CN1962932A - Method and device for preparing rare earth doped gallium nitride light-emitting film - Google Patents
Method and device for preparing rare earth doped gallium nitride light-emitting film Download PDFInfo
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- CN1962932A CN1962932A CN 200610125202 CN200610125202A CN1962932A CN 1962932 A CN1962932 A CN 1962932A CN 200610125202 CN200610125202 CN 200610125202 CN 200610125202 A CN200610125202 A CN 200610125202A CN 1962932 A CN1962932 A CN 1962932A
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Abstract
The invention discloses a preparing method of gallium nitride luminous film doped by rare earth, which is characterized by the following: controlling the substrate temperature within 0-500 Deg C; adopting nitrogen or composite gas of nitrogen and argon as splashing gas; proceeding magnetic control splashing for metal gallium of doped rare earth powder in the vacuum; sedimenting rare earth doped gallium nitride luminous film on the substrate of target position. The invention also provides magnetic control splashing device to prepare the product, which contains vacuum chamber; the rotary substrate rack with substrate and 3-5 magnetic targets are set in the vacuum chamber; the magnetic control target is set on the substrate, which makes substrate bottom parallel the magnetic control target; each magnetic control target connects DC anode directly; the cooling chamber is set in the magnetic control target, which possesses cooling dielectric inlet an outlet.
Description
Technical field
The present invention relates to a kind of method and apparatus that is used to prepare rare earth doped gallium nitride light-emitting film.
Background technology
Present domestic preparation GaN:Re device generally use metal organic chemical vapor deposition (MOCVD) or molecular beam epitaxy (MBE) method under 800～1100 ℃ of high temperature on sapphire or Si substrate epitaxy form.The principle of metal organic chemical vapor deposition (MOCVD) is: the organometallic compound and the nitrogen of gallium react, and generate gan and organism, are a kind of equilibrium chemistry reaction technologies; This technology prepares rare earth doped gallium nitride (GaN:Re) luminescent device need inject rare earth element with ion beam technology usually in gallium nitride film, rare earth element is the bigger heavy element of quality, ion implantationly must cause serious lattice damage.Molecular beam epitaxy (MBE) technology then is that the pure metal gallium is at high temperature evaporated, react with the plasma body of nitrogen, generate gallium nitride film, prepare rare earth doped gallium nitride (GaN:Re) luminescent device only need mix rare earth element or contain rare earth element in gallium compound, but it is at high temperature to react, and is a kind of high temperature technology of preparing.MBE equipment and running cost are all very expensive.Concerning film crystal indicating meter and solar cell, because the general glass substrate that adopts is made flow process and need be finished at a lower temperature, above-mentioned two kinds of methods all are unsuitable for this Application Areas.
Summary of the invention
The object of the present invention is to provide a kind of method and apparatus that is used to prepare rare earth doped gallium nitride light-emitting film, this method and apparatus can prepare rare earth doped gallium nitride light-emitting film at a lower temperature on substrate.
Technical scheme provided by the invention is: a kind of method for preparing rare earth doped gallium nitride light-emitting film, utilize magnetron sputtering technique, under 0～500 ℃, vacuum condition, with the mixed gas of nitrogen or nitrogen and argon gas as sputter gas, the gallium that is doped with rare earth powder is carried out magnetron sputtering, make gallium nitride light-emitting film rear-earth-doped on the substrate deposition that is located at the target position place.
The present invention can at room temperature make substrate deposition one deck gallium nitride film earlier; Substrate temperature is heated to below 500 ℃ or 500 ℃, substrate is added the negative bias of 0～1000V, and on the gallium nitride film of substrate deposition the adulterated gallium nitride film of deposition of rare-earth.
Above-mentioned rare earth is Tm, Er or/and the Pr powder, the ratio doping≤10atm.% of described rare earth.
Above-mentioned vacuum condition is 0.1～4Pa.
The present invention also provides a kind of magnetic control sputtering device for preparing rare earth doped gallium nitride light-emitting film, comprise vacuum chamber, be provided with rotatable substrate holder and 3～5 magnetic controlling targets in the vacuum chamber, be equiped with substrate on the substrate holder, substrate is located at the magnetic controlling target top and makes substrate surface parallel with the magnetic control target surface, and each magnetic controlling target connects the direct supply negative electrode respectively; Be provided with cooling room in the magnetic controlling target, cooling room is provided with cooling medium inlet and outlet.
Above-mentioned substrate holder is provided with lining heat.
Above-mentioned substrate is added with continuously adjustable negative bias in the 0-1000V.
The present invention has that depositing temperature is low, the film forming area is big, film-Ji strong adhesion, growth velocity height, pollution-free, doping process simple and characteristics such as not damaged, is particularly suitable for preparing on glass substrate rare earth doped gallium nitride (GaN:Re) luminescent device.The present invention adopts magnetron sputtering technique; utilize magnetic field to change the electronic motion direction, constraint and prolongation trajectory of electron motion are in the anomalous glow discharge that forms high density plasma; bombardment causes target as sputter to positive ion to target, makes it have high speed, low temperature two big characteristics.
Description of drawings
Fig. 1 is the structural representation of magnetic control sputtering device of the present invention;
Fig. 2 is the A-A enlarged view of Fig. 1.
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is described further:
As depicted in figs. 1 and 2, the present invention includes vacuum chamber 14, vacuum chamber 14 is provided with vacuum orifice 4, be provided with the magnetic controlling target 5 of 3 horizontal positioned and rotatable substrate holder 13 (substrate holder 13 is fixed on the turning axle 9 by drive mechanism) in the vacuum chamber 14, substrate holder 13 and magnetic controlling target 5 relative and parallel placements, and distance adjustable (can realize by the turning axle 9 of up-down adjustment substrate holder 13) is so that optimize processing parameter.Be equiped with substrate 12 on the substrate holder 13, substrate 12 is located at magnetic controlling target 5 tops and makes substrate surface parallel with the magnetic control target surface, and each magnetic controlling target 5 connects direct supply negative electrode 8 respectively; Be provided with cooling room 6 in the magnetic controlling target 5, cooling room 6 is provided with heat-eliminating medium 7 imports and outlet.The magnetic controlling target pond is arranged in the vacuum chamber,, can make the substrate on it be positioned at any target position (promptly aiming at magnetic controlling target 5) by the rotation of substrate holder, thus can be on a slice substrate the mix GaN:Re film of different rare earth elements of sputtering sedimentation.And, regulate the thickness of the different element films that mix by regulating the time that substrate is positioned at different target position.
Target pond 3 base plates of magnetic controlling target 5 adopt the good red copper of thermal conductivity, and each target pond 3 is following with isolating pipeline water flowing energising, with cooling and the bias voltage control that circulated in the target pond.Iron boron strong magnet is placed at each magnetic controlling target back side, and the magnetic field arranged direction is identical, forms closed, target surface magneticstrength 500Gauss; Each independent target magnetic field layout type all is a unbalanced magnetic field simultaneously.Simultaneously in order further to improve film-Ji sticking power, the negative bias 2 that the substrate holder 13 of this device is installed 0-1000V.This device can also increase target pond quantity, reaches the purpose of the complicated photoelectric device of preparation.
Substrate holder among the present invention is installed well heater and thermopair 1, can accurately control underlayer temperature.Gas 10 flows can be by mass flowmeter 11 controls.Vacuum system can be made up of diffusion pump and mechanical pump, also can adopt molecular pump.Working gas is nitrogen, argon gas mixed gas during deposition.Flow with 11 pairs of gases 10 of mass flowmeter is controlled.
The present invention is different with general both at home and abroad at present device preparation facilities, and it is a kind of many target position magnetron sputtering technique, is used in low temperature depositing GaN:Re film on the glass substrate, is the magnetically controlled DC sputtering technology.Can accurately control the number of plies and the thickness of GaN:Re film, each layer one or more rare earth element that can accurately mix.
In a word, technology provided by the invention has the advantage of the characteristics GaN of the different rare earth elements of many target position dopant deposition, and depositing temperature is below 500 ℃.Having overcome the present generally defective of the high growth temperature method of employing and the shortcoming of controlled doping heavy element flexibly in the world, is a kind of preparation technology in low temperature that is suitable for preparing rare earth doped gallium nitride (GaN:Re) luminescent device on glass substrate.
Embodiment 1
3 magnetic controlling target ponds are arranged, the single rare earth powder (particle diameter 10 μ m) of wherein mix respectively in the gallium in 2 target ponds Tm and Er in vacuum chamber.Tm is 1at.% to the doping ratio of target, and Er is 10at.% to the doping ratio of target.Another target pond rare earth element that undopes.The adjustment substrate holder is 11cm to the distance of target surface.Be evacuated down to 10
-4Below the pa, behind the vacustat, the mixed gas of logical nitrogen and argon gas 1: 99 (volume ratio) makes working vacuum reach 4.0Pa, keeps the vacuum tightness of this moment constant.Open cooling-water machine, the temperature in target pond is cooled to below 10 ℃.The dc sputtering power of this target is opened in the top, target pond that substrate is rotated to there be not doped with rare-earth elements, substrate is not heated, and first low temperature depositing one deck amorphous gallium nitride film deposits 5 minutes.Open heating unit, make substrate temperature be heated to 500 ℃.Open grid bias power supply, on substrate holder, add the negative bias of 50V.Connection is doped with the direct supply in the magnetic controlling target pond of Tm, and the metal gallium target that is doped with Tm was carried out glow discharge 30 minutes.The direct supply that disconnection is doped with the magnetic controlling target pond of Tm starts electric motor, and its direct supply is connected in the top, magnetic controlling target pond that the firm substrate that deposited is rotated to be doped with Er, carries out magnetron sputtering 30 minutes.Disconnect dc sputtering power, grid bias power supply, substrate heating temperature and mixed gas successively.Substrate is cooled to below 50 ℃, still keeps logical water coolant in the process of cooling, finish up to cooling.To vacuum chamber venting, open body of heater and can obtain one three layers of gallium nitride film are arranged on same substrate, be doped with the gallium nitride film of Tm and Er in every layer of gallium nitride film respectively.Film is further processed the gallium nitride illumination device of the green glow that can obtain turning blue.
Embodiment 2
3 magnetic controlling target ponds are arranged, earlier the rare earth nano powder (particle diameter 100nm) of doping Tm and Er in the gallium in a target pond in vacuum chamber.The doping of Tm is 0.8at.%, and the doping of Er is 1at.%.Mix and have the rare earth nano powder (particle diameter 80nm) of Eu element in second target pond, the mass content of the rare earth nano powder of Eu element is 0.5at.%.The 3rd target pond rare earth element that undopes.The adjustment substrate holder is 10cm to the distance of target surface.Be evacuated down to 10
-4Below the pa, up to vacustat.The mixed gas of logical nitrogen and argon gas 3: 5 (volume ratio) makes working vacuum reach 0.1Pa, keeps the vacuum tightness of this moment constant.Open cooling-water machine, the temperature in target pond is cooled to below 10 ℃.The dc sputtering power of this target is opened in the top, target pond that substrate is rotated to there be not doped with rare-earth elements, to the substrate heating, and biasing not, first low temperature depositing one deck amorphous gallium nitride film deposits 5 minutes.Open heating unit, make substrate temperature be heated to 300 ℃.Open grid bias power supply, on substrate holder, add the negative bias of 100V.Connection is doped with the direct supply in the magnetic controlling target pond of Tm, and the metal gallium target that is doped with Tm was carried out glow discharge 40 minutes.The direct supply that disconnection is doped with the magnetic controlling target pond of Tm starts electric motor, and its direct supply is connected in the top, magnetic controlling target pond that the firm substrate that deposited is rotated to be doped with Er, carries out magnetron sputtering 40 minutes.Disconnect dc sputtering power, grid bias power supply, substrate heating temperature and mixed gas successively.Substrate is cooled to below 50 ℃, still keeps logical water coolant in the process of cooling, finish up to cooling.To the vacuum chamber venting, to open body of heater and can obtain a film that on same substrate, deposits two layers of gan, one deck is doped with Tm and Er, and another layer is doped with Eu.Film is further processed the gallium nitride illumination device that can obtain emitting white light.
Embodiment 3
3 magnetic controlling target ponds are arranged in vacuum chamber, the rare earth nano powder (particle diameter 50nm) of doping Tm and Er in the gallium of elder generation in a target pond, the doping of Tm is 0.5at.%, the doping of Er is 2.0at.%.Mix and have the rare earth nano powder (particle diameter 50nm) of Eu element and the nanometer powder (particle diameter 50nm) of Tm in second target pond, the mass content of the rare earth nano powder of Eu element is 1.0at.%, and the Tm doping is 1.0at.%.The 3rd target pond rare earth element that undopes.The adjustment substrate holder is 8cm to the distance of target surface.Be evacuated down to 10
-4Below the Pa, behind the vacustat.Logical nitrogen makes working vacuum reach 0.5Pa, keeps the vacuum tightness of this moment constant.Open cooling-water machine, the temperature in target pond is cooled to below 10 ℃.The dc sputtering power of this target is opened in the top, target pond that substrate is rotated to there be not doped with rare-earth elements, to the substrate heating, and biasing not, first low temperature depositing one deck amorphous gallium nitride film deposits 5 minutes.Open heating unit, make substrate temperature be heated to 300 ℃.Open grid bias power supply, on substrate holder, add the negative bias of 100V.Connection is doped with the direct supply in the magnetic controlling target pond of Tm, and the metal gallium target that is doped with Tm was carried out glow discharge 40 minutes.The direct supply that disconnection is doped with the magnetic controlling target pond of Tm starts electric motor, and its direct supply is connected in the top, magnetic controlling target pond that the firm substrate that deposited is rotated to be doped with Er, carries out magnetron sputtering 40 minutes.Disconnect dc sputtering power, grid bias power supply, substrate heating temperature and mixed gas successively.Substrate is cooled to below 50 ℃, still keeps logical water coolant in the process of cooling, finish up to cooling.To the vacuum chamber venting, to open body of heater and can obtain a film that on same substrate, deposits two layers of gan, one deck is doped with Tm and Er, and another layer is doped with Tm and Eu.Film is further processed the gallium nitride illumination device that can obtain emitting white light.
Claims (7)
1. method that is used to prepare rare earth doped gallium nitride light-emitting film, it is characterized in that: utilize magnetron sputtering technique, under 0～500 ℃, vacuum condition, with the mixed gas of nitrogen or nitrogen and argon gas as sputter gas, the gallium that is doped with rare earth powder is carried out magnetron sputtering, make gallium nitride light-emitting film rear-earth-doped on the substrate deposition that is located at the target position place.
2. method according to claim 1 is characterized in that: at room temperature make earlier substrate deposition one deck gallium nitride film; Then substrate temperature is heated to below 500 ℃ or 500 ℃, substrate is added the negative bias of 0～1000V, and on the gallium nitride film of substrate deposition the adulterated gallium nitride film of deposition of rare-earth.
3. method according to claim 1 and 2 is characterized in that: described rare earth is Tm, Er or/and the Pr powder, the ratio doping≤10atm.% of described rare earth.
4. method according to claim 1 and 2 is characterized in that: above-mentioned vacuum condition is 0.1～4Pa.
5. magnetic control sputtering device for preparing rare earth doped gallium nitride light-emitting film, comprise vacuum chamber, it is characterized in that: be provided with rotatable substrate holder and 3～5 magnetic controlling targets in the vacuum chamber, be equiped with substrate on the substrate holder, substrate is located at the magnetic controlling target top and makes substrate surface parallel with the magnetic control target surface, and each magnetic controlling target connects the direct supply negative electrode respectively; Be provided with cooling room in the magnetic controlling target, cooling room is provided with cooling medium inlet and outlet.
6. magnetic control sputtering device according to claim 5, it is characterized in that: substrate holder is provided with lining heat.
7. according to claim 5 or 6 described magnetic control sputtering devices, it is characterized in that: substrate is added with continuously adjustable negative bias in the 0-1000V.
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| CN200610125202A CN100594255C (en) | 2006-11-30 | 2006-11-30 | Method and device for preparing rare earth doped gallium nitride light-emitting film |
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| CN103242846B (en) * | 2012-02-10 | 2016-01-13 | 海洋王照明科技股份有限公司 | Titanium phosphate light-emitting film, its preparation method and electroluminescent device |
| CN103289688A (en) * | 2012-02-28 | 2013-09-11 | 海洋王照明科技股份有限公司 | Titanium doped aluminate luminescent film as well as preparation method and application thereof |
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