CN111257077B - Method and device for preparing lithium niobate nano dot domain structure by ion beam irradiation - Google Patents
Method and device for preparing lithium niobate nano dot domain structure by ion beam irradiation Download PDFInfo
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Abstract
The invention relates to a method and a device for preparing a lithium niobate nano dot domain structure by ion beam irradiation. The method of the invention 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) Setting the rotating speed of a sample table, starting an ion source, and carrying out ion beam irradiation on a lithium niobate sample, wherein the rotating speed of the sample table is 6-80 revolutions per minute; 4) And placing the irradiated lithium niobate crystal in a high temperature furnace for heat treatment at the temperature of 80-350 ℃ for 0.2-3 hours. The invention utilizes ion bombardment to induce the formation of self-organized nano-dot domain structures on the surface of the sample, and can control the characteristics of the obtained nano-domain structures by regulating ion beam parameters.
Description
Technical Field
The invention relates to the technical field of nano-dot domain structure preparation in the field of ferroelectric crystal nano-domain engineering, in particular to a method and a device for preparing a lithium niobate nano-dot 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.
The preparation method of the dot domain structure has various methods, such as 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 is poor due to the lateral growth of the prepared domain structure, so that the difficulty of 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-dot 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 dot 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;
setting the rotating speed of a sample table, starting an ion source, and performing ion beam irradiation on a lithium niobate sample, wherein the rotating speed of the sample table is 6-80 revolutions per minute;
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 density 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 density 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 nano dot domain structure by the ion beam irradiation comprises a substrate movement system, an ion source system, a vacuum system and a control system, and is characterized in that: the substrate movement system comprises a base, a shaft sleeve, a base platform and a X, Y bidirectional movement platform, wherein the cross section of the base platform is T-shaped, the shaft sleeve is sleeved on the outer side of the small end of the base platform, and the base is fixed at the end part of the shaft sleeve; the end face of the large end of the base station is fixedly connected with the X, Y bidirectional moving platform, and a cooling channel is arranged in the large end of the base station.
The cooling channel is connected with a central pipeline, the outer end of the central pipeline is connected with a rotary joint, the rotary joint is connected with a corrugated pipe, circulating water enters the cooling channel from the central pipeline of the base station after passing through the corrugated pipe, and enters a water outlet on the rotary joint after circulating in the cooling channel, so that the substrate table is kept at a constant temperature of 10-30 ℃.
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. in the method provided by the invention, the rotation process enables the surface structure of the sample to uniformly grow in all directions, so that a regular nanometer self-assembled dot structure is formed;
3. the nano structure on the surface of the sample under different ion beam parameters is controllable, and the preparation of nano domain structures with different scales can be realized by changing the ion beam parameters and the heat treatment time by using the ion beam irradiation technology. The preparation device and the preparation method of the lithium niobate crystal nano domain structure can realize batch preparation of the dot domain structure with the size of tens to hundreds of nanometers;
4. 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 irradiation with Ar ion beam at different parameters;
fig. 5 is a domain structure of the surface of the lithium niobate sample after Ar ion beam irradiation.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
A method for preparing a lithium niobate nano dot 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;
setting the rotating speed of a sample table, starting an ion source, and performing ion beam irradiation on a lithium niobate sample, wherein the rotating speed of the sample table is 6-80 revolutions per minute;
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 dot domain structure by the ion beam irradiation adopts a device which comprises 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 shaft sleeve 102, a base 103 and a X, Y bidirectional motion platform 105, wherein the cross section of the base 103 is T-shaped, the shaft sleeve 102 is sleeved outside the small end of the base 103, and the base 101 is fixed at the end part of the shaft sleeve 102; the end face of the large end of the base 103 is fixedly connected with a X, Y bi-directional motion platform 105, and a cooling channel 104 is arranged in the large end of the base 103. The cooling channel 104 is connected with a central pipeline, the outer end of the central pipeline is connected with a rotary joint 106, and the rotary joint 106 is connected with a corrugated pipe 107 to achieve a better sealing effect. The circulating water enters the cooling channel 104 from the central pipeline of the base 103 after passing through the corrugated pipe 107, and enters the water outlet on the rotary joint 106 after circulating in the cooling channel 104, so as to realize the constant temperature of the substrate table at 10-30 ℃.
In the invention, self-organized dot-shaped or dot-cone-shaped nano structures with different characteristic sizes are formed on the surface of a sample after ion beam irradiation, so that nano dot domains with different sizes are formed by polarization, the size of each nano dot domain is 50-500nm, the size of each nano dot domain is related to the parameter selection of the ion beam, and the nano structures are dot-shaped or dot-cone-shaped structures; the nano domain is in a dot domain structure.
Example 1:
a method for preparing a lithium niobate nano dot 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 an 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 ion bombardment equipment to 5 multiplied by 10 < -4 > 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 3 multiplied by 10 < -2 > Pa; the sample stage cooling water is maintained at 22 ℃;
setting the rotation speed of a sample stage to be 20 revolutions per minute, starting an ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incident angle θion=15°, jion=265 μa/cm2, 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 120 ℃ and the time is 1.5 hours.
Example 2:
a method for preparing a lithium niobate nano dot 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 an incident angle of an ion beam to reach a working angle; adjusting X, Y the bidirectional moving platform (105) to enable the center of the ion source to coincide with the center of the workpiece;
step (2), vacuumizing ion bombardment equipment to 5 multiplied by 10 < -4 > 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 3 multiplied by 10 < -2 > Pa; the sample stage cooling water is maintained at 22 ℃;
setting the rotation speed of a sample stage to be 20 revolutions per minute, starting a Xe ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incident angle θion=60°, jion=265 μa/cm2, 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 100 ℃ and the time is 2 hours.
Examples 1 and 2 are examples of the preparation of lithium niobate nanodot domain structures by Xe ion beam irradiation, the surface morphology of the samples is shown in fig. 2, and the observed domain structures are shown in fig. 3, using Atomic Force Microscopy (AFM).
Example 3:
a method for preparing a lithium niobate nano dot 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 an 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 ion bombardment equipment to 5 multiplied by 10 < -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 ℃;
setting the rotation speed of a sample stage to be 30 revolutions per minute, starting an Ar ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incident angle θion=15°, jion=400 μa/cm2, ion beam energy eion=1000 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 120 ℃ and the time is 1.5 hours.
Example 4:
a method for preparing a lithium niobate nano dot 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 an 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 ion bombardment equipment to 5 multiplied by 10 < -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 ℃;
setting the rotation speed of a sample stage to be 30 revolutions per minute, starting an Ar ion source to perform an ion beam irradiation experiment, and setting ion beam irradiation parameters: ion beam incident angle θion=60°, jion=400 μa/cm2, 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 100 ℃ and the time is 2 hours.
Examples 3 and 4 are examples of preparing lithium niobate nanodot domain structures by Ar ion beam irradiation, the surface morphology of the samples is shown in fig. 4, and the observed domain structures are shown in fig. 5, using Atomic Force Microscopy (AFM).
Claims (2)
1. A method for preparing a lithium niobate nano dot 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, the ion beam etching equipment is pumped to high vacuum, and the vacuum degree is lower than 2 multiplied by 10 -3 Pa; introducing high-purity 99.999% inert gas argon or xenon, and controlling gas flow by using a gas flowmeter to keep working vacuum at 2×10 -2 Pa to 8X 10 - 2 Pa;
Setting the rotating speed of a sample table, starting an ion source, and performing ion beam irradiation on a lithium niobate sample, wherein the rotating speed of the sample table is 6-80 revolutions per minute;
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 density 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;
the device adopted by the method for preparing the lithium niobate nano dot 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),
the substrate motion system (1) comprises a base (101), a shaft sleeve (102), a base (103) and a X, Y bidirectional motion platform (105), wherein the cross section of the base (103) is T-shaped, the shaft sleeve (102) is sleeved on the outer side of the small end of the base (103), and the base (101) is fixed at the end part of the shaft sleeve (102); the end face of the large end of the base station (103) is fixedly connected with a X, Y bidirectional motion platform (105), and a cooling channel (104) is arranged in the large end of the base station (103);
the cooling channel (104) is connected with a central pipeline, the outer end of the central pipeline is connected with a rotary joint (106), the rotary joint (106) is connected with a corrugated pipe (107), circulating water enters the cooling channel (104) from the central pipeline of the base station (103) after passing through the corrugated pipe (107), and enters a water outlet on the rotary joint (106) after circulating in the cooling channel (104), so that the substrate table is kept at a constant temperature of 10-30 ℃.
2. A method for preparing a lithium niobate nano dot 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, the ion beam etching equipment is pumped to high vacuum, and the vacuum degree is lower than 2 multiplied by 10 -3 Pa; introducing high-purity 99.999% inert gas argon or xenon, and controlling gas flow by using a gas flowmeter to keep working vacuum at 2×10 -2 Pa to 8X 10 - 2 Pa;
Setting the rotating speed of a sample table, starting an ion source, and performing ion beam irradiation on a lithium niobate sample, wherein the rotating speed of the sample table is 6-80 revolutions per minute;
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 Ar, the ion beam energy E is 900-1350eV, the ion beam current density 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 nano dot 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),
the substrate motion system (1) comprises a base (101), a shaft sleeve (102), a base (103) and a X, Y bidirectional motion platform (105), wherein the cross section of the base (103) is T-shaped, the shaft sleeve (102) is sleeved on the outer side of the small end of the base (103), and the base (101) is fixed at the end part of the shaft sleeve (102); the end face of the large end of the base station (103) is fixedly connected with a X, Y bidirectional motion platform (105), and a cooling channel (104) is arranged in the large end of the base station (103);
the cooling channel (104) is connected with a central pipeline, the outer end of the central pipeline is connected with a rotary joint (106), the rotary joint (106) is connected with a corrugated pipe (107), circulating water enters the cooling channel (104) from the central pipeline of the base station (103) after passing through the corrugated pipe (107), and enters a water outlet on the rotary joint (106) after circulating in the cooling channel (104), so that the substrate table is kept at a constant temperature of 10-30 ℃.
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