CN105908229A - Method for adjusting three-dimensional photonic crystal band gap through lithiation method - Google Patents
Method for adjusting three-dimensional photonic crystal band gap through lithiation method Download PDFInfo
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- CN105908229A CN105908229A CN201610280254.2A CN201610280254A CN105908229A CN 105908229 A CN105908229 A CN 105908229A CN 201610280254 A CN201610280254 A CN 201610280254A CN 105908229 A CN105908229 A CN 105908229A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/02—Electroplating of selected surface areas
- C25D5/022—Electroplating of selected surface areas using masking means
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/54—Electroplating: Baths therefor from solutions of metals not provided for in groups C25D3/04 - C25D3/50
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/08—Germanium
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
- C30B30/02—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using electric fields, e.g. electrolysis
Abstract
The invention discloses a method for adjusting a three-dimensional photonic crystal band gap through a lithiation method. The method for adjusting the three-dimensional photonic crystal band gap through the lithiation method aims at solving the problems that an existing method for adjusting the three-dimensional photonic crystal band gap is narrow in adjusting range and low in precision. The method for adjusting the photonic crystal band gap includes the steps that copper foil is perpendicularly put into PS microsphere emulsion to be cultivated, and copper foil on which a PS colloid template grows is obtained; secondly, GeC14 is added to (EMIM)TF2N, and an electrolyte is obtained; thirdly, a three-electrode electrolytic cell is used, a potentiostatic method is used for electrodeposition of germanium, and a three-dimensional germanium film is obtained; and fourthly, the lithium embedding and lithium removing processes are conducted in a three-electrode system, and therefore the three-dimensional photonic crystal band gap is adjusted. By means of the method, the direction of voltage is controlled so that the germanium film with the three-dimensional photonic crystal structure is correspondingly subjected to the lithium embedding and removing processes, and due to the fact that volume expansion of Ge is large, the adjusting range of the method is very large.
Description
Technical field
The present invention relates to a kind of method regulating three-D photon crystal band gap.
Background technology
This concept of photonic crystal is proposed by Yablonovitch and John the earliest, and it is by the medium of different refractivity
The artificial micro-structure of periodic arrangement, has photonic bandgap.When the frequency of light is positioned in the range of photon band gap, light will
It is prohibited to propagate.Due to the existence of photon band gap, photonic crystal has many brand-new physical propertys, becomes the world today
One study hotspot.
Affect photon band gap because have two kinds: the dielectric constant ratio of dielectric material or refractive index ratio and the structure of photonic crystal.
Therefore, change photon band gap general also from these two aspects consideration: one is to change refractive index to be modulated, and two is that change photon is brilliant
Body periodic structure is modulated.Because changing photonic crystal periodic structure to need by complicated equipment and complex operation, institute
Select to change its band gap by change photonic crystal refractive index with the present invention.
Summary of the invention
The adjustable range that the invention aims to solve the method for existing regulation three-D photon crystal band gap is narrower, precision
Low problem, and a kind of method utilizing lithiumation method regulation three-D photon crystal band gap is provided.
The present invention utilizes the method for lithiumation method regulation three-D photon crystal band gap to follow these steps to realize:
One, Copper Foil is put in hydrochloric acid solution and soaks, then use acetone, methyl alcohol and ultra-pure water ultrasonic cleaning 5～20min successively,
Copper Foil after being cleaned, then with water as solvent, configuration volume fraction is the PS microballoon emulsion of 0.1%～0.3%, will be clear
Copper Foil after washing vertically is put in PS microballoon emulsion, and at 50～70 DEG C incubated 48～120h, obtaining growth has PS glue
The Copper Foil of body template；
Two, by ionic liquid (EMIM) TF2N (the double trifluoro sulfonic amine salt solvent of 1-methyl-3-ethyl imidazol(e)) puts into gloves
Case carries out second distillation, at H2O and O2Under conditions of content is respectively less than 1ppm, by GeCl4Add (EMIM) TF2N
In, dissolve and after shaking up, stand 12～24h, obtain the electrolyte that molar concentration is 0.01～1mol/L；
Three, using the electrolytic cell of three electrodes, with platinum loop for electrode, filamentary silver is reference electrode, and the growth described in step one has
The Copper Foil of PS colloid template is working electrode, uses potentiostatic method, control deposition voltage in the electrolyte that step 2 obtains
Carry out electro-deposition germanium for-1.5～-2V, then take out working electrode, clean, obtain three-dimensional ordered macroporous germanium (3DOM after drying
Ge) film (germanium photonic crystal)；
Four, three-dimensional ordered macroporous germanium film step 3 obtained is as working electrode, lithium band as reference electrode with to electrode,
With LiPF6, EC (ethylene carbonate), the mixed liquor of DEC (diethyl carbonate) be electrolyte, in three-electrode system
Carry out embedding and removing process, thus regulate three-D photon crystal band gap.
It is the direction by controlling voltage that the present invention regulates the principle of three-D photon crystal photon band gap, makes have three-dimensional photon brilliant
Correspondingly there is embedding lithium and de-lithium process in the germanium film of body structure.Germanium can be with the lithium ion in electrolyte during removal lithium embedded
Form Li4.4Ge alloy so that germanium material occurs the biggest Volume Changes.Therefore, along with embedding and the abjection of lithium ion,
Germanium photonic crystal volumetric expansion, structure changes (aperture diminishes, and hole wall is thickening), causes the refraction of three-D photon crystal
Rate changes, thus realizes the regulation to three-D photon crystal photon band gap.And owing to Ge volumetric expansion is up to 370%,
Theoretical embedding lithium specific capacity is relatively big (1600mAh g-1), therefore the method regulation model of this regulation three-D photon crystal photon band gap
Enclose the biggest.The beneficial effects of the present invention is the regulation achieved three-D photon crystal band gap, method of operating is safe, simple
Single, adjustable range is big, precision is high, continuously adjustable.
Accompanying drawing explanation
Fig. 1 is three-dimensional ordered macroporous germanium (3DOM Ge) film scanning electron microscope (SEM) photograph before lithiumation that embodiment one obtains；
Fig. 2 is three-dimensional ordered macroporous germanium (3DOM Ge) film scanning electron microscope (SEM) photograph after lithiumation that embodiment one obtains；
Fig. 3 is three-dimensional ordered macroporous germanium (3DOM Ge) film reflectance spectrum figure of (b) after (a) and lithiumation before lithiumation.
Detailed description of the invention
Detailed description of the invention one: present embodiment utilizes the method for lithiumation method regulation three-D photon crystal band gap to follow these steps to reality
Execute:
One, Copper Foil is put in hydrochloric acid solution and soaks, then use acetone, methyl alcohol and ultra-pure water ultrasonic cleaning 5～20min successively,
Copper Foil after being cleaned, then with water as solvent, configuration volume fraction is the PS microballoon emulsion of 0.1%～0.3%, will be clear
Copper Foil after washing vertically is put in PS microballoon emulsion, and at 50～70 DEG C incubated 48～120h, obtaining growth has PS glue
The Copper Foil of body template；
Two, by ionic liquid (EMIM) TF2N (the double trifluoro sulfonic amine salt solvent of 1-methyl-3-ethyl imidazol(e)) puts into gloves
Case carries out second distillation, at H2O and O2Under conditions of content is respectively less than 1ppm, by GeCl4Add (EMIM) TF2N
In, dissolve and after shaking up, stand 12～24h, obtain the electrolyte that molar concentration is 0.01～1mol/L；
Three, using the electrolytic cell of three electrodes, with platinum loop for electrode, filamentary silver is reference electrode, and the growth described in step one has
The Copper Foil of PS colloid template is working electrode, uses potentiostatic method, control deposition voltage in the electrolyte that step 2 obtains
Carry out electro-deposition germanium for-1.5～-2V, then take out working electrode, clean, obtain three-dimensional ordered macroporous germanium (3DOM after drying
Ge) film (germanium photonic crystal)；
Four, three-dimensional ordered macroporous germanium film step 3 obtained is as working electrode, lithium band as reference electrode with to electrode,
With LiPF6, EC (ethylene carbonate), the mixed liquor of DEC (diethyl carbonate) be electrolyte, in three-electrode system
Carry out embedding and removing process, thus regulate three-D photon crystal band gap.
Present embodiment prepares polystyrene (PS) colloid template initially with vertical deposition method, at copper after configuration electrolyte
Paper tinsel substrates germanium, obtains three-dimensional ordered macroporous germanium film, finally carries out embedding and removing process in three-electrode system, right
The band gap of three-D photon crystal is adjusted.
There is bigger volumetric expansion in germanium sill during lithiumation (embedding and removing), its volumetric expansion is up to 370%.
Therefore the germanium generation lithiumation process with three-dimensional photon crystal structure can be made by controlling the direction of voltage so that it is crystal is tied
Structure changes, and causes the refractive index of three-D photon crystal to change, thus realizes three-D photon crystal photon band gap
Regulation.Safely, simply, adjustable range is big, precision is high, continuously adjustable for method of operating.
Detailed description of the invention two: Copper Foil is put into volumetric concentration by present embodiment step one unlike detailed description of the invention one
It is that the hydrochloric acid solution of 10%～30% soaks 5～10s.Other step and parameter are identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment unlike detailed description of the invention one or two step 3 at H2O and O2Contain
Under conditions of amount is respectively less than 1ppm, in the electrolyte that step 2 obtains, carry out electro-deposition germanium with potentiostatic method.Other step
And parameter is identical with detailed description of the invention one or two.
Detailed description of the invention four: present embodiment clear described in step 3 unlike one of detailed description of the invention one to three
Wash is to use isopropanol to be carried out working electrode surface.Other step and parameter and one of detailed description of the invention one to three phase
With.
Detailed description of the invention five: present embodiment step 3 unlike one of detailed description of the invention one to four controls deposition electricity
Pressure is for-1.5～-2V, and sedimentation time is 10～30min.Other step and parameter are identical with one of detailed description of the invention one to four.
Detailed description of the invention six: the three-dimensional that present embodiment step 3 unlike one of detailed description of the invention one to five obtains
The thickness of ordered big hole germanium (3DOM Ge) film is 0.5～5 μm.Other step and parameter and detailed description of the invention one to
One of five identical.
Detailed description of the invention seven: present embodiment unlike one of detailed description of the invention one to six step 4 at H2O and
O2Under conditions of content is respectively less than 1ppm, three-dimensional ordered macroporous germanium film step 3 obtained is as working electrode, lithium band
As reference electrode with to electrode.Other step and parameter are identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: the electrolysis described in present embodiment step 4 unlike one of detailed description of the invention one to seven
In liquid, the volume ratio of EC Yu DEC is 1:0.5～1:2.Other step and parameter are identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: present embodiment unlike one of detailed description of the invention one to eight step 4 in three electrode body
The process carrying out embedding lithium in system is to use cyclic voltammetry to bear to sweep, and sweep limits is 0～2V, and sweep speed is 0.1mV/s.
Other step and parameter are identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment unlike one of detailed description of the invention one to eight step 4 in three electrode body
The process carrying out de-lithium in system is to use cyclic voltammetry just to sweep, and sweep limits is 0～2V, and sweep speed is 0.1mV/s.
Other step and parameter are identical with one of detailed description of the invention one to eight.
Embodiment one: the present embodiment utilizes the method for lithiumation method regulation three-D photon crystal band gap to follow these steps to implement:
One, Copper Foil is put in the hydrochloric acid solution that volumetric concentration is 10% immersion 5s, more successively with acetone, methyl alcohol and ultrapure
Water ultrasonic cleaning 5min, the Copper Foil after being cleaned, then with water as solvent, configure the PS that volume fraction is 0.2% micro-
Ball emulsion, the Copper Foil after cleaning vertically is put in PS microballoon emulsion, and incubated 72h at 60 DEG C, obtaining growth has
The Copper Foil of PS colloid template；
Two, by double for ionic liquid 1-methyl-3-ethyl imidazol(e) trifluoro sulfonic amine salt solvent (EMIM) TF2N puts in glove box
Carry out second distillation, at H2O and O2Under conditions of content is respectively less than 1ppm, by GeCl4Add (EMIM) TF2In N,
Dissolving stands 12h after shaking up, and obtains the electrolyte that molar concentration is 0.1mol/L；
Three, using the electrolytic cell of three electrodes, with platinum loop for electrode, filamentary silver is reference electrode, and the growth described in step one has
The Copper Foil of PS colloid template is working electrode, at H2O and O2Under conditions of content is respectively less than 1ppm, obtain in step 2
Electrolyte in carry out electro-deposition germanium, at H with potentiostatic method2O and O2Under conditions of content is respectively less than 1ppm, it is heavy to control
Long-pending voltage is-1.7V, and sedimentation time is 20min, takes out working electrode, cleans, obtains three-dimensional ordered macroporous germanium after drying
(3DOM Ge) film (germanium photonic crystal)；
Four, at H2O and O2Under conditions of content is respectively less than 1ppm, 3DOM Ge germanium film step 3 obtained is made
For working electrode, lithium band is as reference electrode with to electrode, with LiPF6, EC (ethylene carbonate), DEC (carbonic acid two
Ethyl ester) mixed liquor be electrolyte, in three-electrode system use cyclic voltammetry carry out embedding and removing process (scanning model
Enclosing is 0～2V, and sweep speed is 0.1mV/s, and after the first direction of scanning is first negative just, i.e. first embedding lithium takes off lithium again), thus regulate three
Dimensional photonic crystal band gap；
Wherein in the electrolyte of step 4, the volume ratio of EC Yu DEC is 1:1, wherein LiPF in electrolyte6Concentration be
1mol/L。
The reflectance spectrum figure of Fig. 3 demonstrates that the 3DOM Ge of different pore size can realize band gap the reddest during removal lithium embedded
Outer regulation in visible wavelength region, adjustable range is big, precision is high.
Claims (10)
1. the method utilizing lithiumation method regulation three-D photon crystal band gap, it is characterised in that be to follow these steps to realize:
One, Copper Foil is put in hydrochloric acid solution and soaks, then use acetone, methyl alcohol and ultra-pure water ultrasonic cleaning 5～20min successively,
Copper Foil after being cleaned, then with water as solvent, configuration volume fraction is the PS microballoon emulsion of 0.1%～0.3%, will clean
After Copper Foil vertically put in PS microballoon emulsion, at 50～70 DEG C incubated 48～120h, obtaining growth has PS colloid
The Copper Foil of template；
Two, by ionic liquid (EMIM) TF2N puts into and carries out second distillation in glove box, at H2O and O2Content is respectively less than
Under conditions of 1ppm, by GeCl4Add (EMIM) TF2In N, dissolving and stand 12～24h after shaking up, obtaining molar concentration is
The electrolyte of 0.01～1mol/L；
Three, using the electrolytic cell of three electrodes, with platinum loop for electrode, filamentary silver is reference electrode, and the growth described in step one has
The Copper Foil of PS colloid template is working electrode, carries out electro-deposition germanium with potentiostatic method in the electrolyte that step 2 obtains, and controls
Deposition voltage is-1.5～-2V, and sedimentation time is 10～30min, then takes out working electrode, cleans, obtains three-dimensional after drying
Ordered big hole germanium film；
Four, three-dimensional ordered macroporous germanium film step 3 obtained is as working electrode, lithium band as reference electrode with to electrode,
With LiPF6, the mixed liquor of EC, DEC be electrolyte, three-electrode system carries out embedding and removing process, thus regulates
Three-D photon crystal band gap.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
Copper Foil is put into and is soaked 5～10s in the hydrochloric acid solution that volumetric concentration is 10%～30% by step one.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
Step 3 is at H2O and O2Under conditions of content is respectively less than 1ppm, carry out with potentiostatic method in the electrolyte that step 2 obtains
Electro-deposition germanium.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
Cleaning described in step 3 is to use isopropanol to be carried out working electrode surface.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
It is-1.5～-2V that step 3 controls deposition voltage, and sedimentation time is 10～30min.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
The thickness of the three-dimensional ordered macroporous germanium film that step 3 obtains is 0.5～5 μm.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
Step 4 is at H2O and O2Under conditions of content is respectively less than 1ppm, the three-dimensional ordered macroporous germanium film that step 3 is obtained as
Working electrode, lithium band is as reference electrode with to electrode.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
In electrolyte described in step 4, the volume ratio of EC Yu DEC is 1:0.5～1:2.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, it is characterised in that
It is to use cyclic voltammetry to bear to sweep that step 4 carries out the process of embedding lithium in three-electrode system, and sweep limits is 0～2V, scanning speed
Degree is 0.1mV/s.
A kind of method utilizing lithiumation method regulation three-D photon crystal band gap the most according to claim 1, its feature exists
The process carrying out de-lithium in step 4 in three-electrode system is to use cyclic voltammetry just to sweep, and sweep limits is 0～2V, scanning
Speed is 0.1mV/s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019173945A1 (en) * | 2018-03-12 | 2019-09-19 | 中国科学院半导体研究所 | Direct bandgap light-emitting silicon-based material and preparation method therefor, and on-chip light-emitting device |
| CN110987822A (en) * | 2019-11-19 | 2020-04-10 | 广西大学 | Method for detecting volatile organic compound |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435110A (en) * | 2008-12-04 | 2009-05-20 | 哈尔滨工业大学 | Preparation of germanium three-dimensional photonic crystal |
| CN102864473A (en) * | 2012-10-22 | 2013-01-09 | 哈尔滨工业大学 | Preparation method of three-dimensional ordered macroporous silicon or germanium film |
| CN103616764A (en) * | 2013-11-26 | 2014-03-05 | 哈尔滨工业大学 | Method for adjusting photonic band gap of three-dimensional photonic crystal through voltage |
-
2016
- 2016-04-29 CN CN201610280254.2A patent/CN105908229B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101435110A (en) * | 2008-12-04 | 2009-05-20 | 哈尔滨工业大学 | Preparation of germanium three-dimensional photonic crystal |
| CN102864473A (en) * | 2012-10-22 | 2013-01-09 | 哈尔滨工业大学 | Preparation method of three-dimensional ordered macroporous silicon or germanium film |
| CN103616764A (en) * | 2013-11-26 | 2014-03-05 | 哈尔滨工业大学 | Method for adjusting photonic band gap of three-dimensional photonic crystal through voltage |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019173945A1 (en) * | 2018-03-12 | 2019-09-19 | 中国科学院半导体研究所 | Direct bandgap light-emitting silicon-based material and preparation method therefor, and on-chip light-emitting device |
| CN110987822A (en) * | 2019-11-19 | 2020-04-10 | 广西大学 | Method for detecting volatile organic compound |
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