CN111313218A - Preparation method of microsphere cavity - Google Patents

Preparation method of microsphere cavity Download PDF

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CN111313218A
CN111313218A CN202010104921.8A CN202010104921A CN111313218A CN 111313218 A CN111313218 A CN 111313218A CN 202010104921 A CN202010104921 A CN 202010104921A CN 111313218 A CN111313218 A CN 111313218A
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disc
etching
layer
photoresist
silicon
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CN111313218B (en
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姜校顺
李胜军
李�昊
刘洋
肖敏
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Nanjing University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01SDEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/05Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
    • H01S3/08Construction or shape of optical resonators or components thereof
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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Abstract

The invention provides a preparation method of a microsphere cavity. The preparation method comprises the following steps: selecting a substrate, wherein the substrate comprises a supporting layer and a device layer which are compounded; forming a photoresist layer on the device layer, and forming a photoresist disc after photoetching and developing; etching the device layer material outside the photoresist disc area by taking the photoresist disc as a mask, then removing the photoresist disc, and forming a device disc on the supporting layer; etching-refluxing: etching the supporting layer material around the device disc to form a supporting column for supporting the device disc; melting the edge of the device disc by using a laser irradiator and inwards shrinking the edge of the device disc to the edge of the top end of the support pillar to form a device ring core; and repeating the etching-refluxing steps to gradually reduce the diameters of the support columns and the device ring core until a microsphere cavity is formed. The method provided by the invention can ensure that the device disc does not crack or fall off in the process of preparing the large-size microsphere cavity, and the diameter of the prepared microsphere cavity is improved.

Description

Preparation method of microsphere cavity
Technical Field
The invention belongs to the technical field of optical resonant cavities, and particularly relates to a preparation method of a microsphere cavity.
Background
Optical resonator has been playing a part in modern opticsThe essential role, which is not only the cornerstone of the laser-related field; meanwhile, the method is widely applied to the aspects of accurate measurement and detection, and plays a great role in the field of nonlinear optics. However, certain characteristics of conventional optical resonators greatly limit their range of use, such as their size, weight, alignment and stability issues, among others. To address these issues, efforts have been made in recent years to develop integrated optical microcavities, including theoretical studies of integrated optical microcavities, fabrication processes, performance testing, and related applications. The optical resonant cavity refers to an optical component which has a function of spatially and temporally locally enhancing and frequency selecting light waves. The limiting effect in time is characterized by a quality factor Q, and the local effect in space is characterized by a mode volume VeffTo indicate.
The whispering gallery mode optical microcavity is a special optical resonant cavity, and the light field can form a stable mode by total reflection in the inner wall of the optical resonant cavity. The most widely studied optical microcavities are currently the following three: a microsphere cavity, a microdisk cavity and a microring core cavity. CN110718841A discloses a method for preparing an on-chip integrated silicon-based microsphere cavity, which comprises the following steps: obtaining an SOI substrate, wherein the SOI substrate comprises a device layer at the top, a supporting layer at the bottom and an oxide layer positioned between the device layer and the supporting layer, the device layer is a Si layer, and the oxide layer is SiO2The supporting layer is a Si layer; spin-coating a photoresist layer on the device layer by using a spin coater; developing after exposure by a photoetching machine, and transferring a circular pattern with a set size onto the photoresist layer; etching a top silicon column and a bottom silicon column in sequence on the device layer, wherein the diameter of the top surface of the bottom silicon column is smaller than that of the top silicon column, and the top silicon column is of a cylindrical structure; removing the photoresist layer; after the top silicon pillar structure is heated and melted for a set time through laser irradiation, the top silicon pillar structure forms a spherical microcavity.
The silicon oxide microsphere cavity on the chip prepared by the prior art has the following problems: when a micro-sphere cavity with a larger diameter is manufactured, the micro-sphere cavity with the larger diameter needs to be refluxed, and the edge of the micro-sphere cavity with the larger diameter is easy to crack and fall off, so that part of silicon oxide is lost, and the diameter of the manufactured micro-sphere cavity is limited. The large diameter of the microsphere cavity is beneficial to improving the quality factor of the microsphere cavity.
Therefore, it is necessary to develop a new method for preparing a microsphere cavity to increase the size of the prepared optical microsphere cavity.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a microsphere cavity. The method can ensure that the device disc does not crack or fall off in the process of preparing the large-size microsphere cavity, and the diameter of the prepared microsphere cavity is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a microsphere cavity, which comprises the following steps:
(1) selecting a substrate, wherein the substrate comprises a supporting layer and a device layer which are compounded;
(2) forming a photoresist layer on the device layer of the substrate, and forming a photoresist disc on the device layer after photoetching and developing;
(3) etching the device layer material outside the photoresist disc area by taking the photoresist disc as a mask, then removing the photoresist disc, and forming a device disc on the supporting layer;
(4) etching-refluxing:
etching: etching the supporting layer material around the device disc to form a supporting column for supporting the device disc; refluxing: irradiating the device disc by laser to enable the edge of the device disc to be melted and to be contracted inwards to the edge of the top end of the support column to form a device ring core;
(5) repeating the etching-refluxing steps on the support pillar and the device ring core to gradually reduce the diameters of the support pillar and the device ring core until a microsphere cavity is formed;
in the step of etching-reflowing, after each etching, the diameter of the top end of the support column is smaller than that of the device disc or the device ring core.
The inventor finds that the silicon dioxide layer on the commercial silicon oxide wafer is grown by oxidizing the silicon wafer at about 1000 ℃, and because of the different thermal expansion coefficients of silicon dioxide and silicon, the silicon dioxide layer can bear stress after the silicon dioxide layer is grown and the silicon wafer is finally cooled down. When a silicon oxide microsphere cavity on a larger-diameter piece is to be manufactured, the diameter of a formed silicon oxide disc needs to be large, according to a traditional one-time heating and melting method, when silicon is etched by xenon difluoride to form a silicon column, silicon combined with the interface of the silicon oxide disc is less and less along with the etching, the exposed area of the silicon oxide disc is larger and larger, the borne stress is larger and larger, and finally the silicon oxide disc can crack and fall off and cannot form a large-diameter silicon oxide disc, so that the size of the finally manufactured silicon oxide microsphere cavity is limited. Similar to this, other substrates having different thermal expansion coefficients, different from the device layer material, also have the same problem.
The invention adopts the means of 'step etching-refluxing', a small part of the supporting columns are etched firstly, then reflows, and then the etching-refluxing steps are repeated until the micro-sphere cavity is formed finally. After reflow, the edge of the device disc is melted and contracted, the stress is released, and meanwhile, the edge of the device disc is rolled to form a ring core, so that the thickness of the edge is increased, the capability of bearing the stress is stronger, the diameter of the device disc is greatly reduced after multiple etching-reflow, and the stress cannot be reproduced to influence. By the method, the problem that the large-size device disc is easy to crack and fall off due to internal stress in the prior art is solved, and the size of the prepared microsphere cavity is increased.
As a preferred technical solution of the present invention, the material of the support layer is silicon.
In a preferred embodiment of the present invention, the device layer is made of silicon dioxide.
As a preferred technical scheme of the invention, the thickness of the device layer is 1-12 μm; for example, it may be 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm or 12 μm.
As a preferred embodiment of the present invention, in the step (3), the diameter of the device disk is 120 times or more of the thickness of the device layer, and may be, for example, 120 times, 125 times, 130 times, 135 times, 140 times, 145 times, 150 times, 155 times, 160 times, or the like of the thickness of the device layer; preferably 120-fold and 150-fold.
It should be noted that the thickness of the device layer and the diameter of the device disk need to be selected according to the size of the microsphere cavity to be prepared (ensuring equal volume), and the larger the thickness of the device layer, the smaller the diameter of the device disk. Although the diameter of the device disc can be reduced by increasing the thickness of the device layer, and the risk of cracking and falling off of the device disc can be reduced to a certain extent, so that the microsphere cavity is prepared by heating and melting in one step, the larger the thickness of the device layer, the longer the manufacturing time is, the higher the cost is, and the available thickness of the device layer is limited.
As a preferred technical scheme of the invention, the etching method in the step (3) is etching by using hydrofluoric acid solution.
Preferably, the method for removing the photoresist disc in the step (3) is as follows: dissolving with degumming agent.
As a preferred technical scheme of the invention, in the etching-refluxing step, the etching method is to etch by using xenon difluoride gas.
In the step of etching-refluxing, after each etching, the reduction value of the radius of the top end of the support column does not exceed 20 times of the thickness of the device layer; for example, it may be 20 times, 19 times, 18 times, 17 times, 15 times, 13 times, 12 times, 10 times, 8 times, or 5 times the thickness of the device layer, etc.
It should be noted that when the support layer is not etched, it corresponds to a support column of the same size as the device disk. Thus, the initial radius of the support post tips can be considered to be the same as the radius of the device disk. In the invention, the supporting columns cannot be etched too much at one time, so that the stress of the exposed device layer can be ensured to be in a bearable range, and the device disc or the device ring core cannot crack or fall off.
As a preferred technical scheme of the invention, in the step of refluxing, the wavelength of the adopted laser is 10.6 μm, and the power is 15-30W; for example, it may be 15W, 16W, 18W, 20W, 22W, 25W, 28W, 30W, or the like.
As a preferred embodiment of the present invention, the preparation method further comprises: the device disk or device ring core is preheated with a laser before each reflow.
Preferably, the laser used for preheating has a wavelength of 10.6 μm and a power of 40-100%, excluding 100%, of the lowest power for melting the device disk or device ring core; for example, it may be 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, or 95%, etc.
The device disc or the device ring core is preheated before backflow, so that impurities such as water and organic matters on the surface of the device disc or the device ring core can be removed, and the quality factor of the microsphere cavity is improved. The laser power adopted for preheating needs to ensure that the device material is not melted; and can not be too low, otherwise, the preheating function cannot be realized.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method provided by the invention solves the problem that the device disc cracks and falls off due to internal stress in the process of preparing the large-size microsphere cavity, improves the diameter of the prepared microsphere cavity, and improves the diameter and is beneficial to improving the quality factor of the microsphere cavity.
Drawings
FIG. 1 is a schematic view of the structure of a substrate used in an embodiment of the present invention;
FIG. 2 is a schematic diagram of a structure of a photoresist-coated substrate in an embodiment of the invention;
FIG. 3 is a schematic diagram of a photolithography method according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a substrate after development in an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a substrate after etching a silicon dioxide layer according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of a substrate with the photoresist puck removed in an embodiment of the present invention;
FIG. 7 is a schematic structural diagram of a silicon pillar and a silicon dioxide disk after a first etching of a silicon layer according to an embodiment of the present invention;
FIG. 8 is a schematic structural diagram of a silicon column and a silica ring core after a first reflow in an embodiment of the present invention;
FIG. 9 is a schematic structural diagram of a silicon pillar and a silicon dioxide ring core after the silicon pillar is etched for the last time in the embodiment of the present invention;
FIG. 10 is a schematic structural diagram of a silica microsphere cavity formed after the last reflow in the embodiment of the present invention.
FIG. 11 is a bimodal Lorentz plot of the cavity quality factor values of silica microspheres prepared in example 1 of the present invention measured by linewidth method;
FIG. 12 is a graph showing a ring curve of the cavity quality factor of silica microspheres prepared in example 1 of the present invention measured by a fast scan method;
fig. 13 is a schematic structural view of a silicon pillar and a silicon dioxide disk after a silicon layer is once etched in comparative example 1 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings. It should be understood by those skilled in the art that the specific embodiments are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a method for preparing a microsphere cavity, which comprises the following steps:
(1) selection substrate
A commercial silicon oxide thin film substrate was selected, the configuration of which is shown in FIG. 1, and which is composed of two layers of silicon and silicon dioxide, wherein the thickness of the silicon dioxide layer is 12 μm.
(2) Lithographic development
As shown in fig. 2, 3, 4, an adhesive is baked on the silicon oxide thin film substrate to enhance the photoresist adhesion, followed by spin coating S1813 photoresist, transferring the reticle pattern onto the photoresist using a photolithography machine, and developing to leave a photoresist disk (1800 μm diameter) on top of the silicon dioxide layer.
(3) Etching with hydrofluoric acid
The silicon dioxide layer is etched using hydrofluoric acid with added buffer with the photoresist disk as a mask. Exposing the silicon dioxide layer outside the photoresist disc area and directly reacting with hydrofluoric acid solutionContact to generate chemical reaction, the equation is SiO2+6HF=H2SiF6+2H2O, fluosilicic acid (H) produced2SiF6) The solution is dissolved in water, and the reaction speed of the hydrofluoric acid solution and the silicon is very slow at normal temperature, so that the silicon dioxide layer outside the photoresist disc area can be corroded, and the silicon layer can be prevented from being corroded. Thus, only the silicon dioxide disk and the photoresist disk thereon remain on the silicon layer, as shown in FIG. 5. The photoresist is then dissolved with a special stripper to completely remove the residual reactants, thereby forming a silicon dioxide disk on the silicon layer, as shown in fig. 6.
(4) Step-by-step etch-reflow
Etching: the silicon substrate around the silicon dioxide disc is etched by using xenon difluoride gas to form a silicon column supporting the silicon dioxide disc, as shown in fig. 7, but the silicon column cannot be etched too much at one time, but only a part of the silicon column is etched (240 μm is etched inwards each time, namely, the radius of the silicon dioxide disc is used as the initial radius of the top end of the silicon column, and the radius of the top end of the silicon column is reduced by 240 μm after each etching), so that the edge of the silicon dioxide disc is not too far away from the silicon column, and therefore, the internal stress is in a tolerable range, and the silicon dioxide disc cannot crack and fall off.
Preheating: the silica disk was irradiated (power 6W) with a carbon dioxide laser to remove surface impurities.
Refluxing: the silica disk was irradiated (power 30W) with a carbon dioxide laser, causing the edge of the silica disk to melt and shrink inward to the top edge of the silicon column, forming a silica ring core, as shown in fig. 8. The wavelength of the carbon dioxide laser is 10.6 microns, the silicon dioxide has a strong absorption effect on laser with the wavelength of 10.6 microns, the absorbed light field energy is converted into self heat energy, when the laser energy density reaches a certain degree, the edge of the silicon dioxide disc can begin to be heated and melted, the silicon dioxide close to the middle area is in contact with a silicon wafer, the heat is conducted out at a higher speed, the temperature is lower than that at the edge, and therefore the silicon dioxide can not be melted at the moment. Due to surface tension, the silica at the edges will shrink inward and form a ring, which is in fact a microring core cavity.
After reflow, the silica at the edge melts and shrinks, and the stress is released. Meanwhile, the edge of the silicon dioxide disc is rolled to form a ring core, the thickness of the edge is increased, and the capability of bearing stress is stronger, so that the silicon dioxide disc cannot be cracked and fall off.
Then, the above-mentioned "etching-reflowing" steps are repeated for three times, and the diameter of the silicon dioxide ring core is greatly reduced and the stress is not restored, and at this time, the supported silicon pillar is etched to be thin (the top diameter is 50 μm), as shown in fig. 9. Then, the mixture was refluxed to form a microsphere cavity (about 330 μm in diameter as measured by an optical microscope), as shown in FIG. 10.
When the Q value (quality factor) of the microsphere cavity is measured, the coupling of the fiber cone and the microsphere cavity is needed, laser is input from one side of the fiber cone by a laser, and the output power is detected by a photoelectric detector from the other side of the fiber cone. And (3) obtaining transmittance curves under different wavelengths through wavelength scanning of a laser, and fitting the intrinsic loss of the microsphere cavity according to the transmittance curves so as to obtain a Q value. According to different wavelength scanning speeds of the laser, Q measuring methods are divided into a line width method and a fast scanning method, the wavelength scanning speed of the laser is low in the line width method, and the wavelength scanning speed of the laser is high in the fast scanning method. The quick scanning method can inhibit the heat effect of the microcavity, and theoretically, the measurement result is more accurate. The quality factor of the silica microsphere cavity prepared in this example was measured by linewidth method, and a bimodal lorentzian curve obtained by data fitting is shown in fig. 11, and the intrinsic quality factor Q0=7.1×108. The quality factor of the silica microsphere cavity prepared in this example was measured by fast-scan method, and the Ringing curve obtained by data fitting is shown in FIG. 12, the intrinsic quality factor Q0=7.0×108
Example 2
This example provides a method for preparing a microsphere cavity, which is different from example 1 in that the thickness of the silicon dioxide layer is 10 μm, the diameter of the silicon dioxide disk is 1500 μm, and in the etching-reflowing step, the top end of the silicon pillar is etched inward 200 μm each time. The diameter of the prepared silicon dioxide microsphere cavity is 270 mu m, and the intrinsic quality factor Q of the silicon dioxide microsphere cavity is measured by a line width method0=6.4×108Measuring the intrinsic quality factor Q by fast scanning method0=6.5×108
Example 3
This example provides a method for preparing a microsphere cavity, which is different from example 1 in that the thickness of the silicon dioxide layer is 8 μm, the diameter of the silicon dioxide disk is 1000 μm, and the top end of the silicon pillar is etched inward 160 μm each time in the etching-reflowing step. The diameter of the prepared silicon dioxide microsphere cavity is 200 mu m, and the intrinsic quality factor Q of the silicon dioxide microsphere cavity is measured by a line width method0=5.4×108Measuring the intrinsic quality factor Q by fast scanning method0=5.4×108
Comparative example 1
A method for preparing a cavity for a microsphere is provided, which is different from example 1 in that the silicon pillar is etched to a tip diameter of 350 μm in step (4) (as shown in fig. 13), and then reflowing is performed.
Comparative example 1 since the silicon pillars were too many and the exposed area of the silicon dioxide disk was too large to endure the internal stress, the peeling occurred during the etching.
Comparative example 2
A method for preparing a microsphere cavity is provided, which is different from the method of example 1 in that the distance of each inward etching of the top end of the silicon pillar in the step (4) is 300 μm.
Comparative example 2 cracking occurred during etching because of excessive silicon pillars, excessive exposed area of the silicon dioxide disk, and excessive internal stress.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A preparation method of a microsphere cavity is characterized by comprising the following steps:
(1) selecting a substrate, wherein the substrate comprises a supporting layer and a device layer which are compounded;
(2) forming a photoresist layer on the device layer of the substrate, and forming a photoresist disc on the device layer after photoetching and developing;
(3) etching the device layer material outside the photoresist disc area by taking the photoresist disc as a mask, then removing the photoresist disc, and forming a device disc on the supporting layer;
(4) etching-refluxing:
etching: etching the supporting layer material around the device disc to form a supporting column for supporting the device disc; refluxing: irradiating the device disc by laser to enable the edge of the device disc to be melted and to be contracted inwards to the edge of the top end of the support column to form a device ring core;
(5) repeating the etching-refluxing steps on the support pillar and the device ring core to gradually reduce the diameters of the support pillar and the device ring core until a microsphere cavity is formed;
in the step of etching-reflowing, after each etching, the diameter of the top end of the support column is smaller than that of the device disc or the device ring core.
2. The method according to claim 1, wherein the material of the support layer is silicon.
3. The method according to claim 1 or 2, wherein the material of the device layer is silicon dioxide.
4. The production method according to any one of claims 1 to 3, wherein the device layer has a thickness of 1 to 12 μm.
5. The method according to any one of claims 1 to 4, wherein the diameter of the device disc in step (3) is 120 times or more, preferably 120 times 150 times the thickness of the device layer.
6. The production method according to any one of claims 1 to 5, wherein the etching in the step (3) is performed by etching with a hydrofluoric acid solution;
preferably, the method for removing the photoresist disc in the step (3) is as follows: dissolving with degumming agent.
7. The production method according to any one of claims 1 to 6, wherein in the etching-refluxing step, the etching method is xenon difluoride gas etching.
8. The method of any of claims 1-7, wherein in the step of etching-reflowing, the radius of the top of the support posts decreases by no more than 20 times the thickness of the device layer after each etching.
9. The production method according to any one of claims 1 to 8, wherein in the step of reflowing, a laser having a wavelength of 10.6 μm and a power of 15 to 30W is used.
10. The production method according to any one of claims 1 to 9, characterized by further comprising: preheating the device disc or the device ring core by adopting laser before each backflow;
preferably, the pre-heating is performed using a laser having a wavelength of 10.6 μm and a power of 40-100%, excluding 100%, of the lowest power that melts the device disk or device ring core.
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CN112525858A (en) * 2020-11-27 2021-03-19 中红外激光研究院(江苏)有限公司 Gas sensor based on microcavity thermotropic ringing effect and gas concentration measuring method

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CN101349780A (en) * 2008-08-30 2009-01-21 中北大学 Plane annular micro-cavity
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