CN113484941A - Method for preparing microlens array coupling reflecting layer structure - Google Patents
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Abstract
The invention provides a preparation method of a micro-lens array coupling reflection layer structure, which is characterized by comprising the following steps: preparing a micro-lens array on a substrate, wherein the micro-lens array comprises quantum dots and an upper cover layer covering the quantum dots, and the surface of the upper cover layer is a raised structure in periodic array arrangement; and peeling the micro lens array from the substrate and transferring the micro lens array onto a broad spectrum reflecting layer to form the micro lens array coupling reflecting layer structure. The invention combines the stripping process to couple the micro-lens array and the reflecting layer structure, and can realize the extraction efficiency of 60 percent. The peeling and transferring process does not need to grow a DBR structure with more pairs, can realize higher extraction efficiency compared with a lower DBR structure, has great advantages in the aspects of subsequent piezoelectric tuning and the like, and has great practical application value and wide application prospect in the fields of quantum light sources, light-emitting diodes, photoelectric detectors and the like.
Description
Technical Field
The invention relates to the technical field of semiconductor materials and devices, in particular to a method for preparing a micro-lens array based on wet etching.
Background
Quantum light sources are key devices for quantum computing, quantum communication, quantum sensing and other applications. The semiconductor quantum dots epitaxially grown by the S-K (Stranski-Krastanov) growth mode have discrete energy levels similar to atoms due to three-dimensional limitation, wherein the discrete two-level transition can prepare a quantum light source which only emits one photon at a time; moreover, the single photon emitted by the semiconductor quantum dot two-level transition has the characteristics of excellent luminous intensity, extremely narrow spectral line width and easiness in multi-physical field adjustment, is easy for light integration, and has huge application prospect in the fields of solid-state quantum physics and quantum information devices. The quantum dot light emission is distributed in the whole space, and the total reflection on the surface of the GaAs body material (the GaAs refractive index is 3.5, and the air is only 1.0, so the total reflection angle is extremely small) causes most of the quantum dot light emission to be totally reflected and dissipated in the body, the photon extraction efficiency is very low (lower than 2%), and the output counting rate is far lower than the intrinsic counting rate. How to improve the extraction efficiency of the semiconductor quantum dots is a technical problem to be overcome urgently in the practical application process of realizing the quantum dot single photon source. In recent years, three types of micro-nano optical structures are mainly developed to improve the photon extraction efficiency: Fabry-Perot micro-column cavity, a bull's eye ring structure and a micro-lens. The micro lens is not limited to a specific space mode or a specific spectrum mode, improves photon extraction efficiency by geometrically converging divergent light into parallel light, is suitable for on-chip high-density batch preparation, and has wide application value in the field of quantum entanglement due to the wide-spectrum enhancement characteristic.
Currently, a common method for fabricating microlenses is to form the microlens topography using in-situ electron beam exposure and plasma etching (ICP). However, the micro-lens prepared by the dry preparation method has rough surface, high positioning precision requirement (below 50 nm) of the whole preparation process, complex process and incapability of preparing a large amount of micro-lens arrays at one time. And the DBR reflecting structure has lower extraction efficiency for the micro-lens array, the preparation of the DBR reflecting structure is more complex, a multilayer structure with more logarithm needs to be grown, and the practicability is lower.
Disclosure of Invention
Technical problem to be solved
In view of the above, the main objective of the present invention is to provide a method for preparing a microlens array coupling reflection layer structure based on wet etching, so as to implement one-time batch preparation of on-chip microlens arrays, couple the microlens arrays to a broad-spectrum reflection layer, greatly improve photon extraction efficiency, and provide a technical basis for the practicality of semiconductor quantum dot single photon sources.
(II) technical scheme
The invention provides a preparation method of a micro-lens array coupling reflection layer structure, which comprises the following steps: preparing a micro-lens array on a substrate, wherein the micro-lens array comprises quantum dots and an upper cover layer covering the quantum dots, and the surface of the upper cover layer is a raised structure in periodic array arrangement; and peeling the micro lens array from the substrate and transferring the micro lens array onto a broad spectrum reflecting layer to form the micro lens array coupling reflecting layer structure.
Optionally, the preparing the microlens array on the substrate includes: sequentially forming a buffer layer, a sacrificial layer, quantum dots and an upper cover layer on a substrate; processing the surface of the upper cover layer to form a mask layer with a circular periodic array; and corroding the mask layer and the upper cover layer to form a micro-lens array.
Optionally, the peeling the microlens array from the substrate and transferring onto the broad spectrum reflection layer comprises: dissociating the substrate to form small-sized substrates; coating a black wax protective layer on the surface of the micro-lens array of the substrate; etching the sacrificial layer by using HF (hydrogen fluoride) so that the substrate and the buffer layer are stripped; the microlens array was transferred to a broad spectrum reflective layer and the black wax protective layer was removed.
Optionally, the broad spectrum reflective layer comprises Au or Ag.
Optionally, the processing the surface of the upper cover layer to form the mask layer with the circular periodic array includes: a negative photoresist is spin-coated on the surface of the upper cover layer; carrying out optical exposure, development and fixation on the negative photoresist to form a circular periodic array hole; depositing a dielectric layer; and stripping and removing the negative photoresist and the dielectric layer outside the circular periodic array holes to form the mask layer.
Optionally, the etching the mask layer and the upper cover layer to form a microlens array includes: preparing a corrosive liquid, wherein the composition of the corrosive liquid is H2O2：H2SO4：H2O; and carrying out anisotropic acid corrosion on the mask layer and the upper cover layer by adopting the corrosive liquid to form a micro-lens array.
Optionally, the volume ratio of the prepared corrosive liquid is H2O2：H2SO4：H2O＝(0.1～10)∶(100～400)∶1000。
Optionally, the sequentially forming a buffer layer, a sacrificial layer, a quantum dot, and an upper cover layer on the substrate includes: and epitaxially growing a GaAs buffer layer, an AlGaAs sacrificial layer, quantum dots and a GaAs upper cover layer on the GaAs substrate.
Optionally, the dielectric layer is deposited by a low-temperature evaporation sputtering process, and the dielectric layer comprises silicon dioxide or silicon nitride material.
Optionally, the stripping away the negative photoresist and the dielectric layer outside the circular periodic array of holes comprises: and sequentially removing the negative photoresist and the dielectric layer outside the circular periodic array holes by adopting acetone and ethanol solution.
(III) advantageous effects
The microlens array prepared by the wet etching method has good surface roughness and low preparation process cost, and is convenient for mass preparation.
The invention adopts the photoetching method of photoetching the circular periodic array holes, then growing the dielectric layer and stripping the dielectric layer in the area outside the circular periodic array holes to form the circular periodic array dielectric layer, thereby avoiding the defect that the subsequent process can not be carried out due to the unclean dielectric layer removal.
The invention adopts the reflecting layer arranged below the quantum dots to reflect the light emitted from the back of the quantum dots, thereby improving the lower surface emission of the quantum dots and improving the light-emitting and collecting efficiency of the quantum dots.
The invention combines the stripping process to couple the micro-lens array and the reflecting layer structure, and can realize the extraction efficiency of 60 percent. In addition, the stripping and transferring process does not need to grow a DBR structure with more pairs, can realize higher extraction efficiency compared with a lower DBR structure, and has great advantages in the aspects of subsequent piezoelectric tuning and the like. The method has great practical application value and wide application prospect in the fields of quantum light sources, light-emitting diodes, photoelectric detectors and the like.
Drawings
FIG. 1 is a flow chart of a method for fabricating a microlens array coupled reflective layer structure provided by the present invention;
FIG. 2 is a schematic structural diagram of a microlens array coupling reflection layer structure according to an embodiment of the present invention;
fig. 3 schematically illustrates a process for preparing a microlens array coupling reflection layer structure according to an embodiment of the present invention.
[ description of reference ]
1-a substrate; 2-a broad spectrum reflective layer; 3-quantum dots; 4-a microlens array;
5-a substrate; 6-a buffer layer; 7-a sacrificial layer; 8-an upper cover layer; 9-a mask layer; 10-protective layer.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.
The invention provides a preparation method of a micro-lens array coupling reflection layer structure, which comprises the following steps: preparing a micro-lens array on a substrate, wherein the micro-lens array comprises quantum dots and an upper cover layer for coating the quantum dots, and the surface of the upper cover layer is a raised structure which is periodically arrayed; and peeling the micro lens array from the substrate and transferring the micro lens array onto the broad spectrum reflecting layer to form a micro lens array coupling reflecting layer structure.
The invention adopts the reflecting layer arranged below the quantum dots to reflect the light emitted from the back of the quantum dots, thereby improving the lower surface emission of the quantum dots and improving the light-emitting and collecting efficiency of the quantum dots. Meanwhile, the micro-lens array and the reflecting layer structure are coupled by combining the stripping process, so that the extraction efficiency can reach 60%. In addition, the stripping and transferring process does not need to grow a DBR structure with more pairs, can realize higher extraction efficiency compared with a lower DBR structure, and has great advantages in the aspects of subsequent piezoelectric tuning and the like. The method has great practical application value and wide application prospect in the fields of quantum light sources, light-emitting diodes, photoelectric detectors and the like.
Further, the preparing the microlens array on the substrate includes: sequentially forming a buffer layer, a sacrificial layer, quantum dots and an upper cover layer on a substrate; processing the surface of the upper cover layer to form a mask layer with a circular periodic array; and corroding the mask layer and the upper cover layer to form the micro-lens array.
In an embodiment of the present invention, referring to fig. 1, the method for manufacturing the microlens array coupled reflective layer structure includes 5 main steps:
and S1, sequentially forming a buffer layer, a sacrificial layer, quantum dots and an upper cover layer on the substrate.
And S2, processing the surface of the upper cover layer to form a mask layer with a circular periodic array.
And S3, etching the mask layer and the upper cover layer to form the micro-lens array.
And S4, stripping the substrate of the micro lens array.
And S5, transferring the micro-lens array to the broad spectrum reflecting layer to form a micro-lens array coupling reflecting layer structure.
Specifically, the preparation of the microlens array on the substrate includes mainly 3 steps of S1, S2, and S3. The buffer layer is formed on the substrate, mainly for filling the deoxidized substrate and reducing the defects. And the quantum dots are covered by the capping layer. By processing the surface appearance of the upper cover layer, the upper cover layer is provided with a raised structure in periodic array arrangement, namely a micro lens array, as shown in fig. 2, a reflecting layer 2 is arranged on a substrate 1, and a quantum dot is coated by a micro lens array 4 to focus light emitted by the quantum dot, so that the vertical light emitting efficiency of the quantum dot light emitting is improved. Meanwhile, the reflecting layer 2 positioned below the quantum dots is a broad-spectrum reflecting layer, and reflects most of light emitted from the quantum dots close to the reflecting layer, so that the micro-lens array 4 focuses the light, and the light-emitting collecting capacity is enhanced.
The conventional method adopts a dry process preparation method, namely, an electron beam Exposure (EBL) is utilized, the electron beam exposure dose is gradually changed in a concentric circle mode to form a pattern of a micro mask, and a micro lens array is formed on a material after ICP etching. Compared with the method for preparing the micro lens by dry etching, the method for preparing the micro lens array has the advantages that the surface of the micro lens is smoother, the requirement on the precision of the preparation process is lower, the optical shape of the lens is more accurate and controllable, and a large number of micro lens arrays can be prepared at one time. Further, the micro-lens array coupling broad spectrum reflecting layer structure can greatly improve the photon extraction efficiency from 2% to 60%.
In an embodiment of the invention, referring to fig. 3, a schematic process diagram of a method for manufacturing a microlens array coupling reflection layer structure according to the invention is shown.
Firstly, the invention forms the structure of the buffer layer 4, the sacrificial layer 7, the quantum dot 3 and the upper cover layer 8 on the substrate 5 in sequence, which can be selected as follows: and epitaxially growing a GaAs buffer layer, an AlGaAs sacrificial layer, InAs quantum dots and a GaAs upper cover layer on the GaAs substrate. The structure is prepared in an epitaxial growth mode, and the GaAs buffer layers grow on the GaAs substrate in a homoepitaxial growth mode and then grow sequentially.
In the embodiment of the invention, the growth temperature of the InAs quantum dots is 500-600 ℃, the growth time is 3-7 min, and the growth rate is 0.005 ML/s; the thickness of the GaAs upper cover layer is 400-1000 nm.
Furthermore, in this embodiment of the present invention, the processing of the surface of the upper cover layer 8 to form the mask layer with a circular periodic array includes: the surface of the upper cover layer 8 is spin-coated with negative photoresist; carrying out optical exposure, development and fixation on the negative photoresist to form a circular periodic array hole; depositing a dielectric layer; and stripping and removing the negative photoresist and the dielectric layer outside the circular periodic array holes to form the mask layer 9.
Specifically, after the circular periodic array of holes of the upper cover layer 8 is formed by a negative photoresist, a low temperature evaporation sputtering process may be used to deposit a dielectric layer, which may comprise silicon dioxide or silicon nitride material. And then sequentially removing the negative photoresist and the dielectric layer outside the circular periodic array holes by adopting acetone and ethanol solution to form a circular periodic array mask layer 9, wherein the circular mask layer has a larger size, in one embodiment of the invention, the diameter of the circular mask layer is 2.5-4 microns, the thickness of the circular mask layer is 100-300 nm, and the interval of the circular periodic array mask layer is 10-100 microns. Therefore, BOE (Buffered Oxide Etch) is needed to be used to further reduce the circular size of the periodic array of the mask layer 9 to 1-3 μm. Wherein, the main component of the etching solution adopted by BOE etching is NH4F4HF and H2And O, the corrosion time is 10-30 seconds. In another embodiment of the present invention, acetone and ethanol solution are sequentially used to remove the negative photoresist and the mask layer 9 except the circular periodic array of holes, and the processing time is 5-20 min.
The invention adopts the photoetching method of photoetching the circular periodic array holes, then growing the dielectric layer and stripping the dielectric layer in the area outside the circular periodic array holes to form the circular periodic array dielectric layer, thereby avoiding the defect that the subsequent process can not be carried out due to the unclean dielectric layer removal.
The wet etching method comprises the following steps: preparing corrosive liquid, wherein the composition of the corrosive liquid is H2O2：H2SO4：H2O; and performing anisotropic acid corrosion on the mask layer and the upper cover layer by using a corrosive liquid to form the micro-lens array. Based on concentrated H2SO4Two-step reaction principle of corrosion liquid formula with extremely dilute H2O2To induce the catalyst, preferential etch formation at the boundaries of the mask layer of a circular periodic array of reduced diameterAnd (4) performing underetching, further performing underetching to form a structure similar to a mask layer microdisk by using an underetched side wall as a base through a capillary effect, and further performing corrosion or removing a mask layer top cover through nitrogen purging to form the microlens array 4. Wherein, the volume ratio adopted for preparing the corrosive liquid is H2O2：H2SO4：H2O is (0.1-10): (100-400): 1000; the temperature of anisotropic acid corrosion is 60-90 ℃; the etching time is 30-100 min.
For the corrosion temperature of anisotropic acid corrosion, if the temperature is too low, the corrosion rate is low, so that the preparation efficiency of the micro-lens array is poor, and if the temperature is too high, the reaction speed is too high, so that the final appearance of the micro-lens array is not easy to accurately control, and therefore, the corrosion temperature of 60-90 ℃ is selected as the proper corrosion temperature in comprehensive consideration.
For the etching time of the anisotropic acid etching, if the time is too short, the shape of the micro lens cannot be formed, and if the time is too long, the etching depth is too deep to damage the structure, and the etching time is selected to be 30-100 min as the appropriate etching time in comprehensive consideration.
After the microlens array 4 is fabricated on the substrate, the microlens array 4 is peeled off from the substrate 5 and transferred onto the broad spectrum reflection layer 2, which in one embodiment of the present invention comprises: dissociating the substrate to form small-sized substrates; coating a black wax protective layer 10 on the surface of the micro-lens array 4 of the substrate; etching the sacrificial layer 7 with HF to peel off the substrate 5 and the buffer layer 2; the microlens array was transferred to the broad spectrum reflective layer and the black wax protective layer 10 was removed. According to the method, the substrate is stripped through HF selective corrosion of the sacrificial layer 7, and the stripped micro-lens array layer is transferred to the substrate of the broad-spectrum reflecting layer, so that a micro-lens array 4 coupling back reflecting layer 2 structure is formed. The broad spectrum reflective layer material comprises Au or Ag.
Specifically, when the sacrificial layer 7 is AlGaAs, the substrate with the microlens array is firstly dissociated into small pieces of about 10 × 10mm, and the surface of the substrate is coated with a black wax protective layer to protect the prepared microlens array structure; and selectively corroding the AlGaAs sacrificial layer for 1-10 h by using 7.5% HF corrosive liquid to strip the original substrate.
The peeling and transferring process does not need to grow a DBR structure with more pairs, can realize higher extraction efficiency compared with a lower DBR structure, and has great advantages in the aspects of subsequent piezoelectric tuning and the like. The method has great practical application value and wide application prospect in the fields of quantum light sources, light-emitting diodes, photoelectric detectors and the like.
It is to be noted that, in the attached drawings or in the description, the implementation modes not shown or described are all the modes known by the ordinary skilled person in the field of technology, and are not described in detail. Further, the above definitions of the various elements and methods are not limited to the various specific structures, shapes or arrangements of parts mentioned in the examples, which may be easily modified or substituted by those of ordinary skill in the art.
It should also be noted that directional terms, such as "upper", "lower", "front", "rear", "left", "right", etc., used in the embodiments are only directions referring to the drawings, and are not intended to limit the scope of the present invention. Throughout the drawings, like elements are represented by like or similar reference numerals. Conventional structures or constructions will be omitted when they may obscure the understanding of the present invention.
And the shapes and sizes of the respective components in the drawings do not reflect actual sizes and proportions, but merely illustrate contents of the embodiments of the present invention. Furthermore, in the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. Unless otherwise indicated, the numerical parameters set forth in the specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by the present invention. In particular, all numbers expressing quantities of ingredients, reaction conditions, and so forth used in the specification and claims are to be understood as being modified in all instances by the term "about". Generally, the expression is meant to encompass variations of ± 10% in some embodiments, 5% in some embodiments, 1% in some embodiments, 0.5% in some embodiments by the specified amount.
Furthermore, the word "comprising" does not exclude the presence of elements or steps not listed in a claim. The word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements.
The use of ordinal numbers such as "first," "second," "third," etc., in the specification and claims to modify a corresponding element does not by itself connote any ordinal number of the element or any ordering of one element from another or the order of manufacture, and the use of the ordinal numbers is only used to distinguish one element having a certain name from another element having a same name.
In addition, unless steps are specifically described or must occur in sequence, the order of the steps is not limited to that listed above and may be changed or rearranged as desired by the desired design. The embodiments described above may be mixed and matched with each other or with other embodiments based on design and reliability considerations, i.e., technical features in different embodiments may be freely combined to form further embodiments.
Similarly, it should be appreciated that in the foregoing description of exemplary embodiments of the invention, various features of the invention are sometimes grouped together in a single embodiment, figure, or description thereof for the purpose of streamlining the invention and aiding in the understanding of one or more of the various disclosed aspects. However, the disclosed method should not be interpreted as reflecting an intention that: that the invention as claimed requires more features than are expressly recited in each claim. Rather, as the following claims reflect, disclosed aspects lie in less than all features of a single foregoing disclosed embodiment. Thus, the claims following the detailed description are hereby expressly incorporated into this detailed description, with each claim standing on its own as a separate embodiment of this invention.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing a micro-lens array coupling reflection layer structure is characterized by comprising the following steps:
preparing a micro-lens array on a substrate, wherein the micro-lens array comprises quantum dots and an upper cover layer covering the quantum dots, and the surface of the upper cover layer is a raised structure in periodic array arrangement;
and peeling the micro lens array from the substrate and transferring the micro lens array onto a broad spectrum reflecting layer to form the micro lens array coupling reflecting layer structure.
2. The method of claim 1, wherein the fabricating the microlens array on the substrate comprises:
sequentially forming a buffer layer, a sacrificial layer, quantum dots and an upper cover layer on a substrate;
processing the surface of the upper cover layer to form a mask layer with a circular periodic array;
and corroding the mask layer and the upper cover layer to form a micro-lens array.
3. The method of claim 2, wherein the step of peeling the microlens array off the substrate and transferring the microlens array onto the broad spectrum reflective layer comprises:
dissociating the substrate to form small-sized substrates;
coating a black wax protective layer on the surface of the micro-lens array of the substrate;
etching the sacrificial layer by using HF (hydrogen fluoride) so that the substrate and the buffer layer are stripped;
the microlens array was transferred to a broad spectrum reflective layer and the black wax protective layer was removed.
4. The method according to claim 1, wherein the broad spectrum reflective layer comprises Au or Ag.
5. The method of claim 2, wherein the processing the surface of the cap layer to form the circular periodic array of mask layers comprises:
a negative photoresist is spin-coated on the surface of the upper cover layer;
carrying out optical exposure, development and fixation on the negative photoresist to form a circular periodic array hole;
depositing a dielectric layer;
and stripping and removing the negative photoresist and the dielectric layer outside the circular periodic array holes to form the mask layer.
6. The method of claim 5, wherein the etching the mask layer and the cap layer to form the microlens array comprises:
preparing a corrosive liquid, wherein the composition of the corrosive liquid is H2O2：H2SO4：H2O；
And carrying out anisotropic acid corrosion on the mask layer and the upper cover layer by adopting the corrosive liquid to form a micro-lens array.
7. The preparation method according to claim 6, wherein the prepared corrosive liquid is prepared by a volume ratio of H2O2∶H2SO4∶H2O＝(0.1～10)∶(100～400)∶1000。
8. The method of claim 2, wherein the sequentially forming the buffer layer, the sacrificial layer, the quantum dot, and the upper cap layer on the substrate comprises:
and epitaxially growing a GaAs buffer layer, an AlGaAs sacrificial layer, quantum dots and a GaAs upper cover layer on the GaAs substrate.
9. The method of claim 5, wherein the dielectric layer is deposited using a low temperature evaporation sputtering process, and the dielectric layer comprises a silicon dioxide or silicon nitride material.
10. The method of claim 5, wherein the stripping away the negative photoresist and the dielectric layer outside the circular periodic array of holes comprises:
and sequentially removing the negative photoresist and the dielectric layer outside the circular periodic array holes by adopting acetone and ethanol solution.
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| CN102983230A (en) * | 2011-09-06 | 2013-03-20 | 三星电子株式会社 | Method of manufacturing quantum dot layer, transfer method, and quantum dot optoelectronic device |
| CN110346931A (en) * | 2019-01-28 | 2019-10-18 | 中山大学 | A kind of certainty quantum light source device and its preparation method and application combining lenticule based on golden reflecting layer |
| CN111403567A (en) * | 2020-04-01 | 2020-07-10 | 中国科学院半导体研究所 | Quantum dot single photon source and wet etching preparation method of microlens array thereof |
| CN112993096A (en) * | 2021-01-20 | 2021-06-18 | 中国石油大学(华东) | Method for processing single photon source integrated device |
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| CN102983230A (en) * | 2011-09-06 | 2013-03-20 | 三星电子株式会社 | Method of manufacturing quantum dot layer, transfer method, and quantum dot optoelectronic device |
| CN110346931A (en) * | 2019-01-28 | 2019-10-18 | 中山大学 | A kind of certainty quantum light source device and its preparation method and application combining lenticule based on golden reflecting layer |
| CN111403567A (en) * | 2020-04-01 | 2020-07-10 | 中国科学院半导体研究所 | Quantum dot single photon source and wet etching preparation method of microlens array thereof |
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