CN107561817A - The method of LiNbO_3 film nanometer-scale periodic polarization - Google Patents
The method of LiNbO_3 film nanometer-scale periodic polarization Download PDFInfo
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- CN107561817A CN107561817A CN201710953193.6A CN201710953193A CN107561817A CN 107561817 A CN107561817 A CN 107561817A CN 201710953193 A CN201710953193 A CN 201710953193A CN 107561817 A CN107561817 A CN 107561817A
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- lithium niobate
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Abstract
A kind of method of LiNbO_3 film nanometer-scale periodic polarization, a nanometer pectinate texture is obtained by being molded first after the whirl coating of lithium niobate monocrystal film sample surface, then metallic diaphragm is coated with nanometer pectinate texture as top electrode, polarization process is carried out by the conductive electrode layer in lithium niobate monocrystal film sample and top electrode again, finally by whirl coating and conductive electrode layer is removed, periodic polarized LiNbO_3 film is obtained.Preparation flow of the present invention facilitates easy to operate, and the nanometer-scale periodic polarization domain reverse structure of large area can be obtained on the lithium niobate monocrystal film of hundreds of nanometer thickness by passing through the present invention.
Description
Technical field
The present invention relates to the technology of a kind of photoelectron, optical communication field, is specifically that one kind is made using nano impression
The method that electrode realizes the polarization of LiNbO_3 film nanometer-scale periodic.
Background technology
Lithium niobate monocrystal film equally has important application in integrated nonlinear optics and device.Have at present more
Kind technology can realize ferroelectricity periodical poling, such as the induction of electric field polarization method, femtosecond laser, AFM electricity on lithium niobate monocrystal film
The methods of polarization and electron-beam direct writing.Femtosecond laser induction, AFM electric polarization and direct electronic beam writing technology can prepare micron
And nanoscale domain inversion structures.The polarization pattern of complexity can be prepared by point by point scanning, but the speed of preparation structure but has
Limit.Prepare large area structure and consuming time length, the inferior position of lack of homogeneity be present, be unsuitable for the polarization structure for preparing large area.
Traditional electric polarization realizes that periodical poling but has many good qualities:Cycle can accomplish very little, can be carried out in room temperature and repeatability is fine.
Room temperature electrical-poling method is quite ripe, and this is also the technology used when prepared by commercial periodic polarized crystal.But by broadening
The limitation of effect, the domain structure of large period can only be prepared using electric field polarization method, it is difficult to directly prepare nanoscale periodical poling knot
Structure.Conventional polar method is primarily limited to the preparation method of polarization comb electrode and the limitation of lithium niobate crystal body thickness.Prepare
Sub-micron domain inversion structures need deep-UV lithography or electron beam lithography to prepare a nanometer comb electrode, and this method
Have the shortcomings that cost is high, program is complicated, time-consuming.When the lithium columbate crystal to millimeters thick polarizes, due to inverting farmland
Horizontal broadening effect in rearwardly growth course, the minor cycle, which inverts, easily produces the merging of adjacent reversion farmland in the manufacturing process of farmland
The problems such as.The achieved Minimum Polarization cycle is also generally 3 μm or so.
The content of the invention
The present invention is unable to reach nano level defect for prior art polarization cycle, proposes a kind of LiNbO_3 film nanometer
The periodic polarized method of level, makes comb electrode, then pass through extra electric field on lithium niobate monocrystal film using nano impression
Polarization method carries out periodic electrodes, can prepare nanometer-scale periodic poled lithium niobate monocrystal thin films.Due to electrode width and
Lithium niobate crystal body thickness all in nanoscale, can avoid the horizontal broadening effect in polarization time domain growth course, and can be hundreds of
Nanometer-scale periodic polarization structure, and required polarizing voltage very little are directly prepared on the LiNbO_3 film of nanometer thickness.
The present invention is achieved by the following technical solutions:
Present invention molding first after the whirl coating of lithium niobate monocrystal film sample surface obtains a nanometer pectinate texture, is then receiving
Metallic diaphragm is coated with as top electrode in rice pectinate texture, then passes through the conductive electrode layer in lithium niobate monocrystal film sample and top
Electrode carries out polarization process, finally by whirl coating and conductive electrode layer is removed, obtains periodic polarized LiNbO_3 film.
Described lithium niobate monocrystal film sample include lithium niobate substrate and set gradually silicon dioxide layer thereon,
Conductive electrode layer and lithium niobate monocrystal film layer, wherein:Lithium niobate monocrystal film layer passes through ion implantation technique and Direct Bonding
Technology is combined to obtain, and thickness is hundred nano-scale.
Described conductive electrode layer is made up of gold, platinum or other metals.
Described whirl coating, spin-on material are not limited to PMMA (polymethyl methacrylate), PDMA, photoresist etc., are preferably
One layer of PMMA solution of spin coating on lithium niobate monocrystal film sample.
Described molding refers to, before whirl coating solidification, the mould of nanoscale electrode is pressed in above, and in environment under low pressure
Lower application pressure so that the cavity in whirl coating filling mould;Pressing mold process terminates solidify afterwards and formed with the figure overlapped with mould
Shape simultaneously removes mould.
Described mould, its pattern are preferably nanometer pectinate texture,
Described is coated with, using but be not limited to evaporation or magnetron sputtering, the thickness for the metal film being coated be more than imprint nano
The depth of cutting in pectinate texture, so as to obtain the nano-electrode of large area broach rule.
Described metal film uses but is not limited to the good conductivities such as gold, silver, chromium and is easy to the material of plated film.
Described polarization process refers to, grounding electrode is set in the lithium niobate substrate of lithium niobate monocrystal film sample,
Between top electrode and grounding electrode apply polarization electric impulse signal, polarized electric field direction caused by the polarization electric impulse signal with
The spontaneous polarization on lithium niobate farmland is opposite.
Because LiNbO_3 film thickness is in the case of hundreds of nanometers, according to lithium columbate crystal coercive field 21kV/mm, outer power-up
Field polarizing voltage is very low, not more than air puncture voltage, solves the problem of air-isolation.When external electric field poling is more than niobium
During the coercive field of sour crystalline lithium, the reversion of lithium niobate domain structure can be realized.And electrode width and lithium niobate crystal body thickness are all
In nanoscale, the horizontal broadening effect in polarization time domain growth course can be avoided.
Technique effect
Compared with prior art, the present invention prepares micro-nano electrode by nano-imprinting method on LiNbO_3 film, enters
And the reversion of LiNbO_3 film domain structure is realized by extra electric field.The polarization cycle of preparation is sub-micron or hundred nano-scale, and
It is suitable for preparing large area domain inversion structures.The nanometer comb electrode utilized prepares simple.By nano-imprinting method in niobium
Nanometer comb electrode is prepared on sour lithium film, is a kind of easy and effective and high yield method.External electric field poling voltage is very low,
Solve the problem of air-isolation, simplify polarization device.
Brief description of the drawings
Fig. 1 be it is proposed by the present invention using nano impression make electrode realize the periodic polarized original of lithium niobate monocrystal film
Manage schematic diagram;
Fig. 2 is the structural representation of lithium niobate monocrystal film of the present invention;
Fig. 3 is the flow chart of implementation steps of the present invention.
In figure:Lithium niobate monocrystal film sample 1, nano impression mould 2, metallic substrates 3, top electrode 4, grounding electrode 5, niobic acid
Lithium substrate 11, silicon dioxide layer 12, conductive electrode 13, lithium niobate monocrystal film layer 14, whirl coating layer 15, pectination grating electrode 16,
Poled lithium niobate film 141, nanostructured 151.
Embodiment
It is niobic acid specifically as shown in Figure 2 a using the lithium niobate monocrystal film sample of two kinds of different structures in the present embodiment
Lithium substrate 11, silicon dioxide layer 12, conductive electrode 13, lithium niobate monocrystal film layer 14, whirl coating layer 15;And shown in Fig. 2 b, it is
Lithium niobate substrate 11, conductive electrode 13, silicon dioxide layer 12, lithium niobate monocrystal film layer 14, whirl coating layer 15, used two kinds
LiNbO_3 film structure is basically identical, other in electric polarization implementation process in addition to the polarizing voltage value of application is slightly different
Step method is consistent.
Described lithium niobate monocrystal film cuts for Z-direction, thickness 300-700nm.
The present embodiment comprises the following steps:
As shown in Fig. 2 one layer of PMMA layer of whirl coating is as whirl coating layer 15 first in lithium niobate monocrystal film layer 14.The whirl coating
Layer 15 is specially the PMMA methyl phenyl ethers anisole solution of content 6%, and whirl coating speed is 1000r/min, whirl coating time 1min, the PMMA of gained
The thickness of whirl coating layer 15 is about 0.5 μm.
As shown in Figure 3 a, nanostructured is transferred to by PMMA whirl coating layers by the metallic mold for nano-imprint 2 of pectination formwork structure
On 15, by applying pressure under environment under low pressure so that the cavity in PMMA materials filling mould.After pressing mold process terminates,
PMMA solidifies, and is formed with the figure overlapped with mould, then removes mould.
The structural cycle of described metallic mold for nano-imprint is 500-800nm, depth 500nm;The nano-imprint stamp is not
It is limited to grating type, other structures are equally applicable.
As shown in Figure 3 b, by plating layer of metal on evaporation or magnetically controlled sputter method whirl coating layer 15 after imprinting
Film, as top electrode 4, the thickness of the metal film is more than the groove depth of imprinted pattern, nanostructured is filled, so as to obtain big face
The nanometer pectination grating electrode 16 of product broach rule.
Described metal film can be the good conductivities such as gold, silver, chromium and be easy to the material of plated film.
As shown in Figure 3 c, lithium niobate monocrystal film upper/lower electrode is connected with AWG and applies the electric arteries and veins of polarization
Signal is rushed, polarized electric field direction is opposite with the spontaneous polarization on lithium niobate farmland caused by the polarization electric impulse signal.
For+Z cutting LiNbO_3 film, then top electrode connect positive source, hearth electrode connects power cathode;Cut for-Z
LiNbO_3 film then contrast.
As shown in Figure 3 d, polarize electric impulse signal amplitude according to lithium columbate crystal coercive field 21kV/mm sizes and pole
The distance between polarizing electrode determines.Because the thickness of LiNbO_3 film is generally 300-700nm, required polarizing voltage is 6.3-
14.7V.When hearth electrode is below silicon dioxide layer, polarizing voltage needs correspondingly to improve.Electric-field intensity needs to be more than niobic acid
Lithium coercive field but the breakdown field strength for being less than silica again.The polarizing voltage of lithium niobate is about 21V/ μm, titanium dioxide
The breakdown field strength of silicon layer is about 25V/ μm.
Top electrode and PMMA whirl coatings layer 15 are washed away using acetone, obtains periodic polarized LiNbO_3 film sample, is such as schemed
Shown in 3e.
Above-mentioned specific implementation can by those skilled in the art on the premise of without departing substantially from the principle of the invention and objective with difference
Mode local directed complete set is carried out to it, protection scope of the present invention is defined by claims and not by above-mentioned specific implementation institute
Limit, each implementation in the range of it is by the constraint of the present invention.
Claims (9)
- A kind of 1. method of LiNbO_3 film nanometer-scale periodic polarization, it is characterised in that first in lithium niobate monocrystal film sample Molding obtains a nanometer pectinate texture after the whirl coating of product surface, and metallic diaphragm is then coated with nanometer pectinate texture as top electrode, Polarization process is carried out by the conductive electrode layer in lithium niobate monocrystal film sample and top electrode again, finally by remove whirl coating and Conductive electrode layer, obtain periodic polarized LiNbO_3 film;Described lithium niobate monocrystal film sample includes lithium niobate substrate and sets gradually silicon dioxide layer, conduction thereon Electrode layer and lithium niobate monocrystal film layer.
- 2. according to the method for claim 1, it is characterized in that, described conductive electrode layer is gold or platinum.
- 3. the method according to claim 11, it is characterized in that, described whirl coating, specially in lithium niobate monocrystal film sample Upper one layer of PMMA solution of spin coating.
- 4. according to the method for claim 1, it is characterized in that, described molding refers to, before whirl coating solidification, by nanoscale The mould of electrode is pressed in above, and applies pressure under environment under low pressure so that the cavity in whirl coating filling mould;Pressing mold process knot Beam solidify afterwards form with the figure overlapped with mould and remove mould.
- 5. according to the method for claim 4, it is characterized in that, described mould, its pattern is nanometer pectinate texture.
- 6. according to the method for claim 1, it is characterized in that, described is coated with, using evaporation or magnetron sputtering, wherein:Plating The thickness of the metal film of system is more than the depth of the cutting in imprint nano pectinate texture, so as to obtain receiving for large area broach rule Rice electrode.
- 7. according to the method for claim 1, it is characterized in that, described polarization process refers to, in lithium niobate monocrystal film sample Grounding electrode is set in the lithium niobate substrate of product, applies polarization electric impulse signal, the polarization between top electrode and grounding electrode Polarized electric field direction caused by electric impulse signal is opposite with the spontaneous polarization on lithium niobate farmland.
- 8. the method according to claim 11, it is characterized in that, when the thickness of the lithium niobate monocrystal film sample is 300- During 700nm, polarizing voltage 6.3-14.7V.
- 9. a kind of nanometer-scale periodic polarization structure, it is characterised in that be prepared into by any of the above-described claim methods described Arrive.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109061910A (en) * | 2018-09-11 | 2018-12-21 | 南开大学 | A method of preparing the sub-micron period micro- disk chamber of any polarization pattern lithium niobate |
CN112013975A (en) * | 2020-08-06 | 2020-12-01 | 济南量子技术研究院 | Miniaturized up-conversion single photon detector |
CN112835262A (en) * | 2021-01-04 | 2021-05-25 | 南京大学 | Preparation method of magnesium-doped lithium niobate domain structure |
CN113820901A (en) * | 2021-08-26 | 2021-12-21 | 华南理工大学 | On-chip integrated frequency doubling device and preparation method thereof |
CN114836837A (en) * | 2022-05-27 | 2022-08-02 | 桂林百锐光电技术有限公司 | Method for changing reversal domain width of potassium titanyl phosphate crystal material |
CN115116829A (en) * | 2022-08-29 | 2022-09-27 | 中北大学 | Method for preparing lithium niobate single crystal film domain wall enhanced force electric coupling response device |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109061910A (en) * | 2018-09-11 | 2018-12-21 | 南开大学 | A method of preparing the sub-micron period micro- disk chamber of any polarization pattern lithium niobate |
CN109061910B (en) * | 2018-09-11 | 2022-08-02 | 南开大学 | Method for preparing submicron periodic randomly polarized pattern lithium niobate microdisk cavity |
CN112013975A (en) * | 2020-08-06 | 2020-12-01 | 济南量子技术研究院 | Miniaturized up-conversion single photon detector |
CN112835262A (en) * | 2021-01-04 | 2021-05-25 | 南京大学 | Preparation method of magnesium-doped lithium niobate domain structure |
CN112835262B (en) * | 2021-01-04 | 2023-03-14 | 南京大学 | Preparation method of magnesium-doped lithium niobate domain structure |
CN113820901A (en) * | 2021-08-26 | 2021-12-21 | 华南理工大学 | On-chip integrated frequency doubling device and preparation method thereof |
CN114836837A (en) * | 2022-05-27 | 2022-08-02 | 桂林百锐光电技术有限公司 | Method for changing reversal domain width of potassium titanyl phosphate crystal material |
CN115116829A (en) * | 2022-08-29 | 2022-09-27 | 中北大学 | Method for preparing lithium niobate single crystal film domain wall enhanced force electric coupling response device |
CN115116829B (en) * | 2022-08-29 | 2022-11-22 | 中北大学 | Method for preparing lithium niobate single crystal film domain wall enhanced force electric coupling response device |
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