CN115332051A - Novel gallium nitride nickel nitrogen vacancy color center and preparation method thereof - Google Patents
Novel gallium nitride nickel nitrogen vacancy color center and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a novel gallium nitride nickel nitrogen vacancy color center and a preparation method thereof, and mainly solves the problems of high color center preparation cost, high optical excitation energy and limited application in the prior art. The scheme comprises the following steps: in the gallium nitride crystal lattice, nickel atom is used to replace one gallium atom and the nitrogen vacancy nearest to the gallium atom, and the atomic arrangement presents C 3v Symmetrical, and C 3v The symmetry axis passing through the centers of the nickel atoms and the nitrogen vacancy and being equal to three spaced gallium atomsVertical in the plane; the preparation method comprises the steps of firstly growing a cubic phase gallium nitride film by adopting a metal organic chemical vapor deposition method, then carrying out ion implantation on the cubic phase gallium nitride film, doping nickel ions of specific types, repairing crystal lattice damage through high-temperature annealing, generating a large number of single vacancies through electron irradiation, and then carrying out rapid annealing. The invention can effectively reduce the optical excitation energy required by operating the color center, reduce the preparation cost of the color center, and can be widely applied to the fields of measurement, communication, simulation, high-performance calculation and the like.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and further relates to a color center in a solid system, in particular to a novel gallium nitride nickel nitrogen vacancy color center and a preparation method thereof, which can be used for quantum sensing devices.
Background
The color center in the solid system has wide application prospect in the fields of sensing and measuring, communication, simulation, high-performance calculation and the like. Through years of development, the nitrogen vacancy NV color center in diamond plays an important role in emerging quantum technology due to the excellent optical property and long spin coherence time. Although the potential of NV color centers in diamond is shown in quantum technology application, the hardness is high, the micro-nano processing and doping difficulty is large, and great challenges are faced in the aspect of practicability. Therefore, it is important to search other wide bandgap semiconductor materials with mature technology and low cost as the host material of the color center.
As a third generation semiconductor material, gaN has a wide direct band gap of 3.4eV, excellent chemical stability, good thermal conductivity; the high-quality GaN film single crystal with mature growth technology avoids the interference of other defect impurities on the spin state of the color center, has weak spin-orbit coupling, and is a main body material very suitable for preparing the color center. The transition metal element has a unique electronic structure, can regulate and control the magnetism of a main material and realize ideal spin injection, and is favorable for realizing paramagnetic color center with intrinsic spin conservation optical excitation.
In the patent document with the application publication number of CN 111705305B, a nano-diamond titanium color center is disclosed, wherein mixed liquid of nano-diamond seed crystals and small transition metal particles is adopted to realize a diamond substrate with uniformly distributed mixed seed crystals through ultrasonically implanting the diamond substrate, a nano-diamond film is regrown on the surface of the diamond substrate after the crystal implantation is finished, and the diamond with the transition metal color center is obtained through a high-temperature annealing method. The preparation method realizes relatively pure transition metal color center of the nano diamond. However, the diamond film produced by this method is composed of many small grains, rather than a "single crystal structure", and such a grain structure seriously affects the electrical and optical properties of diamond. In addition, the color center concentration obtained by the method is low, accurate position control is difficult to realize, and the optical excitation energy required by spin-to-bit state measurement of the color center is high.
The color centers present in Mg-doped gallium nitride film samples are published by the authors of YU Zhou et al in their article "Room temperature solid-state four entities in the collection range". The sample realizes the color center with the radiant fluorescence peak at the near infrared band, high brightness and optical stability, and the color center is easier to form in the p-type gallium nitride. However, the conductivity of the gallium nitride p-type doped layer remains limited, preventing the application of the device.
The transition metal color center taking diamond as a main material is a single photon source with excellent characteristics in a near infrared band, but the diamond has high hardness and high processing difficulty, so that the practical application of the color center in the diamond is limited. High-quality gallium nitride films are also suitable materials for preparing color centers, the existing gallium nitride color centers are easier to form in p-type gallium nitride, but the conductivity of a p-type doped layer of the gallium nitride is limited, so that the application of the gallium nitride color centers is limited. Therefore, a novel color center material having low optical excitation energy, easy processing, and stable existence in n-type gallium nitride is desired.
Disclosure of Invention
The invention aims to provide a novel gallium nitride nickel nitrogen vacancy color center and a preparation method thereof aiming at the defects of the prior art. The method is used for solving the problems that the existing color center has high preparation cost and high optical excitation energy, and only exists in a p-type doped layer with limited conductivity in a gallium nitride host. Firstly, cubic gallium nitride is used as an epitaxial layer, and a brand-new structure of a gallium nitride nickel nitrogen vacancy color center is formed through nickel ion injection and electron irradiation and then thermal annealing; the invention can improve the position of the corresponding fermi surface when the gallium nitride electric neutral color center exists stably, reduce the optical excitation energy required by operating the color center and reduce the preparation cost of the color center.
The specific scheme for realizing the aim comprises the following steps: in the gallium nitride crystal lattice, nickel atoms are used for replacing one gallium atom and the nitrogen vacancy which is nearest to the gallium atom forms a complex, namely a gallium nitride nickel nitrogen vacancy color center; the atomic arrangement of the complex exhibits C 3v Is symmetrical, and C 3v The axis of symmetry passes through the centers of the nickel atoms and nitrogen vacancies and is perpendicular to the plane of the three equally spaced gallium atoms. The method for preparing the gallium nitride nickel nitrogen vacancy color center comprises the following steps:
(1) Selecting a substrate and pretreating the substrate to obtain a pretreated flat substrate;
(2) Growing an unintentionally doped epitaxial layer, namely a cubic phase gallium nitride film, on a flat substrate by adopting a Metal Organic Chemical Vapor Deposition (MOCVD) method;
(3) And (3) carrying out ion implantation on the epitaxial layer:
injecting 170keV nickel ions into the gallium nitride film to obtain an ion-injected sample, and performing rapid annealing at 800 ℃ on the sample in a nitrogen atmosphere;
(4) Applying 10MeV energy to the sample obtained in step (3), and 5X 10 17 cm -2 Carrying out electron irradiation with dose, and carrying out rapid annealing at 600-800 ℃ on the sample subjected to electron irradiation in a nitrogen atmosphere;
(5) And finishing the preparation of the gallium nitride nickel nitrogen vacancy color center.
Compared with the prior art, the invention has the following advantages:
firstly, because the invention adopts gallium nitride as the main material, the processing difficulty of the color center is reduced, thereby reducing the production cost of the color center.
Secondly, because the invention adopts the cubic gallium nitride as the main material, the splitting between the ground state and the excited state of the color center is reduced due to the large lattice constant of the cubic gallium nitride, thereby reducing the optical excitation energy for controlling the color center, and the property is more excellent than that of the diamond color center.
Thirdly, because the invention adopts nickel and nitrogen vacancy codoping, the formation energy of the designed color center is low, the color center has higher chemical stability, and the corresponding fermi surface is close to the bottom of the conduction band when the electrically neutral color center exists stably, so that the color center can exist in the n-type doped gallium nitride stably.
Description of the drawings:
FIG. 1 is a schematic view of a process for preparing a vacant color center in accordance with the present invention;
FIG. 2 is a density of states diagram and band structure diagram of a vacancy color center in the present invention;
FIG. 3 is a bit pattern coordinate diagram of a vacant color center in the present invention;
FIG. 4 is a schematic diagram of the structure of a vacant color center in the present invention;
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Referring to fig. 4, the present invention provides a novel gallium nitride nickel nitrogen vacancy color center, which comprises:
in the gallium nitride crystal lattice, nickel atoms are used for replacing one gallium atom and a nitrogen vacancy which is nearest to the gallium atom to form a complex, namely a gallium nitride nickel nitrogen vacancy color center; the atomic arrangement of the complex exhibits C 3v Is symmetrical, and C 3v The axis of symmetry passes through the centers of the nickel atoms and nitrogen vacancies and is perpendicular to the plane of the three equally spaced gallium atoms.
Referring to the attached figure 1, the invention provides a novel preparation method of a gallium nitride nickel nitrogen vacancy color center, which utilizes an ion injection method to dope nickel ions of specific types, repairs lattice damage through high-temperature annealing, generates a large number of single vacancies through electron irradiation, and then rapidly anneals to finish the preparation; the method specifically comprises the following steps:
step 1, selecting a substrate and pretreating the substrate to obtain a pretreated flat substrate; substrates that may be selected include gallium arsenide substrates, sapphire substrates, gallium nitride substrates, and the like. In the pretreatment process in the embodiment, the substrate is cleaned in an ultrasonic cleaning machine, and then cleaned with acetone for 3-5 minutes, cleaned with ethanol for 3-5 minutes and cleaned with isopropyl alcohol for 3-5 minutes in sequence, so as to remove oil stains on the surface of the substrate; then soaking the substrate in hydrochloric acid aqueous solution for 3 to 5 minutes to remove an oxide layer on the surface; finally, deionized water is used for ultrasonic cleaning, and the product is taken out and dried by nitrogen.
And 2, growing an unintentionally doped epitaxial layer, namely the cubic phase gallium nitride film on the flat substrate by adopting a Metal Organic Chemical Vapor Deposition (MOCVD) method. In this example, MOCVD was used to grow an unintentionally doped epitaxial layer by using TMGa and NH 3 As a gallium source and a nitrogen source, the flow rates of the gallium source and the nitrogen source are respectively 120sccm and 1200sccm; with H 2 As a gallium source carrier gas; is first H at 1150 deg.C 2 Baking the substrate for 10 minutes in the atmosphere, then cooling to 550-580 ℃ to grow a GaN buffer layer for 5 minutes, and then heating to 900 ℃ to grow an undoped GaN epitaxial layer; the thickness of the epitaxial layer is 2-5 μm;
and 3, performing ion implantation on the epitaxial layer:
170keV nickel ions are implanted into the GaN film, with the conventional implantation dosage of 1 × 10 16 cm -2 Obtaining a sample after ion implantation, and carrying out rapid annealing at 800 ℃ on the sample in a nitrogen atmosphere;
step 4, using 10MeV energy and 5X 10 to the sample obtained in the step 3 17 cm -2 Carrying out electron irradiation with dose, and carrying out rapid annealing at 600-800 ℃ on the sample subjected to electron irradiation in a nitrogen atmosphere;
and 5, finishing the preparation of the gallium nitride nickel nitrogen vacancy color center.
The color center in the solid system has wide application prospect in the fields of sensing and measuring, communication, simulation, high-performance calculation and the like. The GaN material has a wide direct band gap of 3.4eV, excellent chemical stability and good thermal conductivity, is a semiconductor material resistant to strong radiation in a severe environment, and is widely applied to the fields of 5G communication, aerospace and the like; the high-quality GaN film single crystal avoids interference of other defect impurities on a color center spin state, has weak spin-orbit coupling, and is a main body material very suitable for preparing a color center. The transition metal element has a unique electronic structure, can regulate and control the magnetism of a main material and realize ideal spin injection, and is favorable for realizing paramagnetic color center with intrinsic spin conservation optical excitation. The potential of NV color centers in diamond is shown in quantum technology application, but the diamond has high hardness and large difficulty in micro-nano processing and doping, and faces great challenges in the aspect of practicability. The existing gallium nitride color centers are not artificially and intentionally prepared, the formation of the color centers is not controlled, and the types and positions of the color centers are uncertain, so that the application of the gallium nitride color centers is limited. The invention prepares the novel gallium nitride nickel nitrogen vacancy color center by nickel ion injection and electron irradiation, does not need higher production cost of a color center host material, reduces the optical excitation energy of the color center, reduces the lattice relaxation and has wider application.
The invention has not been described in detail in part of its common general knowledge to those skilled in the art.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A novel gallium nitride nickel nitrogen vacancy color center is characterized in that: in the gallium nitride crystal lattice, nickel atoms are used for replacing one gallium atom and a nitrogen vacancy which is nearest to the gallium atom to form a complex, namely a gallium nitride nickel nitrogen vacancy color center; the atomic arrangement of the complex exhibits C 3v Symmetrical, and C 3v The axis of symmetry passing through the centers of the nickel atoms and nitrogen vacancies andperpendicular to the plane of the three equally spaced gallium atoms.
2. A novel preparation method of gallium nitride nickel nitrogen vacancy color center is characterized in that an ion injection method is utilized, specific nickel ions are doped, after high-temperature annealing is carried out to repair crystal lattice damage, a large number of single vacancies are generated through electron irradiation, and then rapid annealing is carried out to complete preparation; the method specifically comprises the following steps:
(1) Selecting a substrate and pretreating the substrate to obtain a pretreated flat substrate;
(2) Growing an unintentionally doped epitaxial layer, namely a cubic phase gallium nitride film on a flat substrate by adopting a Metal Organic Chemical Vapor Deposition (MOCVD) method;
(3) And (3) carrying out ion implantation on the epitaxial layer:
injecting 170keV nickel ions into the gallium nitride film to obtain an ion-injected sample, and performing rapid annealing at 800 ℃ on the sample in a nitrogen atmosphere;
(4) Applying 10MeV energy to the sample obtained in step (3), and 5X 10 17 cm -2 Carrying out electron irradiation with dose, and carrying out rapid annealing at 600-800 ℃ on the sample subjected to electron irradiation in a nitrogen atmosphere;
(5) And finishing the preparation of the gallium nitride nickel nitrogen vacancy color center.
3. The method of claim 2, wherein: the substrate selected in the step (1) comprises a gallium arsenide substrate, a sapphire substrate and a gallium nitride substrate.
4. The method of claim 2, wherein: the pretreatment in the step (1) comprises the steps of cleaning the substrate in an ultrasonic cleaning machine, and then sequentially cleaning the substrate with acetone for 3-5 minutes, cleaning the substrate with ethanol for 3-5 minutes and cleaning the substrate with isopropyl alcohol for 3-5 minutes to remove oil stains on the surface of the substrate; then soaking the substrate in hydrochloric acid aqueous solution for 3 to 5 minutes to remove an oxide layer on the surface; finally, deionized water is used for ultrasonic cleaning, and the mixture is taken out and dried by nitrogen.
5. The method of claim 2, wherein: in the step (2), an unintentionally doped epitaxial layer is grown by adopting a Metal Organic Chemical Vapor Deposition (MOCVD) method, and trimethyl gallium (TMGa) and ammonia gas (NH) are respectively used 3 As gallium and nitrogen sources with H 2 As a gallium source carrier gas; is first H at 1150 deg.C 2 Baking the substrate for 10 minutes in the atmosphere, then cooling to 550-580 ℃ to grow a GaN buffer layer for 5 minutes, and then heating to 900 ℃ to grow an undoped GaN epitaxial layer.
6. The method of claim 5, wherein: the flow rates of the gallium source and the nitrogen source are 120sccm and 1200sccm respectively.
7. The method according to claim 2 or 5, characterized in that: the thickness of the epitaxial layer is 2-5 mu m.
8. The method of claim 2, wherein: in the step (3), 170keV nickel ions are implanted into the gallium nitride film with an implantation dosage of 1 × 10 16 cm -2 。
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