CN102545060B - Preparation method of micro laser diode array - Google Patents
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Abstract
The invention relates to a preparation method of a micro laser diode array. The preparation method comprises the steps of: spin-coating a layer of p-type polymer semiconductor film on the surface of a P-type gallium nitride (GaN) film, wherein the p-type polymer semiconductor film can be selected from polyvinylcarbazole (PVK), polyfluorene (PF), poly(p-phenylenevinylene) (PPV), poly-3-alkylthiophene (P3HT) and derivatives thereof and other p-type polymer semiconductors; then integrating with a single zinc oxide (ZnO) microrod on the surface of a p-type polymer film to form a heterojunction; plating a transparent conducting film to transparent glass, wherein the transparent conducting film can be selected from indium tin oxide (ITO), zinc aluminum oxide (ZAO) and the like; then plating a layer of gold (Au) electrode at one end of transparent conductive glass; then buckling the transparent conductive glass on the microrod on which the surface is integrated with ZnO; then injecting epoxy ethyl ester to the gap between the transparent conductive glass and p-GaN; and finally, preparing an electrode with ohmic contact on the surface of p-GaN to form an integral device.
Description
Technical field
The present invention's design utilizes Vapor Transport or hydro thermal method to prepare high-quality single crystal ZnO micron bar, isolate single ZnO micron bar and have the p-type gallium nitride of p-type polymer (as: PVK, PF, PPV, P3HT and derivative thereof etc.) film to be combined it and spin coating and form the pn knot, the transparent conducting glass (as: ITO, ZAO etc.) that one end is coated with the Au electrode is buckled on the integrated ZnO micron bar array, then between transparent conducting glass and p-type GaN, pour epoxy ethyl ester, the structure of annealed immobilising device.The electrode that has ohmic contact in the preparation of GaN one end surfaces at last, the device of complete.The luminous micro laser array that said method obtains can obtain the high-quality little laser emission of ultraviolet electric pump echo wall die.
Background technology
Since Japanese scientist and American scientist had been found ultraviolet radiation in ZnO film and the nano wire in succession, ZnO became the ideal material of design ultraviolet laser.Ultraviolet excitation mode in the ZnO micro nano structure can be divided into three kinds: Random Laser, Fabry-Perot laser,, echo wall die laser.In Random Laser, coherent feedback is by the spontaneous formation of backhaul scattering, it results from the disorder distribution nano particle usually, in the nanostructure of polycrystal film and other pattern, the condition that laser produces is that the size of scattering object approaches or less than wavelength, the path of the transmission of laser is in the gap of nanostructure rather than inside, positive feedback mechanism can be explained with Anderson localization theory: when light is propagated in Disordered Media, when if the mean free path of scattered photon in medium is less than or equal to wavelength, light may produce the backhaul scattering, thereby forms a closed annular light path.If light along the gain in the loop communication process greater than loss, and move all phase places and change into
Integral multiple, just may form oscillating laser.Because the crystal boundaries scattering is serious, so the optical loss in the Random Laser light path is large, and lasing threshold is very high at random usually, and excitation mode is unfixing.F-P type laser is by certain nanostructure with parallel crystal face, produces such as nano wire, nanometer rods and nano thin-film etc., and two parallel crystal faces must be comparatively ideal planes.Its operation principle is similar to traditional F-P chamber type laser, and two parallel surfaces are equivalent to two chamber mirrors, yet reflectivity is lower at the interface owing to the ZnO two ends, so the threshold value of F-P module lasing is also higher.Echo Wall module lasing utilize light path in ZnO hexagon micron bar in constantly total reflection form, optical total-reflection can effectively be strapped in light in the cavity, so optical loss and faint, so the laser emission that ZnO echo wall die micron bar can be exported high-quality-factor and low threshold value.
At present, the ultraviolet of above-mentioned three kinds of pattern ZnO swashs to penetrate at optical pumping and can realize that people have all adopted pulse laser pumping ZnO micro nano structure so that population is reversed so that optical gain greater than optical loss with formation laser emission.Existing research work has begun to put forth effort on development ZnO electroluminescence.Because people are difficult to obtain stable p-type ZnO material.Therefore the researcher forms the pn knot at p-type silicon or p-type GaN superficial growth ZnO film usually, and this film pn knot can only form Random Laser at the most owing to lack suitable cavity body structure, existing a plurality of seminars report.ZnO micron bar monocrystalline has the hexagonal Wurzite structure, and a desirable laser cavity configuration is provided, and the Whispering-gallery-mode of formation has lower laser threshold, fixing zlasing mode and outbound course.The preparation of the echo wall die microcavity laser diode of N-shaped ZnO micron bar/ZnO resilient coating/p-type GaN structure has been reported.But this kind structure is because the middle technique that relates to ion beam etching and use the mask plate plated electrode causes the manufacture craft more complicated, and in the course of processing easily with the micron bar shift position, even destroy ZnO monocrystalline micron bar, be unfavorable for industrialization.
Based on the problems referred to above, here we have proposed a kind of new structure n-ZnO micron bar/film/p-GaN of p-type polymer semiconductor, single ZnO micron bar is integrated in spin coating has the p-GaN surface conjunction of p-type thin polymer film to form the pn knot, the p-type polymer buffer layer that adds links together upper strata ZnO micron bar and the p-GaN of lower floor effectively, guaranteed good electricity contact, improved the total reflection condition in the micron bar cavity, loss is reduced, gain improves.Transparent conducting glass (as: ITO, ZAO) etc. directly covers on integrated ZnO micron bar, has avoided the technique of etching more complicated, has reached again good electricity contact simultaneously.Pour epoxy ethyl ester between transparent conducting glass and p-GaN, the internal structure of immobilising device makes device stable, and increase useful life.
Summary of the invention
Technical problem:The preparation method who the purpose of this invention is to provide a kind of little diode laser matrix.Its laser output wavelength is regulated by regulating ZnO micron bar diameter.
Technical scheme:In the present invention, utilize Vapor Transport or hydro thermal method making ZnO micron bar array, choose single ZnO micron bar and it is combined with the p-type GaN of spin coating p-type polymer (as: PVK, PF, PPV, P3HT and derivative thereof etc.) film and forms pn and tie, next the transparent conducting glass (as: ITO, ZAO etc.) that an end is coated with the Au electrode is buckled in above the p-GaN that the surface is integrated with the ZnO micron bar, then injection ring 2-ethoxyethyl acetate between transparent conducting glass and p-GaN is by annealing immobilising device internal structure.The electrode that has ohmic contact in the preparation of p-GaN surface at last finally obtains N-shaped ZnO micron bar/p-type polymer/p-GaN micro laser array.
The present invention is by the following technical solutions:
The first step: purity is 99.99% ZnO powder and carbon dust according to mass ratio 1:1 mixed grinding, gets
0.3～0.5Restraining this mixture inserts in the ceramic boat.The silicon chip that will approach with ceramic boat aperture area size is done with the nitrogen punching behind acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning, and silicon wafer polishing is faced down covers the ceramic boat top.Subsequently ceramic boat being pushed temperature is
1000～1200 ° of CTube furnace in.Process
30～60Minute the reaction, ZnO micron bar array grows in silicon chip surface (seeing accompanying drawing 1), the crystal structure of single ZnO micron bar is hexagonal Wurzite structure (seeing accompanying drawing 2).Also can adopt hydro thermal method making ZnO micron bar array.
Second step: with the p-type gallium nitride of 2 centimetres of sizes of 1 cm x through acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning after, dry up preparation with nitrogen
0.1～0.4Mg/mL p-type polymer (as: PVK, PF, PPV, P3HT and derivative thereof etc.) chloroformic solution is spun on the sample surfaces for preparing with it.Spin speed accelerates to the setting rotating speed by inactive state within 2 seconds
2000～4000Rev/min, keep subsequently this rotating speed
15～25In second, form thickness approximately
20～30The p-type thin polymer film of nanometer.
The 3rd step: from ZnO micron bar array, select single ZnO micron bar, it is kept flat be integrated into p-type thin polymer film surface.This layer film has been joined together to form pn knot (seeing accompanying drawing 3a) effectively with upper strata ZnO micron bar and the p-type GaN of lower floor.
The 4th step: behind 2 centimetres of big or small transparent conducting glass of 1 cm x (as: ITO, ZAO etc.) process acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning, dry up with nitrogen, utilize electron beam evaporation plating, plate at the one end surfaces
20～30Nanometer thickness Au electrode.
The 5th step: transparent conducting glass is buckled in keeps flat the upper of integrated good ZnO micron bar, then between transparent conducting glass and p-type GaN, inject epoxy second fat, compress annealing about one hour, annealing temperature
120～150Degree centigrade (seeing accompanying drawing 3b).
The 6th step: with chloroform or acetone solvent the p-type thin polymer film on the end of p-type GaN is washed off, then utilized electron beam evaporation plating, plate two-layer electrode, form the Ni/Au electrode (seeing accompanying drawing 3c) of 30～40 nano thickness.
The 7th step: the pn junction device that makes is carried out electrical properties measure, and measure the electric pump laser spectroscopy.
Beneficial effect:Compared with prior art, the present invention has the following advantages:
1, the present invention utilizes the smooth monocrystalline micron ZnO micron bar in border to form the Echo Wall microcavity of nature, and the p-type thin polymer film has improved the total reflection condition in the microcavity as resilient coating simultaneously, makes its optical loss little, and gain improves, and more is conducive to the formation of little laser.
2, the present invention adopts transparent conducting glass (as: ITO, ZAO etc.) to cover on integrated ZnO micron bar, has evaded the complicated technology of ion beam etching, mask plated electrode, has greatly simplified technical process, is conducive to industrialization.
3, the package curing of the present invention by injection ring 2-ethoxyethyl acetate annealing the internal structure of device, it is stable, firm to be conducive to device, has improved useful life.
4, the ZnO micron bar diameter of the present invention preparation is adjustable, so the zlasing mode of micro laser and wavelength are adjustable, have more practical value.
Description of drawings
Fig. 1 gas phase transmission is sent out the ZnO micron bar array of preparation.
The single ZnO micron bar of Fig. 2 SEM figure.
Fig. 3 (a-c) transparent conducting glass/N-shaped ZnO micron bar/little laser two of PVK polymer/p-type GaN
Utmost point pipe array prepares schematic diagram.
The little diode laser matrix preparation of Fig. 4 (a-c) ITO/n type ZnO micron bar/PVK/p type GaN signal
Figure.
Fig. 5 ITO/n type ZnO micron bar/little diode laser matrix electric pump of PVK/p type GaN spectrum.
Embodiment(take the ZnO micron bar of preparation cavity diameter as 14 microns, ITO/n-ZnO micron bar/little diode laser matrix of PVK film/p-GaN is example)
The first step: purity is 99.99% ZnO powder and carbon dust according to mass ratio 1:1 mixed grinding, gets 0.5 this mixture of gram and insert in the ceramic boat.The silicon chip of 3 centimetres of 2 cm x behind acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning, is done with the nitrogen punching, and silicon wafer polishing is faced down to be covered and the ceramic boat top.Ceramic boat is pushed in the tube furnace that temperature is 1150 ° of C subsequently.Through reaction in 40 minutes, ZnO micron bar array grew in silicon chip surface (seeing accompanying drawing 1), and the crystal structure of single ZnO micron bar is hexagonal Wurzite structure (seeing accompanying drawing 2).
Second step: with the p-GaN of 2 centimetres of 1 cm x through acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning after, dry up with nitrogen, prepare 0.1 mg/mL PVK chloroformic solution, it is spun on p-type GaN surface.Spin speed is accelerated to by inactive state within 2 seconds and sets 2900 rev/mins of rotating speeds, keeps subsequently 20 seconds of this rotating speed, forms the PVK film of about 20 nanometers of thickness.
The 3rd step: from ZnO micron bar array, select single ZnO micron bar, it is kept flat be integrated into the PVK film surface.This layer film has been joined together to form the pn knot effectively with upper strata ZnO micron bar and the p-GaN of lower floor.(seeing accompanying drawing 4a)
The 4th step: with the ITO transparent conducting glass of 2 centimetres of 1 cm x through acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning after, dry up with nitrogen, a surperficial end plates the thick Au electrode of 30nm.
The 5th step:, the ITO transparent conducting glass is buckled on the p-GaN substrate of integrated good ZnO micron bar, then with injecting epoxy second fat, compress annealing one hour, 150 degrees centigrade of annealing temperatures (seeing accompanying drawing 4b).
The 6th step: with chloroform or acetone organic solvent the PVK film of p-GaN one end is washed off, then utilized electron beam evaporation plating, show the two-layer electrode of preparation at p-GaN, obtaining thickness is the Ni/Au electrode (seeing accompanying drawing 4c) of 30 nanometers.
The 7th step: the pn junction device that makes is carried out electrical properties measure, and measure electric pump laser spectroscopy (seeing accompanying drawing 5).
Claims (3)
1. the preparation method of a little diode laser matrix is characterized in that this little diode laser matrix is N-shaped ZnO micron bar/p-type polymer/little diode laser matrix of p-type GaN, and this preparation method is:
The first step: purity is 99.99% ZnO end and carbon dust according to mass ratio 1:1 mixed grinding, gets an amount of mixture and insert in the ceramic boat; The silicon chip that will approach with ceramic boat aperture area size is done with the nitrogen punching behind acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning, and silicon wafer polishing is faced down to be covered and the ceramic boat top; Subsequently ceramic boat is pushed in the tube furnace that temperature is 1000～1200 ° of C, through reaction in 30～60 minutes, ZnO micron bar array grew in silicon chip surface;
Second step: behind p-GaN substrate process acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning, dry up with nitrogen, the chloroformic solution of preparation 0.1～0.4mg/mL p-type semi-conducting polymer, it is spun on the p-GaN surface, spin speed accelerates to 2000～4000 rev/mins of setting rotating speeds by inactive state within 2 seconds, keep subsequently 15～25 seconds of this rotating speed, forming thickness is the p-type thin polymer film of 20～30 nanometers;
The 3rd step: select single ZnO micron bar from ZnO micron bar array, it is kept flat be integrated into p-type thin polymer film surface, this layer p-type thin polymer film has been joined together to form the pn knot effectively with upper strata ZnO micron bar and the p-GaN of lower floor;
The 4th step: transparent conducting glass is behind acetone, absolute ethyl alcohol and deionized water successively ultrasonic cleaning, do with the nitrogen punching, utilize electron beam evaporation plating, plate 20～30 nanometer thickness Au electrodes at its surperficial end, form good ohmic contact, to guarantee the carrier injection of high concentration;
The 5th step: transparent conducting glass is buckled on the integrated good ZnO micron bar array, then injects transparent epoxy second fat between transparent conducting glass and p-GaN, compress annealing, annealing temperature is 120～150 degrees centigrade;
The 6th step: with chloroform or acetone the p-type thin polymer film on the end of p-GaN is washed off, then utilized electron beam evaporation plating, plate two-layer electrode, form the Ni/Au electrode of 30～40 nano thickness; Form at last N-shaped ZnO micron bar/PVK polymer/little diode laser matrix of p-type GaN heterojunction;
The 7th step: last N-shaped ZnO micron bar/PVK polymer/little diode laser matrix of p-type GaN heterojunction that forms of the 6th step is carried out the electrical properties measurement, and measure the electric pump laser spectroscopy.
2. the preparation method of little diode laser matrix according to claim 1 is characterized in that described p-type semi-conducting polymer is: Polyvinyl carbazole PVK, poly-fluorenes PF, poly-to styrene support PPV or poly--3 alkylthrophene P3HT and derivatives thereof.
3. the preparation method of little diode laser matrix according to claim 1 is characterized in that described transparent conducting glass is tin indium oxide ITO, oxygen zinc-aluminium ZAO.
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