CN115000279A - Quantum dot color conversion layer microarray and preparation method and application thereof - Google Patents
Quantum dot color conversion layer microarray and preparation method and application thereof Download PDFInfo
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Abstract
According to the quantum dot color conversion layer microarray and the preparation method and application thereof disclosed by the invention, the nano-pore structure is prepared to be used as the quantum dot bearing layer, and the light blocking material is filled in the pixel channel, so that the quantum dots are uniformly dispersed, and the light intensity and the light purity are effectively improved; the preparation method has the advantages of simple process flow, high operability and wide application range; the full-color display device prepared by combining the quantum dot color conversion layer microarray prepared by the invention and the GaN-based blue light Micro-LED microarray avoids the technical bottleneck of mass transfer of red and green, reduces the production cost and improves the production efficiency.
Description
Technical Field
The invention belongs to the technical field of Micro LED display, and particularly relates to a quantum dot color conversion layer microarray. The invention also relates to a preparation method of the quantum dot color conversion layer microarray. The invention further relates to an application of the quantum dot color conversion layer microarray.
Background
Micro LEDs are considered to replace next generation display technology for LCD and OLED displays. On the basis of high LED efficiency, the Micro LED has the advantages of high pixel, high contrast, self-luminescence, low energy consumption, long service life and the like. However, the current challenge of Micro LED display technology in manufacturing is still a huge transfer process, how to prepare Micro red, green and blue Micro LED chips, and how to place the three-color chips on the driving panel quickly and accurately limits the way of mass production of Micro LEDs. In order to avoid the process bottleneck of mass transfer, many current research reports mainly focus on using quantum dot materials to prepare color conversion layers to realize full-color display of Micro LEDs, such as schemes of depositing quantum dot films, quantum dot photoresists and the like, but all have the problems of poor dispersion uniformity of quantum dots, low purity and intensity of red light and green light and the like.
Disclosure of Invention
The invention aims to provide a quantum dot color conversion layer microarray, which solves the problems of poor dispersion uniformity of quantum dots and low purity and intensity of red light and green light in the existing scheme.
The invention also aims to provide a preparation method of the quantum dot color conversion layer microarray, which has the advantages of simple process flow and high operability and can be suitable for preparing devices with various sizes.
The invention further aims to provide application of the quantum dot color conversion layer microarray to a full-color Micro LED device, and the application prospect is wide.
The first technical scheme adopted by the invention is as follows: quantum dot color conversion layer microarray, including the GaN epitaxial layer, seted up grid shape channel on the GaN epitaxial layer, the nanometer pore structure has all been seted up in the single GaN epitaxial layer pixel region that grid shape channel separation formed, has injected red quantum dot and green quantum dot respectively into in the nanometer pore structure of two in the adjacent three GaN epitaxial layer pixel region.
The first technical solution of the present invention is also characterized in that,
the nano-pore structure is a plurality of long-strip holes and is vertically arranged in the pixel point region of the single GaN epitaxial layer.
And black epoxy resin glue is filled in the grid-shaped channel and is used for preventing optical crosstalk among the GaN pixel points.
And a water-oxygen barrier layer is arranged above the GaN epitaxial layer to protect the stability of the quantum dot material in the nanopore structure.
The GaN epitaxial layer grows on a Si or sapphire substrate, the GaN epitaxial layer sequentially comprises a buffer layer, an intrinsic GaN layer, a first N-type GaN layer and a second N-type GaN layer from bottom to top, the bottom end of a channel is arranged to the first N-type GaN layer, the depth of the channel cannot exceed the depth of the first N-type GaN layer, and a thin layer of the first N-type GaN layer needs to be reserved to serve as a current conduction layer of an electrochemical corrosion process.
The second technical scheme adopted by the invention is as follows: the preparation method of the quantum dot color conversion layer microarray comprises the following steps:
step 1, growing a silicon film layer on a GaN epitaxial layer of a Si or sapphire substrate by utilizing Plasma Enhanced Chemical Vapor Deposition (PECVD). The GaN epitaxial layer is prepared by Metal Organic Chemical Vapor Deposition (MOCVD), the structure of the GaN epitaxial layer from bottom to top is a buffer layer, an intrinsic GaN layer, a first N-type GaN layer and a second N-type GaN layer in sequence, and the thickness of each structural layer is determined according to specific process design;
step 2, spinning and coating negative photoresist on the silicon film layer in the step 1, wherein the photomask plate graph is a pixel point microarray graph, the size and the interval of the pixel points can be designed according to the matched pixel point size of the Micro LED microarray, and the photoresist microarray is obtained after exposure and development by using an ultraviolet contact type exposure machine;
step 3, evaporating a metal Cr film layer on the photoresist microarray in the step 2 by using a vacuum electron beam evaporation device (Ebeam) as a hard mask, wherein the thickness of the metal Cr film layer is set according to the depth of etching GaN; carrying out a negative photoresist metal stripping process after the metal Cr film layer is evaporated, stripping and removing Cr metal at the pixel point spacing, and forming a metal Cr microarray after stripping;
step 4, taking the metal Cr microarray in the step 3 as a hard mask, and etching the silicon film layer by utilizing Inductively Coupled Plasma (ICP) to form a metal Cr and silicon composite microarray;
step 5, etching the GaN epitaxial layer by utilizing ICP (inductively coupled plasma) by taking the metal Cr and silicon composite microarray obtained in the step 4 as a hard mask, wherein the etching depth sequentially penetrates through the whole second N-type GaN layer from top to bottom, and the etching is stopped until the first N-type GaN layer is etched to form a GaN microarray; the first N-type GaN layer has a residual thin layer thickness and is used as a current conducting layer of a subsequent electrochemical corrosion process;
step 6, coating black epoxy resin glue in the GaN microarray in the step 5 in a spinning mode, ensuring that the black epoxy resin glue can be completely infiltrated into a channel of the GaN microarray, and curing the black epoxy resin glue;
step 7, performing a thinning and polishing process of black epoxy resin adhesive on the GaN microarray obtained in the step 6 by using Chemical Mechanical Polishing (CMP) until the metal Cr film layer and the silicon film layer are completely removed and the second N-type GaN layer is exposed;
step 8, performing electrochemical corrosion on the GaN microarray in the step 7 by using an anodic oxidation machine, wherein an oxalic acid solution can be selected as a corrosive liquid, the concentration of the oxalic acid can be selected to be 10-80%, the corrosion voltage can be selected to be 1-50V, the corrosion depth of the GaN nanopore structure is determined according to parameters such as the concentration of the corrosive solution, the corrosion voltage and the corrosion duration, and the GaN nanopore structure microarray which is approximately vertical is obtained after corrosion;
step 9, spin-coating a positive photoresist on the surface of the GaN nanopore structure microarray, firstly defining a red color conversion region on the GaN nanopore structure microarray by utilizing ultraviolet lithography, injecting red quantum dots into a nanopore structure of the red color conversion region by utilizing spraying equipment, then defining a green color conversion region and injecting green quantum dots, and finally forming an RGB array;
and step 10, sputtering and depositing a water-oxygen barrier layer on the RGB array in the step 9 by using magnetron sputtering (Sputter) to protect the stability of the quantum dot material in the nanopore structure, wherein the thickness of the water-oxygen barrier layer is determined according to the protection effect.
The second technical solution of the present invention is also characterized in that,
the vacuum infiltration and solidification in the step 6 are specifically as follows: and vacuumizing the GaN microarray subjected to spin coating for 10-20 min in vacuum equipment, wherein the vacuum degree range can be 0.01-0.1 Pa, so that the black epoxy resin adhesive can be better soaked into a channel of the GaN microarray, and then curing for 1-2 h at the temperature of 100-130 ℃.
The thinning and polishing in the step 7 are divided into 2 stages, in the first stage, the silicon film layer is used as a first stop layer for the chemical mechanical polishing of the black epoxy resin adhesive, and the black epoxy resin adhesive is polished until the silicon film layer stops polishing; in the second stage, a second N-type GaN layer is used as a second stop layer for the chemical mechanical polishing of the black epoxy resin adhesive, and the black epoxy resin adhesive is polished until the silicon film layer is completely removed and the second N-type GaN layer is exposed;
the silicon film layer is a silicon oxide film layer or a silicon nitride film layer and is used as a hard mask for etching the gallium nitride material; the water-oxygen barrier layer is a silicon nitride film layer or other compact medium materials, and the service life of the quantum dots is protected.
The third technical scheme adopted by the invention is as follows: the application of the quantum dot color conversion layer microarray is characterized in that the quantum dot color conversion layer microarray and a matched GaN-based Micro LED microarray device are bonded in an alignment mode to form a full-color Micro LED device.
The invention has the beneficial effects that: according to the quantum dot color conversion layer microarray and the preparation method thereof, the nano-pore structure is prepared to serve as the quantum dot bearing layer, and the light blocking material is filled in the pixel channel, so that quantum dots are uniformly dispersed, and the light intensity and the light purity are effectively improved; the preparation method has the advantages of simple process flow, high operability and wide application range; the full-color display device prepared by combining the quantum dot color conversion layer microarray prepared by the invention and the GaN-based blue light Micro-LED microarray avoids the technical bottleneck of mass transfer of red and green, reduces the production cost and improves the production efficiency.
Drawings
FIG. 1 is a flow chart of a method of making a quantum dot color conversion layer microarray of the present invention;
FIG. 2 is a schematic structural diagram of the quantum dot color conversion layer microarray of the present invention obtained in step 1;
FIG. 3 is a schematic diagram of the structure obtained in step 2 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 4 is a schematic structural diagram of the quantum dot color conversion layer microarray of the present invention obtained in step 3;
FIG. 5 is a schematic diagram of the structure obtained in step 4 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 6 is a schematic diagram of the structure obtained in step 5 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 7 is a schematic diagram of the structure obtained in step 6 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 8 is a schematic diagram of the structure obtained in step 7 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 9 is a schematic diagram of the structure obtained in step 8 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 10 is a schematic diagram of the structure obtained in step 9 of the method for preparing a color conversion layer microarray of quantum dots according to the present invention;
FIG. 11 is a schematic diagram of a quantum dot color conversion layer microarray fabricated according to the method of the present invention;
FIG. 12 is a spectrum of a quantum dot color conversion layer microarray of the present invention excited with blue light.
In the figure, 101 is a substrate, 102 is a GaN epitaxial layer, 103 is a silicon film layer, 104 is a photoresist microarray, 105 is a metal Cr microarray, 106 is a black epoxy resin adhesive, 107 is a red quantum dot, 108 is a green quantum dot, and 109 is a water oxygen barrier layer.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a quantum dot color conversion layer microarray and a preparation method thereof, which are exemplified by 8um to 8um pixel points of the conversion layer microarray and 4um pixel point spacing, as shown in figure 1, the specific implementation steps are as follows:
(1) a 1um thick silicon oxide film layer 103 is grown on the GaN epitaxial layer 102 of the Si or sapphire substrate 101 by PECVD. The related GaN epitaxial layer 102 is prepared by MOCVD, the structure and the thickness of the GaN epitaxial layer 102 from bottom to top are a buffer layer 0.5um, an intrinsic GaN layer 1.5um, a first N-type GaN layer 5um and a second N-type GaN layer 2um in sequence, and the total thickness of the epitaxial layer is 9um (figure 2);
(2) a negative photoresist is spin-coated on the silicon film layer 103, the photomask graph is a pixel microarray graph, the size of the pixel is 8um x 8um, the distance between the pixels is 4um, the wafer is exposed by an ultraviolet contact exposure machine, and a photoresist microarray 104 (figure 3) with the polarity opposite to that of the photomask graph is obtained after development;
(3) evaporating a metal Cr film layer with the thickness of 200nm by using Ebeam as a hard mask for etching the GaN; stripping negative glue metal after evaporating the metal Cr film layer, stripping Cr metal at the pixel point spacing, and finally forming a metal Cr microarray 105 (figure 4);
(4) using metal Cr as a hard mask, etching the 1um silicon film layer 103 by utilizing ICP, and adopting an over-etching mode (figure 5) to ensure that the silicon film layer 103 is completely etched;
(5) taking the metal Cr and silicon composite microarray as a composite hard mask, etching the GaN epitaxial layer 102 by utilizing ICP (inductively coupled plasma) until the first N-type GaN layer is remained with a thin layer thickness, wherein the remained N-type GaN thin layer is used as a current conducting layer of a subsequent electrochemical corrosion process, and forming a GaN microarray after the etching is finished (figure 6);
(6) coating black epoxy resin glue 106 in a channel of a GaN microarray in a spinning mode, vacuumizing the glued wafer in 0.01-0.1 Pa vacuum equipment for 10-20 min to ensure that the black epoxy resin glue 106 can be better soaked into the channel, and then curing the black epoxy resin glue 106 according to the curing condition of the glue, wherein the parameters of curing at 100-130 ℃ for 1-2 hours are used; the coating thickness of the black epoxy glue 106 is optimal to exactly fill the depth of the channel completely, so that the problem that the thinning and polishing efficiency of a subsequent glue layer is influenced by the excessively thick glue layer of the black epoxy glue 106 above the GaN microarray (figure 7) is avoided;
(7) the wafer coated with the black epoxy resin glue 106 is subjected to a thinning and polishing process by utilizing CMP; the polishing is divided into 2 stages, wherein in the first stage, the silicon film layer 103 is used as a stop layer, and the black epoxy resin glue 106 is polished until the silicon film layer 103 stops; in the second stage, the second N-type GaN layer is used as a polishing stop layer, and the black epoxy resin glue 106 is polished until the silicon film layer 103 is completely removed and the second N-type GaN layer is exposed; here, it is necessary to ensure that the silicon film layer 103 is removed completely, a polishing procedure may be set to over-polish the second N-type GaN layer of 0.5um or wet-remove the silicon film layer 103 by soaking the wafer with BOE solution (fig. 8);
(8) carrying out electrochemical corrosion on the GaN microarray by using an anodic oxidation machine platform to obtain an approximately vertical GaN nanopore structure microarray with the corrosion depth of about 5um (figure 9);
(9) spin-coating a positive photoresist on the surface of a wafer, firstly defining a red color conversion region on a GaN nanopore structure microarray by utilizing ultraviolet lithography, injecting red quantum dots 107 into the nanopore structure of the red color conversion region by utilizing spraying equipment, then defining a green color conversion region and injecting green quantum dots 108, and finally forming an RGB array (figure 10);
(10) a layer of silicon nitride or other dielectric material is deposited on the wafer with the implanted red and green quantum dots as a water-oxygen barrier layer 109 by using Sputter to protect the stability of the quantum dot material in the nano-pore structure (fig. 11).
After the steps are completed, the quantum dot color conversion layer microarray and the matched GaN-based Micro LED microarray device are subjected to para-position bonding by using a high-precision para-position bonding machine table, wherein the pixel point size of the Micro LED microarray can be 3-5 um, and finally the full-color Micro LED device is formed.
According to the quantum dot color conversion layer microarray prepared in the mode, the nano-pore structure is used as the quantum dot bearing layer, so that quantum dots are uniformly dispersed, the problem of uneven distribution of the quantum dots in a quantum dot film is solved, and meanwhile, the light emitting intensity is effectively improved by utilizing the scattering effect of the nano-pore structure on light; the problem of light crosstalk between pixels is solved by filling light blocking materials in the pixel channels, so that the purity of red light and green light is improved. In addition, the process flow is simple, the operability is high, the application range is wide, and the method is suitable for preparing devices with various sizes, for example, the obtained quantum dot color conversion layer microarray is combined with a GaN-based blue light Micro-LED microarray to prepare a full-color display device, and the quantum dot color conversion technology only needs a blue light LED chip as an excitation light source while having high color gamut and high color purity, so that the technical bottleneck of mass transfer of red and green is avoided, the cost is reduced, and the production efficiency is improved; and the combination of the Micro LED device and the quantum dot color conversion technology has wide application prospect in the fields of novel Micro display devices, AR/VR and the like.
Fig. 12 is a spectrum test chart of the quantum dot color conversion layer microarray after being excited by blue light, and it can be seen that under the same test conditions, a weak blue light peak position is displayed in the spectrum chart of the quantum dot film structure, but no blue light peak position is displayed in the spectrum chart of the structure of the invention, which means that the purity of red light excited by the blue light of the invention is obviously superior to that of the quantum dot film structure, and the intensity of the red light of the invention is improved by about 20% compared with that of the red light of the quantum dot film structure.
Claims (10)
1. The quantum dot color conversion layer microarray is characterized by comprising a GaN epitaxial layer (102), wherein a grid-shaped channel is formed in the GaN epitaxial layer (102), a nanopore structure is formed in a single GaN epitaxial layer pixel region formed by the grid-shaped channel in a separated mode, and red quantum dots and green quantum dots are respectively injected into two nanopore structures in three adjacent GaN epitaxial layer pixel regions.
2. The quantum dot color conversion layer microarray as claimed in claim 1, wherein the nanopore structure is a plurality of elongated holes vertically opened in a pixel region of a single GaN epitaxial layer.
3. The quantum dot color conversion layer microarray of claim 1, wherein the grid shaped channels are filled with black epoxy glue.
4. The quantum dot color conversion layer microarray according to claim 1, wherein a water oxygen barrier layer (109) is disposed above the GaN epitaxial layer (102).
5. The microarray of quantum dot color conversion layer according to claim 1, wherein the GaN epitaxial layer (102) is grown on a Si or sapphire substrate (101), the GaN epitaxial layer (102) has a buffer layer, an intrinsic GaN layer, a first N-type GaN layer, and a second N-type GaN layer in sequence from bottom to top, and the bottom of the trench is opened to the first N-type GaN layer.
6. The preparation method of the quantum dot color conversion layer microarray is characterized by comprising the following steps of:
step 1, growing a buffer layer, an intrinsic GaN layer, a first N-type GaN layer and a second N-type GaN layer on a substrate (101) in sequence to serve as a GaN epitaxial layer (102), and growing a silicon film layer (103) on the second N-type GaN layer;
step 2, spinning and coating negative photoresist on the silicon film layer (103) obtained in the step 1, wherein the photomask plate graph is a pixel point microarray graph, and exposing and developing by using an ultraviolet contact type exposure machine to obtain a photoresist microarray (104);
step 3, evaporating a metal Cr film layer on the photoresist microarray (104) obtained in the step 2, and stripping and removing Cr metal at the pixel point interval after the metal Cr film layer is evaporated to form a metal Cr microarray (105);
step 4, etching the silicon film layer (103) by taking the metal Cr microarray (105) obtained in the step 3 as a hard mask to form a metal Cr and silicon composite microarray;
step 5, etching the GaN epitaxial layer (102) by taking the metal Cr and silicon composite microarray obtained in the step 4 as a hard mask until the bottom of the first N-type GaN layer is etched, and forming a GaN microarray after etching is finished;
step 6, spin-coating black epoxy resin glue (106) in the GaN microarray obtained in the step 5, and after the spin-coating is finished, performing vacuum infiltration and curing;
step 7, thinning and polishing the GaN microarray obtained in the step 6 until the metal Cr film layer and the silicon film layer (103) are completely removed and the second N-type GaN layer is exposed;
step 8, carrying out electrochemical corrosion on the GaN microarray obtained in the step 7 to obtain a GaN nanopore structure microarray;
step 9, spin-coating a positive photoresist on the surface of the GaN nanopore structure microarray obtained in the step 8, defining a red color conversion region and a green color conversion region through ultraviolet lithography, injecting red quantum dots (107) into the nanopore structure of the red color conversion region, and injecting green quantum dots (108) into the nanopore structure of the green color conversion region to obtain an RGB array;
and 10, depositing a water-oxygen barrier layer (109) above the RGB array obtained in the step 9 to obtain the RGB array.
7. The method for preparing a quantum dot color conversion layer microarray as claimed in claim 6, wherein the vacuum infiltration and curing in step 6 specifically comprises: and vacuumizing the GaN microarray subjected to spin coating in vacuum equipment for 10-20 min at the vacuum degree range of 0.01-0.1 Pa, and curing at the temperature of 100-130 ℃ for 1-2 h.
8. The method for preparing a microarray of color conversion layers of quantum dots according to claim 6, wherein the thinning polishing in step 7 comprises two stages, the first stage is polishing to stop the silicon film layer (103) with the silicon film layer (103) as a stop layer; in the second stage, the silicon film layer (103) is completely removed with the second N-type GaN layer as a stop layer until the second N-type GaN layer is exposed.
9. The method of claim 6, wherein the silicon film layer (103) is a silicon oxide film layer or a silicon nitride film layer, and the water-oxygen barrier layer (109) is a silicon nitride film layer.
10. The application of the quantum dot color conversion layer microarray is characterized in that the quantum dot color conversion layer microarray in claim 1 and a matched GaN-based Micro LED microarray device are bonded in an aligned mode to form a full-color Micro LED device.
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