CN102358936A - Preparation method of photonic crystal multilayer film - Google Patents
Preparation method of photonic crystal multilayer film Download PDFInfo
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- CN102358936A CN102358936A CN2011102828198A CN201110282819A CN102358936A CN 102358936 A CN102358936 A CN 102358936A CN 2011102828198 A CN2011102828198 A CN 2011102828198A CN 201110282819 A CN201110282819 A CN 201110282819A CN 102358936 A CN102358936 A CN 102358936A
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Abstract
The invention relates to a preparation method of a photonic crystal multilayer film. Aiming at application state of the photonic crystal to optical materials, an electrically conductive glass is used as a substrate, and titanium oxide and copper are used as films; TiO2 films and Cu films are sputtered on the substrate through magnetron sputtering; the TiO2 film and the Cu film alternatively arranged form a 14-layer multilayer film structure; then the multilayer film are treated with low temperature tempering to increase physical properties and mechanical properties of the multilayer film. The preparation method employs an advanced and rigorous technology with detailed and accurate technical parameters; the product has good quality, high purity and good optical performance; therefore, provided is an ideal preparation method of the photonic crystal multilayer film.
Description
Technical field
The present invention relates to a kind of preparation method of photon crystal multi-layer film, belong to the preparation of optical material and the technical field of application.
Background technology
Photonic crystal is a kind of new optical material that occurs in recent years, is by two kinds of different artificial crystal materials that the material periodic arrangement constitutes of dielectric parameter; Be since the sub-semiconductor material of relay is used, to be hopeful to open up the novel material in electronic information epoch most.
Photonic crystal is with the principal character that exists for of forbidden photon band and photon local, and its characteristic makes photonic crystal be applied in integrated, light interconnection, the optical communication field of low-light electron device.
The bandgap structure of photonic crystal is most important characteristic, also is the basis of photonic crystal applications exploitation, and the forbidden band self-energy loss of the photonic crystal of assembly of thin films structure is lower, but energy gap is limited, and the total-angle high-reflection that broad occurs is penetrated very difficult; And metallic substance is compared with this type photonic crystal, though in wide range of frequency, having very strong reflectivity under the incident direction arbitrarily, absorption has caused bigger power loss; Because there is serious absorption in most materials being lower than visible light wave range, studies less; But, become important research project owing to there is the potential application prospect.
Magnetron sputtering technique is one of important film deposition techniques, has obtained application in electronics, electric, optics, semi-conductor, aviation, system mirror, artistic pottery and porcelain, Handicraft decorative field, photon crystal multi-layer film magnetron sputtering technique preparation also capable of using.
Summary of the invention
Goal of the invention
The objective of the invention is situation to background technology; Adopt magnetically controlled DC sputtering, radiofrequency magnetron sputtering technology; Splash-proofing sputtering metal, ceramic multilayer film on conductive glass; With optical property, the mechanical property that increases substantially photon crystal multi-layer film, make photon crystal multi-layer film be able in the high-performance optical electronic product, use.
Technical scheme
The chemical substance material that the present invention uses is: titanium oxide target, copper target, acetone, absolute ethyl alcohol, deionized water, argon gas, its combination consumption is following: with millimeter, milliliter, centimetre
3Be measure unit
Photon crystal multi-layer film is 14 layers of structure, is made up of basic unit, titanium oxide layer, copper layer, titanium oxide layer, and the I layer is a basic unit, i.e. conductive glass ITO layer, and the II layer is a titanium oxide layer; The III layer is the copper layer, and the IV layer is a titanium oxide layer, and the V layer is the copper layer, and the VI layer is a titanium oxide layer; The VII layer is the copper layer, and the VIII layer is a titanium oxide layer, and IX is the copper layer, and X is a titanium oxide layer; The XI layer is the copper layer, and the XII layer is a titanium oxide layer, and the XIII layer is the copper layer, and the XIV layer is a titanium oxide layer.
The preparation method is following:
(1) the chemical substance material that preparation is needed will carry out selected, and carries out quality purity control:
(2) clean the conductive glass substrate
1. the conductive glass substrate is vertically placed ultrasonic cleaner, add acetone 100mL, carry out ultrasonic cleaning, time 20min dries after the cleaning;
2. the conductive glass substrate is placed another ultrasonic cleaner, add absolute ethyl alcohol 100mL and carry out ultrasonic cleaning, time 20min dries then;
3. conductive glass is placed another ultrasonic cleaning machine, carry out supersound washing with deionized water 200mL, time 20min dries after the washing;
(3) drying
Conductive glass substrate after cleaning is placed quartz boat, places vacuum drying oven dry then, 50 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying 30min, input protection gas argon gas when dry;
(4) magnetron sputtering prepares photon crystal multi-layer film
The preparation of photon crystal multi-layer film is carried out in the magnetron sputtering stove, vacuumize, argon shield, magnetically controlled DC sputtering, rf magnetron sputtering, outer water cycle cooling completion down;
1. put the conductive glass substrate
Open the magnetron sputtering stove, place on the worktable conductive glass is straight, face up;
2. open outer water circulation cooling device, carry out outer water cycle cooling;
3. extract furnace air
Close the magnetron sputtering stove, the open vacuum pump extracts furnace air, and making the interior pressure of stove is 0.0008Pa;
4. regulate operating air pressure in the stove
Open argon bottle, argon gas valve, in stove, import argon gas, argon gas input speed 30cm
3/ min makes the interior invariablenes pressure of liquid of stove at 6.0Pa;
5. open the worktable rotary electric machine, make at the uniform velocity both forward and reverse directions rotation of worktable, velocity of rotation 5r/min, and carry out the both forward and reverse directions conversion, the both forward and reverse directions conversion interval time is 3min;
6. open the rf magnetron sputtering modulator, make the conductive glass on the titanium oxide target alignment work platform, carry out rf magnetron sputtering; Sputtering power 100W, radio-frequency voltage 80V, RFC 0.15A; Sputter rate 0.67nm/min, sputtering time 120min, sputtered layer thickness 80nm; Be titanium oxide layer, i.e. the II layer;
7. open the magnetically controlled DC sputtering modulator, make the conductive glass on the copper target alignment work platform, carry out sputter, sputtering power 10W; Volts DS 300V, galvanic current 0.036A, sputter rate 7.7nm/min, sputtering time 4.5min; Sputtered layer thickness 30nm is copper layer, i.e. III layer;
8. open the rf magnetron sputtering modulator, make the conductive glass on the titanium oxide target alignment work platform, carry out rf magnetron sputtering; Sputtering power 100W, radio-frequency voltage 80V, RFC 0.15A; Sputter rate 0.67nm/min, sputtering time 120min, sputtered layer thickness 80nm; Be titanium oxide layer, i.e. the IV layer;
9. open the magnetically controlled DC sputtering modulator, make the conductive glass on the copper target alignment work platform, carry out sputter, sputtering power 10W; Volts DS 300V, galvanic current 0.036A, sputter rate 7.7nm/min, sputtering time 4.5min; Sputtered layer thickness 30nm is copper layer, i.e. V layer;
10. open the rf magnetron sputtering modulator, make the conductive glass on the titanium oxide target alignment work platform, carry out rf magnetron sputtering; Sputtering power 100W, radio-frequency voltage 80V, RFC 0.15A; Sputter rate 0.67nm/min, sputtering time 120min, sputtered layer thickness 80nm; Be titanium oxide layer, i.e. the VI layer;
opens the magnetically controlled DC sputtering modulator, makes the conductive glass on the copper target alignment work platform, carries out sputter; Sputtering power 10W; Volts DS 300V, galvanic current 0.036A, sputter rate 7.7nm/min; Sputtering time 4.5min; Sputtered layer thickness 30nm is copper layer, i.e. XI layer;
opens the rf magnetron sputtering modulator, makes the conductive glass on the titanium oxide target alignment work platform, carries out rf magnetron sputtering; Sputtering power 100W; Radio-frequency voltage 80V, RFC 0.15A, sputter rate 0.67nm/min; Sputtering time 120min; Sputtered layer thickness 80nm is titanium oxide layer, i.e. the XIV layer;
After
sputter is accomplished; Close the sputter modulator; Close the worktable motor; Make product under argon shield and outer water cycle are cooled off, cool to 25 ℃ with the furnace;
Open the magnetron sputtering stove, take out conductive glass, i.e. conductive glass photon crystal multi-layer film;
(5) vacuum and low temperature tempering
The conductive glass photon crystal multi-layer film is placed quartzy product boat, place the low-temperaturetempering stove then, carry out low-temperaturetempering, 200 ℃ of tempering temperatures, vacuum tightness 1.3Pa, tempering time 60min;
Take out after the low-temperaturetempering, be end product: photon crystal multi-layer film;
(6) detect, analyze, characterize
Pattern, thicknesses of layers, composition, the optical property of photon crystal multi-layer film product of preparation carried out check and analysis to be characterized;
With field emission scanning electron microscope SEM photon crystal multi-layer film being carried out pattern characterizes;
With ultraviolet-visible spectrophotometer the optical property of photon crystal multi-layer film is tested;
With X ray small-angle diffraction appearance the crystalline structure of photon crystal multi-layer film is tested;
Conclusion: photon crystal multi-layer film is a laminate structure, and thicknesses of layers is a nano level, and the reflectivity of multilayer film band gap at the 300-350nm place reaches more than 85%, and multi-layer film structure is titanium oxide and copper;
(7) store
Photon crystal multi-layer film is stored in the brown transparent Glass Containers, airtight keeping in Dark Place, and place cleaning, shady and cool dry place, moistureproof, sun-proof, acid-proof alkali salt erosion, 25 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has tangible advance, is to the applicable cases of photonic crystal in optical material, adopts conductive glass to cook substrate; Do rete with titanium oxide, copper,, on substrate, repeat sputter titanium oxide layer, copper layer through magnetron sputtering; Form multi-layer film structure, then multilayer film is carried out low-temperaturetempering, improve the chemical physics performance and the mechanical property of multilayer film; This preparing method's technology is advanced, tight, and technical parameter is accurately full and accurate, good product quality; Having good optical property, is the preparation method of very good photon crystal multi-layer film.
Description of drawings
Fig. 1 is the state graph of photon crystal multi-layer film magnetron sputtering
Fig. 2 is the photon crystal multi-layer film structure iron
Fig. 3 photon crystal multi-layer film cross-sectional scans Electronic Speculum structure iron
Fig. 4 is a photon crystal multi-layer film uv drs collection of illustrative plates
Fig. 5 is a photon crystal multi-layer film X-ray diffraction intensity collection of illustrative plates
Shown in the figure, list of numerals is following:
1, magnetron sputtering stove, 2, the stove seat, 3, bell, 4, image display, 5, PL, 6, power switch; 7, titanium oxide target source modulator, 8, copper target source modulator, 9, vacuum pump switch, 10, furnace chamber, 11, left viewing window, 12 right viewing windows 13, escape pipe; 14, worktable, 15, titanium oxide radio frequency target, 16, the titanium oxide target, 17, copper d.c. sputtering target, 18, the copper target; 19, argon bottle, 20, the argon gas valve, 21, tunger tube, 22, argon gas, 23, vacuum pump; 24, vacuum valve, 25, valve tube, 26, conductive glass, 27, photon crystal multi-layer film, 28, the water-cooled case; 29, water-cooled pump, 30, water cooling tube, 31, rotary electric machine, 32, the worktable rotating switch, 33, the water-cooled switch.
I, conductive glass, II, titanium oxide layer, III, copper layer, IV, titanium oxide layer, V, copper layer; VI, titanium oxide layer, VII, copper layer, VIII, titanium oxide layer, IX, copper layer, X, titanium oxide layer; XI, copper layer, XII, titanium oxide layer, XIII, copper layer, XIV, titanium oxide layer.
Embodiment
Below in conjunction with accompanying drawing the present invention is described further:
Shown in Figure 1, be the state graph of photon crystal multi-layer film magnetron sputtering, each location, connecting relation want correct, according to quantity proportioning, operation according to the order of sequence.
The value of the chemical substance material that preparation is used is to confirm by the scope that is provided with in advance, with millimeter, milliliter, centimetre
3Be measure unit.
The preparation of photon crystal multi-layer film is carried out in the magnetron sputtering stove; The bottom of magnetron sputtering stove 1 is a stove seat 2, on the anterior control panel of stove seat 2, is provided with image display 4, PL 5, power switch 6, titanium oxide target source modulator 7, copper target source modulator 8, vacuum pump switch 9, worktable rotating switch 32, water-cooled switch 33; The top of magnetron sputtering stove 1 is bell 3, on bell 3, is provided with escape pipe 13, titanium oxide radio frequency target 15, copper d.c. sputtering target 17, and gos deep into respectively in the furnace chamber 10, and connect titanium oxide target 16, copper target 18 respectively; Bottom in furnace chamber 10 is provided with worktable 14, is rotary electric machine 31 in the worktable 14, and horizontal positioned conductive glass 26 on worktable 14 is photon crystal multi-layer film 27 on conductive glass 26; About the top of magnetron sputtering stove 1, be provided with left viewing window 11, right viewing window 12; Right part at stove seat 2 is provided with vacuum pump 23, and through in vacuum valve 24, the valve tube 25 UNICOM's furnace chambers 10; Left part at stove seat 2 is provided with argon bottle 19, and through in argon gas valve 20, the tunger tube 21 UNICOM's furnace chambers 10, and input argon gas 22; Left outside at magnetron sputtering stove 1 is provided with water-cooled case 28, and carries out outer water cycle cooling through water-cooled pump 29, water cooling tube 30 around the sputter furnace chamber; Titanium oxide radio frequency target 15 is regulated and control by titanium oxide target source modulator; Copper d.c. sputtering target 17 is by 8 regulation and control of copper target source modulator; Water-cooled pump 29 is by 33 controls of water-cooled switch; Vacuum pump 23 is by vacuum pump switch 9 controls; Worktable rotary electric machine 31 is by 32 controls of worktable trip switch.
Shown in Figure 2, be the photon crystal multi-layer film structure iron, amount to 14 layers of structure, the bottom is conductive glass I for basic unit; Basic unit top is titanium oxide layer II, and titanium oxide layer top is copper layer III, and copper layer top is titanium oxide layer IV, and titanium oxide layer top is copper layer V; Copper layer top is titanium oxide layer VI, and titanium oxide layer top is copper layer VII, and copper layer top is titanium oxide layer VIII; Titanium oxide layer top is copper layer IX, and copper layer top is titanium oxide layer X, and titanium oxide layer top is copper layer XI; Copper layer top is titanium oxide layer XII, and titanium oxide layer top is copper layer XIII, and copper layer top is titanium oxide layer XIV.
Shown in Figure 3ly do, photon crystal multi-layer film cross-sectional scans Electronic Speculum structure iron, can be known by figure: each rete combines closely, and what color was shinny is the copper layer, and gray is titanium oxide layer, and film thickness is 800nm.
Shown in Figure 4, be photon crystal multi-layer film uv drs spectrogram, can be known by figure: the film in 4 cycles reached for 88%, 6 cycle in 300-450nm scope internal reflection rate film reaches 92% in 300-450nm scope internal reflection rate.
Shown in Figure 5, be photon crystal multi-layer film X-ray diffraction intensity collection of illustrative plates, can know by figure: can find out that through X-ray diffraction analysis multilayer film has the characteristic peak of titanium oxide and copper, the titanium oxide peak height, the copper peak is low.
Claims (3)
1. the preparation method of a photon crystal multi-layer film, it is characterized in that: the chemical substance material of use is: titanium oxide target, copper target, acetone, absolute ethyl alcohol, deionized water, argon gas, its combination consumption is following: with millimeter, milliliter, centimetre
3Be measure unit
Photon crystal multi-layer film is 14 layers of structure, is made up of basic unit, titanium oxide layer, copper layer, titanium oxide layer, and the I layer is a basic unit, i.e. conductive glass ITO layer, and the II layer is a titanium oxide layer; The III layer is the copper layer, and the IV layer is a titanium oxide layer, and the V layer is the copper layer, and the VI layer is a titanium oxide layer; The VII layer is the copper layer, and the VIII layer is a titanium oxide layer, and IX is the copper layer, and X is a titanium oxide layer; The XI layer is the copper layer, and the XII layer is a titanium oxide layer, and the XIII layer is the copper layer, and the XIV layer is a titanium oxide layer.
The preparation method is following:
(1) the chemical substance material that preparation is needed will carry out selected, and carries out quality purity control:
(2) clean the conductive glass substrate
1. the conductive glass substrate is vertically placed ultrasonic cleaner, add acetone 100mL, carry out ultrasonic cleaning, time 20min dries after the cleaning;
2. the conductive glass substrate is placed another ultrasonic cleaner, add absolute ethyl alcohol 100mL and carry out ultrasonic cleaning, time 20min dries then;
3. conductive glass is placed another ultrasonic cleaning machine, carry out supersound washing with deionized water 200mL, time 20min dries after the washing;
(3) drying
Conductive glass substrate after cleaning is placed quartz boat, places vacuum drying oven dry then, 50 ℃ of drying temperatures, vacuum tightness 18Pa, time of drying 30min, input protection gas argon gas when dry;
(4) magnetron sputtering prepares photon crystal multi-layer film
The preparation of photon crystal multi-layer film is carried out in the magnetron sputtering stove, vacuumize, argon shield, magnetically controlled DC sputtering, rf magnetron sputtering, outer water cycle cooling completion down;
1. put the conductive glass substrate
Open the magnetron sputtering stove, place on the worktable conductive glass is straight, face up;
2. open outer water circulation cooling device, carry out outer water cycle cooling;
3. extract furnace air
Close the magnetron sputtering stove, the open vacuum pump extracts furnace air, and making the interior pressure of stove is 0.0008Pa;
4. regulate operating air pressure in the stove
Open argon bottle, argon gas valve, in stove, import argon gas, argon gas input speed 30cm
3/ min makes the interior invariablenes pressure of liquid of stove at 6.0Pa;
5. open the worktable rotary electric machine, make at the uniform velocity both forward and reverse directions rotation of worktable, velocity of rotation 5r/min, and carry out the both forward and reverse directions conversion, the both forward and reverse directions conversion interval time is 3min;
6. open the rf magnetron sputtering modulator, make the conductive glass on the titanium oxide target alignment work platform, carry out rf magnetron sputtering; Sputtering power 100W, radio-frequency voltage 80V, RFC 0.15A; Sputter rate 0.67nm/min, sputtering time 120min, sputtered layer thickness 80nm; Be titanium oxide layer, i.e. the II layer;
7. open the magnetically controlled DC sputtering modulator, make the conductive glass on the copper target alignment work platform, carry out sputter, sputtering power 10W; Volts DS 300V, galvanic current 0.036A, sputter rate 7.7nm/min, sputtering time 4.5min; Sputtered layer thickness 30nm is copper layer, i.e. III layer;
8. open the rf magnetron sputtering modulator, make the conductive glass on the titanium oxide target alignment work platform, carry out rf magnetron sputtering; Sputtering power 100W, radio-frequency voltage 80V, RFC 0.15A; Sputter rate 0.67nm/min, sputtering time 120min, sputtered layer thickness 80nm; Be titanium oxide layer, i.e. the IV layer;
9. open the magnetically controlled DC sputtering modulator, make the conductive glass on the copper target alignment work platform, carry out sputter, sputtering power 10W; Volts DS 300V, galvanic current 0.036A, sputter rate 7.7nm/min, sputtering time 4.5min; Sputtered layer thickness 30nm is copper layer, i.e. V layer;
10. open the rf magnetron sputtering modulator, make the conductive glass on the titanium oxide target alignment work platform, carry out rf magnetron sputtering; Sputtering power 100W, radio-frequency voltage 80V, RFC 0.15A; Sputter rate 0.67nm/min, sputtering time 120min, sputtered layer thickness 80nm; Be titanium oxide layer, i.e. the VI layer;
After
sputter is accomplished; Close the sputter modulator; Close the worktable motor; Make product under argon shield and outer water cycle are cooled off, cool to 25 ℃ with the furnace;
closes the argon gas valve and stops defeated argon gas, closes outer water circulating cooling pump;
Open the magnetron sputtering stove, take out conductive glass, i.e. conductive glass photon crystal multi-layer film;
(5) vacuum and low temperature tempering
The conductive glass photon crystal multi-layer film is placed quartzy product boat, place the low-temperaturetempering stove then, carry out low-temperaturetempering, 200 ℃ of tempering temperatures, vacuum tightness 1.3Pa, tempering time 60min;
Take out after the low-temperaturetempering, be end product: photon crystal multi-layer film;
(6) detect, analyze, characterize
Pattern, thicknesses of layers, composition, the optical property of photon crystal multi-layer film product of preparation carried out check and analysis to be characterized;
With field emission scanning electron microscope SEM photon crystal multi-layer film being carried out pattern characterizes;
With ultraviolet-visible spectrophotometer the optical property of photon crystal multi-layer film is tested;
With X ray small-angle diffraction appearance the crystalline structure of photon crystal multi-layer film is tested;
Conclusion: photon crystal multi-layer film is a laminate structure, and thicknesses of layers is a nano level, and the reflectivity of multilayer film band gap at the 300-350nm place reaches more than 85%, and multi-layer film structure is titanium oxide and copper;
(7) store
Photon crystal multi-layer film is stored in the brown transparent Glass Containers, airtight keeping in Dark Place, and place cleaning, shady and cool dry place, moistureproof, sun-proof, acid-proof alkali salt erosion, 25 ℃ ± 2 ℃ of storing temps, relative humidity≤10%.
2. the preparation method of a kind of photon crystal multi-layer film according to claim 1; It is characterized in that: the preparation of photon crystal multi-layer film is carried out in the magnetron sputtering stove; The bottom of magnetron sputtering stove (1) is stove seat (2), on the anterior control panel of stove seat (2), is provided with image display (4), PL (5), power switch (6), titanium oxide target source modulator (7), copper target source modulator (8), vacuum pump switch (9), worktable rotating switch (32), water-cooled switch (33); The top of magnetron sputtering stove (1) is bell (3), on bell (3), is provided with escape pipe (13), titanium oxide radio frequency target (15), copper d.c. sputtering target (17), and gos deep into respectively in the furnace chamber (10), and connect titanium oxide target (16), copper target (18) respectively; Bottom in furnace chamber (10) is provided with worktable (14), is rotary electric machine (31) in the worktable (14), goes up horizontal positioned conductive glass (26) at worktable (14), goes up at conductive glass (26) to be photon crystal multi-layer film (27); About the top of magnetron sputtering stove (1), be provided with left viewing window (11), right viewing window (12); Right part at stove seat (2) is provided with vacuum pump (23), and through in vacuum valve (24), valve tube (25) the UNICOM's furnace chamber (10); Left part at stove seat (2) is provided with argon bottle (19), and through in argon gas valve (20), tunger tube (21) the UNICOM's furnace chamber (10), and input argon gas (22); Be provided with water-cooled case (28) in the left outside of magnetron sputtering stove (1), and carry out outer water cycle cooling around the sputter furnace chamber through water-cooled pump (29), water cooling tube (30); Titanium oxide radio frequency target (15) is regulated and control by titanium oxide target source modulator (7); Copper d.c. sputtering target (17) is regulated and control by copper target source modulator (8); Water-cooled pump (29) is controlled by water-cooled switch (33); Vacuum pump (23) is controlled by vacuum pump switch (9); Worktable rotary electric machine (31) is controlled by worktable trip switch (32).
3. the preparation method of a kind of photon crystal multi-layer film according to claim 1, it is characterized in that: photon crystal multi-layer film is 14 tunic layer structure, is made up of basic unit, titanium oxide layer, copper layer, titanium oxide layer; The bottom is conductive glass layer I, and basic unit top is titanium oxide layer II, and titanium oxide layer top is copper layer III; Copper layer top is titanium oxide layer IV, and titanium oxide layer top is copper layer V, and copper layer top is titanium oxide layer VI; Titanium oxide layer top is copper layer VII, and copper layer top is titanium oxide layer VIII, and titanium oxide layer top is copper layer IX; Copper layer top is titanium oxide layer X, and titanium oxide layer top is copper layer XI, and copper layer top is titanium oxide layer XII; Titanium oxide layer top is copper layer XIII, and copper layer top is titanium oxide layer XIV.
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| CN104378083A (en) * | 2014-11-05 | 2015-02-25 | 东晶锐康晶体（成都）有限公司 | Low-cost quartz crystal resonator wafer |
| CN108963724A (en) * | 2018-08-01 | 2018-12-07 | 中国工程物理研究院电子工程研究所 | Dielectric-metal photonic crystal, preparation method and terahertz pulse generator |
| CN109470131A (en) * | 2018-11-05 | 2019-03-15 | 三河市衡岳真空设备有限公司 | The detection method of thickness under vacuum state |
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