CN110098287A - The manufacturing method of AlN template and LED epitaxial slice - Google Patents
The manufacturing method of AlN template and LED epitaxial slice Download PDFInfo
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- CN110098287A CN110098287A CN201910209256.6A CN201910209256A CN110098287A CN 110098287 A CN110098287 A CN 110098287A CN 201910209256 A CN201910209256 A CN 201910209256A CN 110098287 A CN110098287 A CN 110098287A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 238000000151 deposition Methods 0.000 claims abstract description 136
- 239000000758 substrate Substances 0.000 claims abstract description 69
- 230000008021 deposition Effects 0.000 claims abstract description 30
- 238000005137 deposition process Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 11
- 230000006835 compression Effects 0.000 abstract description 5
- 238000007906 compression Methods 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 125000004429 atom Chemical group 0.000 description 28
- 229910052782 aluminium Inorganic materials 0.000 description 25
- 230000012010 growth Effects 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 20
- 238000005240 physical vapour deposition Methods 0.000 description 15
- 238000010586 diagram Methods 0.000 description 12
- 230000002776 aggregation Effects 0.000 description 11
- 238000004220 aggregation Methods 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 10
- 230000004888 barrier function Effects 0.000 description 9
- 239000010980 sapphire Substances 0.000 description 8
- 229910052594 sapphire Inorganic materials 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000000137 annealing Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 3
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- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- 229910016920 AlzGa1−z Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
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- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
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- LALRXNPLTWZJIJ-UHFFFAOYSA-N triethylborane Chemical group CCB(CC)CC LALRXNPLTWZJIJ-UHFFFAOYSA-N 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0062—Processes for devices with an active region comprising only III-V compounds
- H01L33/0066—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound
- H01L33/007—Processes for devices with an active region comprising only III-V compounds with a substrate not being a III-V compound comprising nitride compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/12—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a stress relaxation structure, e.g. buffer layer
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Led Devices (AREA)
Abstract
The invention discloses a kind of AlN template and the manufacturing methods of LED epitaxial slice, belong to technical field of semiconductors.Manufacturing method includes: to be sequentially depositing multiple AlN sublayers on substrate, obtains AlN template, and on the direction far from substrate, the depositing temperature of multiple AlN sublayers is gradually increased；Wherein, it is sequentially depositing multiple AlN sublayers on substrate, comprising: after one AlN sublayer of deposition, interrupt the deposition of AlN sublayer；It is depositing in the deposition break period after an AlN sublayer, the depositing temperature of AlN sublayer is being increased；Deposit next AlN sublayer.Manufacturing method provided by the invention can improve the uniformity of the AlN film of formation, reduce the compression in AlN film, improve the luminous efficiency of LED.
Description
Technical field
The present invention relates to technical field of semiconductors, in particular to the system of a kind of AlN template and LED epitaxial slice
Make method.
Background technique
In recent years, light emitting diode (Light Emitting Diode, abbreviation LED) is used as new generation of green light source, just
It is being widely used in the fields such as illumination, backlight, display, instruction.
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 often using AlN film as buffer layer
It is placed between Sapphire Substrate and GaN.
In the implementation of the present invention, the inventor finds that the existing technology has at least the following problems:
Existing AlN film is usually to grow under the conditions of cryogenic thermostat, may result in the AlN film grown
It is in uneven thickness, to influence the crystal quality of GaN epitaxial layer grown on it, reduce the luminous efficiency of LED.Meanwhile
Due to that, there are compression, can make AlN film that warpage occur, and the depositing temperature of AlN film is got between AlN and GaN epitaxial layer
The warpage of height, AlN film is more serious.Therefore, according to high temperature constant temperature growing AIN film, and AlN layers and subsequent GaN be will lead to
Matching between epitaxial layer is poor, and the wavelength uniformity of epitaxial wafer is poorer, and the luminous efficiency of LED is lower.
Summary of the invention
The embodiment of the invention provides a kind of AlN template and the manufacturing methods of LED epitaxial slice, can improve
The uniformity of the AlN film of formation reduces the compression in AlN film, improves the luminous efficiency of LED.The technical solution is such as
Under:
In a first aspect, providing a kind of manufacturing method of AlN template, the manufacturing method includes:
It is sequentially depositing multiple AlN sublayers on substrate, obtains AlN template, on the direction far from the substrate, Duo Gesuo
The depositing temperature for stating AlN sublayer is gradually increased；
It is described to be sequentially depositing multiple AlN sublayers on substrate, comprising:
After depositing an AlN sublayer, the deposition of the AlN sublayer is interrupted；
It is depositing in the deposition break period after an AlN sublayer, the depositing temperature of the AlN sublayer is being increased；
Deposit next AlN sublayer.
Further, the depositing temperature of each AlN sublayer during the deposition process remains unchanged.
Further, the difference of the depositing temperature of two adjacent AlN sublayers is 50~100 DEG C.
Further, the difference of the depositing temperature of two adjacent AlN sublayers is equal.
Further, the depositing temperature of each AlN sublayer during the deposition process is gradually increased.
Further, the depositing temperature of each AlN sublayer is 500~700 DEG C.
Further, the thickness of each AlN sublayer is equal.
Further, each AlN sublayer with a thickness of 5~8nm.
Further, the deposition break period after one AlN sublayer of every deposition is t, 5≤t≤10s.
Second aspect, provides a kind of manufacturing method of LED epitaxial slice, and the manufacturing method includes:
AlN template is manufactured using manufacturing method described in first aspect；
In the AlN template growing epitaxial layers.
Technical solution provided in an embodiment of the present invention has the benefit that
By depositing multiple AlN sublayers on substrate, AlN template is obtained.Since the thickness of AlN film is thicker, Al atom
Aggregation it is more serious, therefore far from substrate direction on, the depositing temperature of multiple AlN sublayers is gradually increased, and can gradually be added
The diffusivity of Al atom in strong each AlN sublayer, reduces the aggregation of Al atom, so as to improve formation AlN film it is uniform
Property, guarantee the crystal quality of the GaN epitaxial layer grown on AlN film, and then improve the luminous efficiency of LED.Meanwhile the present invention
By after depositing an AlN sublayer, interrupting the deposition of AlN sublayer, and the deposition break period after depositing an AlN sublayer
It is interior, the depositing temperature of AlN sublayer is increased, the AlN sublayer deposited can be made to keep a period of time in certain temperature, with
The stress accumulated in release AlN sublayer, then proceedes to deposit next AlN sublayer, the mode of the interruption of growth can reduce AlN
The stress accumulated in layer improves the AlN layers of matching between subsequent GaN epitaxial layer to reduce the warpage of AlN, improves outer
Prolong the wavelength uniformity of piece, and then improves the luminous efficiency of LED.
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 the depositional model schematic diagram of traditional AlN film；
Fig. 2 is a kind of structural schematic diagram of PVD equipment 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 structural schematic diagram of AlN template provided in an embodiment of the present invention；
Fig. 5 is the manufacturing method flow chart of another kind AlN template provided in an embodiment of the present invention；
Fig. 6 is a kind of depositional model schematic diagram of multiple AlN sublayers provided in an embodiment of the present invention；
Fig. 7 is the depositional model schematic diagram of the multiple AlN sublayers of another kind provided in an embodiment of the present invention；
Fig. 8 is a kind of manufacturing method flow chart of LED epitaxial slice provided in an embodiment of the present invention；
Fig. 9 is a kind of structural schematic diagram 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.
In order to better understand the present invention, below in conjunction with the depositional model of AlN film traditional under brief description of the drawings:
Fig. 1 is the depositional model schematic diagram of traditional AlN film, as shown in Figure 1, traditional AlN film is using low temperature
Made of the growth pattern growth of constant temperature.Illustratively, by substrate be placed on PVD (Physical Vapor Deposition,
Physical vapour deposition (PVD)) in equipment, deposition obtains AlN film on substrate.
Fig. 2 is a kind of structural schematic diagram of PVD equipment provided in an embodiment of the present invention, as shown in Fig. 2, PVD equipment includes
Magnetron 210, Al target 220, substrate pallet 230, heating fluorescent tube 240 and the power supply set gradually from top to bottom (does not show in figure
Out), Al target 220 is connect with the cathode of power supply, and substrate pallet 230 is arranged on the anode of power supply.Magnetron 210 is for providing
Magnetic field, for providing electric field, reaction gas will form power supply under the action of the Coulomb force of the Lorentz force in magnetic field and electric field
Gas ions nearby move in a circle along target material surface.Substrate 100 is placed on substrate pallet 230, and heating fluorescent tube 240 is for heating
Substrate pallet 230, to change substrate temperature, to change the depositing temperature of AlN film.
PVD equipment further includes the baffle 250 being arranged between Al target 220 and substrate pallet 230, and baffle 250 is removable
To between Al target 220 and substrate pallet 230, for interrupting the growth of AlN film.
Illustratively, as shown in Fig. 2, when baffle 250 be arranged in the substrate 100 on Al target 220 and substrate pallet 230 it
Between when, baffle 250 can play barrier effect so that formed AlN film be deposited on baffle 250, without deposit to lining
On bottom 100.When baffle 250 is arranged when except Al target 320 and substrate 200, the AlN film of formation can be deposited on substrate
On 100.
Specifically, the forming process of AlN film is as follows: Sapphire Substrate is placed on the substrate pallet of PVD equipment,
Apply voltage between power cathode and anode, the Ar atom in Ar gas is ionized under voltage effect, and ionization process makes part Ar
Atom ionization becomes Ar ion and electronics.Electronics accelerates to fly to substrate, and Ar during flying to substrate under voltage effect
Ar atom in gas collides, and ionizes out a large amount of Ar ion and new electronics, and new electronics continues and Ar atomic collision, production
Raw more Ar ions and electronics.Ar ion accelerates bombardment Al target under voltage effect, and Al target can sputter Al atom, Al
Atom and N2N atomic reaction in gas, AlN film is formed on the substrate.
But with the deposition of AlN film, AlN film, the non-shape in surface also will form in the partial region of Al target material surface
The sputter rate in the region of AlN film is formed with faster at the region specific surface of AlN film, therefore the not formed AlN film in surface
The part Al atom that sputters of region can be deposited directly on substrate, AlN film is then formed in conjunction with N atom again.When splashing
When the Al atom shot out is deposited directly on substrate, may some regions aggregation on substrate, the Al of concentrating portions is former
Son cannot form AlN film with N atom fast reaction, therefore will cause the thickness of the AlN film of Al atom aggregation zone formation
It is relatively thin, so that the uniformity of AlN film is deteriorated.
The embodiment of the invention provides a kind of manufacturing methods of AlN template, can guarantee the crystal quality of AlN film
Under the premise of, improve the uniformity of the AlN film of formation.Fig. 3 is a kind of manufacturing method of AlN template provided in an embodiment of the present invention
Flow chart, as shown in figure 3, the manufacturing method includes:
Step 301 provides a substrate.
In the present embodiment, substrate can be Sapphire Substrate.
After executing step 301, before executing step 302, which can also include:
It places the substrate on the substrate pallet of PVD equipment, substrate is sent into the reaction chamber of PVD equipment；
The reaction chamber of PVD equipment is vacuumized, starts to carry out heat temperature raising to substrate while vacuumizing, works as substrate vacuum
It is evacuated to lower than 1*10-7When torr, by heating temperature stablize at 400~600 DEG C, substrate is toasted, baking time be 2~
12min。
Optionally, target-substrate distance (i.e. the distance of Al target to substrate pallet) can be set to 40~90mm, be conducive to serving as a contrast
Uniform AlN film is formed on bottom.
Optionally, before executing step 302, which can also include:
Step a, Ar, N are passed through into the reaction chamber of PVD equipment2And O2, and chamber pressure is made to maintain 1~12mtorr.
Wherein, the Ar and N being passed through2Flow-rate ratio be 1:2~1:10, Ar and N2Flow be 20~300sccm, O2Stream
Amount is Ar and N20%~5%, O of the sum of flow2Flow be 0~3sccm.
By being passed through O in the reaction chamber to PVD2, making to mix O in multiple AlN sublayers, a part of O atom 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 centainly abnormal
Become, increases the lattice constant of AlN sublayer, keep the lattice constant of AlN sublayer and subsequent GaN epitaxial layer closer, be conducive to reduce
Compression in GaN material improves the warpage of GaN epitaxial layer.
Step b, the temperature setting of fluorescent tube will be heated to the depositing temperature of multiple AlN sublayers.
In the present embodiment, the depositing temperature of multiple AlN sublayers is 500~700 DEG C, at this time the deposition of multiple AlN sublayers
Temperature is lower, it is ensured that the crystal quality of the multiple AlN sublayers deposited.
Step c, after so that depositing temperature is stablized 10~60s, power supply is opened, opens baffle, pre-sputtering is carried out to Al target
10~20s.
In the present embodiment, power supply uses the pulse power, and the pulse frequency of the pulse power immobilizes, 200kHz~
Between 300kHz range, the duty ratio of the pulse power is remained unchanged, between 20%~70%.The power of the pulse power is kept not
Become, between 1kw~6kw.
Step 302 is sequentially depositing multiple AlN sublayers on substrate, obtains AlN template.
Wherein, on the direction far from substrate, the depositing temperature of multiple AlN sublayers is gradually increased.
Further, step 302 may include:
After depositing an AlN sublayer, the deposition of AlN sublayer is interrupted；
It is depositing in the deposition break period after an AlN sublayer, the depositing temperature of AlN sublayer is being increased；
Deposit next AlN sublayer.
On the one hand, since there are compression between multiple AlN sublayers (hereinafter referred to as AlN layers) and GaN epitaxial layer, can make
AlN layers of generation warpage, AlN layers of depositing temperature is higher, and AlN layers of warpage is more convex, between AlN layers and subsequent GaN epitaxial layer
Matching is poorer, and the wavelength uniformity of epitaxial wafer is poorer, lower so as to cause the luminous efficiency of LED.Therefore by multiple AlN
The depositing temperature of sublayer is set as being gradually risen by low temperature, is conducive to discharge the stress in multiple AlN sublayers.On the other hand, more
The depositing temperature of a AlN sublayer is higher, and the diffusivity of Al atom is better, if but the depositing temperature of multiple AlN sublayers begins
High value is maintained eventually, and AlN layers of warpage can be partially convex always, is unfavorable for the control of warpage, and can make the heavy of multiple AlN sublayers
Accumulated temperature degree influences the service life of Al target close to the melting temperature of Al target.Therefore, by the depositing temperature of each AlN sublayer
It is set as being gradually risen by low, the depositing temperature of multiple AlN sublayers can be prevented persistently to be maintained close to the fusing point temperature of Al target
Degree.
Fig. 4 is a kind of structural schematic diagram of AlN template provided in an embodiment of the present invention, as shown in figure 4, AlN template 400 is wrapped
The multiple AlN sublayers 420 for including substrate 410 and being deposited on substrate 410.
Optionally, the thickness of each AlN sublayer 420 is equal.Set quantitative for the thickness of each AlN sublayer, then only
The diffusivity of Al atom and the warpage degree of AlN sublayer in the i.e. changeable AlN sublayer of depositing temperature need to be changed, so as to
To the value of optimal depositing temperature.
In another implementation of the invention, the thickness of each AlN sublayer can also be unequal.For example, along more
The thickness of the stacking direction of a AlN sublayer 420, each AlN sublayer is gradually reduced.
Optionally, each AlN sublayer 420 with a thickness of 5~8nm.It can guarantee accumulate in each AlN sublayer at this time
Biggish stress generates warpage.
In another implementation of the invention, the thickness of each AlN sublayer 420 might be less that 5nm or be greater than
8nm。
Optionally, the overall thickness of multiple AlN sublayers 420 is 10~70nm, can both guarantee multiple AlN sublayers 420 at this time
Play the role of reducing the lattice mismatch between substrate and GaN epitaxial layer, and can guarantee tire out in multiple AlN sublayers 420
The larger stress of product, generates warpage.
In another implementation of the invention, the overall thickness of multiple AlN sublayers 420 might be less that 10nm, at this time
Multiple AlN sublayers 420 can still play the role of reducing the lattice mismatch between substrate and GaN epitaxial layer.
Illustratively, the first AlN sublayer, the 2nd AlN sublayer and the 3rd AlN sublayer, the first AlN have been sequentially depositing on substrate
The depositing temperature of sublayer, the 2nd AlN sublayer and the 3rd AlN sublayer is 500~700 DEG C, and the depositing temperature of the 3rd AlN sublayer
Greater than the depositing temperature of the 2nd AlN sublayer, the depositing temperature of the 2nd AlN sublayer is greater than the depositing temperature of the first AlN sublayer.
The embodiment of the present invention obtains AlN template by depositing multiple AlN sublayers on substrate.Due to the thickness of AlN film
Thicker, the aggregation of Al atom is more serious, therefore on the direction far from substrate, the depositing temperature of multiple AlN sublayers is gradually increased,
The diffusivity of Al atom in each AlN sublayer can gradually be reinforced, the aggregation of Al atom is reduced, so as to improve the AlN of formation
The uniformity of film guarantees the crystal quality of the GaN epitaxial layer grown on AlN film, and then improves the luminous efficiency of LED.
Meanwhile the present invention is by interrupting the deposition of AlN sublayer, and after depositing an AlN sublayer after depositing an AlN sublayer
It deposits in the break period, the depositing temperature of AlN sublayer is increased, the AlN sublayer deposited can be made to protect in certain temperature
A period of time is held, to discharge the stress accumulated in AlN sublayer, then proceedes to deposit next AlN sublayer, the mode of the interruption of growth
The stress accumulated in AlN sublayer can be reduced, to reduce the warpage of AlN, improves AlN layers between subsequent GaN epitaxial layer
Matching improves the wavelength uniformity of epitaxial wafer, and then improves the luminous efficiency of LED.
The embodiment of the invention provides the manufacturing methods of another AlN template, only exist with the difference of above-described embodiment
In the depositional mode of multiple AlN sublayers is different.Fig. 5 is the manufacturer of another kind AlN template provided in an embodiment of the present invention
Method flow chart, as shown in figure 5, the manufacturing method includes:
Step 501 provides a substrate.
In the present embodiment, substrate is Sapphire Substrate.
Step 502 deposits an AlN sublayer on substrate.
Step 503, the deposition for interrupting AlN sublayer, and the depositing temperature of AlN sublayer is increased.
In the present embodiment, the deposition break period after depositing an AlN sublayer can be t, 5≤t≤10s.T's is specific
Value can be determined according to the heating rate of heating fluorescent tube and the difference of the first depositing temperature and the second depositing temperature.Example
Such as, when the highest heating rate of heating fluorescent tube is about 10 DEG C/s, the difference of the first depositing temperature and the second depositing temperature is 50 DEG C
When, the value of t is 5s.
In specific implementation, the growth that AlN sublayer can be interrupted by moving stop, by the temperature for changing heating fluorescent tube
Degree increases the depositing temperature of AlN sublayer.
Step 504, the next AlN sublayer of deposition.
Step 505 repeats step 503 to step 504, until being sequentially depositing multiple AlN sublayers on substrate, obtains AlN
Template.
Wherein, on the direction far from substrate, the depositing temperature of multiple AlN sublayers is gradually increased.
In a kind of implementation of the present embodiment, the depositing temperature of each AlN sublayer during the deposition process is remained unchanged,
Then each AlN sublayer deposits under the depositing temperature of setting, thereby may be ensured that the diffusion energy of Al atom in each AlN sublayer
Power reduces the aggregation of Al atom in each AlN sublayer.
Optionally, the difference of the depositing temperature of two adjacent AlN sublayers is 50~100 DEG C.At this point it is possible to guarantee each
The depositing temperature gentle transition of AlN sublayer, the depositing temperature between each AlN sublayer will not have big difference or too small.If AlN
Depositing temperature between layer has big difference, and it is larger to will lead to increasing extent of temperature, and the heating-up time needed for heating fluorescent tube is longer, to cause
Production capacity waste.If the depositing temperature difference between AlN sublayer is too small, it will lead to that increasing extent of temperature is smaller, the deposition of each AlN sublayer
Temperature or lower, the effect for reinforcing the diffusivity of Al atom is poor, to the improvement result of the uniformity of the AlN film of formation
It is weaker.
In another implementation of the invention, the difference of the depositing temperature of two adjacent AlN sublayers be might be less that
50 DEG C or it is greater than 100 DEG C, can still plays the effect for reinforcing the diffusivity of Al atom in each AlN sublayer at this time.
Optionally, the difference of the depositing temperature of two adjacent AlN sublayers is equal, equal with the thickness of each AlN sublayer
It matches, the depositing temperature of multiple AlN sublayers can be made uniformly to increase, uniformly to reinforce Al atom in each AlN sublayer
Diffusivity.
Illustratively, the difference of the depositing temperature of two adjacent AlN sublayers is 50 DEG C.
In another implementation of the invention, the deposition temperature of two AlN sublayers of arbitrary neighborhood in multiple AlN sublayers
The difference of degree can also be gradually increased, preferably to reinforce the diffusivity of Al atom with the growth of multiple AlN sublayers.
Fig. 6 is a kind of depositional model schematic diagram of multiple AlN sublayers provided in an embodiment of the present invention, as shown in fig. 6, using
When manufacturing method provided in an embodiment of the present invention deposits multiple AlN sublayers, the depositing temperature of each AlN sublayer during the deposition process
It remains unchanged.
Illustratively, the first AlN sublayer, the 2nd AlN sublayer and the 3rd AlN sublayer have been sequentially depositing on substrate.Wherein
The depositing temperature of one AlN sublayer is 550 DEG C, and the depositing temperature of the 2nd AlN sublayer is 600 DEG C, the depositing temperature of third sublayer is
650℃。
After the first AlN sublayer has deposited, the growth of AlN sublayer, break period t1 are interrupted.In break period t1,
Depositing temperature is increased to 600 DEG C from 550 DEG C, continues to deposit the 2nd AlN sublayer, 0 < t1.Similarly, heavy in the 2nd AlN sublayer
After having accumulated, the growth of AlN sublayer is interrupted, depositing temperature is increased to by break period t2 in break period t2 from 600 DEG C
650 DEG C, continue to deposit the 3rd AlN sublayer, t1=t2.
In another implementation of the invention, the depositing temperature of each AlN sublayer during the deposition process is gradually increased,
Compared with the depositing temperature of each AlN sublayer during the deposition process remains unchanged, the depositing temperature of each AlN sublayer can be with
The growth of its thickness and become larger, it is more preferable to the reinforcing effect of the diffusivity of Al atom, can further improve formation
The uniformity of AlN film.
Fig. 7 is the depositional model schematic diagram of the multiple AlN sublayers of another kind provided in an embodiment of the present invention, as shown in fig. 7, adopting
When depositing multiple AlN sublayers with manufacturing method provided in an embodiment of the present invention, the deposition temperature of each AlN sublayer during the deposition process
Degree is gradually increased.
Illustratively, the first AlN sublayer, the 2nd AlN sublayer and the 3rd AlN sublayer have been sequentially depositing on substrate.Wherein
The deposition temperature range of one AlN sublayer be 500~530 DEG C, the depositing temperature of the first AlN sublayer within the scope of 500~530 DEG C by
Edge up height.The deposition temperature range of 2nd AlN sublayer is 550~580 DEG C, and the depositing temperature of the 2nd AlN sublayer is 550~580
It is gradually risen within the scope of DEG C.The depositing temperature of 3rd AlN sublayer is 600~630 DEG C, and the depositing temperature of the 3rd AlN sublayer is 600
It is gradually risen within the scope of~630 DEG C.
After the first AlN sublayer has deposited, the growth of interruption AlN sublayer, break period t1, in break period t1,
Depositing temperature is increased to 550~580 DEG C from 500~530 DEG C, continues to deposit the 2nd AlN sublayer, 0 < t1.Similarly,
After two AlN sublayers have deposited, interrupt AlN sublayer growth, break period t2, in break period t2, by depositing temperature from
550~580 DEG C are increased to 600~630 DEG C, continue to deposit the 3rd AlN sublayer, t1=t2.
The embodiment of the present invention obtains AlN template by depositing multiple AlN sublayers on substrate.Due to the thickness of AlN film
Thicker, the aggregation of Al atom is more serious, therefore on the direction far from substrate, the depositing temperature of multiple AlN sublayers is gradually increased,
The diffusivity of Al atom in each AlN sublayer can gradually be reinforced, the aggregation of Al atom is reduced, so as to improve the AlN of formation
The uniformity of film guarantees the crystal quality of the GaN epitaxial layer grown on AlN film, and then improves the luminous efficiency of LED.
Meanwhile the present invention is by interrupting the deposition of AlN sublayer, and after depositing an AlN sublayer after depositing an AlN sublayer
It deposits in the break period, the depositing temperature of AlN sublayer is increased, the AlN sublayer deposited can be made to protect in certain temperature
A period of time is held, to discharge the stress accumulated in AlN sublayer, then proceedes to deposit next AlN sublayer, the mode of the interruption of growth
The stress accumulated in AlN sublayer can be reduced, to reduce the warpage of AlN, improves AlN layers between subsequent GaN epitaxial layer
Matching improves the wavelength uniformity of epitaxial wafer, and then improves the luminous efficiency of LED.
Fig. 8 is a kind of manufacturing method flow chart of LED epitaxial slice provided in an embodiment of the present invention, such as Fig. 8 institute
Show, which includes:
Step 801, manufacture AlN template.
In the present embodiment, the manufacturing method of AlN template may refer to step 301 as shown in Figure 3 to step 302, or
Person's step 501 as shown in Figure 5 is to step 505, and details are not described herein by the present invention.
Specifically, after executing the step 801, which can also include:
It is cooled to room temperature to AlN template, AlN template is taken out from PVD equipment, be then placed on graphite pallet and be sent into
MOCVD (Metal-organic Chemical Vapor Deposition, metallo-organic compound chemical gaseous phase deposition) equipment
Reaction chamber in carry out epitaxial material growth.
In the present embodiment, can be using trimethyl gallium or triethyl-gallium as gallium source, high pure nitrogen is as nitrogen source, front three
Base indium is as indium source, and for boron triethyl as boron source, N type dopant selects silane, and P-type dopant selects two luxuriant magnesium.
Further, before executing step 802, which can also include:
AlN template is placed on progress in-situ annealing processing in the reaction chamber of MOCVD, annealing temperature 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 the three-dimensional nucleation being sequentially laminated in AlN template
Layer, two-dimentional retrieving layer, undoped GaN layer, N-type layer, prime multiple quantum well layer, multiple quantum well layer, electronic barrier layer, P-type layer
With p-type ohmic contact layer.Each layer in epitaxial layer can be grown using MOCVD method.Therefore it is controlled in following growth courses
Temperature and pressure actually refer to that MOCVD reacts indoor temperature and pressure.
Step 802, the growing three-dimensional nucleating layer in AlN template.
In the present embodiment, three-dimensional nucleating layer can be GaN layer.
Illustratively, reaction chamber temperature being adjusted to 1000~1080 DEG C, chamber pressure is controlled in 250~550torr,
Growth thickness is the three-dimensional nucleating layer of 400~600nm, and growth time is 10~30min.
Step 803 grows two-dimentional retrieving layer on three-dimensional nucleating layer.
In the present embodiment, two-dimentional retrieving layer can be GaN layer.
Illustratively, reaction chamber temperature being adjusted to 1050~1150 DEG C, chamber pressure is controlled in 100~500torr,
Growth thickness is the two-dimentional retrieving layer of 500~800nm, and growth time is 20~40min.
Step 804 grows undoped GaN layer in two-dimentional retrieving layer.
Illustratively, reaction chamber temperature being adjusted to 1050~1200 DEG C, chamber pressure is controlled in 100~500torr,
Growth thickness is the undoped GaN layer of 1~2um.
Step 805 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-3~1020cm-3。
Illustratively, reaction chamber temperature being adjusted to 1050~1200 DEG C, chamber pressure is controlled in 100~500torr,
Growth thickness is the N-type layer of 1~3um.
Step 806 grows prime multiple quantum well layer in N-type layer.
Wherein, prime multiple quantum well layer can be by the In in 5~10 periodsaGa1-aN/GaN superlattice structure composition, 0 < a <
0.5.Wherein, InaGa1-aN layers of thickness can be 1~2nm, and the thickness of GaN layer can be 8~15nm.
Specifically, step 806 may include:
Reaction chamber temperature is adjusted to 760 DEG C~840 DEG C, chamber pressure control is in 100~300torr, growth
InaGa1-aN layers.
Reaction chamber temperature is adjusted to 820 DEG C~920 DEG C, chamber pressure control grows GaN in 100~300torr
Layer.
Step 807 grows multiple quantum well layer on prime multiple quantum well layer.
Wherein, multiple quantum well layer may include the superlattice structure in 6~12 periods, and each superlattice structure includes
InbGa1-bN well layer and GaN barrier layer, 0.1 <b < 1.Wherein InbGa1-bThe thickness of N well layer can be 3~4nm, the thickness of GaN barrier layer
It can be 9~20nm.
Specifically, step 807 may include:
Reaction chamber temperature is adjusted to 750~830 DEG C, chamber pressure control grows In in 100~500torrbGa1- bN well layer.
Reaction chamber temperature is adjusted to 850~900 DEG C, chamber pressure control grows GaN and build in 100~500torr
Layer.
It should be noted that InbGa1-bIn component in N well layer is greater than In in prime multiple quantum well layeraGa1-aIn N layers
In component.
Step 808 grows electronic barrier layer on multiple quantum well layer.
In the present embodiment, electronic barrier layer can be p-type AlzGa1-zN layers, thickness can be 15~100nm, 0.1 < z <
0.5。
Illustratively, reaction chamber temperature being adjusted to 900~1000 DEG C, chamber pressure is controlled in 100~500torr,
Grow electronic barrier layer.
Step 809, the growing P-type layer on electronic barrier layer.
In the present embodiment, P-type layer can be p-type GaN layer, and with a thickness of 50~300nm, the doping concentration of Mg can be 1
×1018~1 × 1020cm-3。
Illustratively, reaction chamber temperature is adjusted to 850~950 DEG C, chamber pressure control is in 100~600torr, life
Long P-type layer.
Step 810, the growing P-type ohmic 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 850~1000 DEG C, chamber pressure is controlled in 100~600torr,
Growth thickness is the p-type contact layer of 5~100nm.
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.
Fig. 9 is a kind of structural schematic diagram of LED epitaxial slice provided in an embodiment of the present invention, as shown in figure 9, Fig. 9
In LED epitaxial slice be fabricated using manufacturing method shown in Fig. 8, which includes AlN mould
Plate and the three-dimensional nucleating layer 902 being sequentially laminated in AlN template 901, two-dimentional retrieving layer 903, undoped GaN layer 904, N
Type layer 905, prime multiple quantum well layer 906, multiple quantum well layer 907, electronic barrier layer 908, P-type layer 909 and p-type ohmic contact layer
910。
The embodiment of the present invention obtains AlN template by depositing multiple AlN sublayers on substrate.Due to the thickness of AlN film
Thicker, the aggregation of Al atom is more serious, therefore on the direction far from substrate, the depositing temperature of multiple AlN sublayers is gradually increased,
The diffusivity of Al atom in each AlN sublayer can gradually be reinforced, the aggregation of Al atom is reduced, so as to improve the AlN of formation
The uniformity of film guarantees the crystal quality of the GaN epitaxial layer grown on AlN film, and then improves the luminous efficiency of LED.
Meanwhile the present invention is by interrupting the deposition of AlN sublayer, and after depositing an AlN sublayer after depositing an AlN sublayer
It deposits in the break period, the depositing temperature of AlN sublayer is increased, the AlN sublayer deposited can be made to protect in certain temperature
A period of time is held, to discharge the stress accumulated in AlN sublayer, then proceedes to deposit next AlN sublayer, the mode of the interruption of growth
The stress accumulated in AlN sublayer can be reduced, to reduce the warpage of AlN, improves AlN layers between subsequent GaN epitaxial layer
Matching improves the wavelength uniformity of epitaxial wafer, and then improves the luminous efficiency of LED.
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 manufacturing method of AlN template, which is characterized in that the manufacturing method includes:
It is sequentially depositing multiple AlN sublayers on substrate, obtains AlN template, it is multiple described on the direction far from the substrate
The depositing temperature of AlN sublayer is gradually increased；
It is described to be sequentially depositing multiple AlN sublayers on substrate, comprising:
After depositing an AlN sublayer, the deposition of the AlN sublayer is interrupted；
It is depositing in the deposition break period after an AlN sublayer, the depositing temperature of the AlN sublayer is being increased；
Deposit next AlN sublayer.
2. the manufacturing method according to claim 1, which is characterized in that each AlN sublayer during the deposition process heavy
Accumulated temperature degree remains unchanged.
3. manufacturing method according to claim 2, which is characterized in that the difference of the depositing temperature of two adjacent AlN sublayers
Value is 50~100 DEG C.
4. manufacturing method according to claim 2, which is characterized in that the difference of the depositing temperature of two adjacent AlN sublayers
It is worth equal.
5. the manufacturing method according to claim 1, which is characterized in that each AlN sublayer during the deposition process heavy
Accumulated temperature degree is gradually increased.
6. described in any item manufacturing methods according to claim 1~5, which is characterized in that the deposition temperature of each AlN sublayer
Degree is 500~700 DEG C.
7. described in any item manufacturing methods according to claim 1~5, which is characterized in that the thickness phase of each AlN sublayer
Deng.
8. described in any item manufacturing methods according to claim 1~5, which is characterized in that each AlN sublayer with a thickness of
5~8nm.
9. described in any item manufacturing methods according to claim 1~5, which is characterized in that heavy after one AlN sublayer of every deposition
The product break period is t, 5≤t≤10s.
10. a kind of manufacturing method of LED epitaxial slice, which is characterized in that the manufacturing method includes:
AlN template is manufactured using claim 1 to the described in any item manufacturing methods of claim 9；
In the AlN template growing epitaxial layers.
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| CN108091741A (en) * | 2017-11-15 | 2018-05-29 | 华灿光电(苏州）有限公司 | A kind of growing method of LED epitaxial slice |
| CN109065438A (en) * | 2018-07-23 | 2018-12-21 | 中国科学院半导体研究所 | The preparation method of AlN film |
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| CN101901758A (en) * | 2010-06-24 | 2010-12-01 | 西安电子科技大学 | MOCVD growth method of non-polar m-surface GaN film based on m-surface SiC substrate |
| US20140158937A1 (en) * | 2012-12-07 | 2014-06-12 | Samsung Electronics Co., Ltd. | Processes for synthesizing nanocrystals and nanocrystal compositions |
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