CN104966670A - Monocrystalline silicon etching method and etching solution - Google Patents
Monocrystalline silicon etching method and etching solution Download PDFInfo
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- CN104966670A CN104966670A CN201510353482.3A CN201510353482A CN104966670A CN 104966670 A CN104966670 A CN 104966670A CN 201510353482 A CN201510353482 A CN 201510353482A CN 104966670 A CN104966670 A CN 104966670A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
Abstract
The invention provides a monocrystalline silicon etching method and an etching solution. The etching method comprises steps: a layer of silicon oxide firstly grows on the surface of a monocrystalline silicon wafer in a thermal oxidation method; a to-be-etched pattern is then formed on the surface of the monocrystalline silicon wafer in a photoetching method; silicon oxide on the surface of the to-be-etched pattern on the monocrystalline silicon wafer are corroded clearly; and the monocrystalline silicon wafer is immersed in a monocrystalline silicon etching solution after heating to complete etching. The etching solution is a compound comprising tetramethylammonium hydroxide, Triton X-100, isopropanol and water. The etched object is monocrystalline silicon (100). According to the monocrystalline silicon etching solution and the etching method of the invention, the depth ratio of convex side etching to etching can reach 0.39, and etching surface roughness is 1.27nm. Through adjusting the content of each component of the etching solution of the invention, etching morphology can be effectively controlled, and processing of a high-precision micro structure is realized. The monocrystalline silicon etching solution is compatible with CMOS, the etching depth can be precisely controlled, toxicity is low, and pollution is low.
Description
Technical field
The invention belongs to microelectromechanical systems field, be specifically related to a kind of monocrystalline silicon lithographic method and etching liquid.
Background technology
In MEMS (micro electro mechanical system) technique, the wet etching technique that the anisotropic etching characteristic according to monocrystalline silicon grows up has played huge effect in making microdevice, particularly inertia device are as the process of accelerometer.Lithographic technique is mainly divided into dry etching and wet etching.The development of these two kinds of lithographic techniques is always along with the progress of silicon-base miniature transducer and actuator.Compare with the dry etching such as reactive ion etching (RIE, Reactive-Ion Etching), the etching depth of wet etching technique is homogeneous, and three-dimensional structure is enriched, and production efficiency is high, and technique manufacturing process is relatively simple, and processing cost is also more cheap.Because the output signal (curtage) of general transducer is very weak, if it is connected to external circuit, then the impact of parasitic capacitance, resistance etc. can thoroughly cover useful signal.Therefore the method for the external treatment circuit of sensor is adopted can not to obtain the transducer be of high quality.Only have both on a single die integrated, just can have best performance.Therefore, the integrated of system is more and more considered in the processing of actual MEMS (micro electro mechanical system).Tetramethylammonium hydroxide TMAH is a kind of anisotropic etching liquid with excellent etching performance, selectivity is good, hypotoxicity low stain, the most important thing is TMAH and complementary metal oxide semiconductors (CMOS) (CMOS, Complementary Metal Oxide Semiconductor) technique is mutually compatible, meet the development trend of SOC (system on a chip) (SOC, System On A Chip).
In order to improve the etching characteristic of single TMAH etching liquid further; obtain good etching surface and salient angle protection; development of new micro-structural; scientific research personnel proposes and have studied certain methods, as: in single TMAH etching liquid, add metal, additive (mainly surfactant-based additive and alcohol type additive), ultrasonic wave etc.But add metal and can bring impurity into, pollute etching liquid, ultrasonic wave can destroy device architecture.The TMAH wet etching liquid that additive is modified has certain advantage, but still there are some problems, and any one additive selected at present all can not carry out available protecting to salient angle while the smooth etching surface of acquisition.
Summary of the invention
The technical problem that the present invention will solve is to provide a kind of monocrystalline silicon lithographic method, and another technical problem that the present invention will solve is to provide a kind of etching liquid of monocrystalline silicon lithographic method.
The present invention is achieved by the following technical solutions.
A kind of monocrystalline silicon lithographic method, is characterized in, comprises the following steps:
(a). adopt thermal oxidation process to grow the silica of one deck 1 μm of thickness at monocrystalline silicon sheet surface, afterwards at silicon oxide surface coating photoresist, obtain monocrystalline silicon piece to be etched;
(b). scribe figure on the surface of monocrystalline silicon piece to be etched by photoetching method, the pattern line degree of depth, slightly larger than the thickness of photoresist, removes the photoresist on figure;
(c). monocrystalline silicon piece step (b) obtained immerses hydrofluoric acid and ammonium fluoride proportioning is in the solution of 1:4, removes the silica on figure;
(d). monocrystalline silicon piece step (c) obtained, first immerses acetone, removes figure on monocrystalline silicon piece and, with the photoresist of exterior domain, take out subsequently, immerse ethanol and remove the residual acetone of monocrystalline silicon sheet surface, finally take out, by washed with de-ionized water;
(e). the hydrofluoric acid solution of the monocrystalline silicon piece immersion 5% that step (d) is obtained 1 ~ 3 minute, remove the natural oxidizing layer of monocrystalline silicon sheet surface figure, retain figure with the silica of exterior domain, take out subsequently, with washed with de-ionized water, drying;
(f). etching liquid is placed in polytetrafluoroethylcontainer container, adopts water bath heating to control at 70 DEG C ~ 80 DEG C by the etching liquid temperature in container;
G monocrystalline silicon piece that step (e) obtains by () immerses in the etching liquid after step (f) heating water bath, and etch period 2 ~ 3 hours, takes out subsequently, with washed with de-ionized water, drying.
The crystal orientation of the monocrystalline silicon piece in described step (a) is crystal orientation (100).
The etching liquid of monocrystalline silicon lithographic method, is characterized in, described etching liquid comprises following component by weight percentage:
Tetramethylammonium hydroxide 15% ~ 30%
Qu Latong 0 ~ 1%
Isopropyl alcohol 0 ~ 30%
Water 50% ~ 80%.
The content of the Tetramethylammonium hydroxide in described etching liquid is 19% ~ 22%.
The content of the Qu Latong in described etching liquid is 0.1% ~ 0.4%.
The content of the isopropyl alcohol in described etching liquid is 13% ~ 25%.
Determine through lot of experiments, simultaneously containing Tetramethylammonium hydroxide TMAH, the Qu Latong Triton X-100 of proper ratio and the monocrystalline silicon etching liquid of isopropyl alcohol IPA, smooth etching surface and minimum salient angle lateral erosion can be obtained simultaneously.If etching liquid is only containing TMAH and water, not containing Triton X-100 and IPA, not only etching surface is very coarse, and salient angle lateral erosion is also very serious; If etching liquid contains TMAH, Triton X-100 and water, not containing IPA, then etching surface can polish, but salient angle lateral erosion is still more serious; If etching liquid contains TMAH, IPA and water, not containing Triton X-100, etching surface becomes very coarse, but salient angle lateral erosion is very little, substantially can ignore.
In described monocrystalline silicon etching liquid, the purity >99% of Qu Latong Triton X-100, the purity >99% of isopropyl alcohol IPA; Qu Latong Triton X-100 can reduce salient angle lateral erosion ratio; Isopropyl alcohol IPA can improve etching surface smoothness.
In order to prevent the concentration of etching liquid in etching process from changing, polytetrafluoroethylcontainer container is provided with condensation reflux device.
Etching liquid of the present invention controls etch topography by changing additive formula; the lobe shape of the monocrystalline silicon piece after etching and etching surface roughness are changed simultaneously; not only there is smooth etching surface; and salient angle protected effect is obvious; effectively improve convex corner compensation problem; the micro-structural met for embody rule processes the requirement protected roughness and salient angle, for the development of the integrated MEMS (micro electro mechanical system) of high-performance provides technical support.Etching liquid of the present invention changes the conventional wet etching characteristic to monocrystalline silicon, have compatible, simple to operate with CMOS, accurately can control that etching depth, repeatability are strong, hypotoxicity low stain, be easy to realize the advantage of mass.
Accompanying drawing explanation
Fig. 1 is monocrystalline silicon etched features schematic diagram of the present invention;
Fig. 2 is etching result schematic diagram of the present invention;
Fig. 3 is etching result vertical view of the present invention;
Fig. 4 is the profile along Fig. 3 A-A hatching line;
In figure, 1. re-entrant angle inclined-plane, re-entrant angle inclined-plane 64. the 4th, re-entrant angle inclined-plane 63. the 3rd, re-entrant angle 52. second re-entrant angle 53. the 3rd re-entrant angle 54. the 4th re-entrant angle 61. first re-entrant angle inclined-plane 62. second, boss inclined-plane 51. first, boss inclined-plane 44. the 4th, boss inclined-plane 43. the 3rd, etching surface 2. boss 31. first salient angle 32. second salient angle 33. the 3rd salient angle 34. the 4th salient angle 41. first boss inclined-plane 42. second.
Embodiment
Fig. 1 is etched features schematic diagram in monocrystalline silicon etching liquid of the present invention, and Fig. 2 is etching result schematic diagram of the present invention, and Fig. 3 is etching result vertical view of the present invention, and Fig. 4 is the profile of the A-A hatching line along Fig. 3.
Below in conjunction with accompanying drawing 1 ~ Fig. 4, the invention will be further described.
In embodiment and comparative example, represent that salient angle protects situation with salient angle lateral erosion and etching depth ratio, ratio is less, and salient angle protected effect is better; Represent the smooth surface degree after etching by etching surface roughness, roughness value is less, and etching surface smoothness is better.
Embodiment 1
In the etching liquid of embodiment 1, each constituent content is 0.2% for Tetramethylammonium hydroxide TMAH is 19%, Qu Latong Triton X-100 by weight percentage, and isopropyl alcohol IPA is 25%, and all the other are water.Etching object is the monocrystalline silicon piece of resistivity 1 ~ 10 cm, crystal orientation (100).First adopt thermal oxidation process to grow the silica of one deck 1 μm of thickness at monocrystalline silicon sheet surface, afterwards at silicon oxide surface coating photoresist, obtain monocrystalline silicon piece to be etched; Scribe figure on the surface of monocrystalline silicon piece to be etched by photoetching method, the pattern line degree of depth, slightly larger than the thickness of photoresist, removes the photoresist on figure; It is in the solution of 1:4 that the monocrystalline silicon piece of acquisition is immersed hydrofluoric acid and ammonium fluoride proportioning, removes the silica on figure; Immerse acetone after taking-up, remove figure on monocrystalline silicon piece and, with the photoresist of exterior domain, take out subsequently, immerse ethanol and remove the residual acetone of monocrystalline silicon sheet surface, finally take out, by washed with de-ionized water; The monocrystalline silicon piece obtained is immersed the hydrofluoric acid solution 1 minute of 5%, remove the natural oxidizing layer on monocrystalline silicon piece figure, retain figure with the silica of exterior domain, take out subsequently, with washed with de-ionized water, drying; Etching liquid is placed in polytetrafluoroethylcontainer container, adopts water bath heating to control at 70 DEG C by the etching liquid temperature in container; Immersed in the etching liquid after heating water bath by the monocrystalline silicon piece obtained, etch period 2 hours, takes out subsequently, with washed with de-ionized water, drying.Monocrystalline silicon piece has etched rear light microscope, scanning electron microscopy (SEM, scanning electron microscope) or scanning probe microscopy (AFM, atomic force microscope) observes salient angle lateral erosion and etching depth compares and etching surface roughness.The monocrystalline silicon piece listing the present embodiment in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
The etch topography of the monocrystalline silicon piece that etching obtains has etching surface 1, boss 2; Wherein, the roughness of etching surface 1 is 1.09; The first salient angle 31, second salient angle 32 in protected boss 2, the 3rd salient angle 33, the 4th salient angle 34 lateral erosion area are all very little, and salient angle lateral erosion is 0.61 with etching depth ratio.
The first boss inclined-plane 42, boss inclined-plane 41, second in described boss 2, the 3rd boss inclined-plane 43, the 4th boss inclined-plane 44 are all 54.7 ° with etching surface 1 angle.
First re-entrant angle inclined-plane 62, re-entrant angle inclined-plane 61, second of described composition first re-entrant angle 51, second re-entrant angle 52, the 3rd re-entrant angle 53, the 4th re-entrant angle 54, the 3rd re-entrant angle inclined-plane 63, the 4th re-entrant angle inclined-plane 64 are all 54.7 ° with etching surface 1 angle.
Embodiment 2
The difference of the present embodiment and embodiment 1 is, each constituent content of monocrystalline silicon etching liquid is 0.3% for Tetramethylammonium hydroxide TMAH is 20%, Qu Latong Triton X-100 by weight percentage, and isopropyl alcohol IPA is 19%, and all the other are water.The hydrofluoric acid solution of monocrystalline silicon piece immersion 5% 2 minutes, etching liquid temperature is 75 ° of C, and etch period is 2.5 hours.The monocrystalline silicon piece listing the present embodiment in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Embodiment 3
The difference of the present embodiment and embodiment 1 is, each constituent content of monocrystalline silicon etching liquid is 0.3% for Tetramethylammonium hydroxide TMAH is 22%, Qu Latong Triton X-100 by weight percentage, and isopropyl alcohol IPA is 13%, and all the other are water.The hydrofluoric acid solution of monocrystalline silicon piece immersion 5% 3 minutes, etching liquid temperature is 80 DEG C, and etch period is 2.5 hours.The monocrystalline silicon piece listing the present embodiment in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Embodiment 4
The difference of the present embodiment and embodiment 1 is, each constituent content of monocrystalline silicon etching liquid is 0.1% for Tetramethylammonium hydroxide TMAH is 20%, Qu Latong Triton X-100 by weight percentage, and isopropyl alcohol IPA is 19%, and all the other are water.Etching liquid temperature is 70 DEG C, and etch period is 3 hours.The monocrystalline silicon piece listing the present embodiment in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Embodiment 5
The difference of the present embodiment and embodiment 1 is, each constituent content of monocrystalline silicon etching liquid is 0.4% for Tetramethylammonium hydroxide TMAH is 19%, Qu Latong Triton X-100 by weight percentage, and isopropyl alcohol IPA is 25%, and all the other are water.Etching liquid temperature is 70 DEG C, and etch period is 2 hours.The monocrystalline silicon piece listing the present embodiment in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Comparative example 1
In the etching liquid of comparative example 1, by weight percentage for Tetramethylammonium hydroxide TMAH is 30%, all the other are water.Etching object is the monocrystalline silicon piece of resistivity 1 ~ 10 cm, crystal orientation (100).First adopt thermal oxidation process to grow the silica of one deck 1 μm of thickness at monocrystalline silicon sheet surface, afterwards at silicon oxide surface coating photoresist, obtain monocrystalline silicon piece to be etched; Scribe figure on the surface of monocrystalline silicon piece to be etched by photoetching method, the pattern line degree of depth, slightly larger than the thickness of photoresist, removes the photoresist on figure; It is in the solution of 1:4 that the monocrystalline silicon piece of acquisition is immersed hydrofluoric acid and ammonium fluoride proportioning, removes the silicon oxide layer on figure; Immerse acetone after taking-up, remove figure on monocrystalline silicon piece and, with the photoresist of exterior domain, take out subsequently, immerse ethanol and remove the residual acetone of monocrystalline silicon sheet surface, finally take out, by washed with de-ionized water; The monocrystalline silicon piece obtained is immersed the hydrofluoric acid solution 1 minute of 5%, remove monocrystalline silicon sheet surface natural oxidizing layer, take out subsequently, with washed with de-ionized water, drying; Etching liquid is placed in polytetrafluoroethylcontainer container, adopts water bath heating to control at 70 DEG C by the etching liquid temperature in container; Immersed in the etching liquid after heating water bath by the monocrystalline silicon piece obtained, etch period 2 hours, takes out subsequently, with washed with de-ionized water, drying.The monocrystalline silicon piece listing this comparative example in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Comparative example 2
This comparative example 2 with the difference of comparative example 1 is, each constituent content of monocrystalline silicon etching liquid is 0.5% for Tetramethylammonium hydroxide TMAH is 20%, Qu Latong Triton X-100 by weight percentage, and all the other are water.The hydrofluoric acid solution of monocrystalline silicon piece immersion 5% 2 minutes, etching liquid temperature is 75 DEG C, and etch period is 2 hours.The monocrystalline silicon piece listing this comparative example 2 in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Comparative example 3
This comparative example 3 with the difference of comparative example 1 is, each constituent content of monocrystalline silicon etching liquid is 15% for Tetramethylammonium hydroxide TMAH by weight percentage, and isopropyl alcohol IPA is 13%, and all the other are water.The hydrofluoric acid solution of monocrystalline silicon piece immersion 5% 3 minutes, etching liquid temperature is 80 DEG C, and etch period is 2.5 hours.The monocrystalline silicon piece listing this comparative example 3 in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Comparative example 4
This comparative example 4 with the difference of comparative example 1 is, each constituent content of monocrystalline silicon etching liquid is 1% for Tetramethylammonium hydroxide TMAH is 25%, Qu Latong Triton X-100 by weight percentage, and isopropyl alcohol IPA is 30%, and all the other are water.The hydrofluoric acid solution of monocrystalline silicon piece immersion 5% 2 minutes, etching liquid temperature is 80 DEG C, and etch period is 3 hours.The monocrystalline silicon piece listing this comparative example 4 in table 1 immerses the time of 5% hydrofluoric acid, etching liquid temperature, etch period, salient angle lateral erosion and etching depth ratio and etching surface roughness.
Table 1
Claims (6)
1. a monocrystalline silicon lithographic method, is characterized in that, comprises the following steps:
(a). adopt thermal oxidation process to grow the silica of one deck 1 μm of thickness at monocrystalline silicon sheet surface, afterwards at silicon oxide surface coating photoresist, obtain monocrystalline silicon piece to be etched;
(b). scribe figure on the surface of monocrystalline silicon piece to be etched by photoetching method, the pattern line degree of depth is greater than the thickness of photoresist, removes the photoresist on figure;
(c). monocrystalline silicon piece step (b) obtained immerses hydrofluoric acid and ammonium fluoride proportioning is in the solution of 1:4, removes the silica on figure;
(d). monocrystalline silicon piece step (c) obtained, first immerses acetone, removes figure on monocrystalline silicon piece and, with the photoresist of exterior domain, take out subsequently, immerse ethanol and remove the residual acetone of monocrystalline silicon sheet surface, finally take out, by washed with de-ionized water;
(e). the hydrofluoric acid solution of the monocrystalline silicon piece immersion 5% that step (d) is obtained 1 ~ 3 minute, remove the natural oxidizing layer of monocrystalline silicon sheet surface figure, retain figure with the silica of exterior domain, take out subsequently, with washed with de-ionized water, drying;
(f). etching liquid is placed in polytetrafluoroethylcontainer container, adopts water bath heating to control at 70 DEG C ~ 80 DEG C by the etching liquid temperature in container;
(g). monocrystalline silicon piece step (e) obtained immerses in the etching liquid after step (f) heating water bath, and etch period 2 ~ 3 hours, takes out subsequently, with washed with de-ionized water, drying.
2. monocrystalline silicon lithographic method according to claim 1, is characterized in that: the crystal orientation of the monocrystalline silicon piece in step (a) is crystal orientation (100).
3. a monocrystalline silicon etching liquid for claim 1, is characterized in that: described etching liquid comprises following component by weight percentage:
Tetramethylammonium hydroxide 15% ~ 30%
Qu Latong 0 ~ 1%
Isopropyl alcohol 0 ~ 30%
Water 50% ~ 80%.
4. monocrystalline silicon etching liquid according to claim 3, wherein the content of Tetramethylammonium hydroxide is 19% ~ 22%.
5. monocrystalline silicon etching liquid according to claim 3, wherein the content of Qu Latong is 0.1% ~ 0.4%.
6. monocrystalline silicon etching liquid according to claim 3, wherein the content of isopropyl alcohol is 13% ~ 25%.
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| CN107316829A (en) * | 2017-07-06 | 2017-11-03 | 中北大学 | Gas phase lithographic method and vapor etching device based on TMAH |
| CN107976723A (en) * | 2017-12-25 | 2018-05-01 | 中国工程物理研究院激光聚变研究中心 | Optical element processing unit (plant) and its system |
| CN109700440A (en) * | 2018-12-18 | 2019-05-03 | 中北大学 | Flexible wearable sensor and its corresponding wearable device and preparation method |
| CN111876157A (en) * | 2020-06-30 | 2020-11-03 | 镇江润晶高纯化工科技股份有限公司 | Preparation and etching method of TMAH etching solution |
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