CN109888070A - AlN template, LED epitaxial slice and its manufacturing method - Google Patents
AlN template, LED epitaxial slice and its manufacturing method Download PDFInfo
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- CN109888070A CN109888070A CN201910060014.5A CN201910060014A CN109888070A CN 109888070 A CN109888070 A CN 109888070A CN 201910060014 A CN201910060014 A CN 201910060014A CN 109888070 A CN109888070 A CN 109888070A
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Abstract
The invention discloses a kind of AlN template, LED epitaxial slice and its manufacturing methods, belong to technical field of semiconductors.AlN template includes substrate and the AlN film deposited on substrate, AlN film includes the first AlN film, insert layer and the 2nd AlN film stacked gradually, insert layer includes multiple AlNO sublayers, and the oxygen content in multiple AlNO sublayers first successively increases again successively reduction along the stacking direction of multiple AlNO sublayers.A part of O atom in AlNO sublayer can substitute N atom, another part O atom will form interstitial atom, and displacement O atom and calking O atom can all make AlN lattice generate certain distortion, increase the lattice constant of AlN film, keep the lattice constant of AlN film and subsequent GaN epitaxial film closer, be conducive to reduce the compression in GaN material, improve the warpage of epitaxial wafer, and then improve the wavelength uniformity of epitaxial layer.
Description
Technical field
The present invention relates to technical field of semiconductors, in particular to a kind of AlN template, LED epitaxial slice and its manufacture
Method.
Background technique
LED (Light Emitting Diode, light emitting diode) is a kind of semiconductor electronic component that can be luminous.As
A kind of efficient, environmentally friendly, green New Solid lighting source, is widely applied rapidly, such as traffic lights, automobile
Inside and outside lamp, landscape light in city, cell phone back light source etc..
Epitaxial wafer is the main composition part in LED, and existing GaN base LED epitaxial wafer includes Sapphire Substrate and life
Long GaN epitaxial layer on a sapphire substrate.Due between sapphire and GaN material there are lattice mismatch and thermal mismatch problem,
And only has lesser lattice between AlN material and GaN material, Sapphire Substrate and mismatch, therefore be often placed in AlN as buffer layer
To between Sapphire Substrate and GaN.Specifically, first at PVD (Physical Vapor Deposition, physical vapour deposition (PVD))
In equipment one layer of AlN film is deposited using PVD method on a sapphire substrate, then grow GaN epitaxial layer on AlN film, is made
LED epitaxial wafer.
In the implementation of the present invention, the inventor finds that the existing technology has at least the following problems:
Since, there are still the unmatched problem of lattice, AlN buffer layer and indigo plant are precious between AlN material and Sapphire Substrate
Stress can be still generated between stone lining bottom, and as the thickness of AlN film gradually increases, the stress of AlN film inner accumulation can be by
It is cumulative big, there is biggish warpage so as to cause epitaxial wafer, so that the wavelength uniformity of epitaxial wafer is deteriorated.
Summary of the invention
The embodiment of the invention provides a kind of AlN template, LED epitaxial slice and its manufacturing method, can be improved outer
Prolong the wavelength uniformity of piece.The technical solution is as follows:
In a first aspect, provide a kind of AlN template, the AlN film deposited including substrate and over the substrate,
The AlN film includes the first AlN film, insert layer and the 2nd AlN film stacked gradually, the insert layer packet
Multiple AlNO sublayers are included, and the oxygen content in the multiple AlNO sublayer is first layer-by-layer along the stacking direction of the multiple AlNO sublayer
Increase and successively reduces again.
Further, the thickness of the multiple AlNO sublayer first successively reduces along the stacking direction of the multiple AlNO sublayer
Successively increase again.
Further, the linear negative of oxygen content in the thickness of the multiple AlNO sublayer and the multiple AlNO sublayer
It closes.
Further, the thickness of the first AlN film is greater than the thickness of the 2nd AlN film.
Second aspect, provides a kind of LED epitaxial slice, and the LED epitaxial slice includes such as first party
AlN template described in face and the epitaxial layer being arranged in the AlN template.
The third aspect, provides a kind of manufacturing method of AlN template, and the manufacturing method includes:
One substrate is provided；
Depositing Al N thin film over the substrate；The AlN film include the first AlN film stacked gradually, insert layer and
2nd AlN film, the insert layer includes multiple AlNO sublayers, and the oxygen content in the multiple AlNO sublayer is along the multiple
The stacking direction of AlNO sublayer first successively increases successively to be reduced again.
Further, the depositing Al N thin film over the substrate, comprising:
Under the atmosphere for being mixed with argon gas, nitrogen and oxygen, splashed using magnetron sputtering technique to Al target
It penetrates, to deposit the AlN film over the substrate；During depositing the AlN film, the oxygen is first gradually increased
Flow, then gradually decrease the flow of the oxygen.
Further, during depositing the AlN film, the flow-rate ratio of the argon gas and the nitrogen gradually increases
Greatly.
Further, magnetron sputtering power supply uses the pulse power, during depositing the AlN film, the pulse
The frequency of power supply is gradually increased.
Fourth aspect, provides a kind of manufacturing method of LED epitaxial slice, and the manufacturing method includes:
One substrate is provided；
Depositing Al N thin film over the substrate；The AlN film include the first AlN film stacked gradually, insert layer and
2nd AlN film, the insert layer includes multiple AlNO sublayers, and the oxygen content in the multiple AlNO sublayer is along the multiple
The stacking direction of AlNO sublayer first successively increases successively to be reduced again；
In the AlN film growing epitaxial layers.
Technical solution provided in an embodiment of the present invention has the benefit that
By the way that AlN film to be set as including the first AlN film, insert layer and the 2nd AlN film stacked gradually, it is inserted into
Layer includes multiple AlNO sublayers, and a part of O atom in AlNO sublayer can substitute N atom, and another part O atom will form calking
Atom, and displacement O atom and calking O atom can all make AlN lattice generate certain distortion, increase the lattice constant of AlN film,
Keep the lattice constant of AlN film and subsequent GaN epitaxial film closer, be conducive to reduce the compression in GaN material, improves outer
Prolong the warpage of piece, and then improves the wavelength uniformity of the epitaxial layer based on AlN template.Oxygen content in multiple AlNO sublayers simultaneously
First successively increase along the stacking direction of multiple AlNO sublayers and successively reduce again, in addition being located at the first AlN that insert layer two sides do not mix O
Film and the 2nd AlN film, the oxygen content in entire AlN film first successively increase to certain value by 0, can sufficiently discharge first
The compression accumulated in AlN film prevents the excess oxygen content being passed through and the crystal quality of insert layer is caused to decline；Then again from
Certain value is reduced to 0, can obtain the AlNO film sublayer compared with high-crystal quality, Oxygen permeation can also be avoided thin to the 2nd AlN
In film, the crystal quality of subsequent epitaxial layer is influenced.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is a kind of structural schematic diagram of AlN template provided in an embodiment of the present invention；
Fig. 2 is a kind of structural schematic diagram of LED epitaxial slice provided in an embodiment of the present invention；
Fig. 3 is a kind of manufacturing method flow chart of AlN template provided in an embodiment of the present invention；
Fig. 4 is a kind of manufacturing method flow chart of LED epitaxial slice provided in an embodiment of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention
Formula is described in further detail.
Fig. 1 is a kind of structural schematic diagram of AlN template provided in an embodiment of the present invention, as shown in Figure 1, the AlN template 100
Including substrate 110 and the AlN film 120 deposited on substrate 110.
AlN film 120 includes the first AlN film 121, insert layer 122 and the 2nd AlN film 123 stacked gradually, insertion
Layer 122 includes multiple AlNO sublayer 122a, and the oxygen content in multiple AlNO sublayer 122a is along the layer of multiple AlNO sublayer 122a
Folded direction first successively increases successively is reduced again.
The embodiment of the present invention is by the way that AlN film to be set as including the first AlN film stacked gradually, insert layer and second
AlN film, insert layer include multiple AlNO sublayers, and a part of O atom in AlNO sublayer can substitute N atom, and another part O is former
Son will form interstitial atom, and displacement O atom and calking O atom can all make AlN lattice generate certain distortion, and it is thin to increase AlN
The lattice constant of film keeps the lattice constant of AlN film and subsequent GaN epitaxial film closer, is conducive to reduce in GaN material
Compression improves the warpage of epitaxial wafer, and then improves the wavelength uniformity of the epitaxial layer based on AlN template.Multiple AlNO simultaneously
Oxygen content in sublayer first successively increases along the stacking direction of multiple AlNO sublayers successively to be reduced again, in addition being located at insert layer two sides
The first AlN film and the 2nd AlN film of O are not mixed, and the oxygen content in entire AlN film first successively increases to certain value by 0, can
Sufficiently to discharge the compression accumulated in the first AlN film, prevents the excess oxygen content being passed through and lead to the crystal matter of insert layer
Amount decline；Then it reduces again from certain value to 0, the AlNO film sublayer compared with high-crystal quality can be obtained, oxygen can also be avoided
It infiltrates into the 2nd AlN film, influences the crystal quality of subsequent epitaxial layer.
Wherein, substrate 110 can be Si, SiC, sapphire, ZnO, GaAs, GaP, MgO, Cu and W substrate.Preferably, it serves as a contrast
Bottom 110 is Sapphire Substrate.
Further, the thickness of multiple AlNO sublayer 122a first successively reduces along the stacking direction of multiple AlNO sublayer 122a
Successively increase again.The variation side of the variation pattern of the thickness of multiple AlNO sublayer 122a and oxygen content in multiple AlNO sublayer 122a
Formula matches, the effect for causing the crystal quality of insert layer 122 to decline to further function as the excess oxygen content for preventing from being passed through,
Oxygen permeation also be can avoid simultaneously into the 2nd AlN film 123, influence the crystal quality of subsequent epitaxial layer.
Optionally, the linear negative of oxygen content in the thickness of multiple AlNO sublayer 122a and multiple AlNO sublayer 122a
It closes.At this point it is possible to guarantee that the oxygen content in each AlNO sublayer 122a will not be excessive or very few, acquisition crystal thereby may be ensured that
The preferable insert layer 122 of quality.
Illustratively, when the oxygen content in AlNO sublayer 122a increases by 0.1%, the thickness of AlNO sublayer 122a reduces
1%.When the oxygen content in AlNO sublayer 122a reduces 0.1%, the thickness of AlNO sublayer 122a increases 1%.
Optionally, AlN film 120 with a thickness of 30~50nm.If the thickness of AlN film 120 is less than 30nm, do not have
Reduce the effect of compression.If the thickness of AlN film 120 is greater than 50nm, it may still build up biggish pressure in AlN film 120 and answer
Power leads to epitaxial wafer warpage.
Further, the thickness of the first AlN film 121 is greater than the thickness of the 2nd AlN film 123.Due to being sputtered in PVD
120 early period of AlN film, obtained 120 uniformity of AlN film is preferable, and stress is smaller, so the first AlN film 121 is arranged
It is more thick a little and not to be passed through oxygen, it is ensured that the crystal quality of the first certain AlN film 121, however persistently sputtered in PVD
During AlN film 120, especially in the later period of sputtering AlN film 120, the formation nitrogen that Al target material surface can be different degrees of
Change aluminium and alumina species, keep deposition rate slack-off, causes reaction gas that cannot fully be sputtered atom A l absorption, it is excessive residual
Remaining reaction gas will hit target, further target material surface formed compound, make target material surface formed aluminium nitride and
Alumina species are more and more, cause the uniformity of 120 thickness of AlN film to be deteriorated, so the 2nd AlN film layer 123 is arranged
The more thinner uniformity to ensure entire AlN film 120.
Illustratively, the first AlN film 121 with a thickness of 10~15nm, the 2nd AlN film 123 with a thickness of 1~5nm.
Illustratively, insert layer 122 with a thickness of 15~20nm.If the thickness of insert layer 122 is less than 15nm, rise not
It arrives, increases the effect of the lattice constant of AlN film 120.Since O is impurity, if the thickness of insert layer 122 is greater than 20nm, and meeting
The O in AlN film 120 is caused to adulterate crystal quality that is excessive and influencing AlN film 120.
Optionally, insert layer 122 includes n AlNO sublayer 122a, 3≤n≤6.If AlNO sublayer 122 in insert layer 122
Number be less than 3, then cannot achieve oxygen content in multiple AlNO sublayers 122 and first successively increase again successively reduction.If insertion
The number of AlNO sublayer 122 is more than 6 in layer 122, then can be excessive due to the number of plies of AlNO sublayer 122, leads to AlNO sublayer 122
Growth course it is relatively complicated.
Fig. 2 is a kind of structural schematic diagram of LED epitaxial slice provided in an embodiment of the present invention, as shown in Fig. 2, should
LED epitaxial slice 200 includes AlN template 100 as shown in Figure 1 and the epitaxial layer being arranged in AlN template 100.
As shown in Figure 1, AlN template 100 includes substrate 110 and the AlN film 120 deposited on substrate 110.AlN film
120 include the first AlN film 121, insert layer 122 and the 2nd AlN film 123 stacked gradually, and insert layer 122 includes multiple
AlNO sublayer 122a, and the oxygen content in multiple AlNO sublayer 122a first successively increases along the stacking direction of multiple AlNO sublayer 122a
Add successively reduction again.
In the present embodiment, epitaxial layer includes undoped GaN layer 210, the N-type layer being sequentially laminated in AlN template 100
220, multiple quantum well layer 230, electronic barrier layer 240, P-type layer 250 and p-type contact layer 260.
Optionally, the thickness of undoped GaN layer 210 can be 1~4um.
Optionally, N-type layer 220 can be to mix the GaN layer of Si, with a thickness of 1~2um.
Optionally, multiple quantum well layer 230 can be by the In in 4~15 periodsaGa1-aN/GaN superlattice structure composition, 0 < a
<0.5.Wherein, InaGa1-aThe thickness of N well layer can be 3~4nm, and the thickness of GaN barrier layer can be 8~20nm.
Optionally, electronic barrier layer 240 can be the Al for mixing MgbGa1-bN layers, 0.1 <b < 0.5, with a thickness of 10~150nm.
Optionally, P-type layer 250 can be to mix the GaN layer of Mg, with a thickness of 10~500nm.
Optionally, p-type contact layer 260 can be the GaN layer of heavily doped Mg, with a thickness of 5~300nm.
The embodiment of the present invention is by the way that AlN film to be set as including the first AlN film stacked gradually, insert layer and second
AlN film, insert layer include multiple AlNO sublayers, and a part of O atom in AlNO sublayer can substitute N atom, and another part O is former
Son will form interstitial atom, and displacement O atom and calking O atom can all make AlN lattice generate certain distortion, and it is thin to increase AlN
The lattice constant of film keeps the lattice constant of AlN film and subsequent GaN epitaxial film closer, is conducive to reduce in GaN material
Compression improves the warpage of epitaxial wafer, and then improves the wavelength uniformity of the epitaxial layer based on AlN template.Multiple AlNO simultaneously
Oxygen content in sublayer first successively increases along the stacking direction of multiple AlNO sublayers successively to be reduced again, in addition being located at insert layer two sides
The first AlN film and the 2nd AlN film of O are not mixed, and the oxygen content in entire AlN film first successively increases to certain value by 0, can
Sufficiently to discharge the compression accumulated in the first AlN film, prevents the excess oxygen content being passed through and lead to the crystal matter of insert layer
Amount decline；Then it reduces again from certain value to 0, the AlNO film sublayer compared with high-crystal quality can be obtained, oxygen can also be avoided
It infiltrates into the 2nd AlN film, influences the crystal quality of subsequent epitaxial layer.
Fig. 3 is a kind of manufacturing method flow chart of AlN template provided in an embodiment of the present invention, as shown in figure 3, the manufacturer
Method includes:
Step 301 provides a substrate.
Wherein substrate can be Si, SiC, sapphire, ZnO, GaAs, GaP, MgO, Cu and W substrate.Preferably, substrate is
Sapphire Substrate.
Step 302, on substrate depositing Al N thin film.
Wherein, AlN film includes the first AlN film, insert layer and the 2nd AlN film stacked gradually, and insert layer includes
Multiple AlNO sublayers, and first successively increase is layer-by-layer again along the stacking direction of multiple AlNO sublayers for the oxygen content in multiple AlNO sublayers
It reduces.
Further, the thickness of multiple AlNO sublayers first successively reduces along the stacking direction of multiple AlNO sublayers and successively increases again
Greatly.
Optionally, the thickness of multiple AlNO sublayers and the oxygen content in multiple AlNO sublayers are linearly negatively correlated.At this point, can
Will not be excessive or very few with the oxygen content guaranteed in each AlNO sublayer, it thereby may be ensured that obtaining crystal quality is preferably inserted into
Layer.
Illustratively, when the oxygen content in AlNO sublayer increases by 0.1%, the thickness of AlNO sublayer reduces 1%.Work as AlNO
When oxygen content in sublayer reduces 0.1%, the thickness of AlNO sublayer increases 1%.
Optionally, AlN film with a thickness of 30~50nm.
Further, the thickness of the first AlN film is greater than the thickness of the 2nd AlN film.
Illustratively, the first AlN film with a thickness of 10~15nm, the 2nd AlN film with a thickness of 1~5nm.
Illustratively, insert layer with a thickness of 15~20nm.
Optionally, insert layer includes n AlNO sublayer, 3≤n≤6.
Specifically, step 302 may include:
Substrate is arranged in vacuum environment, and toasts to substrate by the first step.
Illustratively, Sapphire Substrate is placed on the pallet of SiC material, pallet is put into PVD sputtering machine table, and pass
It send into the reaction chamber of PVD.Then reaction chamber is vacuumized, until the pressure in reaction chamber is lower than 1*10-7torr。
Controlling reaction chamber temperature is 350~700 DEG C, is toasted to substrate, and baking time is 2~12 minutes.
Second step is completed after toasting, under the atmosphere for being mixed with argon gas, nitrogen and oxygen, using magnetron sputtering skill
Art sputters Al target, with depositing Al N thin film on substrate.
During depositing Al N thin film, the flow of oxygen is first gradually increased, then gradually decreases the flow of oxygen, so that
The oxygen content obtained in multiple AlNO sublayers first successively increases again successively reduction along the stacking direction of multiple AlNO sublayers.
Specifically, during depositing Al N thin film, control reaction chamber temperature be 500~700 DEG C, pressure be 1~
10mtorr。
Optionally, the sputtering power of magnetron sputtering is 2~6kW.
In the present embodiment, target-substrate distance can be 40~90mm.Be conducive to uniform AlN is formed on the substrate at this time thin
Film.If target-substrate distance is crossed less than 40mm, part is not combined effectively the Al atom to form AlN that can fall on substrate with N atom, meeting
Cause the impurity contained in the AlN film of deposition more.If target-substrate distance is greater than 90mm, it is unfavorable for AlN film and deposits well
On substrate, AlN film deposition rate is slower.
Optionally, the flow-rate ratio of argon gas and nitrogen is 1:2~1:10.
Illustratively, the flow of argon gas can be 20~80sccm, and the flow of nitrogen can be 50~300sccm.
Further, during depositing Al N thin film, the flow-rate ratio of argon gas and nitrogen is gradually increased.In sputtering sedimentation
During AlN film, the embryo deposit rate of AlN film is very fast, with the progress of sputtering, what target material surface can be different degrees of
Aluminium nitride and alumina species are formed, keeps deposition rate slack-off, leads to reaction gas (N2、O2) it cannot fully be sputtered atom
Al absorbs.The reaction gas of excessive residual will hit target, further form compound in target material surface, make target material surface
Aluminium nitride and alumina species are more and more, and the uniformity of AlN film thickness is caused to be deteriorated, and increase argon gas and nitrogen in the sputtering later period
The flow-rate ratio of gas can reinforce the bombardment to target atom, improve sputter rate, make to keep similar thin in entire sputtering process
Film deposition rate, so as to improve the uniformity of AlN film, the final uniformity for improving epitaxial wafer.
Illustratively, when depositing close to the first AlN film of substrate, the flow-rate ratio of argon gas and nitrogen is minimum, is 1:2.It is heavy
When product is close to the 2nd AlN film layer of epitaxial layer, the flow-rate ratio of argon gas and nitrogen is maximum, is 1:10.
Optionally, the flow of oxygen is the 1%~10% of the sum of argon gas and nitrogen flow.If the flow of oxygen is less than argon gas
With the 1% of the sum of nitrogen flow, then it is unfavorable for the release of AlN stress in thin films.If the flow of oxygen is greater than argon gas and nitrogen stream
The 10% of the sum of amount then will lead to the crystal quality decline of AlN film.
Illustratively, the flow of oxygen can be 0~5sccm.Argon gas, nitrogen, oxygen three total gas couette by PVD
Deposition chambers pressure maintains 1~10mTorr and is preferred.
Optionally, magnetron sputtering power supply uses the pulse power, during depositing Al N thin film, the frequency of the pulse power
It is gradually increased.Due to relatively large in the argon gas in sputtering later period and the ratio of nitrogen, the deposition rate of film is strengthened, at this time
Increase pulse frequency, duty ratio can be improved, increase the service efficiency of power supply.
Optionally, the frequency of the pulse power is 100~350kHz.
Illustratively, when depositing close to the first AlN film of substrate, pulse frequency is minimum, is 100kHz.Deposition is close to outer
When prolonging the 2nd AlN film layer of layer, pulse frequency is maximum, is 350kHz.
Optionally, when depositing Al N thin film, pulse frequency can be incremented by according to 50~100kHz amplitude.
The embodiment of the present invention is by the way that AlN film to be set as including the first AlN film stacked gradually, insert layer and second
AlN film, insert layer include multiple AlNO sublayers, and a part of O atom in AlNO sublayer can substitute N atom, and another part O is former
Son will form interstitial atom, and displacement O atom and calking O atom can all make AlN lattice generate certain distortion, and it is thin to increase AlN
The lattice constant of film keeps the lattice constant of AlN film and subsequent GaN epitaxial film closer, is conducive to reduce in GaN material
Compression improves the warpage of epitaxial wafer, and then improves the wavelength uniformity of the epitaxial layer based on AlN template.Multiple AlNO simultaneously
Oxygen content in sublayer first successively increases along the stacking direction of multiple AlNO sublayers successively to be reduced again, in addition being located at insert layer two sides
The first AlN film and the 2nd AlN film of O are not mixed, and the oxygen content in entire AlN film first successively increases to certain value by 0, can
Sufficiently to discharge the compression accumulated in the first AlN film, prevents the excess oxygen content being passed through and lead to the crystal matter of insert layer
Amount decline；Then it reduces again from certain value to 0, the AlNO film sublayer compared with high-crystal quality can be obtained, oxygen can also be avoided
It infiltrates into the 2nd AlN film, influences the crystal quality of subsequent epitaxial layer.
Fig. 4 is a kind of manufacturing method flow chart of LED epitaxial slice provided in an embodiment of the present invention, such as Fig. 4 institute
Show, which includes:
Step 401 provides a substrate.
Wherein substrate can be Si, SiC, sapphire, ZnO, GaAs, GaP, MgO, Cu and W substrate.Preferably, substrate is
Sapphire Substrate.
Step 402, on substrate depositing Al N thin film.
Wherein, AlN film includes the first AlN film, insert layer and the 2nd AlN film stacked gradually, and insert layer includes
Multiple AlNO sublayers, and first successively increase is layer-by-layer again along the stacking direction of multiple AlNO sublayers for the oxygen content in multiple AlNO sublayers
It reduces.
Further, the thickness of multiple AlNO sublayers first successively reduces along the stacking direction of multiple AlNO sublayers and successively increases again
Greatly.
Optionally, the thickness of multiple AlNO sublayers and the oxygen content in multiple AlNO sublayers are linearly negatively correlated.At this point, can
Will not be excessive or very few with the oxygen content guaranteed in each AlNO sublayer, it thereby may be ensured that obtaining crystal quality is preferably inserted into
Layer.
Illustratively, when the oxygen content in AlNO sublayer increases by 0.1%, the thickness of AlNO sublayer reduces 1%.Work as AlNO
When oxygen content in sublayer reduces 0.1%, the thickness of AlNO sublayer increases 1%.
Optionally, AlN film with a thickness of 30~50nm.
Further, the thickness of the first AlN film is greater than the thickness of the 2nd AlN film.
Illustratively, the first AlN film with a thickness of 10~15nm, the 2nd AlN film with a thickness of 1~5nm.
Illustratively, insert layer with a thickness of 15~20nm.
Optionally, insert layer includes n AlNO sublayer, 3≤n≤6.
Specifically, step 402 may include:
Substrate is arranged in vacuum environment, and toasts to substrate by the first step.
Illustratively, Sapphire Substrate is placed on the pallet of SiC material, pallet is put into PVD sputtering machine table, and pass
It send into the reaction chamber of PVD.Then reaction chamber is vacuumized, until the pressure in reaction chamber is lower than 1*10-7torr。
Controlling reaction chamber temperature is 350~700 DEG C, is toasted to substrate, and baking time is 2~12min.
Second step is completed after toasting, under the atmosphere for being mixed with argon gas, nitrogen and oxygen, using magnetron sputtering skill
Art sputters Al target, with depositing Al N thin film on substrate.
During depositing Al N thin film, the flow of oxygen is first gradually increased, then gradually decreases oxygen flow, so that
Oxygen content in multiple AlNO sublayers first successively increases along the stacking direction of multiple AlNO sublayers successively to be reduced again.
Specifically, during depositing Al N thin film, control reaction chamber temperature be 500~700 DEG C, pressure be 1~
10mtorr。
Optionally, the sputtering power of magnetron sputtering is 2~6kW.
In the present embodiment, target-substrate distance can be 40~90mm.
Optionally, the flow-rate ratio of argon gas and nitrogen is 1:2~1:10.
Illustratively, the flow of argon gas can be 20~80sccm, and the flow of nitrogen can be 50~300sccm.
Further, during depositing Al N thin film, the flow-rate ratio of argon gas and nitrogen is gradually increased.
Illustratively, when depositing close to the first AlN film of substrate, the flow-rate ratio of argon gas and nitrogen is minimum, is 1:2.It is heavy
When product is close to the 2nd AlN film layer of epitaxial layer, the flow-rate ratio of argon gas and nitrogen is maximum, is 1:10.
Optionally, the flow of oxygen is the 1%~10% of the sum of argon gas and nitrogen flow.
Illustratively, the flow of oxygen can be 0~5sccm.Argon gas, nitrogen, oxygen three total gas couette by PVD
Deposition chambers pressure maintains 1~10mTorr and is preferred.
Optionally, magnetron sputtering power supply uses the pulse power, during depositing Al N thin film, the frequency of the pulse power
It is gradually increased.Due to relatively large in the argon gas in sputtering later period and the ratio of nitrogen, the deposition rate of film is strengthened, at this time
Increase pulse frequency, duty ratio can be improved, increase the service efficiency of power supply.
Optionally, the frequency of the pulse power is 100~350kHz.
Illustratively, when depositing close to the first AlN film of substrate, pulse frequency is minimum, is 100kHz.Deposition is close to outer
When prolonging the 2nd AlN film layer of layer, pulse frequency is maximum, is 350kHz.
Optionally, when depositing Al N thin film, pulse frequency can be incremented by according to 50~100kHz amplitude.
AlN template is put into metallo-organic compound chemical gaseous phase deposition equipment by step 403.
Specifically, after executing the step 403, the substrate to be deposited for having AlN buffer layer is cooled to room temperature, and will be deposited with AlN
The substrate of buffer layer takes out from PVD equipment, is then placed on feeding MOCVD (Metal-organic on graphite pallet
Chemical Vapor Deposition, metallo-organic compound chemical gaseous phase deposition) equipment reaction chamber in carry out extension material
The growth of material.
In the present embodiment, using trimethyl gallium or triethyl-gallium gallium source, high pure nitrogen is as nitrogen source, trimethyl indium conduct
Indium source, for boron triethyl as boron source, N type dopant selects silane, and P-type dopant selects two luxuriant magnesium.
Further, step 403 can also include:
The substrate for being deposited with AlN buffer layer is placed on progress in-situ annealing processing, annealing temperature in the reaction chamber of MOCVD
It is 1000~1200 DEG C, annealing pressure is 200~500torr, and annealing time is 5~10min, to remove impurity.
It should be noted that in the present embodiment, epitaxial layer may include be sequentially laminated on it is undoped in AlN template
GaN layer, N-type layer, multiple quantum well layer, electronic barrier layer, P-type layer and p-type contact layer.Each layer in epitaxial layer can use
The growth of MOCVD method.Therefore the temperature and pressure controlled in following growth courses actually refers to that MOCVD reacts indoor temperature
And pressure.
Step 404 grows undoped GaN layer in AlN template.
Illustratively, reaction chamber temperature being adjusted to 1000~1100 DEG C, chamber pressure is controlled in 100~300torr,
Growth thickness is the undoped GaN layer of 1~4um.
Step 405 grows N-type layer in undoped GaN layer.
In the present embodiment, N-type layer can be to mix the GaN layer of Si, and Si doping concentration can be 1018cm-3~1019cm-3。
Illustratively, reaction chamber temperature being adjusted to 1000~1200 DEG C, chamber pressure is controlled in 100~300torr,
Growth thickness is the N-type layer of 1~5um.
Step 406 grows multiple quantum well layer in N-type layer.
In the present embodiment, multiple quantum well layer by 4~15 periods InaGa1-aN/GaN superlattice structure composition, 0 < a <
0.5。
Illustratively, reaction chamber temperature is adjusted to 725~825 DEG C, chamber pressure control is in 100~500torr, life
The long In with a thickness of 3~4nmaGa1-aN well layer.Reaction chamber temperature is adjusted to 845~955 DEG C, chamber pressure is controlled 100
~500torr, growth thickness are the GaN barrier layer of 8~20nm.
Step 407 grows electronic barrier layer on multiple quantum well layer.
Wherein, electronic barrier layer can be the Al for mixing MgbGa1-bN layers, 0.1 <b < 0.5.
Illustratively, reaction chamber temperature being adjusted to 855~1085 DEG C, chamber pressure is controlled in 100~500torr,
Growth thickness is the electronic barrier layer of 10~150nm.
Step 408, the growing P-type layer on electronic barrier layer.
In the present embodiment, P-type layer can be to mix the GaN layer of Mg.
Illustratively, reaction chamber temperature being adjusted to 855~1085 DEG C, chamber pressure is controlled in 100~600torr,
Growth thickness is the P-type layer of 10~500nm.
Step 409, the growing P-type contact layer in P-type layer.
Wherein, p-type contact layer can be the GaN layer of heavily doped Mg, and p-type contact layer be laid on p type semiconductor layer, with core
Ohmic contact is formed between the transparent conductive film or electrode formed in piece manufacture craft.
Illustratively, reaction chamber temperature being adjusted to 855~1065 DEG C, chamber pressure is controlled in 100~600torr,
Growth thickness is the p-type contact layer of 5~300nm.
After above-mentioned steps completion, the temperature of reaction chamber is down to 650~850 DEG C, is carried out at annealing in nitrogen atmosphere
5~15min is managed, room temperature is then gradually decreased to, terminates the epitaxial growth of light emitting diode.
The embodiment of the present invention is by the way that AlN film to be set as including the first AlN film stacked gradually, insert layer and second
AlN film, insert layer include multiple AlNO sublayers, and a part of O atom in AlNO sublayer can substitute N atom, and another part O is former
Son will form interstitial atom, and displacement O atom and calking O atom can all make AlN lattice generate certain distortion, and it is thin to increase AlN
The lattice constant of film keeps the lattice constant of AlN film and subsequent GaN epitaxial film closer, is conducive to reduce in GaN material
Compression improves the warpage of epitaxial wafer, and then improves the wavelength uniformity of the epitaxial layer based on AlN template.Multiple AlNO simultaneously
Oxygen content in sublayer first successively increases along the stacking direction of multiple AlNO sublayers successively to be reduced again, in addition being located at insert layer two sides
The first AlN film and the 2nd AlN film of O are not mixed, and the oxygen content in entire AlN film first successively increases to certain value by 0, can
Sufficiently to discharge the compression accumulated in the first AlN film, prevents the excess oxygen content being passed through and lead to the crystal matter of insert layer
Amount decline；Then it reduces again from certain value to 0, the AlNO film sublayer compared with high-crystal quality can be obtained, oxygen can also be avoided
It infiltrates into the 2nd AlN film, influences the crystal quality of subsequent epitaxial layer.
The foregoing is merely a prefered embodiment of the invention, is not intended to limit the invention, all in the spirit and principles in the present invention
Within, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of AlN template, the AlN film that deposits including substrate and over the substrate, which is characterized in that
The AlN film includes the first AlN film, insert layer and the 2nd AlN film stacked gradually, and the insert layer includes more
A AlNO sublayer, and the oxygen content in the multiple AlNO sublayer first successively increases along the stacking direction of the multiple AlNO sublayer
It successively reduces again.
2. AlN template according to claim 1, which is characterized in that the thickness of the multiple AlNO sublayer is along the multiple
The stacking direction of AlNO sublayer first successively reduces and successively increases again.
3. AlN template according to claim 2, which is characterized in that the thickness of the multiple AlNO sublayer with it is the multiple
Oxygen content in AlNO sublayer is linearly negatively correlated.
4. AlN template according to claim 3, which is characterized in that the thickness of the first AlN film is greater than described second
The thickness of AlN film.
5. a kind of LED epitaxial slice, which is characterized in that the LED epitaxial slice includes such as Claims 1 to 4
Described in any item AlN templates and the epitaxial layer being arranged in the AlN template.
6. a kind of manufacturing method of AlN template, which is characterized in that the manufacturing method includes:
One substrate is provided；
Depositing Al N thin film over the substrate；The AlN film includes the first AlN film stacked gradually, insert layer and second
AlN film, the insert layer includes multiple AlNO sublayers, and the oxygen content in the multiple AlNO sublayer is along the multiple AlNO
The stacking direction of sublayer first successively increases successively to be reduced again.
7. manufacturing method according to claim 6, which is characterized in that the depositing Al N thin film over the substrate, packet
It includes:
Under the atmosphere for being mixed with argon gas, nitrogen and oxygen, Al target is sputtered using magnetron sputtering technique, with
The AlN film is deposited on the substrate；During depositing the AlN film, the flow of the oxygen is first gradually increased,
The flow of the oxygen is gradually decreased again.
8. manufacturing method according to claim 7, which is characterized in that during depositing the AlN film, the argon
The flow-rate ratio of gas and the nitrogen is gradually increased.
9. manufacturing method according to claim 7, which is characterized in that magnetron sputtering power supply uses the pulse power, is depositing
During the AlN film, the frequency of the pulse power is gradually increased.
10. a kind of manufacturing method of LED epitaxial slice, which is characterized in that the manufacturing method includes:
One substrate is provided；
Depositing Al N thin film over the substrate；The AlN film includes the first AlN film stacked gradually, insert layer and second
AlN film, the insert layer includes multiple AlNO sublayers, and the oxygen content in the multiple AlNO sublayer is along the multiple AlNO
The stacking direction of sublayer first successively increases successively to be reduced again；
In the AlN film growing epitaxial layers.
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