CN109270613A - The preparation method of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode - Google Patents
The preparation method of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode Download PDFInfo
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- CN109270613A CN109270613A CN201811029956.9A CN201811029956A CN109270613A CN 109270613 A CN109270613 A CN 109270613A CN 201811029956 A CN201811029956 A CN 201811029956A CN 109270613 A CN109270613 A CN 109270613A
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1847—Manufacturing methods
Abstract
The invention discloses a kind of preparation methods that visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode, material therefor mainly includes that silicon wafer is coated with using surface as coverslip, use material for Cu, Ni, the grid of Ag or Au metal makees anode, make cathode with silicon wafer, micro- thermal poling processing is carried out to chalcogenide glass, using periodical electric field and thermal field method, the printing of the microstructural diffraction grating of a variety of micron orders can be achieved, it can be by adjusting the atmosphere in metal grill size and thermal poling parameter, voltage, temperature and time, to reach the periodicity and pattern of control sample, several times to tens times can be improved with respect to traditional material preparation efficiency in the method for the present invention, disposably required pattern can be printed on optical material sample, realize pattern resolution up to micron even nano-scale, cavity disperse characteristic Controllable with the pattern and atom of size or the composition of molecular structure, preparation efficiency is high.
Description
Technical field
The present invention relates to a kind of preparation methods of optical element, more particularly to a kind of optical element with micro-structure
Preparation method is mainly used in visible-infrared optical system material and device arts.
Background technique
Diffraction optical element (DOE) is the important component of optical field.Since these elements enbrittle mostly, institute
It is easy to damage with them, it is therefore desirable to a kind of stable and less costly electric manufacturing technology.
Thermal poling is widely studied since it can generate second order nonlinear effect in various types of glass.In order to
It realizes the optical functional glass controllable preparation based on micro-structure, needs to be modified glass.Pervious modification focuses primarily upon all
The common micro Process means of such as dry etching and photoetching, disadvantage is that equipment is expensive, complex process, processing efficiency are low
Deng especially photoetching is also influenced by light.2008, it is aobvious that Takagi et al. proposes a kind of simple and feasible solution-
Low-grade fever polarization: using having the anode of periodically micro- lattice to carry out thermal poling to glass, with glass surface formed with
The consistent polarization layer of anode microstructure pattern.In addition, thermal poling is also used for compound glass field, thermal poling quilt again in this field
Referred to as electric field-assisted dissolution (EFAD).2015, Fleming etc. was proved on the compound soda-lime-silica glass of Ag doped with nano using heat
Polarization technique can successfully generate nanostructure.It selectively dissolves silver nano-grain using patterned anode, generates
Periodic patterns are determined there is visible diffraction grating by the shape of anode pattern.But the current light function based on micro-structure
Energy glass preparation efficiency is ideal not enough, and the range of light wavelengths of transmission are also relatively narrow, are not able to satisfy a variety of micron order microstructures
Optical element application needs.
Summary of the invention
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind
The preparation method of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode, it can be disposably by required pattern
Be printed on optical material sample, realize pattern resolution up to micron even nano-scale, cavity disperse characteristic and size
The composition of pattern and atom or molecular structure is controllable, and preparation efficiency is high.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method preparing visible-echelette diffraction grating using the micro- thermal poling technique of grid electrode, with sulphur system
Glass is as sample to be processed, using different silicon wafers as coverslip and cathode, makees anode with metal grill, will be as sun
The metal grill of pole and silicon wafer as cathode are respectively arranged at the chalcogenide glass two sides as sample to be processed, by metal grill
It is set to the silicon wafer as coverslip and between the chalcogenide glass as sample to be processed as anode, forms thermal poling and prepare light
The device of element is learned, and the device that the thermal poling prepares optical element is set in the box of sealing, metal grill uses
With periodically micro- lattice form, the chalcogenide glass as sample to be processed is heated, and is prepared by thermal poling
The metal grill for making anode of the device of optical element and the silicon wafer for making cathode carry out applied voltage, to as sample to be processed
Chalcogenide glass carries out micro- thermal poling processing, to be formed and the metal grill micro-structure figure as anode on chalcogenide glass surface
The consistent polarization layer of case, then will be carried out as the chalcogenide glass of sample to be processed it is cooling after, obtain required having periodically
The chalcogenide glass defraction grating device of grid pattern.
As preferred technical solution of the invention, applied using metal grill size, hot polarized gas atmosphere, thermal poling
The combination parameter of voltage, thermal poling temperature and any one parameter in the thermal poling time or any several parameters, to as to
The treatment process process that the chalcogenide glass of processing sample carries out micro- thermal poling is controlled, to regulate and control as sample to be processed
The periodicity and surface topography of chalcogenide glass surface texture obtain the different required sulphur system glass with periodical grid pattern
Glass defraction grating device.
As preferred technical solution of the invention, the material component and its chemistry of the chalcogenide glass as sample to be processed
Formula are as follows:
(100-x-y)GeS(Se)2·xGa2S(Se)3·yMX；
Wherein, the M in chemical formula be Li, Na, K or Ag, X Cl, Br or I, 0 < x < 40,40≤100-x-y < 100,
The maximum planes of chalcogenide glass as sample to be processed are having a size of 0.8~5cm, with a thickness of 0.5~1.5mm.It is further excellent
0 < x <, 40, the 0 < y < 40 being elected to be in the chemical formula of the material of the chalcogenide glass for sample to be processed.
It is preferred that the material of the above-mentioned metal grill for making anode uses Cu, Ni, Ag or Au.
It is preferred that the square net mesh number of the above-mentioned metal grill for making anode-grid inner width-metal line width correspondingly-sized is
300-58 μm-25 μm of mesh ,-37 μm-25 μm of 400 mesh ,-30 μm-10 μm of 600 mesh, 1000-19 μm-6 μm of mesh ,-11.5 μ of 1500 mesh
M-5 μm or -7.5 μm -5 μm of 2000 mesh.
As preferred technical solution of the invention, the silicon wafer as coverslip and the silicon wafer as cathode are same material
Matter, the width or length dimension of the two are not more than 50mm, and thickness is not more than 0.45mm, and the silicon area as coverslip is less than
The area of silicon wafer as cathode.
As preferred technical solution of the invention, visible-infrared spread out is prepared using the micro- thermal poling technique of grid electrode
The preparation method for penetrating grating, includes the following steps:
A. silicon wafer is made into coverslip, and connects positive pole, at the same make silicon wafer be covered in as anode metal grill it
It above and with positive pole holding is electrically connected, using chalcogenide glass as sample to be processed, other silicon wafer is made into cathode and connects electricity
Source cathode is fixed, and connects heating power supply for the chalcogenide glass as sample to be processed, makes coverslip, metal grill, sulphur
It is glass sample, as the silicon wafer of cathode stacks gradually assembling and form the process unit that thermal poling prepares optical element, and will be hot
Polarizer is set in open box for the process unit of optical element, then adds lid for box, is prepared to thermal poling
The process unit of optical element is sealed；
B. after the sealed box process unit that completion thermal poling prepares optical element in the step a assembled,
Under process control, using the heating device of heat transfer, to be not higher than the heating rate of 10 DEG C/min, from room temperature heating as to from
The chalcogenide glass of reason sample to 100~300 DEG C and is kept the temperature at least 15min, makes the chalcogenide glass as sample to be processed
Equalizing temperature；
C. after completing the equalizing temperature as the chalcogenide glass of sample to be processed in the step b, as wait locate
In the case where 100~300 DEG C of temperature of chalcogenide glass holding for managing sample, anode is made by metal grill and silicon wafer makees cathode, to
The two sides of chalcogenide glass as sample to be processed apply 200~2500V of DC voltage and simultaneously continue 15~120min, to as to
The chalcogenide glass for handling sample carries out micro- thermal poling processing；It is preferred that applying to the two sides of the chalcogenide glass as sample to be processed
250~750V of DC voltage simultaneously continues 30~120min, carries out at micro- thermal poling to the chalcogenide glass as sample to be processed
Reason；As preferred technical solution of the invention, micro- thermal poling processing is being carried out to the chalcogenide glass as sample to be processed
In technical process, when applying DC voltage to the two sides of the chalcogenide glass as sample to be processed, after applied voltage is stablized, electricity
Stream starts gradually decaying until 0A；It is same by computer software always in applied voltage stabilization process and current decay process
The variation of recording voltage and electric current is walked, in case adjusting needed for thermal poling treatment process to thermal poling treatment process parameter setting
Control；
D. after carrying out micro- thermal poling treatment process in the step c, then heating-stopping apparatus heating will be made
Chalcogenide glass for sample to be processed is cooled to room temperature, and in cooling procedure holding simultaneously and applied in the step c
Identical DC voltage continues to apply DC voltage to the two sides of the chalcogenide glass as sample to be processed；
E. it after the step d carries out the cooling chalcogenide glass arrival room temperature as sample to be processed, removes to work
For the DC voltage that the two sides of the chalcogenide glass of sample to be processed apply, the lid of box is opened, what taking-up was handled through thermal poling
Chalcogenide glass, to obtain the required chalcogenide glass defraction grating device with periodical grid pattern.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. the method for the present invention uses metal grid electrode, the micro- pattern resolution of the electrode is up to micron even nanoscale
Not, it is optional in larger range to be conducive to required sample microstructure appearance, and may be reused and required pattern is imprinted on sample；
2. the method for the present invention selects chalcogenide glass substitution simple glass as sample, obtained clearly on chalcogenide glass surface
Lattice, penetrate range of light wavelengths widened visible-infra-red range from visible-range；
3. the method for the present invention once realizes the printing of diffraction grating, several times are can be improved to number in opposite traditional material preparation efficiency
It ten times, has a good application prospect.
Detailed description of the invention
Fig. 1 is that one method of the embodiment of the present invention uses the micro- thermal poling technique of grid electrode to prepare visible-infrared ray diffraction light
The process unit structural schematic diagram of grid.
Fig. 2 is the embodiment of the present invention one at 250V, prepares visible-infrared spread out using the micro- thermal poling technique of grid electrode
Penetrate the optical microscope photograph of grating.
Fig. 3 is the embodiment of the present invention two at 750V, prepares visible-infrared spread out using the micro- thermal poling technique of grid electrode
Penetrate the optical microscope photograph of grating.
Specific embodiment
Above scheme is described further below in conjunction with specific implementation example, the preferred embodiment of the present invention is described in detail such as
Under:
Embodiment one
In the present embodiment, referring to Fig. 1 and Fig. 2, a kind of use micro- thermal poling technique of grid electrode is prepared visible-infrared
The preparation method of diffraction grating, includes the following steps:
A. Cu grid electrode is used, square net mesh number-grid inner width-metal line width of the Cu metal grill of anode is made
Correspondingly-sized is -11.5 μm -5 μm of 1500 mesh, and uses diameter for 10mm, with a thickness of the 60GeS of 0.9mm2·20Ga2S3·
20KCl chalcogenide glass is as optical material sample, and as sample to be processed, using another having a size of 6mm × 6mm × 0.45mm
Outer silicon wafer is cathode, referring to Fig. 1.Silicon wafer is made into coverslip, and connects positive pole, while be covered in silicon wafer as anode
Cu metal grill on and with positive pole holding be electrically connected, using chalcogenide glass as sample to be processed, by other silicon wafer
Make cathode and connect power cathode to be fixed, and connect heating power supply for the chalcogenide glass as sample to be processed, makes lid glass
Piece, chalcogenide glass sample, as the silicon wafer of cathode stacks gradually assembling and forms thermal poling and prepare optical element Cu metal grill
Process unit, and the process unit that thermal poling prepares optical element is set in open box, it is then box plus lid
Son, the process unit for preparing optical element to thermal poling are sealed；
B. after the sealed box process unit that completion thermal poling prepares optical element in the step a assembled,
Under process control, is heated from room temperature with the heating rate of 5 DEG C/min using the heating device of heat transfer and be used as sample to be processed
Chalcogenide glass to 200 DEG C and kept the temperature, keep the temperature 15min in advance before subsequent step added electric field, it is ensured that glass sample
Temperature uniformity makes the equalizing temperature of the chalcogenide glass as sample to be processed；
C. after completing the equalizing temperature as the chalcogenide glass of sample to be processed in the step b, as wait locate
In the case where 200 DEG C of temperature of chalcogenide glass holding for managing sample, anode is made by Cu metal grill and silicon wafer makees cathode, to conduct
The two sides of the chalcogenide glass of sample to be processed apply DC voltage 250V and continue 30min, to the sulphur system as sample to be processed
Glass carries out micro- thermal poling processing；
D. after carrying out micro- thermal poling treatment process in the step c, then heating-stopping apparatus heating will be made
Chalcogenide glass for sample to be processed is cooled to room temperature, and in cooling procedure holding simultaneously and applied in the step c
Identical DC voltage continues to apply DC voltage to the two sides of the chalcogenide glass as sample to be processed；
E. it after the step d carries out the cooling chalcogenide glass arrival room temperature as sample to be processed, removes to work
For the DC voltage that the two sides of the chalcogenide glass of sample to be processed apply, the lid of box is opened, what taking-up was handled through thermal poling
Chalcogenide glass, to obtain the required chalcogenide glass defraction grating device with periodical grid pattern.Using optical microphotograph
Mirror shoots chalcogenide glass defraction grating device sample polarization region surface pattern manufactured in the present embodiment, obtains the optics such as Fig. 2
Microscope photo.
In the present embodiment, Fig. 1 is participated in, visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode
Preparation method, using chalcogenide glass as sample to be processed, using various sizes of silicon wafer as coverslip and cathode, with Cu
Metal grill makees anode, will be respectively arranged at as the Cu metal grill of anode and the silicon wafer as cathode as sample to be processed
Chalcogenide glass two sides, by Cu metal grill be set to the silicon wafer as coverslip and the chalcogenide glass as sample to be processed it
Between be used as anode, form thermal poling and prepare the device of optical element, and the device that the thermal poling prepares optical element is arranged
In the box of sealing, Cu metal grill, which uses, has periodically micro- lattice form, to the sulphur as sample to be processed
Be that glass is heated, and prepared by the metal grill for making anode of the device of optical element to thermal poling and make the silicon wafer of cathode into
Row applied voltage carries out micro- thermal poling processing to the chalcogenide glass as sample to be processed, thus in chalcogenide glass surface shape
At with the consistent polarization layer of Cu metal grill micro structured pattern as anode, then by the chalcogenide glass as sample to be processed
After carrying out cooling, the required chalcogenide glass defraction grating device with periodical grid pattern is obtained, referring to fig. 2.
The present embodiment method uses Cu grid electrode, and the micro- pattern resolution of the electrode is up to micron even nanoscale
Not, it is optional in larger range to be conducive to required sample microstructure appearance, and may be reused and required pattern is imprinted on sample；
The present embodiment selects chalcogenide glass substitution simple glass as sample, has obtained clearly lattice on chalcogenide glass surface,
Its range of light wavelengths penetrated has widened visible-infra-red range from visible-range.The present embodiment can be disposably by needed for
Pattern is printed on optical material sample, realizes pattern resolution up to micron even nano-scale, cavity disperse characteristic and ruler
The composition of very little pattern and atom or molecular structure is controllable, and preparation efficiency is high, and the present embodiment method is prepared with respect to traditional material and imitated
Several times to tens times can be improved in rate, has a good application prospect.
Embodiment two
The present embodiment is basically the same as the first embodiment, and is particular in that:
In the present embodiment, a kind of that visible-infrared ray diffraction is prepared using the micro- thermal poling technique of grid electrode referring to Fig. 3
The preparation method of grating, includes the following steps:
A. Ni grid electrode is used, square net mesh number-grid inner width-metal line width of the Ni metal grill of anode is made
Correspondingly-sized is -11.5 μm -5 μm of 1500 mesh, and uses diameter for 10mm, with a thickness of the 60GeS of 0.9mm2·20Ga2S3·
20KCl chalcogenide glass is as optical material sample, and as sample to be processed, using another having a size of 6mm × 6mm × 0.45mm
Outer silicon wafer is cathode.Silicon wafer is made into coverslip, and connects positive pole, while silicon wafer being made to be covered in the Ni metal as anode
It is electrically connected on grid and with positive pole holding, using chalcogenide glass as sample to be processed, other silicon wafer is made into cathode simultaneously
Connection power cathode is fixed, and connects heating power supply for the chalcogenide glass as sample to be processed, makes coverslip, Ni metal
Grid, chalcogenide glass sample stack gradually assembling and form the process unit that thermal poling prepares optical element as the silicon wafer of cathode,
And be set to the process unit that thermal poling prepares optical element in open box, lid then is added for box, to thermoae
The process unit that change prepares optical element is sealed；
B. this step is the same as example 1；
C. after completing the equalizing temperature as the chalcogenide glass of sample to be processed in the step b, as wait locate
In the case where 200 DEG C of temperature of chalcogenide glass holding for managing sample, anode is made by Ni metal grill and silicon wafer makees cathode, to conduct
The two sides of the chalcogenide glass of sample to be processed apply DC voltage 750V and continue 30min, to the sulphur system as sample to be processed
Glass carries out micro- thermal poling processing；
D. this step is the same as example 1；
E. this step is the same as example 1.
Chalcogenide glass defraction grating device sample polarization region surface manufactured in the present embodiment is shot using optical microscopy
Pattern obtains the optical microscope photograph such as Fig. 3.
The present embodiment method uses Ni grid electrode, and the micro- pattern resolution of the electrode is up to micron even nanoscale
Not, it is optional in larger range to be conducive to required sample microstructure appearance, and may be reused and required pattern is imprinted on sample；
The present embodiment selects chalcogenide glass substitution simple glass as sample, has obtained clearly lattice on chalcogenide glass surface,
Its range of light wavelengths penetrated has widened visible-infra-red range from visible-range.The present embodiment is using silicon wafer as lid glass
Piece, Ni grid make anode, and silicon wafer makees cathode, and the preparation method of micro- thermal poling is carried out to chalcogenide glass.The periodicity electric field and
Thermal field method realizes the microstructural optical element of a variety of micron orders, once realizes defraction grating device, opposite traditional material
Several times to tens times can be improved in preparation efficiency, has a good application prospect.
Embodiment three
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of system preparing visible-echelette diffraction grating using the micro- thermal poling technique of grid electrode
Preparation Method includes the following steps:
A. Ag grid electrode is used, square net mesh number-grid inner width-metal line width of the Ag metal grill of anode is made
Correspondingly-sized is -37 μm -25 μm of 400 mesh, and uses diameter for 50mm, with a thickness of the 40GeS of 1.5mm2·30Ga2S3·30KCl
Chalcogenide glass is as optical material sample, and as sample to be processed, using having a size of 40mm × 40mm × 0.45mm in addition
Silicon wafer be cathode.Silicon wafer is made into coverslip, and connects positive pole, while silicon wafer being made to be covered in the Ag metal mesh as anode
It is electrically connected on lattice and with positive pole holding, using chalcogenide glass as sample to be processed, other silicon wafer is made into cathode and company
It connects power cathode to be fixed, and connects heating power supply for the chalcogenide glass as sample to be processed, make coverslip, Ag metal mesh
Lattice, chalcogenide glass sample stack gradually assembling and form the process unit that thermal poling prepares optical element as the silicon wafer of cathode, and
The process unit that thermal poling prepares optical element is set in open box, then lid is added for box, to thermal poling
The process unit for preparing optical element is sealed；
B. after the sealed box process unit that completion thermal poling prepares optical element in the step a assembled,
Under process control, is heated from room temperature with the heating rate of 10 DEG C/min using the heating device of heat transfer and be used as sample to be processed
Chalcogenide glass to 300 DEG C and kept the temperature, keep the temperature 15min in advance before subsequent step added electric field, it is ensured that glass sample
Temperature uniformity makes the equalizing temperature of the chalcogenide glass as sample to be processed；
C. after completing the equalizing temperature as the chalcogenide glass of sample to be processed in the step b, as wait locate
In the case where 300 DEG C of temperature of chalcogenide glass holding for managing sample, anode is made by Ag metal grill and silicon wafer makees cathode, to conduct
The two sides of the chalcogenide glass of sample to be processed apply DC voltage 2500V and continue 120min, to the sulphur as sample to be processed
It is that glass carries out micro- thermal poling processing；
D. after carrying out micro- thermal poling treatment process in the step c, then heating-stopping apparatus heating will be made
Chalcogenide glass for sample to be processed is cooled to room temperature, and in cooling procedure holding simultaneously and applied in the step c
Identical DC voltage continues to apply DC voltage to the two sides of the chalcogenide glass as sample to be processed；
E. it after the step d carries out the cooling chalcogenide glass arrival room temperature as sample to be processed, removes to work
For the DC voltage that the two sides of the chalcogenide glass of sample to be processed apply, the lid of box is opened, what taking-up was handled through thermal poling
Chalcogenide glass, to obtain the required chalcogenide glass defraction grating device with periodical grid pattern.
The present embodiment method uses Ag grid electrode, and the micro- pattern resolution of the electrode is up to micron even nanoscale
Not, it is optional in larger range to be conducive to required sample microstructure appearance, and may be reused and required pattern is imprinted on sample；
The present embodiment selects chalcogenide glass substitution simple glass as sample, has obtained clearly lattice on chalcogenide glass surface,
Its range of light wavelengths penetrated has widened visible-infra-red range from visible-range.The present embodiment is using silicon wafer as lid glass
Piece, Ag grid make anode, and silicon wafer makees cathode, and the preparation method of micro- thermal poling is carried out to chalcogenide glass.The periodicity electric field and
Thermal field method realizes the microstructural optical element of a variety of micron orders, once realizes defraction grating device, opposite traditional material
Decades of times can be improved in preparation efficiency, has a good application prospect.
Example IV
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of system preparing visible-echelette diffraction grating using the micro- thermal poling technique of grid electrode
Preparation Method applies voltage, thermal poling temperature and thermal poling time using metal grill size, hot polarized gas atmosphere, thermal poling
In any one parameter or any several parameters combination parameter, micro- heat is carried out to the chalcogenide glass as sample to be processed
Polarized treatment process process is controlled, to regulate and control the periodicity and table of the chalcogenide glass surface texture as sample to be processed
Face pattern obtains the different required chalcogenide glass defraction grating devices with periodical grid pattern.The present embodiment uses
Periodical electric field and thermal field method, it can be achieved that the microstructural diffraction grating of a variety of micron orders printing.The present embodiment passes through tune
Whole metal grill size and atmosphere, voltage, temperature and time in thermal poling parameter etc., come reach control sample periodicity with
Pattern.Several times to tens times can be improved with respect to traditional material preparation efficiency in the present embodiment method, and the mesh that can be prepared as needed
Visible-echelette diffraction grating is marked, determines preparation process, there is flexibility and very strong adaptability.
Embodiment five
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of system preparing visible-echelette diffraction grating using the micro- thermal poling technique of grid electrode
Preparation Method, during carrying out micro- thermal poling treatment process to the chalcogenide glass as sample to be processed, to as to be processed
When the two sides of the chalcogenide glass of sample apply DC voltage, after applied voltage is stablized, electric current starts gradually to decay until 0A；?
In applied voltage stabilization process and current decay process, pass through the variation of computer software synchronous recording voltage and current always,
In case regulating and controlling needed for thermal poling treatment process to thermal poling treatment process parameter setting.The present embodiment passes through in thermal poling
To the detection of the Parameters variation of voltage and current during treatment process, data are provided to adjust the adjustment of thermal poling treatment process
Basis obtains optimal process conditions with important value, in case experiment or raw to improving and optimizing thermal poling treatment process
Needed for production.
The above embodiment of the present invention prepares the preparation of visible-echelette diffraction grating using the micro- thermal poling technique of grid electrode
Method can prepare the optical element with high-precision micro- second nonlinear pattern, can be real using electric field, thermal field householder method
Existing a variety of micron orders and the microstructural optical element of nanoscale.The present embodiment method may be implemented have high-precision micro- two
Several times to tens times can be improved in the optical element of rank non-linear susceptibility, opposite traditional material preparation precision.Cavity disperse characteristic with
The pattern and atom of size or the composition of molecular structure are controllable, and preparation efficiency is high.
Combination attached drawing of the embodiment of the present invention is illustrated above, but the present invention is not limited to the above embodiments, it can be with
The purpose of innovation and creation according to the present invention makes a variety of variations, under the Spirit Essence and principle of all technical solutions according to the present invention
Change, modification, substitution, combination or the simplification made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
The skill of the preparation method of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode without departing from the present invention
Art principle and inventive concept, belong to protection scope of the present invention.
Claims (10)
1. a kind of preparation method for being prepared visible-echelette diffraction grating using the micro- thermal poling technique of grid electrode, feature are existed
In:
Using chalcogenide glass as sample to be processed, using different silicon wafers as coverslip and cathode, sun is made with metal grill
Metal grill as anode and the silicon wafer as cathode are respectively arranged at the chalcogenide glass two as sample to be processed by pole
Metal grill is set to the silicon wafer as coverslip and between the chalcogenide glass as sample to be processed as anode, shape by side
The device of optical element is prepared at thermal poling, and the device that the thermal poling prepares optical element is set to the box of sealing
In, metal grill, which uses, has periodically micro- lattice form, the chalcogenide glass as sample to be processed is heated,
And the silicon wafer for preparing the metal grill for making anode of the device of optical element to thermal poling and making cathode carries out applied voltage, to work
Micro- thermal poling processing is carried out for the chalcogenide glass of sample to be processed, to be formed and the gold as anode on chalcogenide glass surface
Belong to the consistent polarization layer of grid micro structured pattern, after then carrying out cooling as the chalcogenide glass of sample to be processed, obtains institute
What is needed has the chalcogenide glass defraction grating device of periodical grid pattern.
2. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 1
Method, it is characterised in that: voltage, thermal poling temperature and heat are applied using metal grill size, hot polarized gas atmosphere, thermal poling
The combination parameter of any one parameter in the polarization time or any several parameters, to the chalcogenide glass as sample to be processed into
The treatment process process of the micro- thermal poling of row is controlled, to regulate and control the week of the chalcogenide glass surface texture as sample to be processed
Phase property and surface topography obtain the different required chalcogenide glass defraction grating devices with periodical grid pattern.
3. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 1
Method, it is characterised in that: the material component and its chemical formula of the chalcogenide glass as sample to be processed are as follows:
(100-x-y)GeS(Se)2·xGa2S(Se)3·yMX；
Wherein, the M in chemical formula be Li, Na, K or Ag, X Cl, Br or I, 0 < x < 40,40≤100-x-y < 100, as
The maximum planes of the chalcogenide glass of sample to be processed are having a size of 0.8~5cm, with a thickness of 0.5~1.5mm.
4. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 3
Method, it is characterised in that: 0 < x <, 40, the 0 < y < 40 in the chemical formula of the material of the chalcogenide glass as sample to be processed.
5. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 1
Method, it is characterised in that: the material of the metal grill for making anode is Cu, Ni, Ag or Au.
6. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 1
Method, it is characterised in that: the square net mesh number of the metal grill for making anode-grid inner width-metal line width correspondence ruler
Very little is-58 μm-25 μm of 300 mesh ,-37 μm-25 μm of 400 mesh ,-30 μm-10 μm of 600 mesh, 1000-19 μm-6 μm of mesh, 1500 mesh-
11.5 μm -5 μm or -7.5 μm -5 μm of 2000 mesh.
7. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 1
Method, it is characterised in that: silicon wafer as coverslip is identical material, the width or length ruler of the two with the silicon wafer as cathode
Very little to be not more than 50mm, thickness is not more than 0.45mm, and is less than the area of the silicon wafer as cathode as the silicon area of coverslip.
8. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 1
Method, which comprises the steps of:
A. silicon wafer is made into coverslip, and connects positive pole, while be covered in silicon wafer on the metal grill as anode simultaneously
It is electrically connected with positive pole holding, using chalcogenide glass as sample to be processed, other silicon wafer is made cathode and connects power supply bear
Pole is fixed, and connects heating power supply for the chalcogenide glass as sample to be processed, makes coverslip, metal grill, sulphur system glass
Glass sample stacks gradually assembling and forms the process unit that thermal poling prepares optical element as the silicon wafer of cathode, and by thermal poling
The process unit for preparing optical element is set in open box, is then added lid for box, is prepared optics to thermal poling
The process unit of element is sealed；
B. after the sealed box process unit that completion thermal poling prepares optical element in the step a assembled, in program
Under control, using the heating device of heat transfer, to be not higher than the heating rate of 10 DEG C/min, is heated from room temperature and be used as sample to be processed
The chalcogenide glass of product is to 100~300 DEG C and is kept the temperature at least 15min, makes the temperature of the chalcogenide glass as sample to be processed
Homogenization；
C. after completing the equalizing temperature as the chalcogenide glass of sample to be processed in the step b, as sample to be processed
In the case that the chalcogenide glass of product is kept for 100~300 DEG C of temperature, anode is made by metal grill and silicon wafer makees cathode, to conduct
The two sides of the chalcogenide glass of sample to be processed apply 200~2500V of DC voltage and continue 15~120min, to as to be processed
The chalcogenide glass of sample carries out micro- thermal poling processing；
D. after carrying out micro- thermal poling treatment process in the step c, heating-stopping apparatus heating, then will as to
The chalcogenide glass of processing sample is cooled to room temperature, and keeps identical as applied in the step c simultaneously in cooling procedure
DC voltage, continue to the two sides of the chalcogenide glass as sample to be processed apply DC voltage；
E. after the step d carries out the cooling chalcogenide glass as sample to be processed and reaches room temperature, remove to as to
The DC voltage that the two sides of the chalcogenide glass of sample apply is handled, the lid of box is opened, takes out the sulphur system handled through thermal poling
Glass, to obtain the required chalcogenide glass defraction grating device with periodical grid pattern.
9. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 8
Method, it is characterised in that: in the step c, apply DC voltage 250 to the two sides of the chalcogenide glass as sample to be processed
~750V simultaneously continues 30~120min, carries out micro- thermal poling processing to the chalcogenide glass as sample to be processed.
10. the preparation of visible-echelette diffraction grating is prepared using the micro- thermal poling technique of grid electrode according to claim 8
Method, it is characterised in that: micro- thermal poling treatment process is carried out to the chalcogenide glass as sample to be processed in the step c
In the process, when applying DC voltage to the two sides of the chalcogenide glass as sample to be processed, after applied voltage is stablized, electric current is opened
Gradually decaying begin until 0A；In applied voltage stabilization process and current decay process, remember always by the way that computer software is synchronous
The variation of voltage and current is recorded, in case regulating and controlling needed for thermal poling treatment process to thermal poling treatment process parameter setting.
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| CN113391383A (en) * | 2021-06-09 | 2021-09-14 | 上海大学 | Preparation method for printing ultramicro-microlens with periodic micro-nano structure gradient refractive index by adopting grid electrode micro-thermal polarization |
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| CN1821132A (en) * | 2006-03-16 | 2006-08-23 | 华东理工大学 | Sulfer-halogen glass having high second-order non-linear polarizability and its heat polarizing method |
| CN101266883A (en) * | 2008-04-11 | 2008-09-17 | 中山大学 | Grid electrode integrated double-side efficient light absorption dye sensitized solar battery |
| CN102109638A (en) * | 2011-03-14 | 2011-06-29 | 浙江大学 | Strip-shaped optical wave guide in glass thermal poling layer |
| JP2014086100A (en) * | 2012-10-20 | 2014-05-12 | Meisho Kiko Kk | Manufacturing method and manufacturing apparatus of nano-uneven patter |
| CN105842767A (en) * | 2016-05-04 | 2016-08-10 | 上海大学 | Equipment for preparing diffractive optical element by adopting microscopic pattern electrode thermal polarization and method thereof |
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|---|---|---|---|---|
| CN1821132A (en) * | 2006-03-16 | 2006-08-23 | 华东理工大学 | Sulfer-halogen glass having high second-order non-linear polarizability and its heat polarizing method |
| CN101266883A (en) * | 2008-04-11 | 2008-09-17 | 中山大学 | Grid electrode integrated double-side efficient light absorption dye sensitized solar battery |
| CN102109638A (en) * | 2011-03-14 | 2011-06-29 | 浙江大学 | Strip-shaped optical wave guide in glass thermal poling layer |
| JP2014086100A (en) * | 2012-10-20 | 2014-05-12 | Meisho Kiko Kk | Manufacturing method and manufacturing apparatus of nano-uneven patter |
| CN105842767A (en) * | 2016-05-04 | 2016-08-10 | 上海大学 | Equipment for preparing diffractive optical element by adopting microscopic pattern electrode thermal polarization and method thereof |
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| CN113391383A (en) * | 2021-06-09 | 2021-09-14 | 上海大学 | Preparation method for printing ultramicro-microlens with periodic micro-nano structure gradient refractive index by adopting grid electrode micro-thermal polarization |
| CN113391383B (en) * | 2021-06-09 | 2022-11-08 | 上海大学 | Preparation method for printing ultramicro-lens with periodic micro-nano structure gradient refractive index by adopting grid electrode micro-thermal polarization |
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