CN111257078B - Method and device for preparing lithium niobate nano domain structure by ion beam irradiation - Google Patents
Method and device for preparing lithium niobate nano domain structure by ion beam irradiation Download PDFInfo
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- CN111257078B CN111257078B CN202010128892.9A CN202010128892A CN111257078B CN 111257078 B CN111257078 B CN 111257078B CN 202010128892 A CN202010128892 A CN 202010128892A CN 111257078 B CN111257078 B CN 111257078B
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Abstract
The invention relates to a method and a device for preparing a lithium niobate nanometer domain structure by ion beam irradiation. Which comprises the following steps: 1) Fixing a lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting to enable the incident angle of the ion beam to reach a working angle; adjusting to enable the center of the ion source to coincide with the center of the workpiece; 2) Pumping the ion beam etching equipment to high vacuum, wherein the vacuum degree is lower than 2 multiplied by 10 < -3 > Pa; introducing high-purity 99.999% inert gas argon or xenon, and controlling the gas flow by using a gas flowmeter to keep the working vacuum at 2X 10-2Pa to 8X 10-2Pa; 3) Starting an ion source, and performing ion beam irradiation on a lithium niobate sample; 4) And placing the irradiated lithium niobate crystal in a high-temperature furnace for heat treatment, wherein the heat treatment temperature is 80-350 ℃ and the time is 0.2-3 hours. The method utilizes ion bombardment to induce formation of self-organized nano domain structures on the surface of a sample, and can control the characteristics of the obtained nano domain structures by regulating ion beam parameters.
Description
Technical Field
The invention belongs to the technical field of nano domain structure preparation in the field of ferroelectric crystal nano domain engineering, and particularly relates to a method and a device for preparing a lithium niobate nano domain structure by ion beam irradiation.
Background
In recent years, a new hot tide, i.e. a hot tide for researching a nano structure, appears in the field of nano materials, so that a new technology for preparing the nano structure by ion beam irradiation is widely focused in the scientific research field. The ion beam irradiation technology is a new idea of simply, economically and widely manufacturing self-organizing nano-structures by utilizing the interaction result of an ion beam sputtering induced roughening mechanism and different surface relaxation mechanisms to enable the surfaces to spontaneously form certain nano-structures. The self-organizing nano structure obtained by the technology has a plurality of advantages: 1. the processing materials are various, and nano structures can be generated on various materials such as insulators, semiconductors, metals, nonmetal and the like; 2. the nanostructure lateral feature size (i.e., period or wavelength of the nanostructure) is small, typically between hundred nanometers and tens of nanometers, and even smaller; 3. the ion beam parameter has high controllability, and the characteristics of the shape, the period, the amplitude, the symmetry and the like of the nano structure can be effectively regulated and controlled by adjusting various parameters in the ion irradiation process, so that the technology has important application prospect in the field of nano manufacturing.
In recent years, methods for preparing domain structures include an external electric field method, an ion implantation method, an electron beam scanning method and the like, and an external electric field polarization technology can prepare a micron-sized single domain structure at room temperature, but extremely high voltage is required to polarize crystals, and the aspect ratio of a periodic domain caused by lateral growth of the prepared domain structure is poor, so that the difficulty in manufacturing a submicron-sized domain is high. Ion implantation technology has the advantages of accurate and controllable concentration and depth distribution of implanted ions, free choice of substrate temperature during ion implantation, and the like, but the ion implantation requires precise vacuum equipment and good experimental conditions. The electron beam scanning technology utilizes electrons to converge into electron beams to scan on the surface of the crystal to directly write domain patterns, and can prepare deeper domain structures, but the domain inversion continuity is poor.
Disclosure of Invention
The invention provides a simple, efficient and low-cost method and a device for preparing a lithium niobate nano domain structure by ion beam irradiation.
In order to solve the problems existing in the prior art, the technical scheme of the invention is as follows: a method for preparing a lithium niobate nano domain structure by ion beam irradiation comprises the following steps:
fixing a lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting to enable the incident angle of an ion beam to reach a working angle; adjusting to enable the center of the ion source to coincide with the center of the workpiece;
step two, the ion beam etching equipment is pumped to high vacuum, and the vacuum degree is generally lower than 2 multiplied by 10 < -3 > Pa; introducing high-purity 99.999% inert gas argon or xenon, and controlling the gas flow by using a gas flowmeter to keep the working vacuum at 2X 10-2Pa to 8X 10-2Pa;
step three, starting an ion source, and performing ion beam irradiation on the lithium niobate sample;
and fourthly, placing the irradiated lithium niobate crystal into a high temperature furnace for heat treatment, wherein the heat treatment temperature is 80-350 ℃ and the time is 0.2-3 hours.
In the third step, the ion beam is Xe, the ion beam energy E is 450-750eV, the ion beam current J is 130-450 mu A/cm < 2 >, the ion beam incidence angle theta is 10-30 degrees or 55-75 degrees, the ion beam action t is 30-300min, and the ion beam incidence angle theta is the included angle between the ion beam and the normal line of the surface of the sample.
In the third step, the ion beam is Ar, the ion beam energy E is 900-1350eV, the ion beam current J is 240-620 mu A/cm < 2 >, the ion beam incidence angle theta is 10-30 degrees or 55-75 degrees, the ion beam action t is 30-300min, and the ion beam incidence angle theta is the included angle between the ion beam and the normal line of the sample surface.
The device adopted by the method for preparing the lithium niobate nanometer domain structure by the ion beam irradiation comprises a substrate movement system, an ion source system, a vacuum system and a control system, wherein the substrate movement system comprises a base, a shaft sleeve, a base platform and a X, Y bidirectional movement platform, the lower end surface of the base platform is fixed on the base platform, the upper end surface of the base platform is fixedly connected with the X, Y bidirectional movement platform, and a cooling channel is arranged in the base platform.
The cooling channel is connected with a central pipeline, circulating water enters the cooling channel from a water inlet on the central pipeline of the base station, and is collected to a water outlet on the central pipeline after circulating in the cooling channel, so that the substrate station is kept at a constant temperature of 10-30 ℃.
The outer end of the central pipeline is connected with a corrugated pipe.
According to the invention, the self-organized nano structure is formed on the surface of the lithium niobate crystal by the irradiation of the ion beam, and meanwhile, certain atoms or atomic groups are sputtered preferentially, so that atoms in the crystal deviate from the original position, and the sputtering and the self-organized nano structure are formed, so that the crystal presents an overall uniform spontaneous polarization state to form the self-organized nano structure, and the spontaneous polarization direction is changed to form a nano domain structure.
Compared with the prior art, the invention has the following advantages:
1. the method is simple, easy to operate, economical and high in machining precision, and is an irreplaceable high-quality method for manufacturing the optical micro-nano structure;
2. the nanometer structure on the surface of the sample under different ion beam parameters is controllable, the ion beam irradiation technology is used, the preparation of nanometer domain structures with different scales can be realized by changing the ion beam parameters and the heat treatment time, and the preparation device and the preparation method of the nanometer domain structure of the lithium niobate crystal can realize batch preparation of the domain structures with the sizes of tens to hundreds of nanometers;
3. the invention can reduce the processing cost and realize the high efficiency and the flexibility of the processing process.
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a nano domain structure of lithium niobate according to the present invention;
FIG. 2 is an AFM image of the surface of a lithium niobate sample after irradiation with Xe ion beam at different parameters;
FIG. 3 is a domain structure of the surface of a lithium niobate sample after Xe ion beam irradiation;
FIG. 4 is an AFM image of the surface of a lithium niobate sample after Ar ion beam irradiation;
FIG. 5 is a domain structure of the surface of a lithium niobate sample after Ar ion beam irradiation;
reference numerals: 1-substrate motion system, 2-ion source system, 3-vacuum system, 4-control system, 101-base, 102-base station, 103-cooling channel, 104-X, Y bidirectional motion platform, 201-beam limiting diaphragm, 202-three grid system, 203-radio frequency or microwave generator, 204-plasma, 205-gas circuit.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
A method for preparing a lithium niobate nano domain structure by ion beam irradiation comprises the following steps:
fixing a lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting to enable the incident angle of an ion beam to reach a working angle; adjusting to enable the center of the ion source to coincide with the center of the workpiece;
step two, the ion beam etching equipment is pumped to high vacuum, and the vacuum degree is generally lower than 2 multiplied by 10 < -3 > Pa; introducing high-purity 99.999% inert gas argon or xenon, and controlling the gas flow by using a gas flowmeter to keep the working vacuum at 2X 10-2Pa to 8X 10-2Pa;
step three, starting an ion source, and performing ion beam irradiation on the lithium niobate sample;
and fourthly, placing the irradiated lithium niobate crystal into a high temperature furnace for heat treatment, wherein the heat treatment temperature is 80-350 ℃ and the time is 0.2-3 hours.
The provided method for preparing the lithium niobate nano domain structure adopts a device comprising a substrate movement system 1, an ion source system 2, a vacuum system 3 and a control system 4. The ion source system 2, the vacuum system 3 and the control system 4 are all in a conventional structure, wherein the ion source system 2 comprises a beam limiting diaphragm 201, a screen grating, an accelerating grating, a three-grating system 202 of the beam grating and a radio frequency or microwave generator 203, the accelerating grating voltage controls the emission angle of the ion beam, the accelerating grating voltage is adjusted to enable the emission angle of the ion beam to be less than +/-5%, and the discharge power of the radio frequency or microwave generator 203 is adjusted to control the extracted beam; the beam limiting diaphragm 201 limits the aperture of the extracted ion beam.
The substrate motion system 1 comprises a base 101, a base 102 and a X, Y bi-directional motion platform 104, wherein the upper end surface of the base 102 is fixed on the base 101, the upper end surface of the base 102 is fixedly connected with the X, Y bi-directional motion platform 104, and a cooling channel 103 is arranged in the base 102.
The cooling channel 103 is connected with a central pipeline, circulating water enters the cooling channel 103 from the central pipeline of the base station 102, and is collected and enters a water outlet after circulating in the cooling channel 103, so that the substrate station is kept at a constant temperature of 10-30 ℃. The outer end of the central pipeline is connected with a corrugated pipe 105, and circulating water is sent into the base station 102 by the corrugated pipe 105, so that a better sealing effect is achieved.
In the invention, self-organizing nano structures with different shapes and characteristic sizes are formed on the surface of a sample after the ion beam irradiation, and then nano domains with different sizes are formed by polarization, wherein the nano domain size is 50-500nm, the nano domain size is related to ion beam parameter selection, and the nano structure shapes comprise but are not limited to: a dot cone-shaped, corrugated self-organizing nanostructure; the nano domains include dot domains, line domains and dendrite domains.
Example 1:
a method for preparing a lithium niobate nano domain structure by ion beam irradiation comprises the following steps:
step (1): fixing a Z tangential lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting a base 101 to enable the incident angle of an ion beam to reach a working angle; adjusting X, Y the bi-directional motion platform 105 to enable the center of the ion source to coincide with the center of the workpiece;
step (2): vacuumizing the ion bombardment equipment to 1.8X10-3 Pa; introducing xenon, and controlling the gas flow of the xenon by using a gas mass flowmeter to ensure that the working vacuum degree is stabilized at 2.6X10-2 Pa; the sample stage cooling water is maintained at 22 ℃;
step (3): starting an ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incidence angle θion=60°, jion=265 μa/cm2, ion beam irradiation time 60min, ion beam energy eion=500 eV; and maintaining the high vacuum for 30min after the irradiation is completed.
Step (4): and taking the lithium niobate crystal after the Xe ion beam irradiation is completed out of the vacuum chamber, and placing the lithium niobate crystal in a high temperature furnace for heat treatment, wherein the heat treatment temperature is 80 ℃ and the time is 3 hours.
A corrugated self-organizing nanostructure is formed on the surface of the sample, and a domain structure is formed by forming small regions with the same spontaneous polarization by the off-site atoms inside the crystal. The surface morphology of the sample was examined using an Atomic Force Microscope (AFM) as shown in fig. 2. Etching the lithium niobate crystal with self-organized nano structure formed by irradiating Xe ion beam with hydrofluoric acid with concentration of 5% -10% for 10min, and treating with polarized light microscope domain structure shown in figure 3 (a). The domain structure observed by applying a voltage to the probe tip by an atomic force microscope is shown in fig. 3 (b).
Example 2:
a method for preparing a lithium niobate nano domain structure by ion beam irradiation comprises the following steps:
step (1): fixing a Z tangential lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting a base 101 to enable the incident angle of an ion beam to reach a working angle; adjusting X, Y the bi-directional motion platform 105 to enable the center of the ion source to coincide with the center of the workpiece;
step (2): vacuumizing the ion bombardment equipment to 5X 10-4Pa; introducing xenon, and controlling the gas flow of the xenon by using a gas mass flowmeter to ensure that the working vacuum degree is stabilized at 3 multiplied by 10 < -2 > Pa; the sample stage cooling water is maintained at 22 ℃;
step (3): starting an ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incidence angle θion=15°, jion=354 μa/cm2, ion beam irradiation time 300min, ion beam energy eion=700 eV; and maintaining the high vacuum for 30min after the irradiation is completed.
Step (4): and taking the lithium niobate crystal after the Xe ion beam irradiation is completed out of the vacuum chamber, and placing the lithium niobate crystal in a high temperature furnace for heat treatment, wherein the heat treatment temperature is 150 ℃ and the time is 0.5 hour.
The surface morphology of the sample was examined using an Atomic Force Microscope (AFM) as shown in fig. 2. Etching the lithium niobate crystal with self-organized nano structure formed by irradiating Xe ion beam with hydrofluoric acid with concentration of 5% -10% for 10min, and treating with polarized light microscope domain structure shown in figure 3 (a). The domain structure observed by applying a voltage to the probe tip by an atomic force microscope is shown in fig. 3 (b).
Example 3:
a method for preparing a lithium niobate nano domain structure by ion beam irradiation comprises the following steps:
step (1): fixing a Z tangential lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting a base 101 to enable the incident angle of an ion beam to reach a working angle; adjusting X, Y the bi-directional motion platform 105 to enable the center of the ion source to coincide with the center of the workpiece;
step (2): vacuumizing the ion bombardment equipment to 6.5X10-4 Pa; argon is introduced, and the gas flow of the argon is controlled by using a gas mass flowmeter, so that the working vacuum degree is stabilized at 3 multiplied by 10 < -2 > Pa; the sample stage cooling water is maintained at 22 ℃;
step (3): starting an ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incidence angle θion=60°, ion beam current density jeon=442 μa/cm2, ion beam irradiation time 120min, ion beam energy eion=1200 eV; and maintaining the high vacuum for 30min after the irradiation is completed.
Step (4): and taking out the lithium niobate crystal irradiated by the Ar ion beam from the vacuum chamber, and placing the lithium niobate crystal in a high-temperature furnace for heat treatment, wherein the heat treatment temperature is 200 ℃ and the time is 1 hour.
The surface morphology of the sample detected by an Atomic Force Microscope (AFM) is shown in figure 4, the lithium niobate crystal which forms the self-organized nano structure after Ar ion beam irradiation is corroded by hydrofluoric acid with the concentration of 5% -10%, the corrosion time is 10min, and the domain structure of the treated sample by a polarized light microscope is shown in figure 5.
The foregoing description is only of the preferred embodiments of the present invention, and is not intended to limit the scope of the present invention.
Claims (1)
1. A method for preparing a lithium niobate nanometer domain structure by ion beam irradiation is characterized in that: the method comprises the following steps:
fixing a lithium niobate sample to be processed on a sample stage of ion beam etching equipment, and adjusting to enable the incident angle of an ion beam to reach a working angle; adjusting to enable the center of the ion source to coincide with the center of the workpiece;
step two, pumping the ion beam etching equipment to high vacuum, wherein the vacuum degree is lower than 2 multiplied by 10 < -3 > Pa; introducing high-purity 99.999% inert gas argon or xenon, and controlling the gas flow by using a gas flowmeter to keep the working vacuum at 2X 10-2Pa to 8X 10-2Pa;
step three, starting an ion source, and performing ion beam irradiation on the lithium niobate sample;
fourthly, placing the irradiated lithium niobate crystal into a high temperature furnace for heat treatment, wherein the heat treatment temperature is 80-350 ℃ and the time is 0.2-3 hours;
in the third step, the ion beam is Xe, the ion beam energy E is 450-750eV, the ion beam current J is 130-450 mu A/cm < 2 >, the ion beam incidence angle theta is 10-30 degrees or 55-75 degrees, the ion beam action t is 30-300min, and the ion beam incidence angle theta is the included angle between the ion beam and the normal line of the surface of the sample;
in the third step, the ion beam is Ar, the ion beam energy E is 900-1350eV, the ion beam current J is 240-620 mu A/cm < 2 >, the ion beam incidence angle theta is 10-30 degrees or 55-75 degrees, the ion beam action t is 30-300min, and the ion beam incidence angle theta is the included angle between the ion beam and the normal of the sample surface;
the device adopted by the method for preparing the lithium niobate nanometer domain structure by the ion beam irradiation comprises a substrate movement system (1), an ion source system (2), a vacuum system (3) and a control system (4), and is characterized in that: the substrate motion system (1) comprises a base (101), a base table (102) and a X, Y bidirectional motion platform (104), wherein the lower end surface of the base table (102) is fixed on the base (101), the upper end surface of the base table (102) is fixedly connected with the X, Y bidirectional motion platform (104), and a cooling channel (103) is arranged in the base table (102);
the cooling channel (103) is connected with a central pipeline, circulating water enters the cooling channel (103) from a water inlet on the central pipeline of the base station (102), and is collected into a water outlet on the central pipeline after circulating in the cooling channel (103), so that the substrate station is kept at a constant temperature of 10-30 ℃;
the outer end of the central pipeline is connected with a corrugated pipe (105).
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