CN105842767B - The device and method of diffraction optical element are prepared using micro- pattern electrode thermal poling - Google Patents
The device and method of diffraction optical element are prepared using micro- pattern electrode thermal poling Download PDFInfo
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- CN105842767B CN105842767B CN201610286749.6A CN201610286749A CN105842767B CN 105842767 B CN105842767 B CN 105842767B CN 201610286749 A CN201610286749 A CN 201610286749A CN 105842767 B CN105842767 B CN 105842767B
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- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/18—Diffraction gratings
- G02B5/1847—Manufacturing methods
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Abstract
The invention discloses the present invention relates to a kind of device and method that diffraction optical element is prepared using micro- pattern electrode thermal poling, the equipment includes compound soda-lime-silica glass, anode, cathode, heating unit, Ag nano particles, thermocouple, insulating ceramics, stainless steel box, the first controller, computer, second controller, gas inlet and outlet, and anode, cathode are located at the both sides of compound soda-lime-silica glass respectively.The thermal field and periodicity electric field equipment can realize a variety of microstructural diffraction optical elements of Nano/micron level.The present invention can come periodicity and pattern that voltage reaches control sample by adjusting periodicity and the pattern of the micro- pattern on thermal poling voltage, temperature, time and Si anodes.The equipment can once realize the microstructural diffraction optical element of large-area nano/micron order, several times to tens times can be improved with respect to traditional material preparation efficiency.
Description
Technical field
The present invention relates to technical field of material, is prepared and spread out using micro- pattern electrode thermal poling more particularly to one kind
Penetrate the device and method of optical element.
Background technology
In recent years, it is seen that-near-infrared optical material is widely used to information technology, laser technology and electronic communication
Deng modern military and civilian high-tech field.Crystalline material such as sapphire and diamond, are obtained aspherical using traditional handicraft
The difficulty of mirror or prism is big, efficiency is low, of high cost, it is difficult to which the optics that meets to develop rapidly, information technology etc. are to the small-sized of material
Change, integrated and functionalization requirement.Soda-lime-silica glass material is because with light loss is low, covering communication windows are more, manufacture work
The advantages that skill is simple, cost is low and physical dimension is unrestricted, before there is wide application in Visible-to-Near InfaRed optics system
Scape.Usually, the controllable printing for realizing microstructure size and distribution is to obtain the key of the performances such as excellent frequency multiplication and diffraction optics
Link.
In order to realize the light function soda-lime-silica glass controllable preparation based on micro-structure, it is necessary to be modified to glass.In the past
Modification focus primarily upon the common micro Process means such as dry etching and photoetching, it is disadvantageous in that, and equipment is expensive, work
Skill is complicated, processing efficiency is low etc., and especially photoetching is also influenced 2008 be subject to optical diffraction, and Takagi et al. proposes one kind
The micro- pattern electrode thermal poling of simple and feasible solution-use, it illustrates as shown in Figure 1：Using aobvious with periodicity
The anode of micro- pattern carries out thermal poling to glass, to form the polarization layer consistent with anode microstructure pattern in glass surface；From
The pattern (distribution and size) and composition (atom or molecular structure etc.) of the micro-structure set out, and be suitable for specific function (such as
Diffraction grating) design, the printing offer basic guarantee of low-cost and high-performance optical material.
The content of the invention
First technical problem to be solved by this invention is to provide a kind of prepared using micro- pattern electrode thermal poling and spread out
The device and method of optical element are penetrated, required pattern can be disposably printed on sample by it, realize that pattern resolution is reachable
Micron even nano-scale, the pattern of micro-structure（Distribution and size）And composition（Atom or molecular structure etc.）Controllable, preparation
It is efficient.
The present invention is to solve above-mentioned technical problem by following technical proposals：One kind is thermoae using micro- pattern electrode
The equipment that change prepares diffraction optical element, it is characterised in that it include compound soda-lime-silica glass, anode, cathode, heating unit,
Ag nano particles, thermocouple, insulating ceramics, stainless steel box, the first controller, computer, second controller, gas inlet and outlet,
Anode, cathode are located at the both sides of compound soda-lime-silica glass respectively, and Ag nano particles are located at the surface of compound soda-lime-silica glass, thermoelectricity
It is even that positioned at the underface of cathode, insulating ceramics prevents corresponding electricity consumption position electric leakage and fixes corresponding component, compound soda-lime-silica glass,
Anode, cathode, heating unit, Ag nano particles, thermocouple, insulating ceramics are all located at stainless steel cassette interior and control thermal poling
During atmosphere and air pressure, heating unit will realize and control that the first controller be connected and record with computer by the first controller
The detailed process of heating, DC voltage will be realized control by second controller, and second controller is connected with computer and records added
The detailed process of voltage and electric current, stainless steel box are equipped with gas inlet and outlet.
Preferably, the thickness of the soda-lime-silica glass is 1 mm, and compound soda-lime-silica glass passes through Ag+- Na+Ion hand over
Change, by Ag+Compound soda-lime-silica glass surface is incorporated into, afterwards by 400 DEG C and H2Under atmosphere, in glass after reduction method heat treatment
Two surfaces of glass respectively obtain the glass that the Ag nano particles of a layer thickness up to 10 mm, 20 ~ 30 nm of particle diameter adulterate, one of them
Then by 12% HF processing, the surface corrosion of about 10 mm of thickness is fallen side.
Preferably, the heating unit is Resistant heating stove, and operating temperature is between 0-400 DEG C.
Preferably, the anode is that the Si plate electrodes with micro- pattern are prepared by focused ion beam or laser,
The lattice constant of micro- pattern is respectively 50,20,10,5,1,0.5 and 0.3 mm, afterwards using magnetron sputtering last layer 30
The chromium film of nm, it is indissociable for preventing from occurring during thermal poling Si pieces and compound soda-lime-silica glass generation anode linkage
Problem；The cathode is common Si pieces.
Preferably, DC voltage added between the anode and cathode is continuously adjustable in the range of 0 ~ 5 kV.
Preferably, the temperature of the heating unit is continuously adjustable in 0 ~ 400 DEG C, and programming rate connects in 0 ~ 20 DEG C/min
It is continuous adjustable.
The method that the present invention prepares diffraction optical element using micro- pattern electrode thermal poling, it comprises the following steps：
Step 1: the Si pieces with micro- pattern and chromium plating film are made into anode connection cathode, single side face carries nanometer Ag
Soda-lime-silica glass, ordinary silicon are made cathode connection anode and are fixed, and connect heating power supply, cover stainless steel lid；
Step 2: the conduit of stainless steel box and vacuum pump are respectively connected with Ar bottles, by vacuum pump by stainless steel
Box is evacuated to 5 Pa, it is necessary to 20 min of time, closes vacuum pump afterwards, toward stainless steel box in insert Ar gas to atmospheric pressure
1.01 MPa, exclude influence of the steam etc. in air to thermal poling；
Step 3: under program, using the heating unit of heat transfer with 10 DEG C/min speed from room temperature heating surface
Soda-lime-silica glass with nanometer Ag keeps the temperature 15 min, it is ensured that glass in advance to 150 ~ 300 DEG C of insulations generally before added electric field
The temperature uniformity of glass sample；
Step 4: in the case where keeping 150 ~ 300 DEG C of required temperature, pass through the Si pieces with periodically micro- pattern
Make anode and common Si pieces make 0.2 ~ 2.0 kV of cathode impressed DC voltage and continue 5 to 60 min, general power-up is pressed onto required electricity
After pressure is stablized, electric current starts decay until 0 A, by the change of computer software recording voltage and electric current at the same time, in case experiment or
Needed for production；
Step 5: after the min of time to go 5 to 60, heating-stopping apparatus heating, makes compound soda-lime-silica glass cold
But to room temperature, but this process keeps the DC voltage added by step 4 at the same time；
Step 6: after required temperature is reached, polarization DC voltage used is removed, stainless steel lid is opened, carefully takes
Go out sample, irradiated using He-Ne laser, verify the diffraction pattern through pattern of glass sample, obtain required diffraction optics
Element；
Step 7: change one piece of surface with nanometer Ag soda-lime-silica glass, using different thermal poling voltage, temperature, when
Between and the Si pieces with the micro- pattern of different cycles make anode, and return to step one.
Preferably, the diffraction optical element is using He-Ne laser irradiation test diffraction property.
The positive effect of the present invention is：This prepares setting for diffraction optical element using micro- pattern electrode thermal poling
Micro- pattern electrode is used for middle, the micro- pattern resolution of the electrode is conducive to required sample up to micron even Nano grade
Product microstructure appearance be may be reused and required pattern is imprinted on sample optional in a big way.This uses micro- pattern
Electrode thermal poling preparation method disposably can prepare micro-structure needed for large area, and the pattern of micro-structure in sample surfaces
Minimum 0.3 mm of size, the diffraction of light does not influence during less than visible wavelength, and the size of sample surfaces micro-structure is controllable, micro-
The component of structure is adjustable, and relative to traditional material scientific research means, its diffraction optical element preparation efficiency can improve several times to number
Ten times.
Brief description of the drawings
Fig. 1 is the structure diagram for the equipment that the present invention prepares diffraction optical element using micro- pattern electrode thermal poling.
Embodiment
Present pre-ferred embodiments are provided below in conjunction with the accompanying drawings, with the technical solution that the present invention will be described in detail.
As shown in Figure 1, the present invention prepares the equipment of diffraction optical element including compound using micro- pattern electrode thermal poling
Soda-lime-silica glass 1, anode 2, cathode 3, heating unit 4, Ag nano particles 5, thermocouple 6, insulating ceramics 7, stainless steel box 8,
First controller 9, computer 10, second controller 11, gas inlet and outlet 12, anode 2, cathode 3 are located at compound sodium calcium silicon glass respectively
The both sides of glass 1, Ag nano particles 5 are located at the surface of compound soda-lime-silica glass 1, and thermocouple 6 is located at the underface of cathode 3, insulation
Ceramics prevent that corresponding electricity consumption position from leaking electricity and fixed corresponding component, compound soda-lime-silica glass 1, anode 2, cathode 3, heating unit 4,
Ag nano particles 5, thermocouple 6, insulating ceramics 7 are all located at the inside of stainless steel box 8 and can control the gas during thermal poling
Atmosphere and air pressure, heating unit 4 will be realized control by the first controller 9, and the first controller is connected with computer 10 and records heating
Detailed process, DC voltage will be realized control by second controller 11, and second controller 11 is connected with computer 10 and records added
The detailed process of voltage and electric current, stainless steel box 8 are equipped with gas inlet and outlet 12.
The heating unit is Resistant heating stove, and operating temperature is between 0-400 DEG C.
The thickness of the compound soda-lime-silica glass 1 is 1 mm, and compound soda-lime-silica glass passes through Ag+- Na+Ion exchange,
By Ag+Compound soda-lime-silica glass surface is incorporated into, afterwards by 400 DEG C and H2Under atmosphere, in glass after reduction method heat treatment
Two surfaces respectively obtain the glass that the Ag nano particles 5 of a layer thickness up to 10 mm, 20 ~ 30 nm of particle diameter adulterate, one of them
Then by 12% HF processing, the surface corrosion of about 10 mm of thickness is fallen side.The anode 2 is by focused ion beam or laser
The Si plate electrodes with micro- pattern are prepared in device, and the lattice constant of micro- pattern is respectively 50,20,10,5,1,0.5 and
0.3 mm, afterwards using the chromium film of 30 nm of magnetron sputtering last layer, for prevent from occurring during thermal poling Si pieces with it is compound
Anode linkage and indissociable problem occur for soda-lime-silica glass, and the micro- pattern resolution of the electrode is up to micron even nanometer
Rank, be conducive to needed for sample microstructure appearance optional in a big way, and may be reused and required pattern is imprinted on sample
On.This disposably can prepare micro- knot needed for large area using micro- pattern electrode thermal poling preparation method in sample surfaces
Structure.Added DC voltage is continuously adjustable in the range of 0 ~ 5 kV between the anode and cathode, in fixed operating temperature and
In the case of less than breakdown voltage, bigger operating voltage, the required thermal poling time is shorter, can according to the actual requirements compared with
Big selection operating voltage.The temperature of the heating unit is continuously adjustable in 0 ~ 400 DEG C, and programming rate is in 0 ~ 20 DEG C/min
It is continuously adjustable in the case of less than breakdown voltage, bigger operating temperature, the required thermal poling time is shorter, can be according to reality
Border demand is in larger selection operating temperature.The cathode is common Si pieces, can so reduce cost.
A variety of microstructural diffraction optical elements of Nano/micron level can be achieved in the present invention, can be by adjusting thermal poling
The periodicity of micro- pattern on voltage, temperature, time and Si anodes and pattern come voltage reach the periodicity of control sample with
Pattern.The equipment can once realize the microstructural diffraction optical element of large-area nano/micron order, with respect to traditional material system
Standby efficiency can improve several times to tens times.
The method that the present invention prepares diffraction optical element using micro- pattern electrode thermal poling includes the following steps following step
Suddenly：
Step 1: the Si pieces with micro- pattern and chromium plating film are made into anode connection cathode, single side face carries nanometer Ag
Soda-lime-silica glass（Its side with nanometer Ag is towards anode）, ordinary silicon make cathode connection anode etc. and fixed by Fig. 1, connect
Heating power supply, covers stainless steel lid；
Step 2: the conduit of stainless steel box and vacuum pump are respectively connected with Ar bottles, by vacuum pump by stainless steel
Box is evacuated to 5 Pa, it is necessary to 20 min of time, closes vacuum pump afterwards, toward stainless steel box in insert Ar gas to atmospheric pressure
1.01 MPa, exclude influence of the steam etc. in air to thermal poling；
Step 3: under program, using the heating unit of heat transfer with 10 DEG C/min speed from room temperature heating surface
Soda-lime-silica glass with nanometer Ag keeps the temperature 15 min, it is ensured that glass in advance to 150 ~ 300 DEG C of insulations generally before added electric field
The temperature uniformity of glass sample；
Step 4: in the case where keeping 150 ~ 300 DEG C of required temperature, pass through the Si pieces with periodically micro- pattern
Make anode and common Si pieces make 0.2 ~ 2.0 kV of cathode impressed DC voltage and continue 5 to 60 min, general power-up is pressed onto required electricity
After pressure is stablized, electric current starts decay until 0 A, by the change of computer software recording voltage and electric current at the same time, in case experiment or
Needed for production；
Step 5: after the min of time to go 5 to 60, heating-stopping apparatus heating, makes compound soda-lime-silica glass cold
But to room temperature, but this process keeps the DC voltage added by step 4 at the same time；
Step 6: after required temperature is reached, polarization DC voltage used is removed, stainless steel lid is opened, carefully takes
Go out sample, using He-Ne laser（Wavelength is 632 nm）Irradiation, verifies the diffraction pattern through pattern of glass sample, obtains
Required diffraction optical element；
Step 7: change one piece of surface with nanometer Ag soda-lime-silica glass, using different thermal poling voltage, temperature, when
Between and the Si pieces with the micro- pattern of different cycles make anode, and return to step one.
The present invention realizes the microstructural diffraction optics member of a variety of Nano/micron levels by thermal field and periodicity electric field equipment
Part.Reach control sample by adjusting the periodicity and pattern of micro- pattern on thermal poling voltage, temperature, time and Si anodes
The periodicity and pattern of product.The equipment can once realize the microstructural diffraction optical element of large-area nano/micron order, phase
Several times to tens times can be improved to traditional material preparation efficiency.Diffraction optical element uses He-Ne laser（Wavelength is 632 nm）
Irradiation test diffraction property, can obtain the diffraction pattern through pattern.According to the effect of diffraction pattern and then to thermal poling
Key factor：The micro- pattern of electrode, thermal poling voltage, temperature, time etc. optimize.
Particular embodiments described above, technical problem, technical solution and the beneficial effect of the solution to the present invention carry out
It is further described, it should be understood that the foregoing is merely the specific embodiment of the present invention, is not limited to
The present invention, within the spirit and principles of the invention, any modification, equivalent substitution, improvement and etc. done, should be included in this
Within the protection domain of invention.
Claims (7)
1. a kind of equipment that diffraction optical element is prepared using micro- pattern electrode thermal poling, it is characterised in that it includes compound
Soda-lime-silica glass, anode, cathode, heating unit, Ag nano particles, thermocouple, insulating ceramics, stainless steel box, the first control
Device, computer, second controller, gas inlet and outlet, anode, cathode are located at the both sides of compound soda-lime-silica glass, nanometer Ag respectively
Grain is located at the surface of compound soda-lime-silica glass, and thermocouple is located at the underface of cathode, and insulating ceramics prevents corresponding electricity consumption position from leaking
Electricity and fixed corresponding component, compound soda-lime-silica glass, anode, cathode, heating unit, Ag nano particles, thermocouple, insulating ceramics
Be all located at stainless steel cassette interior and control thermal poling during atmosphere and air pressure, heating unit will be realized by the first controller
Control, the first controller are connected with computer and record the detailed process of heating, and DC voltage will be realized control by second controller,
Second controller is connected with computer and records the detailed process of institute's making alive and electric current, and stainless steel box is passed in and out equipped with gas
Mouthful.
2. the equipment for preparing diffraction optical element using micro- pattern electrode thermal poling as claimed in claim 1, its feature exist
In the thickness of the soda-lime-silica glass is 1 mm, and compound soda-lime-silica glass passes through Ag+- Na+Ion exchange, by Ag+It is incorporated into
Compound soda-lime-silica glass surface, afterwards by 400 DEG C and H2Under atmosphere, in two surface difference of glass after reduction method heat treatment
The glass that the Ag nano particles of a layer thickness up to 10 mm, 20 ~ 30 nm of particle diameter adulterate is obtained, one of side then passes through 12%
HF processing, the surface corrosion of about 10 mm of thickness is fallen.
3. the equipment for preparing diffraction optical element using micro- pattern electrode thermal poling as claimed in claim 1, its feature exist
In the heating unit is Resistant heating stove, and operating temperature is between 0-400 DEG C.
4. the equipment for preparing diffraction optical element using micro- pattern electrode thermal poling as claimed in claim 1, its feature exist
In the anode is that the Si plate electrodes with micro- pattern, the net of micro- pattern is prepared by focused ion beam or laser
Lattice constant is respectively 50,20,10,5,1,0.5 and 0.3 mm, afterwards using the chromium film of 30 nm of magnetron sputtering last layer, is used for
Prevent from occurring during thermal poling Si pieces and compound soda-lime-silica glass and occur anode linkage and indissociable problem；The cathode
For common Si pieces.
5. the equipment for preparing diffraction optical element using micro- pattern electrode thermal poling as claimed in claim 1, its feature exist
In added DC voltage is continuously adjustable in the range of 0 ~ 5 kV between the anode and cathode.
6. the equipment for preparing diffraction optical element using micro- pattern electrode thermal poling as claimed in claim 1, its feature exist
In the temperature of the heating unit is continuously adjustable in 0 ~ 400 DEG C, and programming rate is continuously adjustable in 0 ~ 20 DEG C/min.
A kind of 7. method that diffraction optical element is prepared using micro- pattern electrode thermal poling, using according in claim 1-6
Any one of them prepares the equipment of diffraction optical element to realize using micro- pattern electrode thermal poling, it is characterised in that the party
Method concretely comprises the following steps：
Step 1: the Si pieces with micro- pattern and chromium plating film are made into anode connection cathode, sodium calcium of the single side face with nanometer Ag
Silica glass, its side with nanometer Ag are made cathode connection anode towards anode, ordinary silicon and are fixed, connect heating power supply, cover
Upper stainless steel lid；
Step 2: the conduit of stainless steel box and vacuum pump are respectively connected with Ar bottles, by vacuum pump by stainless steel box
5 Pa are evacuated to, it is necessary to 20 min of time, closes vacuum pump afterwards, toward stainless steel box in insert Ar gas to atmospheric pressure 1.01
MPa, excludes influence of the steam in air to thermal poling；
Step 3: under program, carried using the heating unit of heat transfer with 10 DEG C/min speed from room temperature heating surface
The soda-lime-silica glass of nanometer Ag keeps the temperature 15 min, it is ensured that hyaloid in advance to 150 ~ 300 DEG C of insulations generally before added electric field
The temperature uniformity of product；
Step 4: in the case where keeping 150 ~ 300 DEG C of required temperature, sun is made by the Si pieces with periodically micro- pattern
Pole and common Si pieces make 0.2 ~ 2.0 kV of cathode impressed DC voltage and continue 5 to 60 min, and it is steady that general power-up is pressed onto required voltage
After fixed, electric current starts decay up to 0 A, by the change of computer software while recording voltage and electric current, in case experiment or production
It is required；
Step 5: after the min of time to go 5 to 60, heating-stopping apparatus heating, allows compound soda-lime-silica glass to be cooled to
Room temperature, but this process keeps the DC voltage added by step 4 at the same time；
Step 6: after required temperature is reached, polarization DC voltage used is removed, stainless steel lid is opened, carefully takes out sample
Product, are irradiated using He-Ne laser, verify the diffraction pattern through pattern of glass sample, obtain required diffraction optical element；
Step 7: change one piece of surface with nanometer Ag soda-lime-silica glass, using different thermal poling voltage, temperature, the time and
Si pieces with the micro- pattern of different cycles make anode, and return to step one.
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| CN201610286749.6A CN105842767B (en) | 2016-05-04 | 2016-05-04 | The device and method of diffraction optical element are prepared using micro- pattern electrode thermal poling |
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| CN201610286749.6A CN105842767B (en) | 2016-05-04 | 2016-05-04 | The device and method of diffraction optical element are prepared using micro- pattern electrode thermal poling |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108732846B (en) * | 2018-05-18 | 2020-09-04 | 上海大学 | Method for preparing optical element with periodic microscopic second-order nonlinear polarizability by adopting grid electrode hot polarization |
| CN108681181B (en) * | 2018-05-18 | 2020-10-16 | 上海大学 | Laser-assisted thermal polarization equipment and method for microscopic second-order nonlinear polarizability optical element |
| CN109270613B (en) * | 2018-09-05 | 2020-10-30 | 上海大学 | Method for preparing visible-infrared diffraction grating by adopting grid electrode micro thermal polarization process |
| US20210347689A1 (en) * | 2018-10-18 | 2021-11-11 | Corning Incorporated | Graphene doping by thermal poling |
| WO2021154698A1 (en) | 2020-01-31 | 2021-08-05 | Corning Incorporated | High throughput electro-thermal poling |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6417968B1 (en) * | 1998-01-27 | 2002-07-09 | René Staub | Diffractive surface pattern |
| CN101388523A (en) * | 2008-10-30 | 2009-03-18 | 上海大学 | Novel organic semi-conductor solid laser and preparation thereof |
| CN105296960A (en) * | 2015-10-28 | 2016-02-03 | 上海大学 | Preparation method of homogenized boron nitride coating |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7067240B2 (en) * | 2001-03-09 | 2006-06-27 | Waveguide Solutions, Inc. | Gray scale fabrication method using a spin-on glass material and integrated optical designs produced therefrom |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6417968B1 (en) * | 1998-01-27 | 2002-07-09 | René Staub | Diffractive surface pattern |
| CN101388523A (en) * | 2008-10-30 | 2009-03-18 | 上海大学 | Novel organic semi-conductor solid laser and preparation thereof |
| CN105296960A (en) * | 2015-10-28 | 2016-02-03 | 上海大学 | Preparation method of homogenized boron nitride coating |
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