CN109285761A - A kind of preparation method of aluminium nitride film - Google Patents
A kind of preparation method of aluminium nitride film Download PDFInfo
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- CN109285761A CN109285761A CN201811094398.4A CN201811094398A CN109285761A CN 109285761 A CN109285761 A CN 109285761A CN 201811094398 A CN201811094398 A CN 201811094398A CN 109285761 A CN109285761 A CN 109285761A
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Abstract
An embodiment of the present invention provides a kind of preparation method of aluminium nitride film, comprising: provides vertical structure graphene nanometer sheet;And aluminium nitride film is formed in the vertical structure graphene nano on piece.The preparation method of an embodiment of the present invention, the buffer layer grown using vertical structure graphene nanometer sheet as aluminium nitride, then aluminium nitride film is formed on graphene buffer layers, atomically flating, stressless aluminium nitride film can be made.
Description
Technical field
The present invention relates to aluminium nitride film, the system of specially a kind of achievable atomically flating, stressless aluminium nitride film
Preparation Method.
Background technique
Aluminium nitride (AlN) is a kind of III-V race's semiconductor with wide direct band gap, has high heat conductance, high machinery strong
The properties such as degree, high chemical stability and strong Radiation hardness, in photoelectron, high temperature high power device and high-frequency wideband communicator
Part application aspect has wide prospect.In addition, AlN can also be mixed to form ternary with gallium nitride (GaN), indium nitride (InN)
Or quaternary compound, it is based on this, it is all effective that the photoelectric device prepared in visible light wave grows to ultraviolet wavelength.
It is industrially given birth at present using hetero-epitaxy (being used as substrate using sapphire or silicon carbide) technology using two-step method
Long AlN film, i.e. elder generation low-temperature epitaxy AlN is as buffer layer, regrowth high-temperature AlN.However, thin using two-step method growing aluminum nitride
Film, complex process, high production cost.However, aluminium nitride is nucleated difficulty in sapphire substrates if being grown using one-step method,
The difficulty further to form a film greatly increases.
Summary of the invention
A primary object of the present invention is providing a kind of preparation method of aluminium nitride film, comprising: provides vertical structure stone
Black alkene nanometer sheet;And aluminium nitride film is formed in the vertical structure graphene nano on piece.
According to an embodiment of the present invention, for the graphene vertical-growth in substrate, the substrate is pyroceram.
According to an embodiment of the present invention, the pyroceram is selected from quartz glass, sapphire glass or high temperature resistant boron
Silica glass.
According to an embodiment of the present invention, the vertical structure graphene nanometer sheet enhances chemistry by direct-current plasma
Vapor deposition is formed in the substrate, and formation temperature is 580 DEG C~1000 DEG C.
According to an embodiment of the present invention, in the growth course of the vertical structure graphene nanometer sheet, growth time
It is 3~15 minutes;Or used carbon source and the flow-rate ratio of hydrogen are (20~50): 20.
According to an embodiment of the present invention, in the growth course of the vertical structure graphene nanometer sheet, applied
Power is 80~1000W.
According to an embodiment of the present invention, in the growth course of the vertical structure graphene nanometer sheet, gas pressure intensity
For 200~1000Pa.
According to an embodiment of the present invention, the aluminium nitride film by Metallo-Organic Chemical Vapor deposition, molecular beam epitaxy,
Hydride gas-phase epitaxy or sputtering method are formed.
According to an embodiment of the present invention, the aluminium nitride film passes through high temperature-Metalorganic Chemical Vapor Deposition growth
It is formed, trimethyl aluminium is as silicon source, and ammonia is as nitrogen source, and nitrogen/hydrogen is as reaction carrier gas.
According to an embodiment of the present invention, the growth air pressure of the aluminium nitride film is 30~100Torr, and gas flow is ammonia
500~2000sccm of gas, 50~120sccm of trimethyl aluminium, growth temperature are 1200 DEG C, growth time 2h.
The preparation method of an embodiment of the present invention, the buffering grown using vertical structure graphene nanometer sheet as aluminium nitride
Layer, then aluminium nitride film is formed on graphene buffer layers, atomically flating, stressless aluminium nitride film can be made.
Detailed description of the invention
Fig. 1 is the flow diagram for preparing aluminium nitride film of an embodiment of the present invention;
Fig. 2A is the atomic force microscope three-dimensional appearance characterization of vertical graphene nanometer sheet made from the embodiment of the present invention 1
Figure;
Fig. 2 B is the Raman characterization figure of vertical graphene nanometer sheet made from the embodiment of the present invention 1;
Fig. 3 A, 3B are that the atomic force microscope phenogram of aluminium nitride film made from the embodiment of the present invention 1 and height count
Distribution map;
Stress phenogram and corresponding Gauss curve fitting of Fig. 4 A for the Raman of aluminium nitride film made from the embodiment of the present invention 1
Curve graph;
Fig. 4 B is the Raman shift comparison of aluminium nitride film made from the embodiment of the present invention 1 and aluminium nitride block;
Fig. 4 C is the stress phenogram of the Raman of aluminium nitride film made from the embodiment of the present invention 2;
Fig. 4 D is the stress phenogram of the Raman of aluminium nitride film made from 3-2 of the embodiment of the present invention;
Fig. 5 A1 is aluminum nitride thin film nucleation 5 minutes scanning electron microscope shape appearance figures of comparative example of the present invention;
Fig. 5 A2 is aluminum nitride thin film nucleation 2 hours scanning electron microscope shape appearance figures of comparative example of the present invention;
Fig. 5 B1 is aluminum nitride thin film nucleation 5 minutes scanning electron microscope shape appearance figures of the embodiment of the present invention 1;
Fig. 5 B2 is the scanning electron microscope shape appearance figure that the aluminium nitride film of the embodiment of the present invention 1 forms a film 2 hours.
Specific embodiment
The exemplary embodiment for embodying feature of present invention and advantage will describe in detail in the following description.It should be understood that
The present invention can have various variations in different embodiments, neither depart from the scope of the present invention, and theory therein
Bright and diagram inherently is illustrated as being used, rather than to limit the present invention.
An embodiment of the present invention provides a kind of preparation method of aluminium nitride film, as shown in Figure 1, being included in 10 table of substrate
It looks unfamiliar long vertical structure graphene layer 20;And aluminium nitride film 30 is formed on vertical structure graphene layer 20.
Compared to the graphene layer of horizontal structure, vertical structure graphene have large specific surface area, there are many active edges
The unique architectural characteristic such as three-dimensional structure of edge, particular vertical.In addition, since vertical graphene nanometer sheet has many edges to lack
It falls into, nucleation site abundant can be provided for the epitaxial growth of aluminium nitride, the nucleation density of aluminium nitride can be dramatically increased, to promote
Rapid fusion, growth into aluminium nitride film, so that aluminium nitride fast filming.
The preparation method of an embodiment of the present invention, the buffering grown using vertical structure graphene nanometer sheet as aluminium nitride
Layer forms AlN film on vertical graphene buffer layers, atomically flating, stressless aluminium nitride film can be made.
In an embodiment, growth of vertical obtains vertical graphene-substrate knot in the graphene of substrate in substrate
Structure provides a kind of new growth substrates for the growth of aluminium nitride film.The preparation method of vertical graphene-substrate is simple, can
Realize industrialization, large area deposition.
In an embodiment, the substrate for growth of vertical graphene can be pyroceram.
In an embodiment, for vertical structure graphene growth pyroceram substrate can for quartz glass,
Sapphire glass, high temperature resistant Pyrex etc., it is however preferred to have the sapphire glass with hexagonal lattice structure similar in aluminium nitride.
In an embodiment, the preparation method of aluminium nitride film includes:
The step of substrate is started the cleaning processing;
The substrate surface growth of vertical graphene nanometer sheet the step of;And
The step of forming aluminium nitride film is deposited in vertical graphene nano on piece.
In an embodiment, substrate such as sapphire wafer substrate can be started the cleaning processing using organic solvent, water,
To obtain clean sapphire substrates.
In an embodiment, organic solvent can be ethyl alcohol, acetone, isopropanol etc..
In an embodiment, the step of starting the cleaning processing to substrate includes: successively to put sapphire wafer piece substrate
Enter ethyl alcohol, acetone, be cleaned by ultrasonic in aqueous isopropanol, is finally cleaned by ultrasonic with deionized water, is dried with nitrogen.
In an embodiment, the growth of vertical graphene nanometer sheet can be carried out in clean process for sapphire-based bottom surface, obtained
To the sapphire substrates of graphene are covered with, wherein the part of the surface that can be sapphire substrates is covered by graphene.
In an embodiment, it can be based on AIXTRON BLACK MAGIC system, enhance chemistry using direct-current plasma
(dc-PECVD) technology of vapor deposition carries out the low-temperature epitaxy of vertical structure graphene nanometer sheet.Using DC plasma and chemical
Gas phase deposition technology vertical graphene nanometer sheet of low-temperature epitaxy directly in substrate can substantially reduce the growth power consumption of graphene,
The energy is saved;And can under cryogenic conditions in such as sapphire substrates large area, rapidly growth of vertical structure graphite
Alkene.
It, can be in addition to Direct current plasma enhanced chemical vapour deposition (dc-PECVD) technology in an embodiment
Select radio frequency plasma enhancing chemical vapor deposition (rf-PECVD) technology or microwave plasma enhanced chemical vapor deposition
Product (MW-PECVD) etc. carries out the growth of graphene nanometer sheet.
In an embodiment, the growth temperature of vertical structure graphene can be 580 DEG C~1000 DEG C, such as 600 DEG C,
650 DEG C, 700 DEG C, 750 DEG C, 800 DEG C, 850 DEG C, 900 DEG C etc..
In an embodiment, the growth temperature of vertical structure graphene is 580 DEG C, can be in argon atmosphere by chamber temperature
Degree is heated to 580 DEG C, then passes to carbon source, carbon source reaches diluted effect in argon atmosphere.
In an embodiment, carbon source can be methane, ethylene, acetylene etc..
It can be 580 DEG C~1000 DEG C by regulation growth temperature, or regulation growth time is in an embodiment
3~15 minutes, or regulation carbon source and the ratio of hydrogen are (20~50): 20 (such as 50sccm:20sccm, 20sccm:
20sccm), perhaps regulation power is 80~1000W or regulation gas pressure intensity is 200~1000Pa etc., and obtaining has difference
Graphene-Sapphire Substrate of coverage, different graphene nanometer sheet density.
In an embodiment, aluminium nitride film can deposit (MOCVD), outside molecular beam by Metallo-Organic Chemical Vapor
Prolong, hydride gas-phase epitaxy, sputtering method etc. are formed.
In an embodiment, aluminum nitride thin is realized by high temperature-Metalorganic Chemical Vapor Deposition (HT-MOCVD)
Film vertical graphene-substrate a step quickly, high growth temperature, wherein using trimethyl aluminium as silicon source, ammonia as nitrogen source,
Nitrogen/hydrogen is as reaction carrier gas.
In an embodiment, the growth conditions of aluminium nitride film can be with are as follows: growth 30~100Torr of air pressure, such as
50Torr, 70Torr, 90Torr etc.;500~2000sccm of ammonia flow, for example, 700sccm, 900sccm, 1000sccm,
1500sccm etc.;Trimethyl aluminium 50~120sccm of flow, such as 60sccm, 80sccm, 100sccm etc.;Growth temperature is 1200
DEG C, growth time 2h.
An embodiment of the present invention provides application of the vertical structure graphene nanometer sheet in aluminium nitride film preparation process,
First pass through in substrate (such as sapphire) surface growth of vertical structure graphite alkene, especially can under cryogenic, large area,
Fast-growth vertical structure graphene, then aluminium nitride film is formed on vertical structure graphene.
The preparation method of an embodiment of the present invention may make nitrogen compared with existing two-step method growing aluminum nitride film
Change aluminium film to be grown directly upon on vertical graphene buffer layers by one-step method, needs not move through low temperature nitride aluminium growth course, greatly
Growth technique is simplified greatly, shortens growth time, to considerably reduce AlN film production cost;In addition, graphene pair
Its growth substrate is without special selectivity, the further expansion range of choice of aluminium nitride hetero-epitaxy substrate.
The preparation method of an embodiment of the present invention can reduce aluminium nitride film and substrate (example due to the insertion of graphene
Such as sapphire wafer piece) effect, to reduce the stress that is subject to of aluminium nitride film that growth obtains.The introducing of stress can be to nitrogen
The structure and performance for changing aluminium film have a huge impact, and can improve the performance of aluminium nitride film by reducing stress.It is specific and
The aluminium nitride film that stress reduces is used for semiconductor devices by speech, helps to reduce polarization, improves hole and electron radiation is multiple
It closes, increases internal quantum efficiency, to further increase device luminous efficiency.
Hereinafter, being described further by specific embodiment to the preparation of the aluminium nitride film of an embodiment of the present invention.Its
In, high levels of three-dimensional is carried out to vertical structure graphene nanometer sheet using atomic force microscope (Bruker Dimension Icon)
Morphology characterization;Using 514 nanometer laser wavelength Raman spectrometer (Horiba, LabRAM HR-8000) to vertical graphene into
Row Raman characterization, and stress analysis is carried out to the aluminium nitride film that growth obtains by Raman spectrum;Use Hitachi S-
4800 scanning electron microscope (acceleration voltage 5-30kV), to different growth substrates (no graphene-based bottom, have it is vertical graphene-based
Bottom), the aluminium nitride of different growth time (5 minutes, 2 hours) carry out surface topography characterization;The density of graphene nanometer sheet passes through
Corresponding atomic force microscope three-dimensional appearance phenogram, which calculates, to be obtained.
Embodiment 1
1) cleaning of sapphire wafer substrate:
Sapphire wafer piece substrate is sequentially placed into ethyl alcohol, acetone, is cleaned by ultrasonic in aqueous isopropanol, is finally spent
Ionized water ultrasonic cleaning, is dried with nitrogen, obtains clean sapphire wafers substrate.
2) growth that vertical graphene nanometer sheet is carried out in sapphire wafers substrate surface, obtains being partially covered with graphene
Low-density graphene nanometer sheet sapphire substrates:
Based on AIXTRON BLACK MAGIC system, carried out using Direct current plasma enhanced chemical vapour deposition technology
The low-temperature epitaxy of vertical structure graphene nanometer sheet.Specific implementation condition are as follows: growth temperature is controlled at 580 DEG C or so, in flow
For chamber temp is heated to 580 DEG C in the argon atmosphere of 200sccm, the application power of 100W then passes to 40sccm methane
Carbon source and 20sccm hydrogen grow 6 minutes, close heating power supply afterwards, when chamber temp drops to room temperature, sample is taken out, is obtained
Obtaining density is 80/micron2Graphene nanometer sheet.
Fig. 2A is the atomic force microscope three-dimensional appearance phenogram of obtained graphene nanometer sheet, shows the stone that growth obtains
Black alkene is made of a series of graphene nanometer sheets, has the three-dimensional structure vertical with growth substrate;Fig. 2 B is corresponding graphene
Raman characterization figure, wherein the presence at the peak D, the peak G and the peak 2D show growth obtain material have graphene feature.
3) sapphire surface that the surface made from step 2) is covered with graphene directly carries out the heavy of high-temperature AlN film
Product, obtains high-quality AlN film:
Aluminium nitride film, specific growth conditions are formed using a step high-temperature metal organic chemical vapour deposition process are as follows: growth
Air pressure 50Torr, ammonia flow 500sccm, trimethyl aluminium flow 60sccm, 1200 DEG C of growth temperature, growth time 2h, growth
It is passed through nitrogen/hydrogen in the process as carrier gas.
Embodiment 2
The density of graphene nanometer sheet can realize that specific one grows example are as follows: the present embodiment by changing growth parameter(s)
The step of with embodiment 1, condition are essentially identical.The growth temperature that the growth conditions of vertical graphene nanometer sheet is 580 DEG C, 100W
Application power, 40sccm CH4And 20sccmH2Carbon source concentration, difference be change growth time, growth time is increased
To 10 minutes, high-density graphite alkene nanometer sheet (about 180/micron are obtained2)。
Embodiment 3-1
The step of the present embodiment and embodiment 1, condition are essentially identical, and difference is that the growth temperature of graphene is 1000
DEG C, the density for obtaining graphene nanometer sheet is 180/micron2.The growth conditions phase of the growth conditions of aluminium nitride and embodiment 1
Together, aluminium nitride-graphene nanometer sheet-Sapphire Substrate composite membrane is further made using MOCVD.
Embodiment 3-2
The step of the present embodiment and embodiment 1, condition are essentially identical, and difference is that the growth temperature of graphene is 800 DEG C,
The density for obtaining graphene nanometer sheet is 100/micron2.The growth conditions of aluminium nitride is identical as the growth conditions of embodiment 1,
Aluminium nitride-graphene nanometer sheet-Sapphire Substrate composite membrane is further made using MOCVD.
Embodiment 4-1
The step of the present embodiment and embodiment 1, condition are essentially identical, and difference is that the power setting for growing graphene is can
The maximum power 1000W of realization, the density for obtaining graphene nanometer sheet is 180/micron2.The growth conditions and reality of aluminium nitride
The growth conditions for applying example 1 is identical, and aluminium nitride-graphene nanometer sheet-Sapphire Substrate composite membrane is further made using MOCVD.
Embodiment 4-2
The step of the present embodiment and embodiment 1, condition are essentially identical, and difference is that the power for growing graphene is 500W,
The density for obtaining graphene nanometer sheet is 100/micron2.The growth conditions of aluminium nitride is identical as the growth conditions of embodiment 1,
Aluminium nitride-graphene nanometer sheet-Sapphire Substrate composite membrane is further made using MOCVD.
Embodiment 5-1
The step of the present embodiment and embodiment 1, condition are essentially identical, and difference is to grow the methane of graphene and hydrogen
Flow is respectively 50sccm, 20sccm, and the density for obtaining graphene nanometer sheet is 120/micron2.The growth conditions of aluminium nitride
It is identical as the growth conditions of embodiment 1, it is compound that aluminium nitride-graphene nanometer sheet-Sapphire Substrate is further made using MOCVD
Film.
Embodiment 5-2
The step of the present embodiment and embodiment 1, condition are essentially identical, and difference is to grow the methane of graphene and hydrogen
Flow is respectively 20sccm, 20sccm, and the density for obtaining graphene nanometer sheet is 120/micron2.The growth conditions of aluminium nitride
It is identical as the growth conditions of embodiment 1, it is compound that aluminium nitride-graphene nanometer sheet-Sapphire Substrate is further made using MOCVD
Film.
Comparative example
In order to verify the effect of vertical graphene, served as a contrast using a step high-temperature metal organic chemical vapour deposition process in sapphire
Bottom carries out the growth of aluminium nitride film, specific growth conditions are as follows: grows air pressure 50Torr, ammonia flow 500sccm, trimethyl aluminium
Flow 60sccm, is passed through nitrogen/hydrogen as carrier gas in growth course by 1200 DEG C of growth temperature, growth time 2h.
Fig. 3 A, 3B, 4A, 4B are respectively atomic force microscope phenogram, the height for the aluminium nitride film that the growth of embodiment 1 obtains
Spend statistical Butut, the stress phenogram based on Raman, the Raman shift comparison diagram with aluminium nitride block.The height of Fig. 3 B statistics
1.3 rans are distributed in, show that the aluminium nitride film that growth obtains is atomically flating.Raman characterization can be used to test nitrogen
Change stress suffered by aluminium film, Fig. 4 A is aluminium nitride E2(high) Raman shift at peak is 657.4cm-1, unstressed with Fig. 4 B
The E of aluminium nitride block2(high) Raman shift (657.4cm at peak-1) identical.Generally use E2(high) peak is relative to unstressed nitrogen
Change the frequency shifts of aluminium to calculate stress intensity suffered by aluminium nitride film.
Fig. 4 C, 4D be respectively embodiment 2, embodiment 3-2 aluminium nitride film based on the stress phenogram of Raman.Fig. 4 A,
The Raman results of 4C, 4D sufficiently show that the aluminium nitride obtained using vertical graphene as buffer growth is unstressed.
Comparative example in Sapphire Substrate growing aluminum nitride film and embodiment 1 in graphene-Sapphire Substrate growth
The morphology characterization of aluminium nitride film is as shown in Fig. 5 A1, Fig. 5 A2, Fig. 5 B1, Fig. 5 B2.It can be seen from the figure that comparative example is blue precious
Island structure is formed using the aluminium nitride that step high temperature method growth obtains on stone lining bottom, can not be formed a film;And embodiment 1 uses graphite
Alkene-Sapphire Substrate can obtain the aluminium nitride film of atomically flating.
Embodiment 1 and embodiment 2 can get the aluminium nitride film of atomically flating, but crystalline quality difference, real
The film quality for applying the nitride of the acquisition of example 1 is more excellent.It is above-mentioned the experimental results showed that, pass through and change the close of vertical graphene nanometer sheet
Degree can regulate and control the growth of nitride.
It is above-mentioned the experimental results showed that, the insertion of the graphene nanometer sheet of the embodiment of the present invention, can reduce aluminium nitride film with
The effect of Sapphire Substrate, to reduce the stress that the aluminium nitride film that growth obtains is subject to.The introducing of stress can be to aluminium nitride
The structure and performance of film have a huge impact, and can improve the performance of aluminium nitride film by reducing stress, have important meaning
Justice.
Unless limited otherwise, term used herein is the normally understood meaning of those skilled in the art.
Embodiment described in the invention is merely for exemplary purpose, the protection scope being not intended to limit the invention,
Those skilled in the art can be made within the scope of the invention various other replacements, changes and improvements, thus, the present invention is not limited to
Above embodiment, and be only defined by the claims.
Claims (10)
1. a kind of preparation method of aluminium nitride film, comprising:
Vertical structure graphene nanometer sheet is provided;And
Aluminium nitride film is formed in the vertical structure graphene nano on piece.
2. according to the method described in claim 1, wherein, the graphene nanometer sheet vertical-growth is in substrate, the substrate
For pyroceram.
3. according to the method described in claim 2, wherein, the pyroceram is selected from quartz glass, sapphire glass or resistance to
High temperature Pyrex.
4. according to the method described in claim 2, wherein, the vertical structure graphene nanometer sheet is increased by direct-current plasma
Extensive chemical vapor deposition is formed in the substrate, and formation temperature is 580 DEG C~1000 DEG C.
5. according to the method described in claim 2, wherein, in the growth course of the vertical structure graphene nanometer sheet, giving birth to
It is for a long time 3~15 minutes;Or used carbon source and the flow-rate ratio of hydrogen are (20~50): 20.
6. according to the method described in claim 2, wherein, in the growth course of the vertical structure graphene nanometer sheet, institute
The power of application is 80~1000W.
7. according to the method described in claim 2, wherein, in the growth course of the vertical structure graphene nanometer sheet, gas
Body pressure is 200~1000Pa.
8. method according to any one of claim 1 to 7, wherein the aluminium nitride film passes through Organometallic Chemistry gas
Mutually deposition, molecular beam epitaxy, hydride gas-phase epitaxy or sputtering method are formed.
9. according to the method described in claim 1, wherein, the aluminium nitride film passes through high temperature-Metallo-Organic Chemical Vapor deposition
Method grows to be formed, and trimethyl aluminium is as silicon source, and ammonia is as nitrogen source, and nitrogen/hydrogen is as reaction carrier gas.
10. according to the method described in claim 9, wherein, the growth air pressure of the aluminium nitride film is 30~100Torr, gas
Flow is 500~2000sccm of ammonia, 50~120sccm of trimethyl aluminium, and growth temperature is 1200 DEG C, growth time 2h.
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