CN112758886B - Large-size optical gyroscope wedge-shaped cavity and preparation method and application thereof - Google Patents
Large-size optical gyroscope wedge-shaped cavity and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a large-size optical gyroscope wedge-shaped cavity and a preparation method and application thereof, wherein the preparation method comprises the following steps: sequentially constructing SiO on the surface of Si wafer 2 An oxide layer and a mask layer; carrying out photoetching exposure treatment on the mask layer in a contact ultraviolet exposure mode, and removing redundant parts in the mask layer; for the SiO 2 BOE corrosion is carried out on the oxide layer, and SiO is formed inside the mask layer 2 Wedge-shaped cavity, followed by removal of the SiO attached thereto 2 A mask layer on the surface of the wedge-shaped cavity; by XeF 2 Etching the surface of the Si wafer by gas, and forming the SiO film on the surface of the Si wafer 2 The inner side of the wedge-shaped cavity forms a Si wedge-shaped cavity. The invention solves the problem that a large-size wedge-shaped cavity is difficult to process and form in the Si-based material, can realize a wedge-shaped structure with a specific inclination angle and a flat surface on the Si-based wafer, obtains optical resonance with an ultra-high quality factor, and has the advantages of simple process, high surface flatness, easiness in realization and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of Si-based optoelectronic devices of optical gyroscopes, and particularly relates to a large-size optical gyroscope wedge-shaped cavity, and a preparation method and application thereof.
Background
The gyroscope is used as an important sensing device for measuring the angular acceleration and the attitude of the carrier, is an important core component of an inertial navigation system, is widely applied to various fields such as aerospace navigation, guidance control, tunnel construction, automobile manufacturing and the like, and has important significance in the research of important technological plans in the industrial field.
The resonant optical gyroscope is used as one development direction of the optical gyroscope, and the working principle of the resonant optical gyroscope is that the angular acceleration change of an object to be detected is calculated by detecting the change of resonance frequency difference caused by the Sagnac effect when two light waves which are reversely transmitted in a resonant cavity return to a starting point, so that the detection of angular velocity sensing is realized; the method has the remarkable advantages of high precision, small volume, low power consumption and the like, and is widely studied. The Si-based resonant optical microcavity gyroscope is miniaturized and integrated to become a development trend of the future gesture detection field, and the ultimate sensitivity of the Si-based resonant optical microcavity gyroscope mainly depends on the product of the diameter D of a resonant cavity and the Q value of a quality factor. Currently, the diameter of a common silicon-based microcavity is in the micrometer scale.
The traditional wedge-shaped resonant cavity is processed by adopting an MEMS (micro electro mechanical System) process, has simple flow and is a main structure for preparing a large-size microcavity; however, due to the limitation of MEMS processing technology, the larger the microcavity diameter D is, the more difficult the uniformity and the surface roughness of the microcavity structure are ensured, and the micrometer-scale surface roughness greatly reduces the Q value of the microcavity structure.
In view of this, it is necessary to develop a wedge structure capable of realizing a specific tilt angle on a Si-based wafer and having a flat surface and a method for preparing a large-sized optical gyro wedge cavity for obtaining an ultra-high quality factor (Q value).
Disclosure of Invention
The invention aims to overcome the defects existing in the prior art and provides a large-size optical gyro wedge-shaped cavity, and a preparation method and application thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a wedge-shaped cavity of a large-size optical gyroscope comprises the following steps:
sequentially constructing SiO on the surface of Si wafer 2 An oxide layer and a mask layer;
carrying out photoetching exposure treatment on the mask layer in a contact ultraviolet exposure mode, and removing redundant parts in the mask layer;
for the SiO 2 BOE corrosion is carried out on the oxide layer, and SiO is formed inside the mask layer 2 Wedge-shaped cavity, followed by removal of the SiO attached thereto 2 A mask layer on the surface of the wedge-shaped cavity;
by XeF 2 Etching the surface of the Si wafer by gasAt the SiO 2 The inner side of the wedge-shaped cavity forms a Si wedge-shaped cavity.
In the technical scheme, the BOE corrosion is performed by adopting a hydrogen fluoride buffer solution for wet corrosion.
Preferably, in the above technical solution, the hydrogen fluoride buffer solution is a mixed aqueous solution of hydrofluoric acid and ammonium fluoride.
Specifically, in the above technical scheme, the proportion of hydrofluoric acid and ammonium fluoride in the hydrogen fluoride buffer solution can influence the corrosion effect to silicon dioxide, when the content of hydrofluoric acid is too high, the corrosion rate is difficult to control, and the too fast corrosion rate can influence the upper surface smoothness degree of wedge chamber, on the contrary, when the content of hydrofluoric acid is too low, the corrosion rate is too slow.
Further preferably, in the above technical solution, the time of the BOE etching is 8-10 hours.
Specifically, in a preferred embodiment of the present invention, the hydrogen fluoride buffer solution is 48-50wt% hydrofluoric acid aqueous solution and 38-42.5wt% ammonium fluoride aqueous solution in a volume ratio of 1: 4.8-6.5.
Specifically, in another preferred embodiment of the present invention, the time of the BOE corrosion is 9 hours.
In the above technical solution, the mask layer is AZ6130 photoresist.
In detail, the AZ6130 photoresist has larger viscosity, and a thicker mask layer can be obtained by spin coating, so that the dropping speed of the mask layer (AZ 6130 photoresist) in wet etching is controlled.
Preferably, in the above technical solution, the thickness of the mask layer is 3.75-4.18 μm.
Further, in the above technical solution, the time of the ultraviolet exposure is 9-12s; further preferably 10s.
In particular, in the technical scheme, the SiO 2 The thickness of the oxide layer is 5-7.5 mu m; preferably 6 μm.
Specifically, in the above technical solution, the above SiO 2 The oxide layer can effectively assist XeF 2 Selective vapor etching of microcavitiesIs used. XeF (XeF) 2 Has a high selectivity to Si, i.e. Si and SiO are present simultaneously in a gaseous atmosphere 2 When XeF 2 The amount of gas etching Si is much higher than for SiO 2 When SiO is used as 2 When the oxide layer is too thick, the lower part of the microcavity etched by the gas phase is close to a cylinder, and the Q value is low; in contrast, when SiO 2 When the oxide layer is too thin, a reasonable protection function cannot be achieved, and the connection part of the upper part and the lower part is fragile and easy to break.
Further, in the above technical scheme, the preparation method of the large-size optical gyroscope wedge-shaped cavity further comprises,
before constructing the mask layer, the surface is provided with SiO 2 And placing the Si wafer of the oxide layer in hexamethyldisiloxane for vapor coating.
In detail, the mask layer and SiO can be enhanced by steaming the oxidized silicon wafer with an adhesive Hexamethyldisiloxane (HMDS) 2 Adhesion between oxide layers.
In detail, in one specific embodiment of the present invention, the method for preparing the wedge-shaped cavity of the large-size optical gyroscope specifically includes the following steps:
s1, thoroughly cleaning Si wafer, placing in a porcelain boat, placing in a vertical single-cavity vertical furnace with an initial temperature of 400-800 ℃, raising the temperature of the vertical single-cavity vertical furnace under the condition of introducing argon or nitrogen, introducing oxygen or oxygen-hydrogen mixed gas when the furnace temperature reaches 800-1100 ℃, controlling oxidation time, and constructing SiO with a thickness of 5.7-6.2 mu m on the surface of the Si wafer 2 The oxide layer is baked for 45-80min at 100-130 ℃ after being thoroughly cleaned again, and is put into hexamethyldisiloxane for vapor coating treatment;
s2, selecting AZ6130 photoresist as a mask layer, and under the condition that the revolution is 2750-2900rpm, forming a mask layer on the SiO 2 Spin coating the surface of the oxide layer to form a mask layer with the thickness of 3.8-4.1 mu m;
s3, selecting a contact type ultraviolet exposure mode, performing ultraviolet exposure on the AZ6130 photoresist mask layer for 9-10S by adopting a MA6 type photoetching machine, and performing ultraviolet exposure on the AZ6130 photoresist mask layer by using methyl ammonium hydroxide and deionized water according to the volume ratio of 1:3.5-5, developing for 30-35s in the developing solution prepared by mixing in proportion, and drying for 9-12min at 140-160 ℃ after the development is completed;
s4, mixing 49wt% of hydrofluoric acid aqueous solution and 40wt% of ammonium fluoride aqueous solution according to the volume ratio of 1:6, mixing the materials in proportion to prepare a hydrogen fluoride buffer solution, immersing the whole pattern area of the Si wafer subjected to the step S3 into the hydrogen fluoride buffer solution for BOE corrosion for 9h, and forming SiO inside the mask layer 2 Wedge-shaped cavity, followed by removal of the SiO attached thereto 2 The mask layer on the surface of the wedge-shaped cavity is annealed for 24 hours at 980-1050 ℃;
s5, adopting Semck desk type XeF 2 The etching system etches the Si wafer after the step S4, the Si wafer and XeF 2 Reaction to form SiF 4 Thereby at the SiO 2 The inner side of the wedge-shaped cavity forms a Si wedge-shaped cavity.
The invention further provides the large-size optical gyroscope wedge-shaped cavity prepared by the preparation method.
The invention also provides the preparation method or the application of the large-size optical gyroscope wedge-shaped cavity prepared by the preparation method in preparation of the optical gyroscope.
The invention forms SiO on the surface of Si wafer 2 Oxide layer and mask layer, siO with HF Buffer (BOE) 2 Etching, namely changing the metering parameter of the HMDS adhesive to control the film forming parameter of the photoresist, so as to control the falling time in etching liquid; the etching rate of the outermost layer near the side of the photoresist-coated region is the fastest, and as the layer etches laterally and longitudinally, the etching solution passes through the photoresist-coated layer and the SiO 2 The middle gap is filled, so that the HMDS adhesive is changed in measurement, the photoresist is easier to gradually fall off according to the sequence from outside to inside, the longitudinal corrosion time of the outermost layer is longest, and the central area is shorter, so that a wedge-shaped structure is formed; removing redundant convex angles on the side wall through corrosion time control, so that the side wall is smooth; the reaction rate is controlled by adjusting the temperature, and the required wedge-shaped structure is taken out from the corrosive liquid; then carrying out thermal annealing to remove residual moisture in the wet etching process step; by etching Si and SiO in the case of etching Si substrates 2 XeF with high selectivity 2 As gasDry etching of Si substrate with reaction gas and XeF 2 For Si and SiO 2 The selection ratio of (2) is greater than 1:100.
compared with the prior art, the invention has the beneficial effects that:
the invention solves the problem that a large-size wedge-shaped cavity is difficult to process and form in a Si-based material, can realize a wedge-shaped structure with a specific inclination angle and a flat surface on a Si-based wafer and obtain optical resonance with an ultra-high quality factor (Q value), has the advantages of simple process, high surface flatness, easiness in realization and the like, and can provide huge assistance for the development of resonant optical gyroscopes and other devices for measuring precise angular velocity in the future.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a wedge-shaped cavity of a large-size optical gyroscope according to an embodiment of the present invention;
in the figure:
1-Si wafer, 2-SiO 2 An oxide layer, 3-AZ6130 photoresist.
Detailed Description
The present invention will be described in further detail with reference to specific examples so as to more clearly understand the present invention by those skilled in the art.
The following examples are only illustrative of the present invention and are not intended to limit the scope of the invention.
The technical means used in the embodiments of the present invention are conventional means well known to those skilled in the art unless otherwise indicated.
All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without making any inventive effort shall fall within the scope of the present invention.
Example 1
The embodiment of the invention provides a preparation method of a wedge-shaped cavity of a large-size optical gyroscope, which is shown in fig. 1, and specifically comprises the following steps:
s1, thoroughly cleaning Si wafer, placing in a porcelain boat, placing in a vertical single-cavity vertical furnace with initial temperature of 600 ℃, and raising the vertical furnace under the condition of introducing argonWhen the temperature of the single-cavity vertical furnace reaches 1000 ℃, oxygen is introduced and the oxidation time is controlled, and SiO with the thickness of 6 mu m is built on the surface of the Si wafer 1 2 Oxide layer 2, which is then thoroughly cleaned again and baked at 120deg.C for 60min, and then put into hexamethyldisiloxane for vapor coating treatment to enhance SiO 2 Adhesion of the oxide layer 2 to the subsequent mask layer 3;
s2, selecting AZ6130 photoresist as a mask layer 3, and under the condition that the rotation number is 2800rpm, performing etching on the SiO 2 Spin-coating the surface of the oxide layer to form a mask layer with the thickness of 4 mu m;
s3, selecting a contact type ultraviolet exposure mode, carrying out ultraviolet exposure on the AZ6130 photoresist mask layer for 10 seconds by adopting a MA6 type photoetching machine, and using methyl ammonium hydroxide and deionized water according to the volume ratio of 1:4, developing for 30s in the developing solution prepared by mixing the components in proportion, and drying for 10min at 150 ℃ after the development is completed;
s4, mixing 49wt% of hydrofluoric acid aqueous solution and 40wt% of ammonium fluoride aqueous solution according to the volume ratio of 1:6, mixing the materials in proportion to prepare a hydrogen fluoride buffer solution, immersing the whole pattern area of the Si wafer subjected to the step S3 into the hydrogen fluoride buffer solution for BOE corrosion for 9h, and forming SiO inside the mask layer 2 Wedge-shaped cavity, followed by removal of the SiO attached thereto 2 The mask layer on the surface of the wedge-shaped cavity is annealed for 24 hours at 1000 ℃;
s5, adopting Semck desk type XeF 2 The etching system etches the Si wafer after the step S4, the Si wafer and XeF 2 Reaction to form SiF 4 Thereby at the SiO 2 The inner side of the wedge-shaped cavity forms a Si wedge-shaped cavity.
Example 2
The embodiment of the invention provides a preparation method of a wedge-shaped cavity of a large-size optical gyroscope, which is similar to the embodiment 1, and specifically comprises the following steps:
s1, thoroughly cleaning Si wafer, placing the Si wafer in a porcelain boat, placing the porcelain boat in a vertical single-cavity vertical furnace with an initial temperature of 600 ℃, raising the temperature of the vertical single-cavity vertical furnace under the condition of introducing argon, introducing oxygen and controlling oxidation time when the furnace temperature reaches 1000 ℃, and constructing SiO with a thickness of 6 mu m on the surface of the Si wafer 1 2 Oxide layer 2, which is then thoroughly cleaned again and baked at 120deg.C for 60min, and then put into hexamethyldisiloxane for vapor coating treatment to enhance SiO 2 Adhesion of the oxide layer 2 to the subsequent mask layer 3;
s2, selecting AZ6130 photoresist as a mask layer 3, and under the condition that the revolution is 2900rpm, forming a mask layer on the SiO 2 Spin-coating the surface of the oxide layer to form a mask layer with the thickness of 3.8 mu m;
s3, selecting a contact type ultraviolet exposure mode, carrying out ultraviolet exposure on the AZ6130 photoresist mask layer for 10 seconds by adopting a MA6 type photoetching machine, and using methyl ammonium hydroxide and deionized water according to the volume ratio of 1:4, developing for 30s in the developing solution prepared by mixing the components in proportion, and drying for 10min at 150 ℃ after the development is completed;
s4, mixing 48.5wt% of hydrofluoric acid aqueous solution and 42wt% of ammonium fluoride aqueous solution according to the volume ratio of 1:5.5 mixing to obtain a hydrogen fluoride buffer solution, and then immersing the whole pattern area of the Si wafer subjected to the step S3 into the hydrogen fluoride buffer solution for BOE corrosion for 9h to form SiO inside the mask layer 2 Wedge-shaped cavity, followed by removal of the SiO attached thereto 2 The mask layer on the surface of the wedge-shaped cavity is annealed for 24 hours at 1000 ℃;
s5, adopting Semck desk type XeF 2 The etching system etches the Si wafer after the step S4, the Si wafer and XeF 2 Reaction to form SiF 4 Thereby at the SiO 2 The inner side of the wedge-shaped cavity forms a Si wedge-shaped cavity.
The surface roughness of the walls of the wedge-shaped cavities prepared in examples 1-2 and the Q value thereof were measured by using a scanning electron microscope and a vector network analyzer, respectively, and the results are shown in Table 1 below.
TABLE 1 detection results of wall surface roughness and Q value of wedge-shaped cavities
From the results in table 1, it can be seen that the surface roughness and Q value of the cavity wall of the large-size optical gyro wedge-shaped cavity prepared by the method of the embodiment of the invention are obviously better than those of the large-size optical gyro wedge-shaped cavity prepared by the MEMS technology in the prior art; the method provided by the embodiment of the invention thoroughly solves the problem that a large-size wedge-shaped cavity is difficult to process and form in the Si-based material, can realize a wedge-shaped structure with a specific inclination angle and a flat surface on the Si-based wafer and obtain optical resonance with an ultra-high quality factor, has the advantages of simple process, high surface flatness, easiness in realization and the like, and has wide application prospect in the preparation of resonant optical gyroscopes and other devices for measuring precise angular velocity.
Finally, the method of the present invention is only a preferred embodiment and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for preparing a wedge-shaped cavity of a large-size optical gyroscope is characterized in that,
the method specifically comprises the following steps:
s1, thoroughly cleaning Si wafer, placing in a porcelain boat, placing in a vertical single-cavity vertical furnace with an initial temperature of 400-800 ℃, raising the temperature of the vertical single-cavity vertical furnace under the condition of introducing argon or nitrogen, introducing oxygen or oxygen-hydrogen mixed gas when the furnace temperature reaches 800-1100 ℃, controlling oxidation time, and constructing SiO with a thickness of 5.7-6.2 mu m on the surface of the Si wafer 2 The oxide layer is baked for 45-80min at 100-130 ℃ after being thoroughly cleaned again, and is put into hexamethyldisiloxane for vapor coating treatment;
s2, selecting AZ6130 photoresist as a mask layer, and under the condition that the revolution is 2750-2900rpm, forming a mask layer on the SiO 2 Spin coating the surface of the oxide layer to form a mask layer with the thickness of 3.8-4.1 mu m;
s3, selecting a contact type ultraviolet exposure mode, performing ultraviolet exposure on the AZ6130 photoresist mask layer for 9-10S by adopting a MA6 type photoetching machine, and performing ultraviolet exposure on the AZ6130 photoresist mask layer by using methyl ammonium hydroxide and deionized water according to the volume ratio of 1:3.5-5, developing for 30-35s in the developing solution prepared by mixing in proportion, and drying for 9-12min at 140-160 ℃ after the development is completed;
s4, mixing 49wt% hydrofluoric acid aqueous solution40% by weight of ammonium fluoride aqueous solution is 1:6, mixing the materials in proportion to prepare a hydrogen fluoride buffer solution, immersing the whole pattern area of the Si wafer subjected to the step S3 into the hydrogen fluoride buffer solution for BOE corrosion for 9h, and forming SiO inside the mask layer 2 Wedge-shaped cavity, followed by removal of the SiO attached thereto 2 The mask layer on the surface of the wedge-shaped cavity is annealed for 24 hours at 980-1050 ℃;
s5, adopting Semck desk type XeF 2 The etching system etches the Si wafer after the step S4, the Si wafer and XeF 2 Reaction to form SiF 4 Thereby at the SiO 2 The inner side of the wedge-shaped cavity forms a Si wedge-shaped cavity.
2. The method for manufacturing a wedge-shaped cavity of a large-size optical gyroscope according to claim 1, wherein in the step S3, an MA6 type photoetching machine is adopted to expose the AZ6130 photoresist mask layer for 10S.
3. The method for manufacturing a wedge-shaped cavity of a large-sized optical gyroscope according to claim 1, wherein in step S1, siO with a thickness of 6 μm is built on the surface of the Si wafer 2 And (5) an oxide layer.
4. The large-size optical gyro wedge-shaped cavity prepared by the preparation method of any one of claims 1-3.
5. Use of the method of any one of claims 1-3 or the large-sized optical gyro wedge cavity of claim 4 for the manufacture of an optical gyro.
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| CN1889233A (en) * | 2006-07-21 | 2007-01-03 | 中国科学院上海微系统与信息技术研究所 | Method for producing CMOS process compatible embedded suspension solenoid structure inductance or mutual inductance |
| CN101114591A (en) * | 2006-07-25 | 2008-01-30 | 杭州科岛微电子有限公司 | Pressure capacitance type sensor substrate cavity-forming method |
| CN101290962A (en) * | 2007-04-19 | 2008-10-22 | 斯坦雷电气株式会社 | Optical device |
| CN104810273A (en) * | 2014-01-26 | 2015-07-29 | 国家电网公司 | Silicon carbide etching method |
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| US7168318B2 (en) * | 2002-08-12 | 2007-01-30 | California Institute Of Technology | Isolated planar mesogyroscope |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1889233A (en) * | 2006-07-21 | 2007-01-03 | 中国科学院上海微系统与信息技术研究所 | Method for producing CMOS process compatible embedded suspension solenoid structure inductance or mutual inductance |
| CN101114591A (en) * | 2006-07-25 | 2008-01-30 | 杭州科岛微电子有限公司 | Pressure capacitance type sensor substrate cavity-forming method |
| CN101290962A (en) * | 2007-04-19 | 2008-10-22 | 斯坦雷电气株式会社 | Optical device |
| CN104810273A (en) * | 2014-01-26 | 2015-07-29 | 国家电网公司 | Silicon carbide etching method |
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