CN112578499B - Preparation method of silicon nitride micro-ring resonant cavity for optical frequency combing - Google Patents
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Abstract
A preparation method of a silicon nitride micro-ring resonant cavity for optical frequency combing comprises the following steps: growing silicon dioxide on the silicon chip as a lower cladding; growing silicon nitride on the lower cladding layer as a buffer layer; growing silicon dioxide on the buffer layer to be used as a mask layer, and preparing the mask layer into a long strip-shaped, square or round periodic structure; growing silicon nitride on the buffer layer with the periodic structure in multiple steps to serve as a waveguide layer, carrying out high-temperature annealing after the growth is finished, and carrying out silicon nitride growth again after cooling until the required thickness of the waveguide layer is reached; spin-coating a layer of polymer on the waveguide layer, then performing nano-imprinting to form a pattern, and removing the nano-imprinting template after the imprinting is finished; transferring the polymer pattern to a silicon nitride waveguide layer by utilizing an ICP (inductively coupled plasma) etching process, organically cleaning the silicon wafer, removing the polymer, and completing pattern transfer to obtain a micro-ring structure and a strip waveguide structure; and continuously growing a layer of silicon dioxide on the waveguide layer to serve as an upper cladding layer, and finishing the preparation of the silicon nitride micro-ring resonant cavity.
Description
Technical Field
The invention discloses a preparation method of a silicon nitride micro-ring resonant cavity for an optical frequency comb, and belongs to the technical field of silicon-based optical device preparation.
Background
The optical frequency comb generated based on the micro-ring resonator (hereinafter referred to as microcavity) is a comb spectrum composed of a series of equally spaced optical frequencies. The device has the advantages of wide coverage range, extremely narrow line width of a single comb tooth, Hertz frequency stability and femtosecond time resolution, can provide a link bridge for various frequency standards such as a microwave frequency standard, an atomic frequency standard and an optical frequency standard, and provides an ideal measuring tool for the fields of length calibration, ultra-fast distance measurement, optical atomic clocks and the like. Microcavity optical frequency combs typically have a large frequency separation and thus have unique advantages in the fields of multi-wavelength light sources, parallel communications and astronomical metrology, precision spectroscopy, and the like. The micro-cavity is generally composed of a ring waveguide with a radius of several micrometers to several hundred micrometers and one or two strip waveguides, has small volume, and can be compatible with a CMOS (complementary metal oxide semiconductor) process, thereby being beneficial to the miniaturization, portability and integration development of devices.
In the development process of the microcavity, the main problem is that the high-quality factor silicon nitride microcavity facing on-chip integration is difficult to obtain. Two factors are involved, namely preparation of a high-quality silicon nitride film and pattern transfer of the ring waveguide and the strip waveguide. In the preparation of the silicon nitride film, in order to meet the requirement that the optical frequency comb is generated to position the waveguide material in a negative dispersion area, the thickness of the silicon nitride film is about 700nm, and when the thickness of the silicon nitride film actually grown by the traditional method exceeds 250nm, cracks can occur due to too large stress, excessive scattering loss is introduced, and the quality factor of the device is influenced. The growth of high quality silicon nitride films is an urgent problem to be solved. In the process of pattern transfer of the waveguide, the quality of the pattern transfer technology is directly related to the quality of the microcavity due to the size of the waveguide and the small distance between the annular waveguide and the strip waveguide (generally hundreds of nanometers). Although the electron beam exposure technique can meet the requirement of small size, the large write field splicing error is introduced due to the large size of the whole chip. But the photoetching machine with less than 1 mu m line is not generally used at present in China.
The high-quality silicon nitride microcavity has great significance for realizing optical frequency comb and device chip formation. The high-quality factor microcavity can provide higher light local capacity and high gain, and on one hand, enough intracavity light field intensity can be provided to realize parametric oscillation; on the other hand, the input power can be effectively reduced to realize an on-chip semiconductor laser and a microcavity integrated device, which is the development trend of microcavity optical frequency comb application in the future. Therefore, optimizing the preparation method of the microcavity device and obtaining the high-quality factor silicon nitride microcavity is an urgent problem to be solved in the application of optical frequency combing.
Disclosure of Invention
The invention aims to solve the problems that the existing micro-ring resonant cavity can not be industrialized and the thickness can not meet the use requirement, and provides a preparation method of a silicon nitride micro-ring resonant cavity for optical frequency combing; the method comprises the steps of firstly adopting a lateral epitaxial growth technology to obtain a high-quality silicon nitride thick waveguide layer, and then adopting a nanoimprint technology to realize waveguide pattern transfer with a pattern size of nanometer level so as to obtain the micro-ring resonant cavity with a high quality factor.
The purpose of the invention is realized by the following technical scheme.
The preparation method of the silicon nitride micro-ring resonant cavity for optical frequency combing comprises the following steps:
the method comprises the following steps: growing a layer of silicon dioxide film on the upper surface of the silicon wafer as a lower cladding;
step two: growing a layer of silicon nitride film on the upper surface of the lower cladding layer as a buffer layer;
step three: growing a layer of silicon dioxide film on the upper surface of the buffer layer to serve as a mask layer, preparing the mask layer into a long-strip-shaped, square-shaped or round periodic structure, wherein the depth of the periodic structure penetrates through the whole mask layer, the exposed silicon nitride buffer layer becomes a nucleation region of a silicon nitride waveguide layer grown next, and nucleation on the surface of the periodic pattern of the mask layer is reduced, so that unevenness of the surface of the waveguide layer caused by the growth of the film with the uneven surface is reduced, the accuracy of film thickness monitoring is facilitated, and a subsequent surface polishing process is avoided;
step four: growing a silicon nitride film on the buffer layer with the periodic structure in multiple steps to serve as a waveguide layer, carrying out high-temperature annealing after the growth is finished, and carrying out silicon nitride film growth again after cooling until the required thickness of the waveguide layer is reached;
step five: spin-coating a layer of polymer on the upper surface of the waveguide layer, performing nano-imprinting on the spin-coated polymer, forming at one time by adopting a nano-imprinting template matched with the substrate in size, and removing the nano-imprinting template after imprinting;
step six: transferring the polymer pattern to a silicon nitride waveguide layer by utilizing an inductively coupled plasma etching (ICP etching) process, organically cleaning a silicon wafer, removing the polymer, and completing pattern transfer to obtain a micro-ring structure and a strip waveguide structure;
step seven: and continuously growing a silicon dioxide film on the waveguide layer to serve as an upper cladding layer, thereby completing the preparation of the silicon nitride micro-ring resonant cavity.
The thickness of the silicon dioxide lower cladding layer is larger than 1 mu m, and the growth method adopts a wet oxidation method or Plasma Enhanced Chemical Vapor Deposition (PECVD).
The silicon nitride buffer layer is subjected to material growth by adopting PECVD or low-pressure chemical vapor deposition (LPCVD), and the thickness of the silicon nitride buffer layer is more than 200 nm.
The silicon dioxide mask layer growth method adopts PECVD, and the thickness is less than 1 mu m.
The preparation method of the periodic structure comprises pattern transfer means such as photoetching, nano-imprinting and the like.
The growth method of the silicon nitride waveguide layer adopts LPCVD, the growth temperature is higher than 1000 ℃, the annealing temperature is higher than 1000 ℃, and the single-time film growth thickness is (100-400) nm.
The total thickness of the silicon nitride waveguide layer is more than 600 nm.
The patterns formed by nanoimprint are micro-ring and strip waveguide structures.
The silicon dioxide upper cladding layer growth method adopts PECVD, and the thickness is more than 1 mu m.
Growing a layer of silicon dioxide film on the upper surface of the silicon wafer as a lower cladding; the thickness of the silicon dioxide lower cladding is more than 1 mu m, and the growth method adopts a wet oxidation method or PECVD; growing a silicon nitride film on the upper surface of the lower cladding as a buffer layer; the silicon nitride buffer layer is subjected to material growth by PECVD or LPCVD, and the thickness of the silicon nitride buffer layer is more than 200 nm; growing a layer of silicon dioxide film on the upper surface of the buffer layer to be used as a mask layer, and preparing the mask layer into a long-strip-shaped, square-shaped or round periodic structure; the silicon dioxide mask layer growth method adopts PECVD, and the thickness is less than 1 mu m; the preparation method of the periodic structure comprises pattern transfer means such as photoetching, nano-imprinting and the like; growing a silicon nitride film on the buffer layer with the periodic structure in multiple steps to serve as a waveguide layer, carrying out high-temperature annealing after the growth is finished, and carrying out silicon nitride film growth again after cooling until the required thickness of the waveguide layer is reached; the growth method of the silicon nitride waveguide layer adopts LPCVD, the growth temperature is more than 1000 ℃, the annealing temperature is more than 1000 ℃, and the single-time film growth thickness is (100-400) nm; the total thickness of the silicon nitride waveguide layer is more than 600 nm; spin-coating a layer of polymer on the upper surface of the waveguide layer, performing nano-imprinting on the spin-coated polymer to form a pattern, and removing the nano-imprinting template after the imprinting is finished; the patterns formed by the nano imprinting are micro-ring and strip waveguide structures; transferring the polymer pattern to a silicon nitride waveguide layer by utilizing an ICP (inductively coupled plasma) etching process, organically cleaning the silicon wafer, removing the polymer, and completing pattern transfer to obtain a micro-ring structure and a strip waveguide structure; continuously growing a silicon dioxide film on the waveguide layer to serve as an upper cladding layer, and completing the preparation of the silicon nitride micro-ring resonant cavity; the silicon dioxide upper cladding layer growth method adopts PECVD, and the thickness is more than 1 mu m.
Advantageous effects
The preparation method of the silicon nitride micro-ring resonant cavity for optical frequency combing adopts the lateral epitaxy technology, and utilizes the mask pattern to block the dislocation of the buffer layer and reduce the cracks of the silicon nitride thick waveguide layer, thereby reducing the scattering loss of the waveguide and improving the quality factor of the microcavity. The nano-imprinting technology provides a preparation method of a nano-scale and accurate micro-ring resonant cavity. The method avoids the write field splicing error introduced in the electron beam exposure, can also realize repeated pattern transfer, and reduces the process cost.
Drawings
FIG. 1 is a flow chart of the manufacturing process of the present invention;
fig. 2 is a schematic structural diagram of a micro-ring resonator.
Detailed Description
The invention is further described with reference to the following figures and examples.
Example 1
Referring to fig. 1 and 2, the present invention provides a method for preparing a silicon nitride micro-ring resonator for an optical frequency comb, comprising:
step 1: after cleaning a silicon wafer, growing a layer of silicon dioxide film on the upper surface of the silicon wafer as a substrate 1 to serve as a lower cladding 2, wherein the thickness of the lower cladding 2 is more than 1 mu m, and the growing method adopts a wet oxidation method or PECVD (plasma enhanced chemical vapor deposition);
step 2: growing a silicon nitride film on the upper surface of the lower cladding layer 2 to serve as a buffer layer 3, wherein the buffer layer 3 is subjected to material growth by adopting PECVD or LPCVD, the thickness is more than 200nm, and the reason for the larger thickness is to enable the silicon nitride layer to generate stress relaxation and reduce stress generated by lattice mismatch in the subsequent growth process;
and step 3: growing a layer of silicon dioxide film on the upper surface of a buffer layer 3 to be used as a mask layer, wherein the thickness of the mask layer is smaller than 1 mu m by adopting PECVD (plasma enhanced chemical vapor deposition), preparing the mask layer into a strip-shaped, square or round periodic structure 4, exposing the buffer layer 3 outside the periodic structure 4, and blocking cracks in the buffer layer 3 by using the periodic structure 4 made of silicon dioxide materials to prevent the cracks from extending upwards into a waveguide layer 5, wherein the periodic structure 4 is prepared by utilizing pattern transfer means such as photoetching or nanoimprint and the like and ICP (inductively coupled plasma) etching to form the periodic structure 4, and a periodic pattern exists in the whole chip range and has a distance of (2-20) mu m between the periodic pattern and an annular waveguide and a strip-shaped waveguide;
and 4, step 4: growing a silicon nitride film on the buffer layer 3 exposed outside the periodic structure 4 in multiple steps to serve as a waveguide layer 5, wherein the growth method of the silicon nitride waveguide layer 5 adopts LPCVD, the growth temperature is more than 1000 ℃, the single film growth thickness is (100-400) nm, high-temperature annealing is carried out after the growth is finished, the annealing temperature is more than 1000 ℃, the annealing time is 1-3 hours, annealing is carried out in a nitrogen atmosphere, the silicon nitride film is grown again after cooling until the required waveguide layer thickness is reached, and the total thickness of the silicon nitride waveguide layer is more than 600 nm;
and 5: spin-coating a layer of polymer on the upper surface of the waveguide layer 5, performing nano-imprinting on the spin-coated polymer to form a pattern, removing a nano-imprinting template after the imprinting is finished, wherein the pattern formed by the nano-imprinting is a micro-ring and strip waveguide structure;
and 6: transferring the polymer pattern to a silicon nitride waveguide layer 5 by utilizing an ICP (inductively coupled plasma) etching process, organically cleaning a silicon wafer, removing the polymer, and completing pattern transfer to obtain a micro-ring 8 and a strip waveguide 7;
and 7: and continuously growing a layer of silicon dioxide film on the waveguide layer 5 to serve as an upper cladding layer 6, wherein the silicon dioxide upper cladding layer is grown by adopting PECVD (plasma enhanced chemical vapor deposition) and the thickness of the silicon dioxide upper cladding layer is more than 1 mu m, and the preparation of the silicon nitride micro-ring resonant cavity is finished.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any modifications, equivalents, improvements, etc. made by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (8)
1. The preparation method of the silicon nitride micro-ring resonant cavity for the optical frequency comb is characterized by comprising the following steps of: the method comprises the following steps:
the method comprises the following steps: the substrate is sequentially provided with a lower cladding layer and a buffer layer;
step two: growing a mask layer on the upper surface of the buffer layer, preparing the mask layer into a periodic structure, wherein the depth of the periodic structure penetrates through the whole mask layer, the exposed silicon nitride buffer layer becomes a nucleation area of a silicon nitride waveguide layer grown next, and nucleation on the surface of a periodic pattern of the mask layer is reduced, so that unevenness of the surface waveguide layer caused by film growth on the uneven surface is reduced, accuracy of film thickness monitoring is facilitated, and a subsequent surface polishing process is avoided;
step four: growing a silicon nitride film on the buffer layer with the periodic structure in multiple steps to serve as a waveguide layer, carrying out high-temperature annealing after the growth is finished, and carrying out silicon nitride film growth again after cooling until the required thickness of the waveguide layer is reached;
step five: spin-coating a layer of polymer on the upper surface of the waveguide layer, performing nano-imprinting on the spin-coated polymer, forming at one time by adopting a nano-imprinting template matched with the substrate in size, and removing the nano-imprinting template after imprinting;
step six: transferring the polymer pattern to a silicon nitride waveguide layer by using an inductive coupling plasma etching process, organically cleaning the silicon wafer, removing the polymer, and completing pattern transfer to obtain a micro-ring structure and a strip waveguide structure;
step seven: and continuously growing a silicon dioxide film on the waveguide layer to serve as an upper cladding layer, thereby completing the preparation of the silicon nitride micro-ring resonant cavity.
2. The method of claim 1 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: the lower cladding is a layer of silicon dioxide film growing on the upper surface of the silicon chip; the buffer layer is a silicon nitride film grown on the upper surface of the lower cladding layer.
3. The method of claim 2 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: and step two, the mask layer is a silicon dioxide film.
4. The method of claim 3 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: the thickness of the silicon dioxide lower cladding is more than 1 mu m, and the growth method adopts a wet oxidation method or Plasma Enhanced Chemical Vapor Deposition (PECVD); the silicon nitride buffer layer adopts PECVD or low-pressure chemical vapor deposition (LPCVD) to carry out material growth, and the thickness is more than 200 nm; the silicon dioxide mask layer growth method adopts plasma enhanced chemical vapor deposition, and the thickness is less than 1 mu m; the growth method of the silicon nitride waveguide layer adopts low-pressure chemical vapor deposition, the growth temperature is higher than 1000 ℃, the annealing temperature is higher than 1000 ℃, and the single-time film growth thickness is (100-400) nm; the silicon dioxide upper cladding layer growth method adopts PECVD, and the thickness is more than 1 mu m.
5. The method of claim 1 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: the preparation method of the periodic structure comprises photoetching and nano-imprinting.
6. The method of claim 1 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: the total thickness of the silicon nitride waveguide layer is more than 600 nm.
7. The method of claim 1 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: the patterns formed by nano-imprinting are micro-ring and strip waveguide structures.
8. The method of claim 1 for preparing a silicon nitride micro-ring resonator for an optical frequency comb, wherein: growing a layer of silicon dioxide film on the upper surface of the silicon wafer as a lower cladding; the thickness of the silicon dioxide lower cladding is more than 1 mu m, and the growth method adopts a wet oxidation method or PECVD (plasma enhanced chemical vapor deposition); growing a silicon nitride film on the upper surface of the lower cladding as a buffer layer; the silicon nitride buffer layer is subjected to material growth by adopting PECVD or LPCVD, and the thickness is more than 200 nm; growing a layer of silicon dioxide film on the upper surface of the buffer layer to be used as a mask layer, and preparing the mask layer into a long-strip-shaped, square-shaped or round periodic structure; the silicon dioxide mask layer growth method adopts PECVD, and the thickness is less than 1 mu m; the preparation method of the periodic structure comprises photoetching and nano-imprinting; growing a silicon nitride film on the buffer layer with the periodic structure in multiple steps to serve as a waveguide layer, carrying out high-temperature annealing after the growth is finished, and carrying out silicon nitride film growth again after cooling until the required thickness of the waveguide layer is reached; the growth method of the silicon nitride waveguide layer adopts LPCVD, the growth temperature is more than 1000 ℃, the annealing temperature is more than 1000 ℃, and the single-time film growth thickness is (100-400) nm; the total thickness of the silicon nitride waveguide layer is more than 600 nm; spin-coating a layer of polymer on the upper surface of the waveguide layer, performing nano-imprinting on the spin-coated polymer to form a pattern, and removing the nano-imprinting template after the imprinting is finished; the patterns formed by nanoimprint lithography are micro-ring and strip waveguide structures; transferring the polymer pattern to a silicon nitride waveguide layer by using an inductive coupling plasma etching process, organically cleaning the silicon wafer, removing the polymer, and completing pattern transfer to obtain a micro-ring structure and a strip waveguide structure; continuously growing a silicon dioxide film on the waveguide layer to serve as an upper cladding layer, and completing the preparation of the silicon nitride micro-ring resonant cavity; the silicon dioxide upper cladding layer growth method adopts PECVD, and the thickness is more than 1 mu m.
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