CN102517551B - Preparation method for three-dimensional photonic crystal - Google Patents
Preparation method for three-dimensional photonic crystal Download PDFInfo
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- CN102517551B CN102517551B CN 201110441138 CN201110441138A CN102517551B CN 102517551 B CN102517551 B CN 102517551B CN 201110441138 CN201110441138 CN 201110441138 CN 201110441138 A CN201110441138 A CN 201110441138A CN 102517551 B CN102517551 B CN 102517551B
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Abstract
The invention relates to a preparation method for a three-dimensional photonic crystal, in particular to a method for preparing the photonic crystal by utilizing a multi-layer film structure and a laser technology and belongs to the technical fields of preparation of films and micronano structures. Multiple layers separated by copper nitride/nitride are prepared by a spattering method or an atomic layer deposition method; and the three-dimensional photonic crystal is prepared by performing femtosecond laser scanning on the multiple layers. A three-dimensional periodic structure can be formed by utilizing a copper nitride low-temperature decomposition effect and combining the multi-layer film structure and the femtosecond laser technology; the thickness of each layer of film can be regulated and controlled; the optical property of the three-dimensional photonic crystal can be regulated and controlled conveniently; the test steps are simple; and repeatability is high.
Description
Technical field
The present invention relates to a kind of preparation method of photonic crystal, refer in particular to and utilize multi-layer film structure and laser technology, the preparation photonic crystal belongs to film preparation, micro-nano structure preparing technical field.
Background technology
Photonic crystal is new ideas and the novel material that late nineteen eighties proposes, and obtains so far unusual swift and violent development, and this material can be controlled the motion of photon as we wish; Because the high-performance optical device that its unique characteristic, photonic crystal can be made brand new principle or can not be made in the past also has important purposes on optical communication, as substituting traditional electron device with photon crystal device, improve the speed of information communication.
Simple and easy for seeking a kind of making, the low structure of while component units dimension, the researchist of Ames has proposed a kind of photonic crystal of laminate structure, forming unit is one dimension dielectric rod [K. M. Ho, C. T. Chan, C. M. Soukoulis, R. Biswas, and M. Sigalas, Solid State Commun. 89,413 (1994)], in every layer, one dimension dielectric rod is arranged in parallel, and distance each other is a; The dielectric rod of the second layer is 90 with the first layer rod angle
oThe 3rd layer of arranges the same with the first layer, but displacement a/2; The 4th layer with the second layer too, but displacement a/2; Layer 5 and the first layer repeat; Such structure has center of area four directions symmetry, when ability c/a=√ 2, is exactly diamond lattic structure especially, and in fact, facing mutually two-layer angle can be 60 to 90
oBetween change, omnidirectional gap is arranged, piled up by alumina rod for the first time on this structural experiment and form [E. Ozbay, A. Abeyta, G. Tuttle, ringides, R. Biswas, M. Sigalas, C. M. Soukoulis, C. T. Chan, and K. M. Ho, Phys. Rev. B50,1945 (1994)], photon band gap is at microwave region (12-14 GHz).
People have also proposed other laminate structure and have made three-D photon crystal [H. Sozuer and J. Dowling, J. Mod. Opt. 41,231 (1994); S. Fan, P. Villeneuve, R. Meade, and J. Joannoupolis, Appl. Phys. Lett. 65,1466 (1994); M. Wanke, O. Lehmann, K. Muller, Q. Z. Wen, and M. Stuke, Science 275,1284 (1997); S. Y. Lin, J. G. Fleming, D. L. Hetherington, B. K. Smith, R. Biswas, K. M. Ho, M. M. Sigalas, W. Zubrzycki, S. R. Kurtz, and J. Bur, Nature 394,251 (1998)]; The structure that MIT group proposes can utilize ripe semiconductor technology to obtain photonic crystal [the S. Fan of optical range, P. Villeneuve, R. Meade, and J. Joannoupolis, Appl. Phys. Lett. 65,1466 (1994)], making processes is that the first step is first with a layer thickness
dSi be deposited on the substrate with MBE or CVD, then etch each other distance and be
aParallel-groove, in groove, fill at last SiO
2Second step regrowth a layer thickness is
hSi; The 3rd step etched the degree of depth directly over the Si of lower floor be that the d width is the groove of w, and then fill SiO in groove
2The 4th step is identical with the first step; After so repeating to finish, down etch cylindrical air hole array on the surface, the cross section of airport can be circular again, also can be oval, removes at last SiO
2Obtain the Si skeleton structure.
Copper nitride is to have a cube anti-ReO
3The crystalline network semiconductor material, quite stable at room temperature, but the rear elemental copper that resolves into easily of being heated, its thermolysis (2Cu
3N → 6Cu+N
2) temperature (360
oAbout C) lower [Z. Q. Liu, W. J. Wang, T. M. Wang, S. Chao and S. K. Zheng, Thermal stability of copper nitride films prepared by rf magnetron sputtering, Thin Solid Films, 325 (1998) 55-59]; Nitrogenize copper film before the copper film that generates after decomposing and the decomposition is very large in the reflectivity difference of infrared and visible region, is expected to become the candidate materials of optical storage media in the light storage device; The Japan scientist utilizes the laser of (780 nm, 7 mW) to decompose copper nitride film in nineteen ninety, has prepared the two dimensional structure of copper nitride/copper; [M. Asano, K. Umeda, and A. Tasaki, Cu
3N Thin film for a new light recording media, Jpn. J. Appl. Phys., 29,1985 (1990)]; Calendar year 2001, the Japan scientist utilizes magnetically controlled sputter method to prepare copper nitride film, and use the beam bombardment copper nitride film, in copper nitride, form respectively copper quantum dot [the Toshikazu Nosaka of 3 μ m * 3 μ m and 1 μ m * 1 μ m, a, Masaaki Yoshitakea, Akio Okamotoa, Soichi Ogawaa and Yoshikazu Nakayama, Thermal decomposition of copper nitride thin films and dots formation by electron beam writing, Applied Surface Science, 169-170 (2001) 358-361].
What previous literature was reported is to utilize laser or electron beam partial thermal degradation at the individual layer copper nitride film, form individual layer copper nitride/copper two-dimensional array, the present invention adopts copper nitride and the alternate multilayer film of other nitride (such as titanium nitride and aluminium nitride), utilizes femtosecond laser to make three-D photon crystal.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of new three-D photon crystal namely adopts the method for sputter or Atomic layer deposition method to prepare multilayer film between copper nitride/TiN phase, adopts femtosecond laser scanning at multilayer film, the preparation three-D photon crystal.
The technical solution used in the present invention comprises the steps:
(1) preparation of multilayer film: utilize sputter or technique for atomic layer deposition to prepare between copper nitride and TiN phase
Multilayer film;
(2) preparation of photonic crystal: utilize femtosecond laser scanning to form the periodic structure photonic crystal.
The invention has the beneficial effects as follows:
Utilize copper nitride low-temperature decomposition effect, again in conjunction with multi-layer film structure and femtosecond laser technology, just can form the three-dimensional periodic structure, select such as titanium nitride, regulate and control the thickness of each layer of multilayer film, optical property that can the conveniently regulating and controlling three-D photon crystal; Experimental procedure is simple, good reproducibility.
Realize that technical scheme of the present invention is:
Selecting glass, plastics, silicon chip or ceramic substrate is substrate material.
One, the preparation method of copper nitride and titanium nitride multilayer film
1, sputter deposition
1.1 the sputter of titanium nitride
Adopt direct current or radio-frequency magnetron sputter method depositing titanium nitride film, the target of sputter is 99.999% high-purity titanium target,, before the sputter gas pressure in vacuum is extracted into and is lower than 8.0 * 10 as reactant gases and working gas with 99.99% high pure nitrogen and 99.99% argon gas
-4Pa, total sputtering pressure is at 0.5 ~ 2 Pa, and underlayer temperature is controlled at room temperature-300
oC, nitrogen/argon airshed ratio is at 4 ~ 2:1, and sputtering power is at 30 ~ 100 W, and monolayer deposition thickness is at 30 ~ 100 nm;
1.2 the sputter of copper nitride
Adopt direct current or magnetron sputtering method or radio-frequency magnetron sputter method cvd nitride copper film at titanium nitride membrane, the target of sputter is 99.999% high-purity copper target,, before the sputter gas pressure in vacuum is extracted into and is lower than 8.0 * 10 as reactant gases and working gas with 99.99% high pure nitrogen and 99.99% argon gas
-4Pa, total sputtering pressure is at 0.5 ~ 2 Pa, and underlayer temperature is controlled at room temperature-300
oC, nitrogen/argon gas ratio is at 10 ~ 1:1, and sputtering power is at 30 ~ 100 W, and monolayer deposition thickness is at 30 ~ 100 nm;
1.3 alternating deposit forms alternate copper nitride and titanium nitride multilayer film.
2, Atomic layer deposition method
2.1 the deposition of titanium nitride
With tetramethoxy titanium (Ti (OCH
3)
3) as the titanium source, prepare nitrogenize with 99.99% high pure nitrogen as nitrogenous source
The titanium film, temperature of reaction is controlled at 180 ~ 300
OC, monolayer deposition thickness is at 30 ~ 100 nm;
2.2 the deposition of copper nitride
On titanium nitride membrane with hexafluoroacetylacetone acid copper (Cu (hfac)
2) as the copper source, prepare Cu with 99.99% high pure nitrogen as nitrogenous source
3The N film, temperature of reaction is controlled at 180 ~ 300
OC, monolayer deposition thickness is at 30 ~ 100 nm;
2.3 alternating deposit forms alternate copper nitride and titanium nitride multilayer film.
Two, the preparation method of copper nitride/titanium nitride three-D photon crystal
Utilize femtosecond laser processing copper nitride/titanium nitride multilayer film, preparation 3 D stereo optical memory: laser apparatus output center wavelength 808 nm, pulse width 30 ~ 100 femtoseconds, repetition rate 10Hz ~ 10kHz; It is burnt that Output of laser is regulated single pulse energy 0.01 ~ 1 milli by attenuator, the micro-nano focusing system arrives the multilayer film lower end to laser focusing, spot diameter was 0.1 ~ 2 micron after light beam focused on, sample is fixed on the XY plane by computer-controlled three-dimensional precise mobile platform, the computer control sample table moves along X and Y-direction, forms the 3 D stereo optical memory by femtosecond laser scanning like this.
(1) at first femtosecond laser is focused on multilayer film and 20 ~ 100nm below the substrate junction, hot spot is positioned at the lower left corner of multilayer film;
(2) computer control sample table moves right along X-direction, and rate travel 0.1 ~ 10mm/s carries out directions X scanning;
(3) directions X moves after the delegation, and the computer control sample table moves forward 0.1 ~ 1.5 μ m along Y-direction, repeats directions X scanning;
(4) repeating step 2 and 3 is until the end of scan.
Description of drawings
Fig. 1 is the copper nitride XRD figure of utilizing the sputtering method preparation among the embodiment 1 in glass substrate;
Fig. 2 is the section S EM figure of multilayer film among the embodiment 1;
Fig. 3 is the dot matrix SEM figure that forms after laser processing among the embodiment 1.
Embodiment
Embodiment 1
Utilize sputtering method and femtosecond laser technology to prepare the 3 D stereo optical memory in glass substrate:
1, the sputtering sedimentation of multilayer film
1.1 utilize d.c. sputtering method depositing titanium nitride film
The chamber base vacuum is 1 * 10
-4Pa, the throughput ratio of argon gas and nitrogen is 3:1, sputtering pressure is 0.8Pa,
Sputtering power 80W, depositing temperature are 100 ℃, deposition 30nm thick film.
1.2 utilize dc magnetron sputtering method cvd nitride copper film
The chamber base vacuum is 1 * 10
-4Pa,, the throughput ratio of argon gas and nitrogen is 1:10, sputtering pressure is 1Pa,
Sputtering power 60W, depositing temperature are 100 ℃, deposition 30nm thick film.
1.3 alternating deposit 10 times forms copper nitride/titanium nitride multilayer film.
2, femtosecond laser scanning
Utilize femtosecond laser processing copper nitride/titanium nitride multilayer film, preparation 3 D stereo optical memory; Sample size is 5 μ m * 5 μ m, and laser apparatus output center wavelength 808nm, pulse width 80fs, repetition rate 1kHz, Output of laser focus on rear spot diameter 0.1 μ m by attenuator regulating impulse energy 0.02 mJ.
(1) at first femtosecond laser is focused on multilayer film and 50 nm places below the substrate junction, hot spot is positioned at the lower left corner of multilayer film;
(2) computer control sample table moves along X-direction, and rate travel 0.25 mm/s carries out directions X scanning;
(3) directions X moves after the delegation, and the computer control sample table moves 0.25 μ m along Y-direction, repeats directions X scanning;
(4) repeating step 2 and 3 is until the end of scan.
Adopt transmission spectrum absorbance spectrum instrument that the photonic crystal of the present invention's preparation is measured at visible light and near-infrared band respectively, experimental result finds do not have obvious transmission band near the visible light, and be that a very strong transmission band has appearred in 1052 nm places at wavelength, the transmission spectrum of test shows that the bandgap center wavelength of photonic crystal is 1052nm.
Embodiment 2
Utilize technique for atomic layer deposition and femtosecond laser technology to prepare the 3 D stereo optical memory at silicon chip:
1, the ald of multilayer film
1.1 the deposition of titanium nitride
With tetramethoxy titanium (Ti (OCH
3)
3) as the titanium source, prepare nitrogenize with 99.99% high pure nitrogen as nitrogenous source
Titanium film, temperature of reaction are controlled at 180 ℃, and monolayer deposition thickness is at 50 nm;
1.2 the deposition of copper nitride
On titanium nitride membrane with hexafluoroacetylacetone acid copper (Cu (hfac)
2) as the copper source, preparing copper nitride film with 99.99% high pure nitrogen as nitrogenous source, temperature of reaction is controlled at 200
OC, monolayer deposition thickness is at 60 nm;
1.3 alternating deposit 15 times forms alternate copper nitride and titanium nitride multilayer film.
2, the preparation method of copper nitride/titanium nitride three-D photon crystal
Utilize femtosecond laser processing copper nitride/titanium nitride multilayer film, preparation 3 D stereo optical memory; Sample size is 5 μ m * 5 μ m, laser apparatus output center wavelength 808 nm, pulse width 40 femtoseconds, repetition rate 100Hz; It is burnt that Output of laser is regulated single pulse energy 0.1 milli by attenuator, and to the multilayer film lower end, spot diameter was 1 micron after light beam focused on laser focusing for the micro-nano focusing system.
(1) at first femtosecond laser is focused on multilayer film and 50 nm places below the substrate junction, hot spot is positioned at the lower left corner of multilayer film;
(2) computer control sample table moves right along X-direction, and rate travel 1mm/s carries out directions X scanning;
(3) directions X moves after the delegation, and the computer control sample table moves forward 0.6 μ m along Y-direction, repeats directions X scanning;
(4) repeating step 2 and 3 is until the end of scan.
Adopt transmission spectrum absorbance spectrum instrument that the photonic crystal of the present invention's preparation is measured at visible light and near-infrared band respectively, the transmission spectrum of test shows that the bandgap center wavelength of photonic crystal is 1531nm.
Embodiment 3
With embodiment 1, during the depositing titanium nitride film, the throughput ratio of argon gas and nitrogen is 4:1, and sputtering pressure is 2Pa,
Sputtering power 40W, depositing temperature are 250 ℃, deposition 80nm thick film; During cvd nitride copper film, the throughput ratio of argon gas and nitrogen is 1:2, and sputtering pressure is 2Pa, and sputtering power 90W, depositing temperature are 200 ℃, deposition 60nm thick film; During femtosecond laser scanning, laser pulse width 100fs, repetition rate 8kHz, Output of laser is by attenuator regulating impulse energy 0.5 mJ, spot diameter 2 μ m after focusing on, femtosecond laser is focused on the following 100nm of multilayer film and substrate junction place, sample table rate travel 5 mm/s, the computer control sample table moves forward 1.5 μ m along Y-direction.
Adopt transmission spectrum absorbance spectrum instrument that the photonic crystal of the present invention's preparation is measured at visible light and near-infrared band respectively, the transmission spectrum of test shows that the bandgap center wavelength of photonic crystal is 1123 nm.
Embodiment 4
With embodiment 2, during the titanium nitride membrane deposition, temperature of reaction is controlled at 300 ℃, and monolayer deposition thickness is at 80 nm; During the copper nitride film deposition, temperature of reaction is controlled at 300 ℃, and monolayer deposition thickness is at 100nm; Utilize femtosecond laser processing copper nitride/titanium nitride multilayer film, laser pulse width 70 femtoseconds, repetition rate 500Hz; It is burnt that Output of laser is regulated single pulse energy 1 milli by attenuator, spot diameter was 1 micron after light beam focused on, femtosecond laser is focused on the following 200nm of multilayer film and substrate junction place, sample table rate travel 8mm/s, the computer control sample table moves forward 0.4 μ m along Y-direction.
Adopt transmission spectrum absorbance spectrum instrument that the photonic crystal of the present invention's preparation is measured at visible light and near-infrared band respectively, the transmission spectrum of test shows that the bandgap center wavelength of photonic crystal is 1239nm.
Claims (3)
1. the preparation method of a three-D photon crystal, it is characterized in that: comprise the step of utilizing sputter or technique for atomic layer deposition to prepare the multilayer film between copper nitride and TiN phase and utilize femtosecond laser scanning to form the step of three-D photon crystal, the described step of utilizing femtosecond laser scanning to form three-D photon crystal is specially:
Step 1: at first femtosecond laser is focused on multilayer film and 20 ~ 100nm below the substrate junction, hot spot is positioned at the lower left corner of multilayer film;
Step 2: multilayer film is fixed on the XY plane by computer-controlled three-dimensional precise mobile platform, and the computer control sample table moves right along X-direction, and rate travel 0.1 ~ 10mm/s carries out directions X scanning;
Step 3:X direction moves after the delegation, and the computer control sample table moves forward 0.1 ~ 1.5 μ m along Y-direction, repeats directions X scanning;
Repeating step 2 and 3 is until the end of scan;
Laser apparatus output center wavelength 808 nm, pulse width 30 ~ 100 femtoseconds, repetition rate 10Hz ~ 10kHz; It is burnt that Output of laser is regulated single pulse energy 0.01 ~ 1 milli by attenuator, and spot diameter was 0.1 ~ 2 micron after light beam focused on.
2. the preparation method of a kind of three-D photon crystal as claimed in claim 1, it is characterized in that: the described step of utilizing sputtering technology to prepare the multilayer film between copper nitride and TiN phase is specially:
(1) sputter of titanium nitride
Adopt direct current or radio-frequency magnetron sputter method depositing titanium nitride film, the target of sputter is 99.999% high-purity titanium target,, before the sputter gas pressure in vacuum is extracted into and is lower than 8.0 * 10 as reactant gases and working gas with 99.99% high pure nitrogen and 99.99% argon gas
-4Pa, total sputtering pressure is at 0.5 ~ 2 Pa, and underlayer temperature is controlled at room temperature-300
oC, nitrogen/argon airshed ratio is at 4 ~ 2:1, and sputtering power is at 30 ~ 100W, and monolayer deposition thickness is at 30 ~ 100 nm;
(2) sputter of copper nitride
Adopt direct current or magnetron sputtering method or radio-frequency magnetron sputter method cvd nitride copper film at titanium nitride membrane, the target of sputter is 99.999% high-purity copper target,, before the sputter gas pressure in vacuum is extracted into and is lower than 8.0 * 10 as reactant gases and working gas with 99.99% high pure nitrogen and 99.99% argon gas
-4Pa, total sputtering pressure is at 0.5 ~ 2 Pa, and underlayer temperature is controlled at room temperature-300
oC, nitrogen/argon gas ratio is at 10 ~ 1:1, and sputtering power is at 30 ~ 100 W, and monolayer deposition thickness is at 30 ~ 100 nm;
(3) alternating deposit forms alternate copper nitride and titanium nitride multilayer film.
3. the preparation method of a kind of three-D photon crystal as claimed in claim 1, it is characterized in that: the described step of utilizing technique for atomic layer deposition to prepare the multilayer film between copper nitride and TiN phase is specially:
(1) deposition of titanium nitride
As the titanium source, the high pure nitrogen with 99.99% prepares titanium nitride membrane as nitrogenous source with the tetramethoxy titanium, and temperature of reaction is controlled at 180 ~ 300
oC, monolayer deposition thickness is at 30 ~ 100 nm;
(2) deposition of copper nitride
On titanium nitride membrane with hexafluoroacetylacetone acid copper as the copper source, the high pure nitrogen with 99.99% prepares copper nitride film as nitrogenous source, temperature of reaction is controlled at 180 ~ 300
oC, monolayer deposition thickness is at 30 ~ 100 nm;
(3) alternating deposit forms alternate copper nitride and titanium nitride multilayer film.
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