CN115083885A - Method for in-situ growth of periodic nanostructure through laser induction - Google Patents

Method for in-situ growth of periodic nanostructure through laser induction Download PDF

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CN115083885A
CN115083885A CN202210508097.1A CN202210508097A CN115083885A CN 115083885 A CN115083885 A CN 115083885A CN 202210508097 A CN202210508097 A CN 202210508097A CN 115083885 A CN115083885 A CN 115083885A
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张子旸
王洪培
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Qingdao Yichen Radisson Technology Co ltd
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    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
    • H01L21/02664—Aftertreatments
    • H01L21/02667—Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth
    • H01L21/02675—Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth using laser beams
    • H01L21/02686—Pulsed laser beam

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Abstract

The invention discloses a method for in-situ growth of a periodic nano structure by laser induction, which comprises the following steps: the method comprises the following steps: carrying out primary growth on the substrate to form a buffer layer, and flattening the surface of the substrate; step two: and continuously growing the substrate while irradiating the substrate by utilizing a plurality of laser beams, wherein the plurality of laser beams form interference on the substrate, and the periodic nano structure is formed after the substrate is continuously grown for 1-4 h. The laser interference is used for inducing in-situ growth on the substrate, so that the complicated processes of photoetching, corrosion, cleaning and the like are avoided, and the cost is reduced. The laser interference induction positioning growth positioning is more accurate, and the accuracy is higher. Meanwhile, the cavity opening operation is avoided, the subsequent structure growth is not polluted, and the structural performance is better.

Description

Method for in-situ growth of periodic nanostructure through laser induction
Technical Field
The invention relates to the field of semiconductor photoelectric materials, in particular to a method for in-situ growth of a periodic nano structure by laser induction.
Background
Periodic nanostructures, which are a group of nanomaterials consisting of single or multiple nano-units/components periodically arranged in ordered patterns (e.g., vertical and lateral superlattices), have great potential applications in energy conversion, electronic and optoelectronic applications due to their special physicochemical properties. Among them, nanostructures such as two-dimensional photonic crystals and bragg reflectors are widely used to enhance the light emission efficiency, absorption efficiency, and raman effect of materials.
At present, methods for preparing the periodic nanostructure mainly comprise photoetching, electron beam exposure, nanoimprint, focused ion beam etching and the like, but the methods are not only complex in operation and low in yield, but also low in processing precision and high in cost, and the development of the methods is restricted.
Therefore, a high-precision, low-cost, and efficient method for preparing periodic nanostructures is needed to solve the above problems.
Disclosure of Invention
It is an object of the present invention to provide a new solution for periodic nanostructure growth.
According to a first aspect of the present invention, there is provided a method of laser induced in situ growth of periodic nanostructures, comprising the steps of:
the method comprises the following steps: carrying out primary growth on the substrate to form a buffer layer, and flattening the surface of the substrate;
step two: and continuously growing the substrate while irradiating the substrate by utilizing a plurality of laser beams, wherein the plurality of laser beams form interference on the substrate, and the periodic nano structure is formed after the substrate is continuously grown for 1-4 h.
Preferably, the substrate includes, but is not limited to, GaAs, InP, Al 2 O 3 Or GaSb, in the first growth, the buffer layer is formed of a material including, but not limited to, one of GaAs, InP, GaSb, GaN, SiC, InAs, or GaP, and in the subsequent growth, the periodic nanostructures are formed of a material including, but not limited to, one of GaAs, InP, GaSb, GaN, SiC, InAs, or GaP.
Preferably, in the second step, the substrate temperature is controlled to be 0-200 ℃ for further growth.
Preferably, in the second step, the multiple laser beams are formed in a manner that: and irradiating one laser beam onto the beam splitter to form two laser beams, and irradiating the two laser beams onto the substrate through the reflectors to form interference.
Preferably, in the second step, the wavelength of the laser beam is 320-488 nm; the pulse width of the laser beam is 2-1000 ns; the average power of the laser beam is 40-100 mW.
Preferably, the laser beam is angled 40-70 degrees from the perpendicular to the substrate.
Preferably, the first growth and the continuous growth adopt a molecular beam epitaxy growth mode or a gas phase epitaxy growth mode.
Preferably, in step one, the substrate is first removed of surface oxide and then subjected to a first growth.
Preferably, in the step one, after the buffer layer is grown for the first time, the lower limiting layer and the active region are grown continuously, and then the step two is performed.
According to one embodiment of the disclosure, laser interference is used for inducing in-situ growth on the substrate, so that complicated processes such as photoetching, corrosion, cleaning and the like are avoided, and the cost is reduced. The laser interference induction positioning growth positioning is more accurate, and the accuracy is higher. Meanwhile, the cavity opening operation is avoided, the subsequent structure growth is not polluted, and the structural performance is better.
Other features of the present invention and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
FIG. 1 is a schematic diagram of an optical path of a laser beam during laser-induced in-situ growth of a periodic nanostructure according to an embodiment of the present invention.
Fig. 2 is a microscopic image of the periodic nanostructure prepared in example one.
Fig. 3 is a schematic diagram of three epitaxial structures of an embodiment.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
Example one
The method for in-situ growth of the periodic nanostructure by laser induction in the embodiment comprises the following steps:
the method comprises the following steps: with GaAs, InP, Al 2 O 3 The method comprises the following steps of taking materials such as GaSb as a substrate, keeping the position of the substrate unchanged, using a molecular beam epitaxy growth Mode (MBE) or a vapor phase epitaxy growth Mode (MOCVD) to grow a buffer layer made of materials such as GaAs, InP, GaSb, GaN, SiC, InAs and GaP with a certain thickness on the substrate for the first time so as to level the surface of the substrate;
step two: controlling the temperature of the substrate to be 0-200 ℃, enabling a plurality of laser beams to form interference irradiation on the substrate, continuously growing for 1-4h by using materials such as GaAs, InP, GaSb, GaN, SiC, InAs, GaP and the like by using MBE or MOCVD, and forming a periodic nano structure after closing the laser irradiation.
By the method, a plurality of laser beams are focused on the substrate to generate interference, periodic nanometer bright and dark stripes are formed in a light spot area on the substrate by the interference, and the heat effect and the temperature at the bright stripes are high; the heat effect at the dark stripe is low, and the temperature is low; the growth of the inducing material at the bright stripes can be controlled by controlling the laser parameters and the growth conditions, and finally the periodic nano structure is formed.
In this embodiment, the substrate includes, but is not limited to, GaAs, InP, Al 2 O 3 Or GaSb, in the first growth, the buffer layer is formed of a material including, but not limited to, one of GaAs, InP, GaSb, GaN, SiC, InAs, or GaP, and in the subsequent growth, the periodic nanostructures are formed of a material including, but not limited to, one of GaAs, InP, GaSb, GaN, SiC, InAs, or GaP.
In this embodiment or other embodiments, in the second step, a laser interference inducing device is used to perform laser interference irradiation, and a plurality of laser beams are formed in the laser interference inducing device as shown in fig. 1, one laser beam is used to be finished through a plano-concave lens 210 and a plano-convex lens 220 and then is incident on a 50:50 beam splitter 300, the beam is equally divided into two beams with equal intensity, and the two beams are totally reflected by a reflector 410 and focused on the substrate 100 to generate interference.
In this or other embodiments, in step two:
the wavelength of the laser beam is 320-488 nm;
the pulse width of the laser beam is 2-1000 ns;
the average power of the laser beam is 40-100mW, the epitaxial quality can be reduced by excessively high power, and the power is too low to grow slowly, so that the required structural effect cannot be achieved finally.
The included angle between the laser beam and the vertical direction of the substrate is 40-70 degrees.
In other embodiments, the wavelength, pulse width, average power, and angle of the laser beam perpendicular to the substrate may be adjusted depending on the growth material and the equipment.
In the embodiment, the polarization states of the laser beams are different, and the periods of light and dark fringes formed by interference are also different, namely the periods of the in-situ grown nano structures are different; if the polarization state of the incident laser beam is a TE mode, the period calculation formula is as follows:
Figure BDA0003638187020000041
if the polarization state of the incident laser beam is a TM mode, the period calculation formula is as follows:
Figure BDA0003638187020000042
wherein: in the formula, Λ is the period of the light and dark stripes, namely the period of the nano structure; λ is the wavelength of the incident laser beam; and theta is the included angle between the laser and the substrate in the vertical direction.
In this or other embodiments, the Ga source is introduced while keeping the As source always on after the buffer layer growth is completed, until the periodic nanostructure is formed.
In this embodiment or other embodiments, in step one, the surface oxide is first removed from the substrate to ensure the purity of the substrate, and then the first growth is performed, so as to ensure the growth quality and growth precision of the periodic nanostructure.
In this embodiment or other embodiments, in the step one, after the buffer layer is grown for the first time, the lower confinement layer and the multiple quantum well active region are continuously grown, and then the step two is performed, so that the periodic nanostructure can be grown by the method alone, and the periodic nanostructure can also be grown in the process of growing the epitaxial structure.
According to the embodiment, the laser interference is used for inducing in-situ growth on the substrate, so that complicated processes such as photoetching, corrosion, cleaning and the like are avoided, and the cost is reduced. The laser interference induction positioning growth positioning is more accurate, and the accuracy is higher. Meanwhile, the cavity opening operation is avoided, the subsequent structure growth is not polluted, and the structural performance is better.
Example two
In this particular example, a 2 "n-type GaAs substrate was exposed to MBE at 580 deg.C to remove surface oxides, then heated to 600 deg.C to grow a 500nm thick n-type GaAs buffer layer, the substrate was cooled to 200 deg.C, and the substrate rotation was stopped. The parameters of the laser interference inducing device are adjusted to be that the wavelength of a laser beam is 355nm, the pulse width is 2ns, the average power is 52mW, the included angle with the vertical direction of the substrate is 64 degrees, and the polarization state of the beam is a TE mode. And turning on a laser light source, and focusing and interfering the laser on the substrate. Meanwhile, the As source in the MBE is normally open, Ga is slowly introduced, and the growth is carried out for 4 hours under the condition, so that the periodic nano structure is obtained. And closing the Ga source, closing the laser induction device, closing the As source, cooling and taking out the substrate. As shown in fig. 2, the growth area was tested using AFM, which resulted in a growth of nanostructures with a period of about 200 nm.
EXAMPLE III
In the specific embodiment, a 2-inch n-type GaAs substrate is subjected to surface oxide removal in MBE at 580 ℃, then the temperature is raised to 600 ℃ to grow a 300 nm-thick n-type GaAs buffer layer, then a 1.2 micron n-type AlGaAs lower limiting layer is sequentially grown, the temperature is lowered to 500 ℃ to grow an InGaAs multi-quantum well active region, and after the growth of the above structure is completed, the temperature of the substrate is lowered to 200 ℃, and the rotation of the substrate is stopped. The parameters of the laser interference inducing device are adjusted as follows: the wavelength of the laser beam is 355nm, the pulse width is 2ns, the average power is 52mW, the included angle with the vertical direction of the substrate is 64 degrees, and the polarization state of the beam is a TE mode. And turning on a laser light source, and focusing and interfering the laser on the substrate. Meanwhile, the As source in the MBE is normally open, Ga is slowly introduced, and the growth is carried out for 4 hours under the condition, so that the periodic grating structure is obtained. Then the laser induction device is closed and the temperature is raised to 600 ℃, the 1.2 micron p-type AlGaAs upper limiting layer continues to grow, and finally the 300nm thick p-type heavily doped GaAs layer is grown to finish the whole epitaxial structure. Thus, an epitaxial structure of the DFB laser fabricated by the in-situ growth method is formed.
Example four
In this particular example, a 2 "n-type GaAs substrate was exposed to MBE at 580 deg.C to remove surface oxides, then heated to 600 deg.C to grow a 500nm thick n-type GaAs buffer layer, the substrate was cooled to 200 deg.C, and the substrate rotation was stopped. The parameters of the laser interference inducing device are adjusted to be that the wavelength of a laser beam is 405nm, the pulse width is 7ns, the average power is 34mW, the included angle with the vertical direction of the substrate is 60 degrees, and the polarization state of the beam is a TE mode. And turning on a laser light source, and focusing and interfering the laser on the substrate. Meanwhile, the As source in the MBE is normally open, Ga is slowly introduced, and the growth is carried out for 4 hours under the condition, so that the periodic nano structure is obtained. And closing the Ga source, closing the laser induction device, closing the As source, cooling and taking out the substrate. The growth area was tested using AFM, which resulted in a growth of nanostructures with a period of about 235 nm.
EXAMPLE five
In this embodiment, a 2-inch n-type InP substrate is subjected to MBE at 500-700 ℃ to remove surface oxide, and then cooled to 400 ℃ to grow a 300nm thick InP buffer layer. And cooling the substrate to room temperature, and stopping the rotation of the substrate. The parameters of the laser interference inducing device are adjusted to be that the wavelength of a laser beam is 355nm, the pulse width is 5ns, the average power is 40mW, the included angle with the vertical direction of the substrate is 64 degrees, and the polarization state of the laser beam is a TE mode. And turning on a laser light source, and focusing and interfering the laser on the substrate. Meanwhile, the P source In the MBE is normally open and is slowly communicated with In, and the MBE grows for 2 hours under the condition, so that the periodic nano structure is obtained. And closing the In source, closing the laser induction device, closing the P source and taking out the substrate slice. The growth area was tested using AFM, which resulted in a growth of nanostructures with a period of about 198 nm.
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.

Claims (9)

1. A method for growing periodic nanostructures in situ by laser induction, comprising the steps of:
the method comprises the following steps: carrying out primary growth on the substrate to form a buffer layer, and flattening the surface of the substrate;
step two: and continuously growing the substrate while irradiating the substrate by utilizing a plurality of laser beams, wherein the plurality of laser beams form interference on the substrate, and the periodic nano structure is formed after the substrate is continuously grown for 1-4 h.
2. The method of claim 1, wherein the substrate comprisesBut are not limited to GaAs, InP, Al 2 O 3 Or GaSb, in the first growth, the buffer layer is formed of a material including, but not limited to, one of GaAs, InP, GaSb, GaN, SiC, InAs, or GaP, and in the subsequent growth, the periodic nanostructures are formed of a material including, but not limited to, one of GaAs, InP, GaSb, GaN, SiC, InAs, or GaP.
3. The method of claim 1, wherein in the second step, the substrate temperature is controlled to 0-200 ℃ for further growth.
4. The method for laser-induced in-situ growth of periodic nanostructures according to claim 1, wherein in step two, the plurality of laser beams are formed by: and irradiating one laser beam onto the beam splitter to form two laser beams, and irradiating the two laser beams onto the substrate through the reflectors to form interference.
5. The method of claim 1, wherein in the step two, the wavelength of the laser beam is 320-488 nm; the pulse width of the laser beam is 2-1000 ns; the average power of the laser beam is 40-100 mW.
6. The method of claim 1, wherein the laser beam is at an angle of 40-70 degrees with respect to the vertical direction of the substrate.
7. The method of any one of claims 1 to 6, wherein the first growth and the further growth are molecular beam epitaxy or vapor phase epitaxy.
8. The method of claim 1, wherein in step one, the substrate is first removed of surface oxide and then subjected to a first growth.
9. The method of claim 1, wherein after the buffer layer is grown for the first time, the lower confinement layer and the active region are grown, and then step two is performed.
CN202210508097.1A 2022-05-11 2022-05-11 Method for in-situ growth of periodic nanostructure through laser induction Pending CN115083885A (en)

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