance figure observed under laser confocal microscope, can be with from Fig. 2
Find out that a kind of method of plasma etching auxiliary laser processing silicon carbide is capable of processing out square hole, and bore edges are relatively advised
Then, hole surface is without obvious uneven.
Embodiment 2, laser employed in the present embodiment are titanium: sapphire laser, processing is circular hole, side length
800 μm of diameter, hole depth is different, depends primarily on working power and the scanning number of plies.
Referring to Fig.1, a kind of method of plasma etching auxiliary laser processing silicon carbide, comprising the following steps:
Step 1, it cleans: taking a piece of semi-insulating 4H-SiC wafer of 4 cun of N-types, with a thickness of 500 μm, crystal orientation<0001>, scribing
The small-sized print for being cut into 1.5cm × 1cm is spare, one kind of is successively impregnated with acetone and ethanol solution, respectively
Ultrasonic cleaning 30 minutes removes surface impurity pollutant and dries；
Step 2, Gold Films Irradiated by Femtosecond Laser processes circular hole: with the quadrangle of normal transparent tape-stripping print, being fixed in dry
On net frosted glass plate, prevent print from moving in laser irradiation process；The frosted glass slide glass of print will be pasted with
It is placed on femtosecond laser processing articles holding table；Titanium: sapphire femto-second laser central wavelength is 800nm, setting program is " spiral shell
Spin line " path processes circular hole, starts to process after having debugged processing program；The power regulating range of femtosecond laser be 400mw~
560mw, scanning speed be 2000 μm/s, 3000 μm/s, 4000 μm/s；
Step 3, corrode: the silicon carbide print laser machined by step 2 is immersed in the mixing of hydrofluoric acid and nitric acid
In solution, first ultrasound 20 minutes, then stand 24 hours；The mixed solution be by volumetric concentration be 68% hydrofluoric acid and
The nitric acid that volumetric concentration is 45% is made after mixing according to the ratio of 1:1；
Step 4, it cleans: after the silicon carbide print that step 3 was corroded takes out, successively using acetone and soaked in absolute ethyl alcohol,
Ultrasonic cleaning 30 minutes, deionized water are dried after rinsing, removal residual acid solution and impurity；
Step 5, the sic wafer on piece pattern mask cleaned according to micro-nano technology technique in step 4；
Step 6: sense coupling (ICP) being carried out to the processed silicon carbide print of step 5, etch thicknesses
It is 40 μm；Sample surface pattern after being processed with optical microscopy, scanning electron microscope and confocal laser scanning microscope,
Working depth and surface roughness are measured, Fig. 3 is to complete the process the pattern of gained circular hole under an optical microscope, can be with from Fig. 3
Find out that a kind of resulting circular hole of method processing of plasma etching auxiliary laser processing silicon carbide is more regular, can effectively remove
High rigidity carbofrax material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Any modifications, equivalent replacements, and improvements etc. done within mind and principle, should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method of plasma etching auxiliary laser processing silicon carbide, it is characterised in that: first with femtosecond laser to material
The irradiation ablation of material acts on, and realizes that the roughing of silicon carbide quickly removes, and is then added with hydrofluoric acid and the removal of nitric acid mixed solution
The impurity on work surface, then plasma etching retrofit is carried out, obtain expected micro-nano structure.
2. a kind of method of plasma etching auxiliary laser processing silicon carbide, which comprises the following steps:
Step 1, it cleans: silicon carbide whisker disk is successively impregnated in acetone and ethanol solution, 15-30 points of ultrasonic cleaning
Clock；
Step 2, Gold Films Irradiated by Femtosecond Laser is processed: the silicon carbide whisker disk that step 1 was cleaned is placed in femtosecond laser processing work
On platform, according to the good machining path of program setting, machined parameters are adjusted, focus laser on the surface of the material and start to scan to add
Work；
Step 3, corrode: the silicon carbide whisker disk laser machined by step 2 is immersed to the mixed solution of hydrofluoric acid and nitric acid
In, first it is cleaned by ultrasonic 15-20 minutes, then stands 24 hours；
Step 4, it cleans: the silicon carbide whisker disk that step 3 was corroded successively is impregnated in acetone and ethanol solution, ultrasound
Cleaning 15-30 minutes, deionized water are dried after rinsing；
Step 5, the sic wafer on piece pattern mask cleaned according to micro-nano technology technique in step 4；
Step 6, plasma etching is carried out to the processed silicon carbide whisker disk of step 5, obtains expected micro-nano structure.
3. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, it is characterised in that:
The silicon carbide whisker disk is any one crystal form including 3C, 4H or 6H.
4. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, it is characterised in that:
The silicon carbide whisker disk is any crystal orientation.
5. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, it is characterised in that:
The processing structure that Gold Films Irradiated by Femtosecond Laser is processed in the step 2 is any one planform that program is realized, including circle
Shape and rectangular shape etc., such as: for circular shape structure, successively processed using helical-like path；For rectangular shape, adopt
Material is successively removed with bow vee path V.
6. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, it is characterised in that:
In the step 2 Gold Films Irradiated by Femtosecond Laser process machined parameters include femtosecond laser power, scanning speed, scan line spacings and
Scan the number of plies.
7. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, it is characterised in that:
Hydrofluoric acid and nitric acid volumetric concentration be in 40%~70% range in the step 3, and according to volume ratio 1:1~1:5 model
Arbitrary proportion in enclosing is mixed to get mixed solution.
8. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, it is characterised in that:
The step 6 plasma etching, which refers to, realizes that the related dry method of material removal is carved using plasma bombardment material surface
Erosion, including sense coupling (ICP) and reactive ion etching (RIE).
9. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, which is characterized in that
The following steps are included:
Step 1, it cleans: a piece of 4 cun of N-types conduction 4H-SiC wafer is taken, with a thickness of 340 μm, relative to<1120>crystal orientation off-axis
4.0 ° ± 0.5 °, the small-sized print that scribing is cut into 1.5cm × 1cm is spare, by one kind of successively in acetone and anhydrous second
Alcohol solution for soaking is cleaned by ultrasonic 15-30 minutes, removes surface impurity pollutant and dries；
Step 2, Gold Films Irradiated by Femtosecond Laser processes square hole: pasting the quadrangle of print with adhesive tape, is fixed in clean hair glass
Glass on piece；The frosted glass slide glass for being pasted with print is placed on femtosecond laser processing articles holding table；Titanium: sapphire femto-second laser
Central wavelength is 800nm, and pulse width is less than 120fs, and setting program is that " bow font " path processes square hole, debugs and processes journey
Start to process after sequence；The power regulating range of femtosecond laser is 30mw~80mw, and scan line spacings are from 2 μm~4 μm, scanning speed
For 2000 μm/s, 3000 μm/s, 4000 μm/s, the scanning number of plies is 2~5 layers；
Step 3, corrode: the silicon carbide print laser machined by step 2 is immersed in the mixed solution of hydrofluoric acid and nitric acid
In, first ultrasound 15 minutes, then stand 24 hours；The mixed solution is the hydrofluoric acid and volume by volumetric concentration for 68%
The nitric acid that concentration is 45% is made after mixing according to the ratio of 1:1；
Step 4, it cleans: after the silicon carbide print that step 3 was corroded takes out, successively using acetone and soaked in absolute ethyl alcohol, ultrasound
Cleaning 15 minutes, deionized water are dried after rinsing, removal residual acid solution and impurity；
Step 5, the sic wafer on piece pattern mask cleaned according to micro-nano technology technique in step 4；
Step 6: sense coupling (ICP) being carried out to the processed silicon carbide print of step 5, etch thicknesses 40
μm。
10. a kind of method of plasma etching auxiliary laser processing silicon carbide according to claim 2, feature exist
In, comprising the following steps:
Step 1, it cleans: taking a piece of semi-insulating 4H-SiC wafer of 4 cun of N-types, with a thickness of 500 μm, crystal orientation<0001>, scribing is cut
It is spare at the small-sized print of 1.5cm × 1cm, one kind of is successively impregnated with acetone and ethanol solution, respectively ultrasound
Cleaning 15-30 minutes removes surface impurity pollutant and dries；
Step 2, Gold Films Irradiated by Femtosecond Laser processes circular hole: pasting the quadrangle of print with adhesive tape, is fixed in clean hair glass
Glass on piece；The frosted glass slide glass for being pasted with print is placed on femtosecond laser processing articles holding table；Titanium: sapphire femto-second laser
Central wavelength is 800nm, setting program is that " helix " path processes circular hole, starts to process after having debugged processing program；Femtosecond
The power regulating range of laser be 400mw~560mw, scanning speed be 2000 μm/s, 3000 μm/s, 4000 μm/s；
Step 3, corrode: the silicon carbide print laser machined by step 2 is immersed in the mixed solution of hydrofluoric acid and nitric acid
In, first ultrasound 15-30 minutes, then stands 24 hours；The mixed solution be by volumetric concentration be 68% hydrofluoric acid and
The nitric acid that volumetric concentration is 45% is made after mixing according to the ratio of 1:1；
Step 4, it cleans: after the silicon carbide print that step 3 was corroded takes out, successively using acetone and soaked in absolute ethyl alcohol, ultrasound
Cleaning 15-30 minutes, deionized water are dried after rinsing, removal residual acid solution and impurity；
Step 5, the sic wafer on piece pattern mask cleaned according to micro-nano technology technique in step 4；
Step 6: sense coupling (ICP) being carried out to the processed silicon carbide print of step 5, etch thicknesses 40
μm。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111477545A (en) * | 2020-04-09 | 2020-07-31 | 浙江大学 | GaN device SiC substrate etching method |
| CN111521070A (en) * | 2020-04-29 | 2020-08-11 | 西安工业大学 | Preparation method of carbon-based low-voltage ignition switch |
| CN111766403A (en) * | 2020-07-20 | 2020-10-13 | 西安交通大学 | Comb micro-accelerometer resisting high-g-value impact and preparation method thereof |
| CN112591707A (en) * | 2020-12-15 | 2021-04-02 | 南方科技大学 | Nano conical array structure and preparation method thereof |
| CN113130305A (en) * | 2021-03-03 | 2021-07-16 | 哈尔滨工业大学 | Method for constructing surface microstructure of silicon carbide single crystal |
| CN115894090A (en) * | 2022-11-17 | 2023-04-04 | 中国工程物理研究院激光聚变研究中心 | Method for preparing high anti-reflection sub-wavelength structure on surface of brittle and hard material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111477545A (en) * | 2020-04-09 | 2020-07-31 | 浙江大学 | GaN device SiC substrate etching method |
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| CN115894090A (en) * | 2022-11-17 | 2023-04-04 | 中国工程物理研究院激光聚变研究中心 | Method for preparing high anti-reflection sub-wavelength structure on surface of brittle and hard material |
| CN115894090B (en) * | 2022-11-17 | 2024-03-22 | 中国工程物理研究院激光聚变研究中心 | Method for preparing high-reflection-resistance sub-wavelength structure on surface of brittle and hard material |
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