WO2024036680A1 - Procédé de préparation d'un réseau de micro-del de nitrure monocristallin basé sur un substrat non-monocristallin - Google Patents

Procédé de préparation d'un réseau de micro-del de nitrure monocristallin basé sur un substrat non-monocristallin Download PDF

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WO2024036680A1
WO2024036680A1 PCT/CN2022/118960 CN2022118960W WO2024036680A1 WO 2024036680 A1 WO2024036680 A1 WO 2024036680A1 CN 2022118960 W CN2022118960 W CN 2022118960W WO 2024036680 A1 WO2024036680 A1 WO 2024036680A1
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single crystal
layer
nitride
dimensional material
array
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王新强
刘放
陈兆营
郭昱成
王涛
盛博文
沈波
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北京大学
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0093—Wafer bonding; Removal of the growth substrate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L27/00—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate
    • H01L27/15—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate including semiconductor components having potential barriers, specially adapted for light emission
    • H01L27/153—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate including semiconductor components having potential barriers, specially adapted for light emission in a repetitive configuration, e.g. LED bars
    • H01L27/156—Devices consisting of a plurality of semiconductor or other solid-state components formed in or on a common substrate including semiconductor components having potential barriers, specially adapted for light emission in a repetitive configuration, e.g. LED bars two-dimensional arrays
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0062—Processes for devices with an active region comprising only III-V compounds
    • H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
    • H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H01L33/0095—Post-treatment of devices, e.g. annealing, recrystallisation or short-circuit elimination

Definitions

  • the present invention relates to the preparation technology of semiconductor light-emitting devices, and in particular to a preparation method of a single crystal nitride Micro-LED array based on a non-single crystal substrate.
  • nitride semiconductors are usually heteroepitaxially grown on single crystal substrates with matching lattice symmetry.
  • high-transmittance single-crystal sapphire substrates are usually selected to prepare nitride light-emitting devices
  • single-crystal silicon or single-crystal silicon carbide substrates are usually selected to prepare electronic devices.
  • the above-mentioned single crystal substrates cannot fully meet the requirements of light emitting efficiency, transparency, heat dissipation and other aspects of light-emitting devices.
  • Single crystal nitride films can be realized by using single crystal two-dimensional material-assisted epitaxy on non-single crystal substrates such as quartz.
  • the epitaxial film will The interface interaction of 2D materials will be stronger than the interface interaction between 2D materials and non-single crystal substrates, causing the epitaxial film to be broken due to partial interface separation during growth or cooling;
  • the thickness of the epitaxial film is less than 1 micron, The dislocation density of epitaxial films is usually higher than 3 ⁇ 10 10 cm -2 , and the half-width of the rocking curve of the corresponding X-ray diffraction (0002) crystal plane is greater than 1 degree, resulting in low electro-optical conversion efficiency of light-emitting devices prepared on it, and electronic devices
  • the current leakage is serious and cannot meet the application requirements in fields such as flexible LED, ultraviolet LED, and radio frequency power devices, especially the research and development requirements in the field of micro-light-
  • the present invention proposes a method for preparing a single crystal nitride Micro-LED array based on a non-single crystal substrate.
  • the preparation method of the single crystal nitride Micro-LED array based on a non-single crystal substrate of the present invention includes the following steps:
  • a) Provide a non-single crystal substrate, which is made of rigid non-metallic materials; perform double-sided polishing of the non-single crystal substrate;
  • the two-dimensional atomic crystal induction layer has a single crystal structure with doped atoms and is exposed to the two-dimensional atomic crystal.
  • the doped atoms on the surface of the induction layer provide surface unsaturated dangling bonds, which serve as nucleation sites for single crystal nitride and provide the required modified surface for single crystal nitride growth;
  • a first through hole array composed of a plurality of periodically two-dimensionally arranged through holes is formed on the first two-dimensional material mask layer, with equal periods of rows and columns. , the depth of each through hole is consistent with the thickness of the first two-dimensional material mask layer, and the diameter of the through hole is less than 2/3 of the first through hole array period;
  • c) Deposit a second layer of single crystal nitride on the first two-dimensional material mask layer.
  • the surface of the first two-dimensional material mask layer other than the first through hole array does not have surface unsaturated dangling bonds and cannot grow single crystals.
  • Nitride the area of the corresponding template layer below the first via array, has surface unsaturated dangling bonds and can grow single crystal nitride to achieve the first dislocation filtering, that is, in the template layer not corresponding to the first via array Dislocations cannot enter the upper second layer of single crystal nitride;
  • a second through hole array composed of a plurality of periodically two-dimensionally arranged through holes on the second two-dimensional material mask layer.
  • the depth of each through hole The thickness of the second two-dimensional material mask layer is consistent, and the period and shape of the second via hole array are consistent with the first via hole array, but the position of the second via hole array is horizontally offset from the first via hole array, and the horizontal offset is Move so that the outer edge of the through holes of the second through hole array is tangent to the outer edge of the through holes of the first through hole array;
  • c) Deposit a third layer of single crystal nitride on the second two-dimensional material mask layer.
  • the surface on the second two-dimensional material mask layer other than the second through hole array area does not have surface unsaturated dangling bonds and cannot grow single crystal nitride.
  • Crystal nitride, the area of the corresponding dislocation filter layer below the second via hole array can grow single crystal nitride to achieve the second dislocation filtering, that is, dislocations in the dislocation filter layer corresponding to the non-second via hole array It cannot enter the third layer of single crystal nitride in the upper layer;
  • a third through hole array composed of a plurality of periodically two-dimensionally arranged through holes is formed on the third two-dimensional material mask layer, with equal periods of rows and columns.
  • the depth of each through hole is consistent with the thickness of the third two-dimensional material mask layer
  • the diameter of the through hole is 1/2 to 3/4 of the third through hole array period
  • the third through hole array period is the same as the first through hole array period. The hole array period is consistent;
  • c) Deposit a single crystal nitride functional structure on the third two-dimensional material mask layer.
  • the surface on the third two-dimensional material mask layer other than the third via hole array area does not have surface unsaturated dangling bonds and cannot grow single crystals.
  • Nitride functional structure, the corresponding area of the single crystal nitride film under the third through hole array can grow the nitride functional structure in a single crystal, and the single crystal nitride functional structure is one of the ultraviolet or visible light emitting diode structures; by controlling the deposition
  • the growth temperature and the stoichiometric ratio of the nitrogen source and Group III source flow rates during the process are such that the lateral size of the single crystal nitride functional structure is equal to the lateral size of the circular via area, and only longitudinal growth is performed, the single crystal nitride functional structure
  • the height is greater than the thickness of the third two-dimensional material mask layer, forming a single crystal nitride Micro-LED array with the same periodic
  • c) Laser is incident from the back of the non-single crystal substrate, and the laser heats the two-dimensional atomic crystal induction layer between the non-single crystal substrate and the template layer through lattice resonance absorption, and melts the two-dimensional atomic crystal induction layer to achieve non-single crystal substrate.
  • the single crystal substrate is separated from the structure above the two-dimensional atomic crystal induction layer to obtain a flexible single crystal nitride Micro-LED array and a reusable non-single crystal substrate.
  • the bandgap width of the non-single crystal substrate is greater than 5eV
  • the lattice mismatch with the nitride semiconductor is greater than 20%
  • the thermal expansion coefficient mismatch is greater than 50%
  • the visible light transparency is greater than 0.99
  • the melting point is high
  • one of quartz, mica, corundum and diamond is used.
  • the two-dimensional atomic crystal induction layer adopts graphene with a single crystal structure having doped atoms.
  • the doped atoms are nitrogen atoms or oxygen atoms, and the proportion of nitrogen atoms or oxygen atoms is greater than 1%.
  • the thickness is 1 to 10nm, and the doped atoms provide surface unsaturated dangling bonds as nucleation sites for nitrides, without the need for additional modification of the two-dimensional atomic crystal induction layer.
  • the first layer of single crystal nitride is grown using metal-organic chemical vapor deposition technology, molecular beam epitaxy, hydride vapor phase epitaxy, magnetron sputtering or pulsed laser deposition technology, and the growth temperature is 900°C ⁇ 1250°C, the stoichiometric ratio of the flow rates of nitrogen source and III source, that is, V/III, is 300 to 1000.
  • the III source is a metal or metal organic source
  • the nitrogen source is ammonia or nitrogen
  • the compound is AlN or a composite structure of AlGaN and AlN, the band gap is greater than 5eV, the thickness of the template layer is 500nm ⁇ 1000nm, and the dislocation density of the template layer is lower than 5 ⁇ 10 10 cm -2 and higher than 1 ⁇ 10 9 cm -2 .
  • the first two-dimensional material mask layer is made of polycrystalline or amorphous graphene, boron nitride or transition metal chalcogenide, with a thickness of 10 nm to 30 nm.
  • step 2) the specific process of mask protection and selective etching is as follows: spin-coat photoresist on the upper surface of the first two-dimensional material mask layer, and pass through the mask with a set periodic shape.
  • the photoresist is processed by template exposure, and the photoresist denatured by exposure is removed through chemical etching, and the undenatured photoresist with a set periodic shape provides mask protection; selective etching uses plasma etching.
  • the first two-dimensional material mask layer with mask protection is directly etched by techniques such as etching or reactive ion etching. The areas without mask protection are etched, and the areas with mask protection are not etched and are removed by chemical cleaning.
  • the remaining photoresist layer will have a set periodic shape transferred from the photoresist layer to the first two-dimensional material mask layer.
  • the shape of the through hole is a cylinder; the period of the first through hole array is 0.1 ⁇ m to 50 ⁇ m.
  • the second layer of single crystal nitride is grown using metal-organic chemical vapor deposition technology, molecular beam epitaxy, hydride vapor phase epitaxy, magnetron sputtering or pulsed laser deposition technology, and the growth temperature is 900°C ⁇ At 1250°C, the stoichiometric ratio of the flow rate of the nitrogen source and the III source, that is, V group/III group, is 300 to 1000.
  • the second layer of single crystal nitride is AlN or a composite structure of AlGaN and AlN, and the bandgap width is greater than 5eV.
  • step 2) the growth temperature is increased to 1000°C to 1350°C, and the group V/group III ratio is increased to 1500 to 5000.
  • the thickness of the dislocation filtering layer is 500nm ⁇ 2000nm, and the dislocation density is lower than 1 ⁇ 10 9 cm -2 .
  • the second two-dimensional material mask layer is composed of polycrystalline or amorphous graphene, boron nitride, transition metal chalcogenide, etc., and has a thickness of 10 nm to 30 nm.
  • the third layer of single crystal nitride is grown using metal-organic chemical vapor deposition technology, molecular beam epitaxy, hydride vapor phase epitaxy, magnetron sputtering or pulsed laser deposition technology, and the growth temperature is 900°C ⁇ At 1250°C, the stoichiometric ratio of the flow rate of the nitrogen source and the III source, that is, V group/III group, is 300 to 1000.
  • the third layer of single crystal nitride is AlN or a composite structure of AlGaN and AlN, and the bandgap width is greater than 5eV.
  • the growth temperature is increased to 1000°C to 1350°C, and the group V/group III ratio is increased to 1500 to 5000.
  • the thickness of the single crystal nitride film is 500nm to 2000nm, and the dislocation density is less than 1 ⁇ 10 8 cm -2 .
  • the third two-dimensional material mask layer is composed of polycrystalline or amorphous graphene, boron nitride, transition metal chalcogenide, etc., and has a thickness of 10 nm to 30 nm.
  • the growth temperature is 900°C to 1250°C, and the stoichiometric ratio of the flow rate of the nitrogen source and the group III source, that is, group V/group III, is 300 to 1000;
  • the single crystal nitride functional structure is the array element It is composed of n-type layer, quantum structure and p-type layer, with a height of 0.5 ⁇ m ⁇ 3 ⁇ m.
  • step 5) a), polymethylmethacrylate (PPMA) or polydimethylsiloxane (PDMS) is spin-coated.
  • PPMA polymethylmethacrylate
  • PDMS polydimethylsiloxane
  • the flexible protective layer is composed of PMMA, transparent conductive film or other flexible organic materials.
  • infrared laser, ultraviolet laser or visible laser is incident from the back side of the non-single crystal substrate; the wavelength of the infrared laser is greater than 800 nm.
  • the present invention obtains a dislocation filter layer with a dislocation density lower than 1 ⁇ 10 9 cm -2 by preparing a two-dimensional material mask layer, and further obtains a single crystal nitride with a dislocation density lower than 1 ⁇ 10 8 cm -2 Thin films can achieve ultra-high quality single crystal nitride functional structures on non-single crystal substrates with large lattice mismatch and large thermal expansion coefficient mismatch.
  • Radio frequency devices, power devices, light-emitting devices and detection devices, etc. have process universality; using laser to destroy the interface between the epitaxial structure and the non-single crystal substrate can achieve lossless separation of the epitaxial structure and multiple times of the non-single crystal substrate Reusable, energy-saving and environmentally friendly, simple process and suitable for mass production.
  • Figure 1 is a cross-sectional view of the template layer obtained by the preparation method of a single crystal nitride Micro-LED array based on a non-single crystal substrate according to the present invention
  • Figure 2 is a cross-sectional view of a dislocation filter layer obtained according to the preparation method of a single crystal nitride Micro-LED array based on a non-single crystal substrate of the present invention
  • Figure 3 is a cross-sectional view of a single crystal nitride film obtained according to the preparation method of a single crystal nitride Micro-LED array based on a non-single crystal substrate of the present invention
  • Figure 4 is a cross-sectional view of a single crystal nitride Micro-LED array prepared according to the method for preparing a single crystal nitride Micro-LED array based on a non-single crystal substrate of the present invention
  • Figure 5 is a cross-sectional view of a flexible single crystal nitride Micro-LED array obtained by the method for preparing a single crystal nitride Micro-LED array based on a non-single crystal substrate of the present invention.
  • a) Provide a non-single crystal substrate 1.
  • the band gap of the non-single crystal substrate is greater than 5eV
  • the lattice mismatch with the nitride semiconductor is greater than 20%
  • the thermal expansion coefficient mismatch is greater than 50%
  • the visible light transparency is greater than 0.99
  • the melting point is greater than Quartz at 1200°C; double-sided polishing of non-single crystal substrates;
  • the two-dimensional atomic crystal induction layer is a single crystal structure with nitrogen doped atoms, and nitrogen atoms account for It is 1.2% and has a thickness of 5nm.
  • the doping atoms exposed on the surface of the two-dimensional atomic crystal induction layer provide surface unsaturated dangling bonds, which serve as nucleation sites for nitride and provide the required modified surface for single crystal nitride growth. ;
  • the first two-dimensional material mask layer is polycrystalline graphene with a thickness of 15 nm;
  • the shape of the through hole is a cylinder; forming a first through hole array composed of a plurality of periodically two-dimensionally arranged through holes on the first two-dimensional material mask layer, rows Equal to the period of the column, the depth of each through hole is consistent with the thickness of the first two-dimensional material mask layer, the diameter of the through hole is 1/2 of the period of the first through hole array, and the period of the first through hole array is 5 ⁇ m;
  • c) Use metal-organic chemical vapor deposition technology to deposit single crystal AlN on the first two-dimensional material mask layer to form a second layer of single crystal nitride.
  • the growth temperature is 1050°C
  • the stoichiometric ratio of the flow rate of the nitrogen source and the III source is That is, Group V/III is 500
  • the bandgap width of the second layer of single crystal nitride is greater than 5eV
  • the surface of the first two-dimensional material mask layer other than the first through hole array does not have surface unsaturated dangling bonds and cannot grow.
  • Single crystal nitride the area of the corresponding template layer below the first via array, has surface unsaturated dangling bonds that can grow single crystal nitride to achieve the first dislocation filtering, that is, the template layer corresponding to the non-first via array
  • the dislocations in cannot enter the upper second layer of single crystal nitride;
  • the growth temperature increases to 1150°C and the Group V/III ratio increases to 2000, causing the thickness of the second layer of single crystal nitride to exceed the thickness of the first two-dimensional material mask layer and continue to grow vertically while expanding laterally.
  • the nearly stress-free state of the lateral expansion process causes the dislocation propagation direction to change from the area of the template layer corresponding to the first via array to the second layer of single crystal nitride. , causing partial annihilation of dislocations to obtain a dislocation filter layer 5 with a dislocation density lower than 1 ⁇ 10 9 cm -2 .
  • the thickness of the dislocation filter layer 5 is 1500nm, as shown in Figure 2;
  • the second two-dimensional material mask layer 6 is made of polycrystalline graphene and has a thickness of 20nm;
  • a second through hole array composed of a plurality of periodically two-dimensionally arranged through holes on the second two-dimensional material mask layer.
  • the depth of each through hole The thickness of the second two-dimensional material mask layer is consistent, and the period and shape of the second through-hole array are consistent with the first through-hole array of the first two-dimensional material mask, but the position of the second through-hole array is consistent with the first through-hole array.
  • the array is offset horizontally along the row direction by the diameter of the through hole;
  • c) Use metal-organic chemical vapor deposition technology to deposit single crystal AlN on the second two-dimensional material mask layer to form the third layer of single crystal nitride.
  • the growth temperature is 1050°C
  • the stoichiometric ratio of the flow rate of the nitrogen source and the III source is That is, Group V/III is 500
  • the bandgap width of the third layer of single crystal nitride is greater than 5eV
  • the surface of the second two-dimensional material mask layer outside the second through hole array area does not have surface unsaturated dangling bonds and cannot Single crystal nitride is grown, and the area of the corresponding dislocation filter layer below the second via hole array can grow single crystal nitride to achieve the second dislocation filtering, that is, the area in the dislocation filter layer corresponding to the second via hole array is not Dislocations cannot enter the upper third layer of single crystal nitride;
  • the growth temperature increases to 1150°C and the Group V/III ratio increases to 2000, causing the thickness of the third layer of single crystal nitride to exceed the thickness of the second two-dimensional material mask layer and continue to grow vertically while expanding laterally.
  • the nearly stress-free state of the lateral expansion process causes the area of the dislocation filter layer corresponding to the second via hole array to expand to the dislocation propagation direction of the third layer of single crystal nitride. Changes occur, causing some dislocations to be annihilated, and a single crystal nitride film 7 with a dislocation density lower than 1 ⁇ 10 8 cm -2 is obtained.
  • the thickness of the single crystal nitride film 7 is 1500nm, as shown in Figure 3;
  • the third two-dimensional material mask layer 8 uses polycrystalline graphene with a thickness of 20nm;
  • a third through hole array composed of a plurality of periodically two-dimensionally arranged through holes is formed on the third two-dimensional material mask layer, with equal periods of rows and columns. , the depth of each through hole is consistent with the thickness of the third two-dimensional material mask layer, the diameter of the through hole is 3/5 of the third through hole array period, and the third through hole array period is consistent with the first through hole array period;
  • the growth temperature is 1050°C
  • the stoichiometric ratio of the flow rate of the nitrogen source and the group III source, that is, group V/group III is 500
  • the nitride is deposited on the third two-dimensional material mask layer Functional structure.
  • the surface of the third two-dimensional material mask layer outside the third via hole array area does not have surface unsaturated dangling bonds and cannot grow nitride functional structures.
  • the corresponding single crystal nitride film below the third via hole array has The area can grow a nitride functional structure, which is one of the ultraviolet or visible light emitting diode structures; by controlling the growth temperature during the deposition process and the stoichiometric ratio of the flow rate of the nitrogen source and the III source, the nitride functional structure can be grown.
  • the lateral size of the structure is equal to the lateral size of the circular through hole area, and only longitudinal growth is performed to form a single crystal nitride Micro-LED array 9 with the same periodic distribution as the third through hole array, and the nitride function in each through hole is
  • the structure is an array element of a single crystal nitride Micro-LED array with a height of 1 ⁇ m, as shown in Figure 4;
  • Infrared laser is incident from the back of the non-single crystal substrate, with a wavelength greater than 800nm.
  • the infrared laser heats the two-dimensional atomic crystal induction layer between the non-single crystal substrate and the template layer through lattice resonance absorption, and melts the two-dimensional atoms.
  • the crystal induction layer realizes the structural separation above the non-single crystal substrate and the two-dimensional atomic crystal induction layer, and obtains a flexible single crystal nitride Micro-LED array and a reusable non-single crystal substrate, as shown in Figure 5.

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Abstract

L'invention concerne un procédé de préparation d'un réseau de micro-DEL de nitrure monocristallin basé sur un substrat non-monocristallin. Une couche de masque de matériau bidimensionnel est préparée pour obtenir une couche de filtre de dislocation ayant une densité de dislocation inférieure à 1×109cm-2, et pour obtenir en outre un film mince de nitrure monocristallin ayant une densité de dislocation inférieure à 1×108cm-2, de telle sorte qu'une structure fonctionnelle de nitrure monocristallin de qualité ultra-élevée peut être mise en œuvre sur un substrat non-monocristallin ayant un grande désaccord de réseau et un grand coefficient de désaccord de dilatation thermique. En plus d'être utilisé pour préparer un dispositif à micro-DEL, le procédé peut en outre être utilisé pour préparer un dispositif radiofréquence, un dispositif d'alimentation en énergie, un dispositif électroluminescent, un dispositif de détection, et analogues, et a une universalité de traitement. La liaison d'interface entre une structure épitaxiale et le substrat non-monocristallin est détruite à l'aide d'un laser, de telle sorte qu'une séparation non destructive de la structure épitaxiale et une utilisation répétée du substrat non-monocristallin peuvent être réalisées, et le procédé est économe en énergie, respectueux de l'environnement, et simple, et est approprié pour une production par lots.
PCT/CN2022/118960 2022-08-16 2022-09-15 Procédé de préparation d'un réseau de micro-del de nitrure monocristallin basé sur un substrat non-monocristallin WO2024036680A1 (fr)

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CN113078046A (zh) * 2021-03-26 2021-07-06 华厦半导体(深圳)有限公司 一种氮化镓同质衬底及其制备方法
CN114678257A (zh) * 2022-03-11 2022-06-28 中国科学院长春光学精密机械与物理研究所 一种基于金属衬底的氮化物模板及其制备方法和应用
CN115050864A (zh) * 2022-08-16 2022-09-13 北京大学 一种基于非单晶衬底的单晶氮化物Micro-LED阵列的制备方法

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