CN113526458B - Method for preparing micro-core annular cavity by wet etching silicon - Google Patents
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Classifications
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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
-
- 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
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/30—Imagewise removal using liquid means
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- Engineering & Computer Science (AREA)
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- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Weting (AREA)
Abstract
A method for preparing a micro-core annular cavity by wet etching silicon comprises the following steps: taking a silicon wafer, wherein the surface of the silicon wafer is a silicon dioxide oxide layer, and obtaining a silicon dioxide disc pattern covered with photoresist on the surface of the silicon wafer by using a photoetching and hydrofluoric acid etching method; secondly, wet etching is carried out on the silicon dioxide disc graph covered with the photoresist by using a hydrofluoric acid-nitric acid mixed solution as an etching solution to obtain a micro-disc cavity; and finally, removing photoresist on the surface of the micro-disc cavity, and performing thermal reflux on the photoresist by using a laser to finish the preparation of the micro-core annular cavity. The invention uses hydrofluoric acid-nitric acid etching to replace dry etching in the preparation process, improves isotropy, so that the etching method is suitable for preparing the ultra-high quality micro-core annular cavity, and realizes 10 in 1550nm wave band 8 The above quality factors, which are comparable to those in the relevant reports. The invention has the advantages of low cost, simple etching equipment, easy maintenance, good robustness to temperature and humidity, and the like.
Description
Technical Field
The present invention relates to micro-nano optical device and semiconductor silicon micro-processing manufacturing field, especially to a method for preparing micro-core annular cavity by wet etching silicon.
Background
The whispering gallery mode optical microcavity has high Quality factor (Q) and small mode volume, is an ideal platform for researching the interaction of light and substances, and has very important application in various fields such as quantum information processing, nonlinear optics, laser sensing, optomechanical and the like. There are many kinds of whispering gallery mode optical microcavities, such as a micro-core annular cavity, a micro-sphere cavity, a micro-bubble cavity, etc., wherein the optical mode of the micro-core annular cavity is sparsely distributed, is easier to control, and is very popular to apply.
Isotropic xenon difluoride (XeF) 2 ) Etching is first used to form silicon pillars to make the micro-core annular cavity, and then a method of making the micro-core annular cavity using reactive ion etching (Reactive ion etching, RIE) emerges. XeF is currently widely used in the art 2 And RIE method for preparing ultra-high quality micro-core annular cavity: xeF is used by various subject groups such as university of California, university of St.Louis Washington, university of California, university of Japanese Qing, university of Beijing and university of Nanj 2 The micro-core annular cavity is prepared by using an RIE etching method from a plurality of subject groups such as Turkey university, madison division of Wis university, japan, and the like.
Studies on both methods show that isotropic silicon etching is necessary in the process, and that the quality factor of the samples prepared from them can reach 10 8 The above, however, has the disadvantage that one is that the two methods require large etching equipment, and therefore, the cost is high; another is that the etching equipment uses a complicated system of vacuum, gas valves, etc., and maintenance is relatively difficult. The preparation of the micro-core annular cavity is an indispensable step in basic research and engineering application, and the requirement of preparing the ultra-high quality micro-core annular cavity in basic and application research is continuously improved at present. Therefore, the preparation method of the ultra-high quality micro-core annular cavity with low cost and easy maintenance has very wide application prospect.
Disclosure of Invention
The inventionProvides a method for preparing a micro-core ring cavity by wet etching silicon, which selects reasonable HF+HNO 3 Proportioning, adjusting parameters in the process, and improving isotropy of etching to obtain a higher quality factor. So as to pass through HF+HNO at room temperature 3 The ultra-high quality micro-core annular cavity is simple and convenient to prepare by etching.
The invention provides a method for preparing a micro-core annular cavity by wet etching silicon, which comprises the following steps:
s1: taking a silicon wafer, wherein the surface of the silicon wafer is a silicon dioxide oxide layer, and obtaining a silicon dioxide disc pattern covered with photoresist on the surface of the silicon wafer by using a photoetching and hydrofluoric acid etching method;
s2: carrying out wet etching on the silicon dioxide disc graph covered with the photoresist, which is obtained in the step S1, by using a hydrofluoric acid-nitric acid mixed solution as an etching solution to obtain a micro-disc cavity;
s3: and removing photoresist on the surface of the micro-disc cavity, and performing thermal reflux on the photoresist by using a laser to finish the preparation of the micro-core annular cavity.
Optionally, the method for preparing the micro-core annular cavity by wet etching silicon comprises the steps.
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the silicon wafer is a monocrystalline silicon wafer;
in the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the resistivity of the silicon wafer is 0.01-0.02 omega cm.
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the silicon wafer is a P-type silicon wafer.
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the thickness of the oxide layer of the silicon wafer is 2-4 mu m, and the thickness is preferably 3 mu m.
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the crystal orientation of the silicon wafer is [111].
In the method for preparing the micro-core annular cavity by wet etching silicon, the volume ratio of hydrofluoric acid and nitric acid (1:19) - (3:17) is prepared when etching solution is prepared; preferably, the volume ratio is 1:9;
the concentration of hydrofluoric acid used in preparing the etching solution is 35wt.% to 60wt.%, preferably the concentration of hydrofluoric acid is 49wt.%;
the concentration of nitric acid used in formulating the etching solution is 60wt.% to 80wt.%, preferably 65.0wt.% to 68.0wt.%.
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the etching rotating speed is optionally 150-300rpm, and preferably 240rpm.
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the photoetching and hydrofluoric acid etching method in the step S1 comprises the following steps of:
a. washing the silicon wafer, namely washing an oxide layer on the surface of the silicon wafer by using one or more of acetone, isopropanol and deionized water, and then drying the silicon wafer;
b. c, surface modification, namely placing the silicon wafer cleaned in the step a on a spin table of a spin coater for rotation, and dripping Hexamethyldisilane (HMDS) on an oxide layer on the surface of the silicon wafer;
c. b, throwing photoresist, namely covering positive photoresist on the oxide layer on the surface of the silicon wafer after modification in the step b, rotating the photoresist through a photoresist homogenizer to uniformly cover the photoresist on the oxide layer on the surface of the silicon wafer after modification, and drying the silicon wafer after completion;
d. c, covering a mask plate on the silicon wafer covered with the positive photoresist, which is obtained in the step c, and then exposing the silicon wafer under ultraviolet light, wherein the mask plate is round; the mask plate is of a common round shape, and the diameter of the round shape is generally 70-200 mu m; the mask plate can be arranged in a plurality of circular arrays.
e. Immersing the silicon wafer obtained in the step d in a developing solution for developing, then cleaning the silicon wafer, and then drying the silicon wafer;
f. c, immersing the silicon wafer with good development condition obtained in the step e in a hydrofluoric acid buffer solution, wherein the positive photoresist is used as an etching mask until all the oxide layer which is not covered by the positive photoresist is etched, and forming a silicon dioxide disc graph with the surface covered by the photoresist on the silicon wafer.
In the method for preparing a micro-core annular cavity by wet etching silicon provided by the invention, the positive photoresist is generally preferably a chemically enhanced positive photoresist, comprising one or more resins containing photoacid-labile groups (such as phenolic resin/diazonaphthoquinone system).
Optionally, the step S1 consists of the above steps a-f.
In the method for preparing the micro-core annular cavity by wet silicon etching, in the step b, the rotating speed of the spin coater is 2000-4000rpm, and the rotating time is 3-10s; preferably, the rotating speed is 3000rpm, and the rotating time is 5s;
in the method for preparing the micro-core annular cavity by wet silicon etching provided by the invention, optionally, in the step c, the rotating speed of the spin coater is 2000-4000rpm, and the rotating time is 30-90s; preferably, the rotating speed is 3000rpm, and the rotating time is 60s;
in the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, optionally, in the step d, the exposure time of ultraviolet light is 20s-60s, the wavelength of the ultraviolet light is 300-400nm, and the power is about 5-15mW/cm 2 ；
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, optionally, in the step e, the developing solution is tetramethyl ammonium hydroxide;
in the method for preparing the micro-core annular cavity by wet silicon etching, optionally, in the step f, the hydrofluoric acid buffer solution is prepared by mixing hydrofluoric acid (49 wt%) and ammonium fluoride (40 wt%) according to the volume ratio of (1-6).
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, in the step S2, the wet etching comprises the following steps:
a) Etching solution is prepared, and hydrofluoric acid solution and nitric acid solution are uniformly mixed; adjusting the initial temperature of the etching solution to room temperature; optionally, the room temperature is in the temperature range of 15-30 ℃;
b) Placing the silicon dioxide disc graph with the surface covered with the photoresist in a container, then placing the container in etching solution, and forming small holes penetrating the inside and the outside of the container at the bottom of the container; in the etching process, the container floats on the surface of the etching solution, and the silicon dioxide disc graph with the surface covered with photoresist is immersed in the etching solution;
in the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, the silicon dioxide disc graph with the surface covered with photoresist is immersed in the etching solution; the etch depth is about one-fourth the diameter of the disk.
Optionally, the step S2 consists of steps a) and b).
In the method for preparing the micro-core annular cavity by wet etching silicon provided by the invention, in the step S3, photoresist on the surface of the micro-disc cavity is removed, and a laser is used for carrying out thermal reflow, and the method comprises the following steps:
1) Washing off the photoresist on the surface of the silicon dioxide disc graph, and then drying;
2) Irradiating the sample by using a laser to form a regular silicon dioxide ring surface so as to finish the preparation of the micro-core ring cavity;
optionally, the step S3 consists of steps 1) and 2).
In the method for preparing the micro-core annular cavity by wet silicon etching provided by the invention, optionally, the wavelength of the laser is 10.6 mu m, the laser pulse frequency is 1Hz, the duty ratio is 10%, the laser power is about 25W-100W, and the pulse number is 1-10.
In the method for preparing the micro-core annular cavity by wet etching silicon, the drying temperature is 100-130 ℃, and the drying time is 1-10min; preferably, the drying temperature is 115 ℃ and the time is 5min.
On the other hand, the invention provides the micro-core annular cavity prepared by the method for preparing the micro-core annular cavity by wet etching silicon.
The invention uses HF+HNO 3 The etching replaces the dry etching in the original process, improves the isotropy of the etching by adjusting the process parameters, and realizes 10 in 1550nm wave band 8 The quality factor is low in cost, and meanwhile, the etching device has the advantages of simplicity and easiness in maintenance. In addition, the wet etching for forming the silicon pillar can be performed at room temperature, the preparation effect has better robustness to temperature change, and the preparation method has better effect onThe change in humidity is insensitive. Such a manufacturing process can be directly applied in many fields, such as laser, sensing, encapsulation, etc.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and drawings.
Drawings
The accompanying drawings are included to provide an understanding of the principles of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain, without limitation, the principles of the invention.
FIG. 1 (a) is a schematic diagram showing a quality factor measurement experiment apparatus, and the inset is [111]]Preparing a scanning electron microscope photo of a micro-core annular cavity by using a crystal orientation silicon wafer; in FIG. 1 (b) is shown the use of HF+HNO 3 The etching method is used for preparing a schematic diagram of the micro-core annular cavity.
Fig. 2 is a top view of a micro-core annular cavity prepared from silicon wafers with different crystal orientations under an optical microscope.
Fig. 3 (a) shows the quality factor obtained by preparing the core-around cavities at different initial temperatures. The quality factors of the samples prepared at different humidities are shown in fig. 3 (b). FIG. 3 (c) shows that the highest quality factor measured at 1550nm band of the core-annular cavity prepared in example 1 in the experiment is 1.05X10 8 The resonance wavelength was about 1549.99nm. FIG. 3 (d) shows the distribution of optical modes, the illustration is a side view of the micro-core ring cavity under a scanning electron microscope, and the left and right sides are respectively composed of HF+HNO 3 And XeF 2 Is prepared.
Detailed Description
The following describes embodiments of the present invention in detail for the purpose of making the objects, technical solutions and advantages of the present invention more apparent. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be arbitrarily combined with each other.
The embodiment of the invention provides a method for preparing a micro-core annular cavity by wet etching silicon, which comprises the following steps:
s1: taking a silicon wafer, wherein the surface of the silicon wafer is a silicon dioxide oxide layer, and obtaining a silicon dioxide disc pattern covered with photoresist on the surface of the silicon wafer by using a photoetching and hydrofluoric acid etching method;
s2: carrying out wet etching on the silicon dioxide disc graph covered with the photoresist, which is obtained in the step S1, by using a hydrofluoric acid-nitric acid mixed solution as an etching solution to obtain a micro-disc cavity;
s3: and removing photoresist on the surface of the micro-disc cavity, and performing thermal reflux on the photoresist by using a laser to finish the preparation of the micro-core annular cavity.
Optionally, the method for preparing the micro-core annular cavity by wet etching silicon comprises the steps.
In the embodiment of the invention, the silicon wafer is a monocrystalline silicon wafer;
in the embodiment of the invention, preferably, the resistivity of the silicon wafer is 0.01-0.02 Ω & cm;
in the embodiment of the invention, optionally, the silicon wafer is P-type boron doped;
in the embodiment of the invention, optionally, the thickness of the oxide layer of the silicon wafer is 2-4 μm, and the thickness is preferably 3 μm;
in the embodiment of the invention, preferably, the crystal orientation of the silicon wafer is [111].
In the embodiment of the invention, the volume ratio (1:19) - (3:17) of hydrofluoric acid and nitric acid is used for preparing etching solution; preferably, the volume ratio is 1:9;
in an embodiment of the present invention, the concentration of hydrofluoric acid used in preparing the etching solution is 35wt.% to 60wt.%, preferably the concentration of hydrofluoric acid is 49wt.%;
in an embodiment of the present invention, the concentration of nitric acid used in preparing the etching solution is 60wt.% to 80wt.%, preferably 65.0wt.% to 68.0wt.%.
In an embodiment of the present invention, the etching rotation speed is optionally 150-300rpm, and preferably, the etching rotation speed is 240rpm.
In the embodiment of the present invention, the photolithography and hydrofluoric acid etching method in step S1 includes the following steps:
a. washing the silicon wafer, namely washing an oxide layer on the surface of the silicon wafer by using one or more of acetone, isopropanol and deionized water, and then drying the silicon wafer;
b. c, surface modification, namely placing the silicon wafer cleaned in the step a on a spin table of a spin coater for rotation, and dripping Hexamethyldisilane (HMDS) on an oxide layer on the surface of the silicon wafer;
c. b, throwing photoresist, namely covering positive photoresist on the oxide layer on the surface of the silicon wafer after modification in the step b, rotating the photoresist through a photoresist homogenizer to uniformly cover the photoresist on the oxide layer on the surface of the silicon wafer after modification, and drying the silicon wafer after completion;
d. c, covering a mask plate on the silicon wafer covered with the positive photoresist, which is obtained in the step c, and then exposing the silicon wafer under ultraviolet light, wherein the mask plate is round; the mask plate is of a common round shape, and the diameter of the round shape is generally 70-200 mu m; the mask plate can be arranged in a plurality of circular arrays.
e. Immersing the silicon wafer obtained in the step d in a developing solution for developing, then washing the silicon wafer, and then drying the silicon wafer;
f. c, immersing the silicon wafer with good development condition obtained in the step e in a hydrofluoric acid buffer solution, wherein the positive photoresist is used as an etching mask until all the oxide layer which is not covered by the positive photoresist is etched, and forming a silicon dioxide disc graph with the surface covered by the photoresist on the silicon wafer.
In embodiments of the present invention, the positive photoresist is generally preferably a chemically amplified positive photoresist comprising one or more resins containing photoacid-labile groups (e.g., phenolic resin/diazonaphthoquinone systems).
Optionally, the step S1 consists of the above steps a-f.
In the embodiment of the invention, in the step b, the rotating speed of the spin coater is 2000-4000rpm, and the rotating time is 3-10s; preferably, the rotating speed is 3000rpm, and the rotating time is 5s;
in the embodiment of the present invention, optionally, in the step c, the rotation speed of the spin coater is 2000-4000rpm, and the rotation time is 30-90s; preferably, the rotating speed is 3000rpm, and the rotating time is 60s;
in an embodiment of the present invention, optionally, in the step d, the exposure time of the ultraviolet light is 20s-60s, the wavelength of the ultraviolet light is 300-400nm, and the power is about 5-15mW/cm 2 ；
In an embodiment of the present invention, optionally, in step e, the developing solution is tetramethylammonium hydroxide;
in an embodiment of the present invention, optionally, in step f, the hydrofluoric acid buffer solution is prepared by mixing hydrofluoric acid (49 wt.%) and ammonium fluoride (40 wt.%) according to a volume ratio of (1-6): 1-6.
In the embodiment of the present invention, in step S2, the wet etching includes the following steps:
a) Preparing etching solution, namely uniformly mixing hydrofluoric acid solution and nitric acid solution; adjusting the initial temperature of the etching solution to room temperature; optionally, the room temperature is in the temperature range of 15-30 ℃;
b) Placing the silicon dioxide disc graph with the surface covered with the photoresist in a container, then placing the container in etching solution, and forming small holes penetrating the inside and the outside of the container at the bottom of the container; in the etching process, the container floats on the surface of the etching solution, and the silicon dioxide disc graph with the surface covered with photoresist is immersed in the etching solution;
in the embodiment of the invention, the silicon dioxide disc graph with the surface covered with photoresist is immersed in the etching solution; the etch depth is about one-fourth the diameter of the disk.
Optionally, the step S2 consists of steps a) and b).
In the embodiment of the present invention, in step S3, removing the photoresist on the surface of the micro-disc cavity, and performing thermal reflow using a laser includes the following steps:
1) Washing off the photoresist on the surface of the silicon dioxide disc graph, and then drying;
2) Irradiating the sample by using a laser to form a regular silicon dioxide ring surface so as to finish the preparation of the micro-core ring cavity;
optionally, the step S3 consists of steps 1) and 2).
In the embodiment of the invention, optionally, the wavelength of the laser is 10.6 μm, the laser pulse frequency is 1Hz, the duty ratio is 10%, the laser power is about 25W-100W, and the number of pulses is 1-10.
In the embodiment of the invention, the drying temperature is 100-130 ℃, and the drying time is 1-10min; preferably, the drying temperature is 115 ℃ and the time is 5min.
On the other hand, the invention provides the micro-core annular cavity prepared by the method for preparing the micro-core annular cavity by wet etching silicon.
Example 1
The raw materials used in this example were as follows:
the resistivity of the silicon wafer is 0.01-0.02 omega cm, the thickness of the oxide layer of the silicon wafer is 3 mu m; the wafer diameter was 10cm (4 inches).
Etching solution volume ratio HF: HNO 3 =1:9, etching rotation speed 240rpm, hydrofluoric acid concentration used to prepare etching solution HF (49 wt.%) and nitric acid concentration used HNO 3 (65.0-68.0wt.％)。
Positive photoresist (Beijing ke Hua microelectronic BP 212-37)
Mask plate, mask plate is circular array
Developing solution (Beijing family Hua microelectronic KMP PD238-II positive photoresist developer, tetramethyl ammonium hydroxide)
Hydrofluoric acid buffer solution (using a mixed configuration of 49wt.% hydrofluoric acid and 40wt.% ammonium fluoride in a volume ratio of 1:6)
FIG. 1 (b) shows the use of HF+HNO 3 The etching method is used for preparing a schematic diagram of the micro-core annular cavity. The specific process steps are as follows:
(1) Spin coating
a. Washing a silicon wafer, sequentially using acetone, isopropanol and deionized water to wash an oxide layer on the surface of the silicon wafer, and then placing the silicon wafer on a heating magnetic stirrer for baking at 115 ℃ for 5min to remove water in the silicon wafer;
b. c, surface modification, namely placing the silicon wafer obtained in the step a on a turntable of a spin coater, and dripping about 8 drops of Hexamethyldisilane (HMDS) at the center of the silicon wafer, wherein the spin speed of the spin coater is 3000rpm, and the spin time is 5s;
c. c, throwing photoresist, namely dropwise adding positive photoresist into the center of the oxide layer on the surface of the silicon wafer after modification in the step b until the diameter is about 5cm, rotating the photoresist uniformly at 3000rpm for 60 seconds, and baking the silicon wafer for 2 minutes at 115 ℃ on a heating magnetic stirrer after finishing.
(2) Exposure to light
Covering the mask plate on the silicon wafer covered with the positive photoresist obtained in the step (1), and then exposing the silicon wafer under an ultraviolet lamp with the wavelength of 365nm and the power of about 10mW/cm 2 Exposure time 40s, mask plate is circular array.
(3) Development process
Immersing the silicon wafer obtained in the step (2) in a developing solution for development, then flushing with deionized water, and baking for 5 minutes at 115 ℃ on a heating magnetic stirrer.
(4) HF etching
Immersing the silicon wafer obtained in the step (3) in a hydrofluoric acid buffer solution, taking the positive photoresist as an etching mask until all the oxide layer which is not covered by the positive photoresist is etched, and forming a silicon dioxide disc graph with the surface covered by the photoresist on the silicon wafer.
(5)HF+HNO 3 Etching
a. Etching solution formulation, 10mL hydrofluoric acid (49 wt.%) and 90mL nitric acid (65.0 wt.% to 68.0 wt.%) were mixed in a jar of 150mL polypropylene;
b. the initial temperature and the ambient temperature of the etching solution are adjusted to 22 ℃;
c. the wide-mouth bottle is placed on a heating magnetic stirrer, and only the stirring function is started, the stirring speed is 240rpm, the stirring can avoid local overheating of the solution, and the diffusion of the etching agent is accelerated;
d. the silicon dioxide disc pattern covered with photoresist is placed in a culture dish of polystyrene, then the culture dish is placed in etching solution, small holes are drilled at the bottom of the culture dish, the culture dish floats on the surface of etching solution in the etching process, a sample is immersed in the etching solution, a large amount of heat is generated during etching, the temperature of each etching time is increased by about 2-3 ℃, and the etching depth is about one quarter of the diameter of the disc.
(6) Thermal reflow of carbon dioxide laser
a. Sequentially using acetone, isopropanol and deionized water to wash off photoresist on the surface of the disc, and placing the disc on a heating magnetic stirrer to bake for 5min at 115 ℃ to dry the surface of the disc;
b. the sample was irradiated with a carbon dioxide laser to complete the preparation of the core annular cavity. The carbon dioxide laser has a wavelength of 10.6 μm, a laser pulse frequency of 1Hz, a duty cycle of 10%, a laser power of about 35W, and a pulse number of 3.
Comparative example 1
Comparative example 1 XeF was used according to the method provided in Nature 421,925-928 (2003) 2 A micro-core annular cavity was prepared as shown in the right-hand insert of fig. 3 (d). In order to be able to compare with example 1, the difference from the above document is mainly that the silicon wafer is used as P-doped boron, [111]The resistivity of the crystal orientation is 0.01-0.02 omega cm, the thickness of the oxide layer of the silicon wafer is 3 mu m, and the diameter of the photoetching mask plate is a disc of 120 mu m. As shown in FIG. 3 (d), xeF is used 2 The method of (comparative example 1) and the use of HF+HNO 3 The highest quality factor of the core-around cavity prepared by the method of (example 1) is on the same order of magnitude.
Test case
1. Characterization of the quality factor of the microcavity
Fig. 1 (a) is a schematic diagram of an experimental apparatus, in which a broken line arrow represents an optical fiber pathway and a solid line arrow corresponds to an electrical pathway. In order to more fully characterize the microchip ring cavity, tunable lasers in three wavebands of 980nm, 1450nm and 1550nm are used as laser sources, respectively. Laser light emitted by the laser is coupled into the microcavity through the fiber taper. The output of the laser is detected by a photodetector whose voltage output is connected to an oscilloscope. During testing, the laser intensity of the output end of the optical fiber cone is adjusted to the magnitude of 3 mu W through an adjustable attenuator to reduce the influence of thermal broadening and other nonlinear effects on the quality factor. An oscilloscope was used to record each observed high Q transmission line. The quality factor in the present invention is a measured quality factor or a load quality factor, which includes intrinsic loss and coupling loss.
2. Testing of silicon wafers with different crystal orientations
FIG. 2 is a top view of a micro-core annular cavity prepared from silicon wafers with different crystal orientations under an optical microscope, and FIG. 2 (a) is [111]]The crystal orientation, FIG. 2 (b) is [100 ]]The crystal orientation, FIG. 2 (c) is [110 ]]And (5) crystal orientation. These samples were prepared using a similar procedure to example 1, except that hf+hno 3 The initial temperature and the ambient temperature of the etching are 24 ℃, and the ambient humidity is 21.2-24.3%. As can be seen from FIG. 2, the anisotropy of each silicon wafer is more clearly observed. The crystal of silicon is diamond structure, belonging to O h The (111), (100) and (110) crystal planes of single crystal silicon correspond to 3 times, 4 times and 2 times rotational symmetry, respectively, from the symmetry point group analysis. The different etch rates for the different crystal orientations result in a silicon pillar plane pattern with rotational symmetry similar to 3, 4, and 2 rotational symmetries. Along [111]]The silicon atoms are arranged in a regular triangle when seen in the crystal orientation direction, so that the symmetry of the plane pattern of the crystal orientation sample is increased from 3 times to 6 times, and the crystal orientation sample is higher than the other two crystal orientations and is closer to a circle with highest plane symmetry. These samples were characterized at 980nm, 1450nm and 1550nm bands, respectively, and the highest load quality factors measured are shown in table 1. [111]The quality factor of the crystal orientation is higher than [100 ]]And [110 ]]And (5) crystal orientation. The silicon pillars can play a role in heat conduction in the thermal reflow process, and the round silicon pillars with smooth surfaces are beneficial to the uniform shrinkage and cooling of silicon dioxide, so that a higher quality factor can be realized. Although [100 ]]And [110 ]]Can also have more than 10 7 But may be due to the presence of many low Q modes, the baseline of the transmission spectrum is not like [111]]The crystal orientation is flat.
TABLE 1 quality factors of samples of different crystal orientations at different wavebands
| Q(×10) | 980nm | 1450nm | 1550nm |
| [111] | 15.5 | 6.54 | 6.26 |
| [100] | 8.44 | 4.66 | 4.48 |
| [110] | 6.56 | 2.87 | 3.00 |
3. Testing of samples prepared at different temperatures and humidities
Using [111]]The samples prepared from the crystal orientation silicon wafer are used for robustness research and comparison of mode distribution, and the laser sources used for testing are all 1550nm wave bands. Temperature and humidity are two very important environmental parameters, where temperature and humidity refer to the temperature and humidity at which HF+HNO is carried out 3 Temperature and humidity during etching. In the robustness study on temperature, the temperature of the solution and the ambient temperature were adjusted to a same value before etching. Fig. 3 (a) shows the quality factors obtained by preparing the micro-core annular cavity at different initial temperatures, the etching initial temperature is 18 ℃ to 28 ℃ to cover the range of room temperature. As can be seen from the figure, using this method, 5X 10 can be obtained at different temperatures 7 The above quality factors. FIG. 3 (b) shows the quality factors of the samples prepared at different humidities. Humidity range is about15% to 45%, the starting temperature of the etching and the ambient temperature are 24 ℃. The samples were immersed in the etchant, so humidity should have no effect on the quality factor of the microchip ring cavity, this assumption being consistent with the data in fig. 3 (b). The highest quality factor measured in the 1550nm band in the experiment was 1.05X10 8 The resonance wavelength was about 1549.99nm, the transmission spectrum was finely scanned as shown in FIG. 3 (c), and the sample tested was obtained using [111]]The crystal orientation sample is prepared at 22 ℃. Mode cleaving is due to the uncoupling of the degeneracy between the forward and reverse optical modes. Both single lorentzian and bislorentzian lines exist in the observed optical mode. FIG. 3 (d) shows the distribution of optical modes, the two samples being composed of HF+HNO, respectively 3 And XeF 2 The left and right illustrations are prepared by two etching methods. HF+HNO 3 The quality factor and XeF of the micro-core annular cavity prepared by the method 2 The etching is equivalent.
Although the embodiments of the present invention are described above, the embodiments are only used for facilitating understanding of the present invention, and are not intended to limit the present invention. Any person skilled in the art can make any modification and variation in form and detail without departing from the spirit and scope of the present disclosure, but the scope of the present disclosure is to be determined by the appended claims.
Claims (23)
1. A method for preparing a micro-core annular cavity by wet etching silicon, wherein the method comprises the following steps:
s1: taking a silicon wafer, wherein the surface of the silicon wafer is a silicon dioxide oxide layer, and obtaining a silicon dioxide disc pattern covered with photoresist on the surface of the silicon wafer by using a photoetching and hydrofluoric acid etching method; the diameter of the silicon dioxide disc pattern covered with the photoresist is 70 μm to 200 μm;
s2: carrying out wet etching on the silicon dioxide disc graph covered with the photoresist, which is obtained in the step S1, by using a hydrofluoric acid-nitric acid mixed solution as an etching solution to obtain a micro-disc cavity;
s3: removing photoresist on the surface of the micro-disc cavity, and performing thermal reflux on the photoresist by using a laser to finish the preparation of the micro-core annular cavity;
in step S2, the wet etching includes the following steps:
a) Preparing etching solution, and uniformly mixing hydrofluoric acid solution and nitric acid solution; adjusting the initial temperature of the etching solution to room temperature; the room temperature is 15-30 ℃;
b) Placing the silicon dioxide disc pattern sample with the surface covered with the photoresist in a container, then placing the container in etching solution, and forming small holes penetrating the inside and the outside of the container at the bottom of the container; in the etching process, the container floats on the surface of the etching solution, and the silicon dioxide disc pattern sample with the surface covered with photoresist is immersed in the etching solution; stirring to avoid local overheating of the solution;
the silicon wafer is a monocrystalline silicon wafer;
the volume ratio of hydrofluoric acid to nitric acid (1:19) - (3:17) when preparing etching solution;
the crystal orientation of the silicon wafer is [111];
the concentration of hydrofluoric acid used in preparing the etching solution is 35 wt-60 wt%;
the concentration of nitric acid used in preparing the etching solution is 60 wt% -80 wt%.
2. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein,
the silicon wafer is a P-type silicon wafer.
3. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the resistivity of the silicon wafer is 0.01-0.02 Ω -cm.
4. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the thickness of the oxide layer of the silicon wafer is 2-4 μm.
5. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 4, wherein the thickness of the oxide layer of the silicon wafer is 3 μm.
6. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the volume ratio of hydrofluoric acid to nitric acid is 1:9 when preparing etching solution.
7. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the concentration of hydrofluoric acid used in preparing the etching solution is 49 wt%.
8. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the concentration of the nitric acid used in preparing the etching solution is 65.0 wt% -68.0 wt%.
9. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the stirring rotation speed of the wet etching in the step S2 is 150-300 rpm.
10. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 9, wherein the stirring rotation speed of the wet etching in the step S2 is 240rpm.
11. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein the photolithography and hydrofluoric acid etching method in step S1 comprises the following steps:
a. washing the silicon wafer, namely washing an oxide layer on the surface of the silicon wafer by using one or more of acetone, isopropanol and deionized water, and then drying the silicon wafer;
b. c, surface modification, namely placing the silicon wafer cleaned in the step a on a spin table of a spin coater, dripping hexamethyldisilane on an oxide layer on the surface of the silicon wafer, and then rotating;
c. b, throwing photoresist, namely covering positive photoresist on the oxide layer on the surface of the silicon wafer after modification in the step b, rotating the photoresist through a photoresist homogenizer to uniformly cover the photoresist on the oxide layer on the surface of the silicon wafer after modification, and drying the silicon wafer after completion;
d. c, covering a mask plate on the silicon wafer covered with the positive photoresist, which is obtained in the step c, and then exposing the silicon wafer under ultraviolet light, wherein the mask plate is round;
e. immersing the silicon wafer obtained in the step d in a developing solution for developing, then washing the silicon wafer, and then drying the silicon wafer;
f. c, immersing the silicon wafer obtained in the step e in a hydrofluoric acid buffer solution, wherein the positive photoresist is used as an etching mask until all the oxide layer which is not covered by the positive photoresist is etched, and forming a silicon dioxide disc graph with the surface covered by the photoresist on the silicon wafer.
12. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 11, wherein,
in the step b, the rotating speed of the spin coater is 2000-4000rpm, and the rotating time is 3-10 s.
13. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 11, wherein in the step b, the rotating speed of the spin coater is 3000rpm, and the rotating time is 5s.
14. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 11, wherein in the step c, the rotating speed of the spin coater is 2000-4000rpm, and the rotating time is 30-90 s.
15. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 14, wherein in the step c, the rotating speed of the spin coater is 3000rpm, and the rotating time is 60s.
16. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 11, wherein in the step d, the exposure time of the ultraviolet light is 20s-60s, the wavelength of the ultraviolet light is 300-400nm, and the power is 5-15mW/cm 2 。
17. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 11, wherein in the step e, the developing solution is tetramethyl ammonium hydroxide.
18. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 11, wherein in the step f, the hydrofluoric acid buffer solution is prepared by mixing hydrofluoric acid and ammonium fluoride according to the volume ratio of (1-6).
19. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 1, wherein in the step S3, photoresist on the surface of the micro-disc cavity is removed and thermally reflowed by using a laser, comprising the following steps:
1) Washing off the photoresist on the surface of the silicon dioxide disc graph, and then drying;
2) And irradiating the sample by using a laser to form a regular silicon dioxide circular surface so as to finish the preparation of the micro-core circular cavity.
20. The method for preparing a micro-core annular cavity by wet etching silicon as claimed in claim 19, wherein the wavelength of the laser is 10.6 μm, the laser pulse frequency is 1Hz, the duty ratio is 10%, the laser power is 25W-100W, and the number of pulses is 1-10.
21. The method for preparing a micro-core annular cavity according to any one of claims 11 to 20, wherein the drying temperature is 100-130 ℃ and the drying time is 1-10 min.
22. The method for preparing a micro-core annular cavity by wet etching silicon according to claim 21, wherein the drying temperature is 115 ℃ and the drying time is 5min.
23. A microchip ring cavity made by the method for preparing a microchip ring cavity by wet etching silicon according to any one of claims 1 to 22.
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