CN101948999B - Low-temperature-doped luminescent aluminum nitride thin film and preparation method thereof - Google Patents

Low-temperature-doped luminescent aluminum nitride thin film and preparation method thereof Download PDF

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CN101948999B
CN101948999B CN2010102938564A CN201010293856A CN101948999B CN 101948999 B CN101948999 B CN 101948999B CN 2010102938564 A CN2010102938564 A CN 2010102938564A CN 201010293856 A CN201010293856 A CN 201010293856A CN 101948999 B CN101948999 B CN 101948999B
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target
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CN101948999A (en
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邱万奇
刘仲武
孙歌
余红雅
钟喜春
曾德长
蔡明�
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South China University of Technology SCUT
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Abstract

The invention discloses a low-temperature-doped luminescent aluminum nitride thin film and a preparation method thereof. The method comprises the following steps: preparing a mosaic target, and placing the mosaic target on a magnetic filtration electric-arc-plating target; chemically cleaning the surface of a matrix; placing the matrix into an electric-arc ion plating machine, and vacuumizing until the background vacuum degree is less than 3.0*10-3Pa; adding bias voltage of -800V; starting a curved arc magnetic filter and the magnetic filtration electric-arc-plating target to perform argon arc plasma bombardment cleaning on the matrix; maintaining current of a magnetic filtration tube, current of the electric-arc target and duty cycle, regulating and controlling the bias voltage to -100 to -400V, introducing nitrogen, and film-coating for 30-90 minutes; and switching off the magnetic filtration electric-arc-plating target and the curved arc magnetic filter, and then taking out a sample to obtain the doped luminescent aluminum nitride thin film. During the preparation process, the temperature of the sample is not more than 180 DEG C, and diffusion heat treatment is not required after deposition. The invention has simple preparation process and easy operation, and electrical and mechanical automatic control can be used in the film-coating course.

Description

A kind of low temperature doping light emitting nitride aluminium film and preparation method thereof
Technical field
The invention belongs to photoluminescence thin film technique field, particularly a kind of low temperature doping light emitting nitride aluminium film and preparation method thereof.
Background technology
Aluminium nitride (AlN) has very wide energy gap (6.2eV), helps preparing the luminescent material of bigger blue light of energy gap and UV-light.Although the various methods that prepare film all can be used for preparing AlN, yet the luminous AlN film of present preparation, mainly still concentrate in the low technology of some ionization levels, as magnetron sputtering method, pulsed laser deposition method and chemical vapor deposition (CVD) method etc., wherein with the doped with Al N film of chemical Vapor deposition process preparation, because of depositing temperature is very high, doped element can form effectively diffusion and become luminescence center in deposition process, directly luminous after the deposition.And with the doped with Al N film of magnetron sputtering and laser splash method preparation, because of depositing temperature is low, doped with Al N film often needs follow-up High temperature diffusion to handle, and makes doped element enter lattice, forms luminescence center.In a word, it is all very high that above method prepares luminous AlN film temperature, and energy expenditure is big, and matrix selects to receive considerable restraint.
Advantages such as arc ion plating has the ionization level height, and depositing temperature is low, and sedimentation velocity is fast are used widely in industrial tight acquisition.Yet the arc ion plating film pollutes because of there being macrobead, is not used in depositing Al N film substantially.Adopt the filtered arc ion plating technique when keeping high ionization level and sedimentation rate, to eliminate the particle contamination of big film.The present invention can directly deposit luminous AlN film at low temperatures with the luminous AlN film of filtered arc ion plating preparation doping.
Summary of the invention
In order to overcome the shortcoming and defect that exists in the prior art, primary and foremost purpose of the present invention is to provide the preparation method of a kind of low temperature doping light emitting nitride aluminium (AlN) film, make present industrial application the most widely arc ion plating apparatus after increasing the arc of curvature magnetic filter, can prepare light emitting nitride aluminium film.
Low temperature doping light emitting nitride aluminium (AlN) film that provides method for preparing to obtain is provided.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of the light emitting nitride aluminium film that mixes comprises following operation steps:
(1) with dopant material cast setting on the fine aluminium target, make and inlay target; And will inlay target and be contained on the magnetic filtered arc plating target;
(2) matrix being carried out surface chemistry cleans; Described matrix is silicon single crystal, quartz or glass;
(3) matrix is packed in the arc ion plating machine, matrix is positioned at the outside 60~100mm in winding pipe exit axis of range curvature arc magnetic filter, apart from the position of winding pipe exit below 60~80mm, takes out base vacuum to less than 3.0 * 10 -3Pa; Matrix biasing-800V~-1000V; Open the arc of curvature magnetic filter, adjust arc of curvature magnetic filter control power supply, adjusting magnetic strainer tube electric current is 3.0~4.6A; Start magnetic filtered arc plating target, adjusting the electric arc target electric current is 60~80A, and voltage is 18~22V, dutycycle 15~25%; Feed high-purity argon 35~45sccm (the standard milliliter number that Standard Curbic Centimiter Per Minute per minute flows through) to vacuum chamber, matrix is carried out the argon arc plasma bombardment clean, scavenging period is 5~15min;
(4) keep the described magnetic strainer tube of step (2) electric current, electric arc target electric current and dutycycle, with the bias voltage regulation and control-100~-400V; Reduce high-purity argon flow to 10~25sccm, feed nitrogen simultaneously, nitrogen flow is 60~70sccm; The beginning deposit aluminum nitride films, depositing time is 30~90min; Along with the increase of depositing time, substrate temperature raises, and substrate temperature is less than 200 ℃ behind deposition 90min;
(5) after plated film finishes, turn off magnetic filtered arc plating target and arc of curvature magnetic filter, and close high-purity argon and nitrogen, rising vacuum degree in vacuum chamber to 3.0~5.0 * 10 -3Pa treats to take out matrix when substrate temperature is cooled to room temperature, and light emitting nitride aluminium film obtains mixing.
The preparation that step (1) is described inlays target is by following operation steps: at diameter is 100mm, height is on the cylindrical fine aluminium target surface of 45mm, the mode of employing mechanical workout processes three diameters apart from 25mm place, target surface center on 120 ° of radial directions be 14.0~15.0mm, the degree of depth is the blind hole of 18~25mm, in a vacuum the dopant material rod is embedded in the blind hole then, the hole axle is a shrink-fit, carry out the stress relief annealing processing to inlaying good target at last, and mechanical workout is to guarantee the planeness of target surface.
The described dopant material of step (1) is chromium (Cr), copper (Cu) or manganese (Mn), selects according to required glow color.
The described chemical cleaning method of step (2) is behind alcohol ultrasonic cleaning 10~15min, oven dry.
Described the taking out in the base vacuum process of step (3) is arranged on 180 ℃~250 ℃ with main Heating temperature, further sloughs moisture, reduces oxygen partial pressure in the coating chamber.
A kind of doping light emitting nitride aluminium film that obtains according to method for preparing.
The inventive method needs to install arc of curvature magnetic filter (hereinafter to be referred as magnetic filter) on common electric arc ion film coating machine, pollute with the macrobead of eliminating in the deposition ionic current; Dopant material is embedded on the fine aluminium electric arc target, with arc of curvature magnetic filtered arc ion plating reactive deposition doped aluminum nitride film, sedimentary doped aluminum nitride film does not need just can obtain photoluminescence through diffusion heat treatments, be placed in the coating process bottom the sample thermocouple measurement to temperature be no more than 180 ℃.
The present invention compared with prior art has following advantage and effect:
(1) the plated film speed of magnetic filtered arc ion plating method wants high than magnetron sputtering, and have with magnetron sputtering quite or be better than the coating quality of magnetron sputtering because ion is coated with diffraction preferably, help preparing large area film;
(2) need not heat in process of plating, in the whole coating process, sample is subjected to the bombardment operative temperature of ionic current can be elevated to 130~180 ℃, more than chemical vapor deposition (CVD) or need the building method of DIFFUSION TREATMENT low;
(3) but the luminous AlN film of the sedimentary doping of the present invention does not need to carry out the just direct sunshine photoluminescence of follow-up DIFFUSION TREATMENT;
(4) preparation technology of the present invention is simple, and easy handling, coating process adopt electric and mechanical control automatically.
Description of drawings
Fig. 1 is a magnetic filtered arc ion plating AlN:Cr film room temperature photoluminescence spectrogram.
Fig. 2 is a magnetic filtered arc ion plating AlN:Cu film room temperature photoluminescence spectrogram.
Fig. 3 is magnetic filtered arc ion plating A1N:Cr, Cu duplicature light at room temperature photoluminescence spectrogram.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done further detailed description, but embodiments of the present invention are not limited thereto.
Embodiment 1
Adopt AIP---01 type multi-arc ion plating film machine, additional magnetic filter device in the coating equipment, coating equipment and magnetic filter all can be buied from market, and wherein magnetic filter is made by the Institute of Low Energy Nuclear Physics, Beijing Normal University; The multi-arc ion plating film machine is manufactured and designed by boat Surface Engineering research and development centre of Shenyang section; The substrate of adopting is a silica glass, more easily buys from the market; That is adopted inlays target, be to be 100mm at diameter, height is on the cylindrical fine aluminium target surface of 45mm, the mode of employing mechanical workout processes three diameters apart from 25mm place, target surface center on 120 degree radial directions be 12mm, the degree of depth is the blind hole of 10mm, in a vacuum pure Cr rod is inlayed wherein then, the hole axle is a shrink-fit, carry out the processing of 300 ℃+120min stress relief annealing to inlaying good target at last, and target surface carried out turning processing, make and inlay the Cr plane rod end and the Al target is in the same plane.
(1) at first with quartz substrate in alcohol behind the ultrasonic cleaning 15min, dry for standby;
(2) will dry good substrate and pack in the AIP-01 type multi-arc ion plating film machine, place the winding pipe exit center position position 60mm of arc of curvature magnetic filter,, allow the positive sample surfaces that bombards of magnetic filtered arc plasma apart from 70mm place, lower end, mouth of pipe center;
(3) 180 ℃~250 ℃ of vacuum chamber heating tube temperature ranges are set, further remove the aqueous vapor of substrate and furnace chamber, vacuumize step by step with mechanical pump, lobe pump, diffusion pump then, when pressure in vacuum tank reduces to 6.5 * 10 -3During Pa, close heating subsequently, equal vacuum chamber cool to room temperature just begins plated film, continues to keep mechanical pump, lobe pump and diffusion pump to vacuumize during cooling, makes vacuum chamber base vacuum degree further be increased to 3 * 10 -3Pa; Power-on water coolant and plated film power supply adjust to clean and to be biased into-800V, and dutycycle is 20%, and argon flow amount is 40sccm, opens magnetic filter, and the electric current of magnetic filter is adjusted into 3.5A, and voltage is 19V; Start magnetic then and filter single arc plating target, the arc target current is 60A, and voltage 29V carries out ion with argon arc plasma jet bombardment sample and cleans, and scavenging period is 10min;
(4) keep magnetic strainer tube electric current, electric arc target electric current and dutycycle, adjustment is biased into-400V; Feed 70sccm nitrogen, argon flow amount is adjusted into 20sccm; Then magnetic filtered arc plating target current is adjusted into 75A, voltage is 25V; The plated film time is 60min, in the coating process with the thermocouple measurement of substrate bottom to temperature be no more than 180 ℃;
(5) after plated film finishes, turn off magnetic filtered arc plating target and arc of curvature magnetic filter, and close high-purity argon and nitrogen, rising vacuum degree in vacuum chamber to 3.0~5.0 * 10 -3Pa treats to take out matrix when substrate temperature is cooled to room temperature, obtains the Cr of mixing photoluminescence AlN film of the present invention.The roughness of film of measuring with atomic force microscope (AFM) is that Ra is 12nm, illustrates that arc of curvature magnetic filtered arc ion plating film eliminated the macrobead pollution, has obtained smooth AlN film; Is 5.4wt.% with XPS measuring to doping Cr content, and be diffused into substantially in the AlN lattice, excite with the incident of 270nm light in the PLM-100 fluorescence spectrophotometer, the photoluminescence spectra that measures is seen Fig. 1, contain 2 peaks in the spectrum, be that remaining oxygen causes that 757nm ruddiness peak is Cr during owing to plated film at the purple light peak of 380nm 3+Ion 3d → 3d transition produces.
Embodiment 2
Adopt AIP---01 type multi-arc ion plating film machine, additional magnetic filter device in the coating equipment, coating equipment and magnetic filter all can be buied from market, and wherein magnetic filter is made by the Institute of Low Energy Nuclear Physics, Beijing Normal University; The multi-arc ion plating film machine is manufactured and designed by boat Surface Engineering research and development centre of Shenyang section; The substrate of adopting is a silica glass, more easily buys from the market; That is adopted inlays target, at diameter is 100mm, height is on the cylindrical fine aluminium target surface of 45mm, the mode of employing mechanical workout processes three diameters apart from 25mm place, target surface center on 120 degree radial directions be 14.4mm, the degree of depth is the blind hole of 20mm, in a vacuum pure Cu rod is inlayed wherein then, the hole axle is a shrink-fit, carry out the processing of 300 ℃+120min stress relief annealing to inlaying good target at last, and target surface carried out turning processing, make and inlay the Cu plane rod end and the Al target is in the same plane.
(1) at first substrate is cleaned, behind alcohol ultrasonic cleaning 15min, oven dry;
(2) will dry good substrate and pack in the AIP-01 type multi-arc ion plating film machine, place winding pipe exit center position position 90mm,, allow the positive sample surfaces that bombards of plasma body apart from 60mm place, lower end, mouth of pipe center apart from the arc of curvature magnetic filter;
(3) 180 ℃~250 ℃ of vacuum chamber heating tube temperature ranges are set, further remove the aqueous vapor of substrate and furnace chamber, vacuumize step by step with mechanical pump, lobe pump, diffusion pump then, when pressure in vacuum tank reduces to 6.5 * 10 -3Pa or when above closes heating subsequently, and equal vacuum chamber cool to room temperature just begins plated film, continues to keep mechanical pump, lobe pump and diffusion pump to vacuumize during cooling, makes vacuum chamber base vacuum degree further be increased to 3 * 10 -3Pa; Power-on water coolant and plated film power supply adjust to clean and to be biased into-800V, and dutycycle is 20%, and argon flow amount is 40sccm, opens magnetic filter, and the electric current of magnetic filter is adjusted into 3.5A, and voltage is 19V.Start magnetic then and filter single arc plating target, the arc target current is 60A, and voltage 29V carries out ion with argon arc plasma jet bombardment sample and cleans, and scavenging period is 10min;
(4) keep magnetic strainer tube electric current, electric arc target electric current and dutycycle, adjustment is biased into-300V, feeds 60sccm nitrogen, the argon flow amount adjustment, and argon flow amount is adjusted into 25sccm, and the electric current that then magnetic is filtered single arc plating target is adjusted into 70A, and voltage is 32V; The plated film time is 60min, in the coating process with the thermocouple measurement that is placed on substrate bottom to temperature be no more than 180 ℃;
(5) after plated film finishes, turn off magnetic filtered arc plating target and arc of curvature magnetic filter, and close high-purity argon and nitrogen, rising vacuum degree in vacuum chamber to 3.0~5.0 * 10 -3Pa treats to take out matrix when substrate temperature is cooled to room temperature, obtains the Cu of mixing photoluminescence AlN film of the present invention.The roughness of film of measuring with atomic force microscope (AFM) is that Ra is 14.4nm, illustrates that arc of curvature magnetic filtered arc ion plating film eliminated the macrobead pollution, has obtained smooth AlN film; Is 11wt.% with XPS measuring to doped with Cu content, and considerable part simple substance Cu is arranged, and has only a small amount of Cu +Ion diffusion forms luminescence center in the AlN lattice, excite with the incident of 370nm light on the PLM-100 fluorescence spectrophotometer, and the photoluminescence spectra that measures is seen Fig. 2, in the spectrum is because 3d at the blue light peak of 448nm 104s 1→ 3d 10Transition produces.
Embodiment 3
Adopt AIP---01 type multi-arc ion plating film machine, additional magnetic filter device in the coating equipment, coating equipment and magnetic filter all can be buied from market, and wherein magnetic filter is made by the Institute of Low Energy Nuclear Physics, Beijing Normal University; The multi-arc ion plating film machine is manufactured and designed by boat Surface Engineering research and development centre of Shenyang section; The substrate of adopting is N type (a 100) silicon, more easily buys from the market; The pure Cr that is adopted inlays pure Al target, be to be 100mm at diameter, height is on the cylindrical fine aluminium target surface of 45mm, adopting mach mode to process three diameters apart from 25mm place, target surface center on 120 degree radial directions is 12mm, the degree of depth is the blind hole of 10mm, in a vacuum pure Cr rod is inlayed wherein then, and the hole axle is a shrink-fit, carry out the stress relief annealing processing to inlaying good target at last, and machining is to guarantee the planeness of target surface.The pure Cu that is adopted inlays pure Al target, at diameter is 100mm, height is on the cylindrical fine aluminium target surface of 45mm, the mode of employing mechanical workout processes three diameters apart from 25mm place, target surface center on 120 degree radial directions be 14.4mm, the degree of depth is the blind hole of 20mm, in a vacuum pure Cu rod is inlayed wherein then, and the hole axle is a shrink-fit, carry out the stress relief annealing processing to inlaying good target at last, and mechanical workout is to guarantee the planeness of target surface.
(1) the pure Al target of at first pure Cu the being inlayed magnetic filtered arc target of packing into;
(2) N type silicon base is cleaned, behind alcohol ultrasonic cleaning 15min, oven dry;
(3) will dry good workpiece and pack in the AIP-01 type multi-arc ion plating film machine, place winding pipe exit center position position 40mm,, allow the positive substrate surface that bombards of plasma body apart from 80mm place, lower end, mouth of pipe center apart from the arc of curvature magnetic filter;
(4) 180 ℃~250 ℃ of vacuum chamber heating tube temperature ranges are set, further remove the aqueous vapor of substrate and furnace chamber, vacuumize step by step with mechanical pump, lobe pump, diffusion pump then, when pressure in vacuum tank reduces to 6.5 * 10 -3Pa or when above closes heating subsequently, and equal vacuum chamber cool to room temperature just begins plated film, continues to keep mechanical pump, lobe pump and diffusion pump to vacuumize during cooling, makes vacuum chamber base vacuum degree further be increased to 3 * 10 -3Pa; Power-on water coolant and plated film power supply adjust to clean and to be biased into-1000V, and dutycycle is 20%, and argon flow amount is 40sccm, opens magnetic filter, and the electric current of magnetic filter is adjusted into 3.5A, and voltage is 19V.Start magnetic then and filter single arc plating target, the arc target current is 60A, and voltage 29V carries out ion with argon arc plasma jet bombardment substrate and cleans, and scavenging period is 5min;
(5) keep magnetic strainer tube electric current, electric arc target electric current and dutycycle, adjustment is biased into-200V, feeds 70sccm nitrogen, the argon flow amount adjustment, and argon flow amount is adjusted into 20sccm, and the electric current that then magnetic is filtered single arc plating target is adjusted into 70A, and voltage is 31~33V; The plated film time is 60min, in the coating process with the thermocouple measurement that is placed on sample bottom to temperature be no more than 180 ℃;
(6) after plated film finishes, turn off magnetic filtered arc plating target and arc of curvature magnetic filter, and close high-purity argon and nitrogen, rising vacuum degree in vacuum chamber to 3.0~5.0 * 10 -3Pa treats to take out matrix when substrate temperature is cooled to room temperature, obtains luminous AlN of the present invention and mixes the Cu film;
(7) the pure Al target of then pure Cr the being inlayed magnetic filtered arc target of packing into;
(8) will mix the Cr film with the AlN for preparing on the silicon base packs in the AIP-01 type multi-arc ion plating film machine in the coating equipment; Placement is apart from the winding pipe exit center position position 40mm of arc of curvature magnetic filter, apart from 80mm place, lower end, mouth of pipe center;
(9) 180 ℃~250 ℃ of vacuum chamber heating tube temperature ranges are set, further remove the aqueous vapor of substrate and furnace chamber, vacuumize step by step with mechanical pump, lobe pump, diffusion pump then, when pressure in vacuum tank reduces to 6.5 * 10 -3Pa or when above closes heating subsequently, and equal vacuum chamber cool to room temperature just begins plated film, continues to keep mechanical pump, lobe pump and diffusion pump to vacuumize during cooling, makes vacuum chamber base vacuum degree further be increased to 3 * 10 -3Pa; Power-on water coolant and plated film power supply adjust to clean and to be biased into-800V, and dutycycle is 20%, and argon flow amount is 40sccm, opens magnetic filter, and the electric current of magnetic filter is adjusted into 3.5A, and voltage is 19V.Start magnetic then and filter single arc plating target, the arc target current is 60A, and voltage 30V carries out ion with argon arc plasma jet bombardment substrate and cleans, and scavenging period is 5min;
(10) keep magnetic strainer tube electric current, electric arc target electric current and dutycycle, adjustment is biased into-200V, feeds 70sccm nitrogen, the argon flow amount adjustment, and argon flow amount is adjusted into 20sccm, and the electric current that then magnetic is filtered single arc plating target is adjusted into 70A, and voltage is 34V; The plated film time is 38min, in the coating process with the thermocouple measurement that is placed on sample bottom to temperature be no more than 110 ℃;
(11) after plated film finishes, turn off magnetic filtered arc plating target and arc of curvature magnetic filter, and close high-purity argon and nitrogen, rising vacuum degree in vacuum chamber to 3.0~5.0 * 10 -3Pa takes out matrix when treating that substrate temperature is cooled to room temperature, obtain of the present inventionly mixing at luminous AlN that sedimentary luminous AlN mixes the duplicature that the Cr film is formed on the Cu film.The roughness of film of measuring with atomic force microscope (AFM) is that Ra is 13.6nm, illustrates that arc of curvature magnetic filtered arc ion plating film eliminated the macrobead pollution, has obtained smooth film; With XPS stripping layer analysis method, measuring doped with Cu content is 7wt.%, and has considerable part to exist with simple substance Cu, has only to be diffused on a small quantity in the AlN lattice, exists with the Cu+ ion, forms luminescence center; The AlN film Cr content that Cr is mixed on the surface is 3wt.%, is present in the AlN lattice with the Cr3+ form, forms luminescence center.On the PLM-100 fluorescence spectrophotometer, excite with the incident of 270nm light, the photoluminescence spectra that measures is seen Fig. 3, in the spectrum the wide region royal purple of 300~400nm only the remaining oxygen ion among the AlN and Cu+ eject jointly, be that Cr3+ ion 3d → 3d transition produces at the ruddiness of 697nm.Here the ruddiness that excites of the blue light that excites of Cu+ and Cr3+ all moves to left than embodiment 1 and embodiment 2 respectively, and the difference of its reason dopant ion concentration causes.
The mode that the foregoing description has been implemented for the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (5)

1. the preparation method of a low temperature doping light emitting nitride aluminium film is characterized in that comprising following operation steps:
(1) with dopant material cast setting on the fine aluminium target, make and inlay target; And will inlay target and be contained on the magnetic filtered arc plating target; Described dopant material is chromium, copper or manganese;
(2) matrix being carried out surface chemistry cleans; Described matrix is silicon single crystal, quartz or glass;
(3) matrix is packed in the arc ion plating machine, matrix is positioned at the outside 60~100mm in winding pipe exit axis of range curvature arc magnetic filter, apart from the position of winding pipe exit below 60~80mm, takes out base vacuum to less than 3.0 * 10 -3Pa; Matrix biasing-800V~-1000V; Open the arc of curvature magnetic filter, adjust arc of curvature magnetic filter control power supply, adjusting magnetic strainer tube electric current is 3.0~4.6A, starts magnetic filtered arc plating target, and adjusting the electric arc target electric current is 60~80A, and voltage is 18~22V, dutycycle 15~25%; Feed high-purity argon 35~45sccm to vacuum chamber, matrix is carried out the argon arc plasma bombardment clean, scavenging period is 5~15min;
(4) keep the described magnetic strainer tube of step (3) electric current, electric arc target electric current and dutycycle, with the bias voltage regulation and control-100~-400V; Reduce high-purity argon flow to 10~25sccm, feed nitrogen simultaneously, nitrogen flow is 60~70sccm; The beginning deposit aluminum nitride films, depositing time is 30~90min, substrate temperature is less than 200 ℃ behind deposition 90min;
(5) after plated film finishes, turn off magnetic filtered arc plating target and arc of curvature magnetic filter, and close high-purity argon and nitrogen, rising vacuum degree in vacuum chamber to 3.0~5.0 * 10 -3Pa treats to take out matrix when substrate temperature is cooled to room temperature, and light emitting nitride aluminium film obtains mixing.
2. the preparation method of a kind of low temperature doping light emitting nitride aluminium film according to claim 1, it is characterized in that: the preparation that step (1) is described inlays target is by following operation steps: at diameter is 100mm, height is on the cylindrical fine aluminium target surface of 45mm, the mode of employing mechanical workout processes three diameters apart from 25mm place, target surface center on 120 ° of radial directions be 14.0~15.0mm, the degree of depth is the blind hole of 18~25mm, in a vacuum the dopant material rod is embedded in the blind hole then, the hole axle is a shrink-fit, carry out the stress relief annealing processing to inlaying good target at last, and mechanical workout is to guarantee the planeness of target surface.
3. the preparation method of a kind of low temperature doping light emitting nitride aluminium film according to claim 1 is characterized in that: the described chemical cleaning method of step (2) is behind alcohol ultrasonic cleaning 10~15min, oven dry.
4. the preparation method of a kind of low temperature doping light emitting nitride aluminium film according to claim 1, it is characterized in that: described the taking out in the base vacuum process of step (3) is arranged on 180 ℃~250 ℃ with main Heating temperature, further slough moisture, reduce oxygen partial pressure in the coating chamber.
5. low temperature doping light emitting nitride aluminium film according to each described method preparation of claim 1~4.
CN2010102938564A 2010-09-26 2010-09-26 Low-temperature-doped luminescent aluminum nitride thin film and preparation method thereof Expired - Fee Related CN101948999B (en)

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