CN108681181B - Laser-assisted thermal polarization equipment and method for microscopic second-order nonlinear polarizability optical element - Google Patents
Laser-assisted thermal polarization equipment and method for microscopic second-order nonlinear polarizability optical element Download PDFInfo
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- CN108681181B CN108681181B CN201810477666.4A CN201810477666A CN108681181B CN 108681181 B CN108681181 B CN 108681181B CN 201810477666 A CN201810477666 A CN 201810477666A CN 108681181 B CN108681181 B CN 108681181B
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- 239000010955 niobium Substances 0.000 claims abstract description 150
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 149
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 43
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- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/355—Non-linear optics characterised by the materials used
- G02F1/3555—Glasses
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/3501—Constructional details or arrangements of non-linear optical devices, e.g. shape of non-linear crystals
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/35—Non-linear optics
- G02F1/37—Non-linear optics for second-harmonic generation
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- Optical Modulation, Optical Deflection, Nonlinear Optics, Optical Demodulation, Optical Logic Elements (AREA)
Abstract
The invention discloses a microscopic second-order nonlinear polarizability lightA laser-assisted thermal polarization equipment and method for optical element features that the Sm doped ITO glass with single surface and side coated with silver lines is used as anode, silicon wafer as cathode and continuous laser with 1064nm wavelength is used3+The ionic niobium borophosphate glass is prepared by micro thermal polarization. The electric field, the thermal field and the laser field auxiliary method can realize optical elements with various micron-sized microstructures. The periodicity and morphology of the sample can be controlled by adjusting the laser parameters and the thermal polarization parameters. The method can realize the optical element with periodic microscopic second-order nonlinear polarizability at one time, realize that the pattern resolution can reach the level of micron or even nanometer, improve the preparation efficiency by several times to dozens of times compared with the traditional material, control the shape of microstructure distribution and size and the components of atomic or molecular structures, and have high preparation efficiency.
Description
Technical Field
The invention relates to a preparation method of an optical element, in particular to a preparation method of an optical element with a microstructure, which is mainly applied to the technical field of visible-near infrared optical system materials and devices.
Background
In recent years, visible-near infrared optical materials have been widely used in modern military and civil high-tech fields such as information technology, laser technology, electronic communication technology, and the like. The difficulty of obtaining aspheric lenses or prisms from crystalline materials such as sapphire and diamond by using the traditional process is high, the efficiency is low, the cost is high, and the requirements of miniaturization, integration and functionalization of materials by rapidly developing optics, information technology and the like are difficult to meet. The oxide glass material has the advantages of low optical loss, more covered optical communication windows, simple manufacturing process, low cost, no limitation on geometric dimension and the like, and has wide application in visible-near infrared optical systemsAnd the application prospect is good. Wherein the niobium borophosphate (Na)2B4O7-NaPO3-Nb2O5BPN glass material for short, can introduce a large amount of high quadratic non-linear coefficient (n)2) Nb of2O5And the printing ink also has strong third-order nonlinear performance, and is paid more and more attention to the realization of the controllable printing of the size and the distribution of a microstructure, which is a key link for obtaining excellent performance such as frequency doubling and optics.
In order to realize the controllable preparation of the optical functional BPN glass based on the microstructure, the glass needs to be modified. Previous modifications have mainly focused on common microfabrication means such as dry etching and photolithography, which have disadvantages in that equipment is expensive, processes are complicated, processing efficiency is low, and the like, and particularly, photolithography is also affected by light.
In 2002, Komatsu et al proposed a simple and feasible solution-writing the desired microscopic single crystal structure in special ion-doped glass using continuous laser; based on the distribution and size of the microstructure and other morphological parameters and the atom or molecular structure and other components, the printing of the optical material with low cost and high performance is suitable for specific function design, such as frequency doubling design and the like, and provides basic guarantee. However, at present, the process of performing thermal polarization on glass by using continuous laser cannot meet the requirement of preparing visible-near infrared optical materials, the process is complex, the patterning resolution is not ideal, and the process controllability and the preparation efficiency need to be improved.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects of the prior art and provide the laser-assisted thermal polarization equipment and the laser-assisted thermal polarization method for the microscopic second-order nonlinear polarizability optical element.
In order to achieve the purpose, the invention adopts the following technical scheme:
a laser-assisted thermal polarization device of a microscopic second-order nonlinear polarizability optical element adopts silver conductive paint for Sm3+ ion-doped niobium Borophosphate (BPN) glass samples, taking a second piece of glass with the surface coated with silver wires as a cover glass arranged above the surface of one side of the sample of the niobium borophosphate glass, taking the second piece of glass as an anode and a silicon wafer as a cathode, arranging a silicon chip below the surface of the other side of the niobium borophosphate glass sample to form a sandwich type device formed by stacking and assembling a second piece of glass, the niobium borophosphate glass sample and the silicon chip, a power supply is connected with the second piece of glass and the silicon chip, a heating power supply is connected with the niobium borophosphate glass sample, arranging a laser above a second piece of glass serving as a cover glass, and enabling continuous laser with the emission wavelength of 1064nm to penetrate through the second piece of glass and reach the surface of the niobium borophosphate glass sample for scanning; and placing the sandwich type device in a sealed box, introducing non-oxidizing gas into the sealed box to form a gas atmosphere, applying voltage to a second piece of glass serving as an anode and a silicon wafer serving as a cathode, applying an electric field to a niobium borophosphate glass sample, applying a thermal field to the niobium borophosphate glass sample, scanning the niobium borophosphate glass sample by using a laser beam, performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample by using the electric field, the thermal field and a laser light field auxiliary method, and cooling the niobium borophosphate glass serving as the sample to prepare the micro second-order nonlinear polarizability optical element.
The second piece of glass is preferably ITO glass.
As a preferred technical scheme of the invention, the second piece of glass coated with silver wires on one side and side surfaces of the second piece of glass is used as an anode, the thickness of the silver wires is not more than 100 mu m, the width of the silver wires is not more than 5mm, the length and width of the plane of the ITO glass are not more than 30mm, and the thickness of the plane of the ITO glass is not more than 1.1 mm; the width or length dimension of the silicon wafer as the cathode is not more than 30mm, and the thickness of the silicon wafer is not more than 0.45 mm.
As a preferable technical scheme of the invention, Sm is doped as a sample3+The width or length dimension of the ionic niobium borophosphate glass is not more than 40mm, and the thickness is not more than 1.0 mm.
YAG continuous laser, emitting laser wavelength is not less than 1064nm, power is not more than 8W, intensity can be controlled to be 0.6-3.4W, laser focusing depth is not more than 20 mu m, scanning time is not more than 5min, and at least 20 times of objective lens is adopted for focusing.
As a preferred technical scheme of the invention, N is introduced into a sealed box2And Ar or a mixed gas of the two gases to form a gas atmosphere of the hot polarization treatment process.
The invention discloses a laser-assisted thermal polarization equipment adopting a microscopic second-order nonlinear polarizability optical element, which is a method for carrying out laser-assisted thermal polarization on the microscopic second-order nonlinear polarizability optical element, and comprises the following steps:
a. adopting silver conductive coating, taking glass coated with silver wires on the surface as a cover glass and an anode, connecting the silver wires with the anode, taking Sm3+ ion-doped niobium Borophosphate (BPN) glass as a sample, taking a silicon wafer as a cathode and connecting the silicon wafer with the cathode for fixing, connecting a heating power supply to the niobium borophosphate glass as the sample, sequentially stacking and assembling the glass as the anode, the niobium borophosphate glass as the sample and the silicon wafer as the cathode in a sandwich manner to form a process device for preparing an optical element by means of thermal polarization, arranging the process device for preparing the optical element by means of thermal polarization in an open box, then adding a cover to the box, and sealing the process device for preparing the optical element by means of thermal polarization;
b. respectively connecting a conduit of a sealed box assembled by the process device for preparing the optical element by thermal polarization in the step a and a vacuum pump with an external gas supply pipeline, firstly vacuumizing the box by the vacuum pump until the air pressure in the box is not higher than 5Pa, then closing the vacuum pump, filling gas of a non-oxidative thermal polarization treatment process into the box to be not lower than 1.3bar, and removing air, water vapor and dust in the box;
c. after the gas atmosphere in the process device for preparing the optical element by hot polarization is set in the step b, a heating device for heat conduction is utilized to heat at the temperature of not less than 10 ℃/m under the control of a programin temperature raising Rate, Sm doped sample was heated from room temperature3+Keeping the temperature of the ionic niobium borophosphate glass at 260-300 ℃, homogenizing the temperature of the niobium borophosphate glass serving as a sample, and enabling the niobium borophosphate glass to be in a uniform thermal field;
d. after the temperature of the niobium borophosphate glass serving as the sample is homogenized in the step c, under the condition that the temperature of the niobium borophosphate glass serving as the sample is kept at 260-300 ℃, applying direct-current voltage to glass serving as an anode and a silicon wafer serving as a cathode, applying an electric field to the niobium borophosphate glass sample, applying a thermal field to the niobium borophosphate glass sample, arranging a laser above the glass serving as the anode, scanning the niobium borophosphate glass sample by using laser beams to emit continuous laser with the wavelength of 1064nm, and performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample by using the electric field, the thermal field and a laser light field auxiliary method;
e. after the micro thermal polarization treatment process in the step d is finished, stopping heating of the heating device, cooling the niobium borophosphate glass serving as the sample to room temperature, keeping the direct-current voltage applied in the step d in the cooling process, and continuing applying an electric field to the niobium borophosphate glass serving as the sample;
f. and e, after the sample niobium borophosphate glass cooled in the step e reaches the room temperature, removing the direct-current voltage applied to the two sides of the sample niobium borophosphate glass, opening the cover of the box, and taking out the sample of the niobium borophosphate glass subjected to thermal polarization treatment, thereby obtaining the required micro second-order nonlinear polarizability optical element.
As a preferred technical scheme of the present invention, in the step d, in the process of performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample, any one parameter or a combination parameter of any several parameters of the laser parameter and the thermal polarization parameter is adopted to control the process of performing laser-assisted thermal polarization treatment on the niobium borophosphate glass serving as the sample on the micro second-order nonlinear polarizability optical element, so as to obtain different required laser-assisted thermal polarizability optical elements of the micro second-order nonlinear polarizability optical element; wherein the laser parameters mainly comprise scanning intensity, focusing depth and scanning time parameters; the thermal polarization parameters mainly comprise thermal polarization gas atmosphere, thermal polarization applied voltage, thermal polarization temperature and thermal polarization time parameters.
As a preferable technical solution of the present invention, in the step d of performing a micro thermal polarization treatment process on the niobium borophosphate glass as a sample, when a direct current voltage is applied to both sides of the niobium borophosphate glass as a sample, after the applied voltage is stabilized, the current starts to gradually decay to 0A; and synchronously recording the changes of the voltage and the current through computer software in the stabilizing process of the applied voltage and the attenuating process of the current all the time so as to be required by the hot polarization treatment process and regulate and control the parameter setting of the hot polarization treatment process.
As a preferred technical scheme of the invention, in the process of performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample in the step d, when a laser field is applied to the niobium borophosphate glass, the laser intensity is controlled to be 0.6-3.4W, the laser focusing depth is not more than 20 μm, and the laser scanning time is not more than 5 min; when an electric field is applied to the niobium borophosphate glass, a laser-assisted thermal polarization treatment process of a microscopic second-order nonlinear polarizability optical element is carried out by applying a direct-current voltage of 1.2-2.5 kV to the glass serving as an anode and a silicon wafer serving as a cathode and keeping the voltage for not less than 60 min; before an electric field is applied to the niobium borophosphate glass serving as a sample, heating the niobium borophosphate glass in advance, keeping the temperature of the niobium borophosphate glass uniform for 15min, and enabling the niobium borophosphate glass to be in the uniform thermal field.
As a preferred embodiment of the present invention, Sm is doped in the above sample3+The chemical formula of the ionic niobium borophosphate glass is 0.96[0.58(0.95 NaPO)3+0.05Na2B4O7)+0.42Nb2O5]+0.04Sm2O3。
Preferably, a confocal micro-raman spectrometer is used to test the performance of the microscopic second-order nonlinear polarizability.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the invention adopts laser-assisted thermal polarization in the method for preparing the high-precision second-order linear non-polarizability optical element, introduces a periodic structure on optical glass point by point or line or a complex structure, has second-order non-linear optical performance, and can write a required pattern on a sample by programming and repeated use;
2. the invention selects ITO glass as an anode, the ITO and the BPN sample surface are in good contact, the discharge is weak, and the prepared optical element has stable and strong chi(2)And weak anodic bonding;
3. the method provided by the invention can realize the optical element with periodic microscopic second-order nonlinear polarizability at one time, can improve the preparation efficiency by several times to tens of times compared with the traditional material, and has a good application prospect.
Drawings
Fig. 1 is a schematic structural diagram of a laser-assisted thermal polarization process apparatus of a microscopic second-order nonlinear polarizability optical element according to an embodiment of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
example one
In this embodiment, a laser-assisted thermal polarization apparatus for a micro-second order nonlinear polarizability optical element is configured such that, for a Sm3+ ion-doped niobium Borophosphate (BPN) glass sample, a silver conductive coating is used, ITO glass with a silver wire coated on a surface thereof is used as a cover glass disposed above a surface of one side of the niobium borophosphate glass sample, ITO glass is used as an anode, a silicon wafer is used as a cathode, and a silicon wafer is disposed below a surface of the other side of the niobium borophosphate glass sample, so as to form a sandwich type apparatus in which the ITO glass, the niobium borophosphate glass sample, and the silicon wafer are stacked and assembled, and a power supply is connected to the ITO glass and the silicon wafer, a heating power supply is connected to the niobium borophosphate glass sample, and a laser is disposed above the ITO glass used as the cover glass, so that continuous laser with an emission wavelength of 1064nm penetrates through the ITO glass and reaches the surface of the niobium borophosphate glass sample for; and placing the sandwich type device in a sealed box, introducing non-oxidizing gas Ar gas into the sealed box to form an inert gas atmosphere, applying voltage to ITO glass serving as an anode and a silicon wafer serving as a cathode, applying an electric field to a niobium borophosphate glass sample, applying a thermal field to the niobium borophosphate glass sample, scanning the niobium borophosphate glass sample by using a laser beam, performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample by using the electric field, the thermal field and a laser light field auxiliary method, cooling the niobium borophosphate glass serving as the sample, and preparing a microscopic second-order nonlinear polarizability optical element, wherein the reference is shown in figure 1. YAG, the laser has emission wavelength of 1064nm and power of 8W, and can be controlled to have intensity of 0.6-3.4W, laser focusing depth of 20 μm, scanning time of 5min, and 20 times of objective lens for focusing.
In this example, referring to fig. 1, a method for performing laser-assisted thermal polarization of a microscopic second-order nonlinear polarizability optical element using a laser-assisted thermal polarization apparatus of the microscopic second-order nonlinear polarizability optical element of this example, the materials used mainly include ITO glass coated with thin silver lines on one side and the side as an anode, silicon wafer as a cathode, and Sm doped ITO glass as a cathode3+The ionic BPN glass is subjected to micro thermal polarization, and the method comprises the following steps:
a. adopting silver conductive paint, using ITO glass with one side and side coated with thin silver wire as anode, the thickness of silver wire is 100 micrometers, width is 5mm, and the planar length and width of ITO glass are 10mm × 10mm, × 1.1.1 mm, connecting the silver wire with anode, and doping Sm to obtain the invented product3+The ionic niobium Borophosphate (BPN) glass is taken as a sample, the length, width and thickness dimensions of the niobium borophosphate glass are respectively 20mm, 20mm and 1.0mm, and the composition chemical formula of the Sm3+ ion-doped niobium borophosphate glass is 0.96[0.58(0.95 NaPO)3+0.05Na2B4O7)+0.42Nb2O5]+0.04Sm2O3The width or length of the silicon wafer as the cathode is 15mm, and the thickness of the silicon wafer is 0.45 mm; the silicon chip is taken as a cathode and is connected with a cathode for fixing, and a heating power supply is connected with the niobium borophosphate glass taken as a sample, so that the glass taken as the anode, the niobium borophosphate glass taken as the sample and the silicon chip taken as the cathode are sequentially laminatedAssembling a sandwich type process device for preparing the optical element by thermal polarization, arranging the process device for preparing the optical element by thermal polarization in an open stainless steel box, adding a stainless steel cover on the box, and sealing the process device for preparing the optical element by thermal polarization;
b. respectively connecting a guide pipe of a sealed stainless steel box assembled by the process device for preparing the optical element by thermal polarization in the step a and a vacuum pump with an external gas supply pipeline, firstly vacuumizing the box by the vacuum pump until the air pressure in the box is 5Pa, and the time is required to be 20min, then closing the vacuum pump, filling Ar gas into the box to be not less than 1.3bar, and taking the Ar gas as the gas of the non-oxidative thermal polarization treatment process to remove air, water vapor and dust in the box, and eliminating the influence of water vapor, dust and the like in the air on thermal polarization;
c. after the setting of the gas atmosphere in the process equipment for the thermal polarization preparation of the optical element is completed in the step b, the Sm doped sample is heated from room temperature at a heating rate of 10 ℃/min by using a heat conduction heating device under the control of a program3+Keeping the temperature of the ionic niobium borophosphate glass at 260 ℃, heating the niobium borophosphate glass and keeping the temperature for 15min to homogenize the temperature of the niobium borophosphate glass serving as a sample, and keeping the niobium borophosphate glass in a uniform thermal field;
d. after the temperature of the niobium borophosphate glass serving as the sample is homogenized in the step c, under the condition that the temperature of the niobium borophosphate glass serving as the sample is kept at 260 ℃, applying direct-current voltage to glass serving as an anode and a silicon wafer serving as a cathode, applying an electric field to the niobium borophosphate glass sample, applying a thermal field to the niobium borophosphate glass sample, arranging a laser above the glass serving as the anode, scanning the niobium borophosphate glass sample by using laser beams to emit continuous laser with the wavelength of 1064nm, and performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample by using the electric field, the thermal field and a laser light field auxiliary method;
in the process of carrying out micro thermal polarization treatment on niobium borophosphate glass serving as a sample, when a laser field is applied to the niobium borophosphate glass, the laser intensity is controlled to be 0.6-3.4W, the laser focusing depth is 20 microns, and the laser scanning time is 5 min; when an electric field is applied to the niobium borophosphate glass, a laser-assisted thermal polarization treatment process of a microscopic second-order nonlinear polarizability optical element is carried out by applying a direct-current voltage of 1.2-2.5 kV through glass serving as an anode and a silicon wafer serving as a cathode for 60 min; in the embodiment, before an electric field is applied to the niobium borophosphate glass serving as a sample, the niobium borophosphate glass is heated in advance and is kept at the temperature for 15min, so that the temperature of the niobium borophosphate glass is kept uniform, and the niobium borophosphate glass is in the uniform thermal field;
e. after the micro thermal polarization treatment process in the step d is finished, stopping heating of the heating device, cooling the niobium borophosphate glass serving as the sample to room temperature, keeping the direct-current voltage applied in the step d in the cooling process, and continuing applying an electric field to the niobium borophosphate glass serving as the sample;
f. and e, cutting off the Ar supply pipeline after the sample niobium borophosphate glass cooled in the step e reaches the room temperature, removing the direct current voltage applied to two sides of the sample niobium borophosphate glass, opening a stainless steel cover of a stainless steel box, and taking out the sample of the heat-polarized niobium borophosphate glass, thereby obtaining the required micro second-order nonlinear polarizability optical element.
And testing the performance of the microscopic second-order nonlinear polarizability by using a confocal microscopic Raman spectrometer, and verifying the microscopic second-order nonlinear polarizability pattern of the glass sample. The present embodiment implements an optical element having microscopic second-order nonlinear polarizability by means of a thermal field and a periodic electric field device. The optical element with high precision and high second-order nonlinear polarizability can be realized, and the precision can be improved by several times to tens of times compared with the preparation precision of the traditional material. The shape of the distribution and the size of the microstructure and the components of the atomic or molecular structure are controllable, and the preparation efficiency is high. The method of the embodiment can introduce periodic structures on the optical glass point by point or line or complex structures and has second-order nonlinear optical performance, and can write required patterns on a sample through programming repeated use.
In the method for preparing the second-order linear non-polarizability optical element with high precision in the embodiment, the optical element is prepared byWith laser-assisted thermal poling, periodic structures are introduced on the optical glass point-by-point or line-by-line or complex structures and have second-order nonlinear optical properties, and the desired pattern can be written on the sample by programmed reuse. Meanwhile, ITO glass is selected as an anode, and the ITO and the BPN sample surface are in good contact and weak in discharge. The prepared optical element has stable and strong chi(2)And weak anodic bonding.
Example two
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for laser-assisted thermal polarization of a microscopic second-order nonlinear polarizability optical element includes the steps of:
a. the step is the same as the first embodiment;
b. respectively connecting the conduit of the sealed stainless steel box assembled by the process device for preparing the optical element by thermal polarization in the step a and a vacuum pump with an external gas supply pipeline, firstly vacuumizing the box by the vacuum pump until the air pressure in the box is 5Pa, and the time is 20min, then closing the vacuum pump, and filling N into the box2The gas is not less than 1.3bar, and is used as the gas of the non-oxidative thermal polarization treatment process to remove air, water vapor and dust in the box and eliminate the influence of the water vapor, the dust and the like in the air on thermal polarization;
c. the step is the same as the first embodiment;
d. the step is the same as the first embodiment;
e. the step is the same as the first embodiment;
f. cutting off N when the sample niobium borophosphate glass cooled in the step e reaches room temperature2And the supply pipeline is used for removing the direct-current voltage applied to two sides of the niobium borophosphate glass serving as the sample, opening a stainless steel cover of the stainless steel box, and taking out the niobium perborate phosphate glass sample subjected to thermal polarization treatment, so that the required microscopic second-order nonlinear polarizability optical element is obtained.
The laser-assisted thermal polarization method of the high-precision microscopic second-order nonlinear polarizability optical element of the embodiment uses materialsComprises using ITO glass with one side and side coated with thin silver wire as anode, silicon wafer as cathode, continuous laser with wavelength of 1064nm to dope Sm3+Ionic niobium Borophosphate (BPN) glass was subjected to a micro-thermal polarization treatment. The electric field, the thermal field and the laser field auxiliary method can realize optical elements with various micron-sized microstructures. The method can realize the optical element with high-precision microscopic second-order nonlinear polarizability, and can improve the precision by several times to tens times compared with the preparation precision of the traditional material. The shape of the distribution and the size of the microstructure and the components of the atomic or molecular structure are controllable, and the preparation efficiency is high.
In this embodiment, a confocal micro-raman spectrometer is used to test the performance of the microscopic second-order nonlinear polarizability, and the microscopic second-order nonlinear polarizability pattern of the glass sample prepared in this embodiment is tested. This example method for preparing a second order linear non-polarizability optical element with high precision employs laser-assisted thermal polarization, introduces periodic structures on an optical glass point by point or line or complex structures and has second order non-linear optical properties, and can write a desired pattern on a sample by programmed reuse. Meanwhile, ITO glass is selected as an anode, and the ITO and the BPN sample surface are in good contact and weak in discharge. The prepared optical element has stable and strong chi(2)And weak anodic bonding.
EXAMPLE III
This embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for laser-assisted thermal polarization of a microscopic second-order nonlinear polarizability optical element includes the steps of:
a. the step is the same as the first embodiment;
b. the step is the same as the first embodiment;
c. after the setting of the gas atmosphere in the process equipment for the thermal polarization preparation of the optical element is completed in the step b, the Sm doped sample is heated from room temperature at a heating rate of 10 ℃/min by using a heat conduction heating device under the control of a program3+Keeping the temperature of the ionic niobium borophosphate glass to 300 ℃, heating the niobium borophosphate glass and keeping the temperature for 15min to obtain the productHomogenizing the temperature of the niobium borophosphate glass of the sample, and placing the niobium borophosphate glass in a uniform thermal field;
d. after the temperature of the niobium borophosphate glass serving as the sample is homogenized in the step c, under the condition that the temperature of the niobium borophosphate glass serving as the sample is kept at 300 ℃, applying direct-current voltage to glass serving as an anode and a silicon wafer serving as a cathode, applying an electric field to the niobium borophosphate glass sample, applying a thermal field to the niobium borophosphate glass sample, arranging a laser above the glass serving as the anode, scanning the niobium borophosphate glass sample by using laser beams to emit continuous laser with the wavelength of 1064nm, and performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample by using the electric field, the thermal field and a laser light field auxiliary method;
in the process of carrying out micro thermal polarization treatment on niobium borophosphate glass serving as a sample, when a laser field is applied to the niobium borophosphate glass, the laser intensity is controlled to be 0.6-3.4W, the laser focusing depth is 20 microns, and the laser scanning time is 5 min; when an electric field is applied to the niobium borophosphate glass, a laser-assisted thermal polarization treatment process of a microscopic second-order nonlinear polarizability optical element is carried out by applying a direct-current voltage of 1.2-2.5 kV through glass serving as an anode and a silicon wafer serving as a cathode for 60 min; in the embodiment, before an electric field is applied to the niobium borophosphate glass serving as a sample, the niobium borophosphate glass is heated in advance and is kept at the temperature for 15min, so that the temperature of the niobium borophosphate glass is kept uniform, and the niobium borophosphate glass is in the uniform thermal field;
e. the step is the same as the first embodiment;
f. the procedure is the same as in the first embodiment.
The laser-assisted thermal polarization method of the high-precision microscopic second-order nonlinear polarizability optical element uses materials which mainly comprise an anode made of ITO glass coated with thin silver wires on one side and the side, a cathode made of silicon wafers, continuous laser with the wavelength of 1064nm and Sm-doped materials3+Ionic niobium Borophosphate (BPN) glass was subjected to a micro-thermal polarization treatment. The electric field, the thermal field and the laser field auxiliary method can realize optical elements with various micron-sized microstructures. The method of the embodiment can realize high precisionCompared with the traditional material preparation precision, the microscopic second-order nonlinear polarizability optical element can improve the precision by several times to tens of times. The shape of the distribution and the size of the microstructure and the components of the atomic or molecular structure are controllable, and the preparation efficiency is high.
Example four
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, in the process of performing micro thermal polarization treatment on the niobium borophosphate glass serving as a sample, any one or a combination of a laser parameter and a thermal polarization parameter is used to control the process of performing laser-assisted thermal polarization treatment on the niobium borophosphate glass serving as the sample on the micro second-order nonlinear polarizability optical element, so as to obtain different required laser-assisted thermal polarizability optical elements of the micro second-order nonlinear polarizability optical element; wherein the laser parameters mainly comprise scanning intensity, focusing depth and scanning time parameters; the thermal polarization parameters mainly comprise thermal polarization gas atmosphere, thermal polarization applied voltage, thermal polarization temperature and thermal polarization time parameters. In the embodiment, the niobium borophosphate glass coated with the thin silver wire on the surface is used as a cover glass as an anode, the silicon wafer is used as a cathode, any one or combination of any parameters of laser parameters, hot polarization gas atmosphere, hot polarization applied voltage, hot polarization temperature and hot polarization time different from those of the previous embodiment is adopted to obtain a richer and diversified hot polarization treatment process, and the niobium borophosphate glass is subjected to micro hot polarization treatment, so that different series of optical elements with periodic micro second-order nonlinear polarizability can be prepared, and more special requirements of more visible-near infrared optical materials and elements are met. The periodic electric field and thermal field method realizes optical elements with various micron-sized microstructures and optical elements with periodic microscopic second-order nonlinear polarizability at one time. The present embodiment implements an optical element having microscopic second-order nonlinear polarizability by means of a thermal field and a periodic electric field device. The periodicity and the morphology of the sample are controlled by adjusting the periodicity and the morphology of the microscopic pattern of laser parameters, thermal polarization voltage, temperature and time. The embodiment can realize the optical element with large area and high second-order nonlinear polarizability at one time, and can improve the preparation efficiency by several times to tens of times compared with the traditional material. The embodiment can further provide key factors for thermal polarization according to the effect of the pattern: different laser parameters and atmosphere, voltage, temperature and time thermal polarization parameters are optimized.
EXAMPLE five
This embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, during the process of performing micro-thermal polarization treatment on the niobium borophosphate glass as a sample, when a direct current voltage is applied to both sides of the niobium borophosphate glass as a sample, after the applied voltage is stabilized, the current starts to gradually decay to 0A; and synchronously recording the changes of the voltage and the current through computer software in the stabilizing process of the applied voltage and the attenuating process of the current all the time so as to be required by the hot polarization treatment process and regulate and control the parameter setting of the hot polarization treatment process. The embodiment provides a data base for adjusting the thermal polarization treatment process by detecting the parameter changes of the voltage and the current in the thermal polarization treatment process, and has important value for perfecting and optimizing the thermal polarization treatment process and obtaining the optimal process condition for experiments or production.
The laser-assisted thermal polarization method of the high-precision microscopic second-order nonlinear polarizability optical element uses materials which mainly comprise an anode made of ITO glass coated with thin silver wires on one side and the side, a cathode made of silicon wafers, continuous laser with the wavelength of 1064nm and Sm-doped materials3+Ionic niobium Borophosphate (BPN) glass was subjected to a micro-thermal polarization treatment. The electric field, the thermal field and the laser field auxiliary method can realize optical elements with various micron-sized microstructures. The method can realize the optical element with high-precision microscopic second-order nonlinear polarizability, and can improve the precision by several times to tens times compared with the preparation precision of the traditional material. The shape of the distribution and the size of the microstructure and the components of the atomic or molecular structure are controllable, and the preparation efficiency is high.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes and modifications can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, so long as the purpose of the present invention is met, and the technical principle and inventive concept of the laser-assisted thermal polarization apparatus and method for the microscopic second-order nonlinear polarizability optical element of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A laser-assisted thermal polarization equipment of a microscopic second-order nonlinear polarizability optical element is characterized in that:
for doping Sm3+An ionic niobium Borophosphate (BPN) glass sample adopts silver conductive paint, a second piece of glass with a silver wire coated on the surface is used as a cover glass arranged above the surface of one side of the niobium borophosphate glass sample, the second piece of glass is used as an anode, a silicon wafer is used as a cathode, the silicon wafer is arranged below the surface of the other side of the niobium borophosphate glass sample, so that a sandwich type device formed by laminating and assembling the second piece of glass, the niobium borophosphate glass sample and the silicon wafer is formed, a power supply is connected to the second piece of glass and the silicon wafer, a heating power supply is connected to the niobium borophosphate glass sample, a laser is arranged above the second piece of glass used as the cover glass, and continuous laser with the emission wavelength of 1064nm penetrates through the second piece of glass and reaches the surface of the niobium borophosphate glass sample to be scanned; and placing the sandwich type device in a sealed box, introducing non-oxidizing gas into the sealed box to form a gas atmosphere, applying voltage to a second piece of glass serving as an anode and a silicon wafer serving as a cathode, applying an electric field to a niobium borophosphate glass sample, applying a thermal field to the niobium borophosphate glass sample, scanning the niobium borophosphate glass sample by using a laser beam, performing micro thermal polarization treatment on the niobium borophosphate glass serving as the sample by using the electric field, the thermal field and a laser light field auxiliary method, and cooling the niobium borophosphate glass serving as the sample to prepare the micro second-order nonlinear polarizability optical element.
2. The laser-assisted thermal polarization apparatus of microscopic second-order nonlinear polarizability optical elements of claim 1, wherein: the second piece of glass is made of ITO glass.
3. The laser-assisted thermal polarization apparatus of microscopic second-order nonlinear polarizability optical elements of claim 1, wherein: coating silver wires on one side and side surfaces of the second piece of glass to form an anode, wherein the thickness of the silver wires is not more than 100 mu m, the width of the silver wires is not more than 5mm, the length and width of the plane of the ITO glass are not more than 30mm, and the thickness of the plane of the ITO glass is not more than 1.1 mm; the width or length dimension of the silicon wafer as the cathode is not more than 30mm, and the thickness of the silicon wafer is not more than 0.45 mm.
4. The laser-assisted thermal polarization apparatus of microscopic second-order nonlinear polarizability optical elements of claim 1, wherein: doping Sm as a sample3+The width or length dimension of the ionic niobium borophosphate glass is not more than 40mm, and the thickness is not more than 1.0 mm.
5. The laser-assisted thermal polarization apparatus of microscopic second-order nonlinear polarizability optical elements of claim 1, wherein: YAG continuous laser, emitting laser wavelength is not less than 1064nm, power is not more than 8W, intensity can be controlled to be 0.6-3.4W, laser focusing depth is not more than 20 mu m, scanning time is not more than 5min, and at least 20 times of objective lens is adopted for focusing.
6. The laser-assisted thermal polarization apparatus of microscopic second-order nonlinear polarizability optical elements of claim 1, wherein: introducing N into a sealed box2And Ar or a mixed gas of the two gases to form a gas atmosphere of the hot polarization treatment process.
7. A method of performing laser-assisted thermal polarization of a microscopic second-order nonlinear polarizability optical element using the laser-assisted thermal polarization apparatus of the microscopic second-order nonlinear polarizability optical element of claim 1, wherein: the method comprises the following steps:
a. adopting silver conductive paint, using glass whose surface is coated with silver wire as cover glass and anode, connecting the silver wire with anode, and doping Sm3+Taking ionic niobium Borophosphate (BPN) glass as a sample, taking a silicon wafer as a cathode and connecting the silicon wafer with a cathode for fixing, connecting a heating power supply to the niobium borophosphate glass as the sample, sequentially stacking and assembling the glass as an anode, the niobium borophosphate glass as the sample and the silicon wafer as the cathode to form a sandwich type, forming a process device for preparing an optical element by thermal polarization, arranging the process device for preparing the optical element by thermal polarization in an open box, then adding a cover to the box, and sealing the process device for preparing the optical element by thermal polarization;
b. respectively connecting a conduit of a sealed box assembled by the process device for preparing the optical element by thermal polarization in the step a and a vacuum pump with an external gas supply pipeline, firstly vacuumizing the box by the vacuum pump until the air pressure in the box is not higher than 5Pa, then closing the vacuum pump, filling gas of a non-oxidative thermal polarization treatment process into the box to be not lower than 1.3bar, and removing air, water vapor and dust in the box;
c. after the setting of the gas atmosphere in the process device for preparing the optical element by hot polarization is finished in the step b, heating Sm doped sample from room temperature at a heating rate of not less than 10 ℃/min by utilizing a heat conduction heating device under the control of a program3+Keeping the temperature of the ionic niobium borophosphate glass at 260-300 ℃, homogenizing the temperature of the niobium borophosphate glass serving as a sample, and enabling the niobium borophosphate glass to be in a uniform thermal field;
d. after the temperature of the niobium borophosphate glass serving as the sample is homogenized in the step c, under the condition that the temperature of the niobium borophosphate glass serving as the sample is kept at 260-300 ℃, direct-current voltage is applied to glass serving as an anode and a silicon wafer serving as a cathode, an electric field is applied to the niobium borophosphate glass sample, a laser is further arranged above the glass serving as the anode, continuous laser with the wavelength of 1064nm emitted by the niobium borophosphate glass sample is scanned by utilizing laser beams, and the niobium borophosphate glass serving as the sample is subjected to micro thermal polarization treatment by utilizing an electric field, a thermal field and a laser light field auxiliary method;
e. after the micro thermal polarization treatment process in the step d is finished, stopping heating the heating device, cooling the niobium borophosphate glass serving as the sample to room temperature, keeping the direct-current voltage applied in the step d in the cooling process, and continuously applying an electric field to the niobium borophosphate glass serving as the sample;
f. and e, after the sample niobium borophosphate glass cooled in the step e reaches the room temperature, removing the direct-current voltage applied to the two sides of the sample niobium borophosphate glass, opening the cover of the box, and taking out the sample of the niobium borophosphate glass subjected to thermal polarization treatment, thereby obtaining the required micro second-order nonlinear polarizability optical element.
8. The method of laser-assisted thermal polarization of microscopic second-order nonlinear polarizability optical elements of claim 7 wherein: in the step d, in the process of carrying out micro thermal polarization treatment on the niobium borophosphate glass serving as the sample, any one parameter or combination parameters of any several parameters of the laser parameter and the thermal polarization parameter are adopted to control the laser-assisted thermal polarization treatment process of the optical element with the micro second-order nonlinear polarizability of the niobium borophosphate glass serving as the sample, so as to obtain different required optical elements with the micro second-order nonlinear polarizability; wherein the laser parameters mainly comprise scanning intensity, focusing depth and scanning time parameters; the thermal polarization parameters mainly comprise thermal polarization gas atmosphere, thermal polarization applied voltage, thermal polarization temperature and thermal polarization time parameters.
9. The method of laser-assisted thermal polarization of microscopic second-order nonlinear polarizability optical elements of claim 7 wherein: in the process of carrying out micro thermal polarization treatment on the niobium borophosphate glass serving as the sample in the step d, when direct current voltage is applied to two sides of the niobium borophosphate glass serving as the sample, after the applied voltage is stable, the current starts to gradually attenuate to 0A; and synchronously recording the changes of the voltage and the current through computer software in the stabilizing process of the applied voltage and the attenuating process of the current all the time so as to be required by the hot polarization treatment process and regulate and control the parameter setting of the hot polarization treatment process.
10. The method of laser-assisted thermal polarization of microscopic second-order nonlinear polarizability optical elements of claim 7 wherein: in the process of carrying out micro thermal polarization treatment on the niobium borophosphate glass serving as the sample in the step d, when a laser field is applied to the niobium borophosphate glass, the laser intensity is controlled to be 0.6-3.4W, the laser focusing depth is not more than 20 mu m, and the laser scanning time is not more than 5 min; when an electric field is applied to the niobium borophosphate glass, a laser-assisted thermal polarization treatment process of a microscopic second-order nonlinear polarizability optical element is carried out by applying a direct-current voltage of 1.2-2.5 kV to the glass serving as an anode and a silicon wafer serving as a cathode and keeping the voltage for not less than 60 min; before an electric field is applied to the niobium borophosphate glass serving as a sample, heating the niobium borophosphate glass in advance, keeping the temperature of the niobium borophosphate glass uniform for 15min, and enabling the niobium borophosphate glass to be in the uniform thermal field.
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