CN107424912A - A kind of preparation method of gallium nitride base nano column array - Google Patents
A kind of preparation method of gallium nitride base nano column array Download PDFInfo
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02631—Physical deposition at reduced pressure, e.g. MBE, sputtering, evaporation
Abstract
The present invention relates to a kind of preparation method of gallium nitride base nano column array, the preparation method of the gallium nitride base nano column array comprises the following steps：Step A：Aln layer, gallium nitride film layer are sequentially formed on a substrate；Step B：The applying silicon oxide film layer on the gallium nitride film layer；Step C：The layer gold of 0.5 1.5nm thickness is deposited on the silica membrane layer；Step D：Evaporation thickness is 10 20nm nickel dam on the layer gold surface, forms metallic nickel island structure.Uniformity of the nanometer island structure that the present invention is prepared using the double film methods of nickel gold in shape, density and size is better than the nano island prepared using conventional method, substantially increases the photoelectric efficiency of related photoelectric device.When realizing the growth of MOCVD secondary epitaxies using gallium nitride nano-pillar, gallium nitride base nano column array prepared by the present invention can be substantially improved gallium nitride quality, and then improve the luminous efficiency of the devices such as LED.
Description
Technical field
The present invention relates to technical field of semiconductors, and in particular to a kind of preparation method of gallium nitride base nano column array.
Background technology
Gallium nitride nanostructured (such as nano-pillar, nano wire) is preparing semiconductor laser, LED, solar cell, spy
Surveying on the devices such as device has boundless application field and good application prospect, and is preparing high-quality gallium nitride crystal
There are huge potentiality on material, (crystal mass is improved by the method for nano-pillar secondary epitaxy).Therefore, gallium nitride nanometer material
Material has certain researching value and meaning.
At present, the preparation method of gallium nitride base nano column array is roughly divided into two kinds：The first utilizes nano impression
Method, it is to realize the duplication of pattern and transfer using traditional mould replica principle, and nitrogen is realized by dry etching means
Change gallium base nanometer column structure.The preparation method is simple to operate, and cost is relatively low.However, there is also defect for this method：1st, imprint
Instrument needs and manufacture material directly contacts, and may cause physical damnification to sample, influence device efficiency；2nd, high quality is prepared
Nano-imprint stamp difficulty it is larger, cost is very high, it is extremely difficult to realizes industrial volume production.Second of preparation method is utilized " from group
Knit nano dot technology " realize gallium nitride base nano column array.It carries out high-temperature thermal annealing to nickel nanometer layer, it is spontaneously formed nickel
Nanoscale island structure, realize gallium nitride nano-pillar as mask, and using dry etching technology.The method is easy to operate,
Cost is relatively low, and technique is simple, it is easy to accomplish volume production.But spontaneously formed because nickel nano dot is heated by nickel metal layer, its chi
Very little, shape, density, spacing are very irregular.As illustrated by figures 1 a-1 c, the SEM of various sizes of nickel metal nano island structure bows
View, the thickness of Fig. 1 a Central Plains nickel metal layer are 10nm, and the thickness of Fig. 1 b Central Plains nickel metal layer is 15nm, Fig. 1 c Central Plains nickel metal
The thickness of layer is 20nm.It follows that when the average-size on nickel metal nano island further increases, its erratic behavior is more bright
It is aobvious.The gallium nitride base nano column array prepared by above two method largely drops there is clearly disadvantageous and defect
The low efficiency of photoelectric device prepared therefrom.Traditional " self-organizing nano dot technology " is to utilize the nickel metal layer to nanometer scale
(10-20nm) carries out high-temperature thermal annealing, and irregular nanometer scale nickel nano dot is spontaneously formed at 850 DEG C or so.
And nano nickel island can coordinate dry etching to realize the nanometer of gallium nitride as the mask for preparing gallium nitride nano-pillar
Column structure.Layer of silicon dioxide film is first plated on gallium nitride film layer first, one is then deposited on silica membrane
Layer nickel metal.Nickel film is set to spontaneously form the nickel nano island of nanometer scale followed by the method for rapid thermal annealing.Finally use
RIE and ICP etches to form a nanometer column structure to silica and GaN.Self-organizing nickel nano island be due to surface tension and
Difference based on the thermal coefficient of expansion between nickel metal and silica in temperature-rise period and what caused huge stress was formed.With
The nickel island that conventional method is prepared as shown in Figure 2 a, gallium nitride nano column array as shown in Figure 3 a, due to the surface of silica
Rougher, the surface tension that nickel island structure is subject in a different direction is more uneven, therefore the nickel nano island and nitrogen formed
Change the nitridation that the shape, size, density of gallium base nano-pillar etc. are also irregular, are prepared using traditional " self-organizing nano dot technology "
The uniformity and repetitive rate of gallium nano-pillar are relatively low.
In addition, when the diameter of nickel nano island reaches more than 300nm, it hardly results in the nickel island of separation.It is irregular to receive
Rice column dimension, shape and density hinder realize high-crystal quality gallium nitride base nanometer column structure and height to a certain extent
Imitate photoelectric device.
As can be seen here, the gallium nitride base nano-pillar battle array prepared using the preparation method of traditional gallium nitride base nano column array
It is very irregular that row prepare nickel nano-dot size, shape, density and the spacing that cost is high, it is difficult to realize volume production, prepares etc., it would be highly desirable to enters
One step is improved.
The content of the invention
It is an object of the invention to provide a kind of preparation method of gallium nitride base nano column array, to overcome prior art to exist
The defects of.
In order to solve the above technical problems, the present invention provides a kind of preparation method of gallium nitride base nano column array, the nitrogen
The preparation method for changing gallium base nano column array comprises the following steps：
Step A：Aln layer, gallium nitride film layer are sequentially formed on substrate；
Step B：The applying silicon oxide film layer on the gallium nitride film layer；
Step C：The layer gold of 0.5-1.5nm thickness is deposited in the silica membrane layer surface；
Step D：Evaporation thickness is 10-20nm nickel dam on the layer gold surface, forms metallic nickel island structure；
Step E：Use etching technics with metallic nickel island structure shape to gallium nitride film layer, silica membrane layer, gold
Layer and nickel dam perform etching, and form nanometer columnar arrays.
In one embodiment of the present of invention, the aln layer includes aln nucleation layer and is formed at the aluminium nitride
Pulse supplying high temperature aln layer on nucleating layer.
In one embodiment of the present of invention, the thickness of the aln nucleation layer is 10-20nm, and its growth temperature is 950-
1100 DEG C, V/III molar flows flow-rate ratio is 90-110, atmospheric pressure value 55-70Torr.
In one embodiment of the present of invention, the thickness of the pulse supplying high temperature aln layer is 75-85nm, and it forms bar
Part be temperature to 1150-1250 DEG C, V/III molar flows ratio is 1650-1750, atmospheric pressure value 220-230Torr.
In one embodiment of the present of invention, the thickness of the gallium nitride film layer is 0.8-1.2um.
In one embodiment of the present of invention, the layer gold is that gold is put into thermal evaporation coil using thermal evaporation coating machine,
It is added into the electric current of 14-16 amperes, makes its distillation evaporation to silica membrane.
In one embodiment of the present of invention, the nickel dam is to utilize thermal evaporation coating machine, under 18-22A electric current, makes it
Distillation is vaporized on the surface of the layer gold.
In one embodiment of the present of invention, the substrate is Sapphire Substrate.
The preparation method of the gallium nitride base nano column array of the present invention has advantages below：
The present invention is based on " self-organizing nano dot " principle, it is proposed that the new method for preparing gallium nitride base nano column array,
The gallium nitride base nano column array of preparation has more preferable uniformity in size, shape, density etc., and preferably repeats
Property.Shape, the size more rule of gallium nitride base nano column array prepared by the present invention, uniformity is more preferable, substantially increases it
The crystal mass of the gallium nitride of photoelectric device efficiency and secondary epitaxy.
Brief description of the drawings
Fig. 1 a are gallium nitride base nano column array prepared by conventional method, when nickel metal layer thickness is 10nm, nickel metal
The SEM top views of nanometer island structure.
Fig. 1 b are gallium nitride base nano column array prepared by conventional method, when nickel metal layer thickness is 15nm, nickel metal
The SEM top views of nanometer island structure.
Fig. 1 c are gallium nitride base nano column array prepared by conventional method, when nickel metal layer thickness is 20nm, nickel metal
The SEM top views of nanometer island structure.
Fig. 2 a are that the SEM of the nickel metal nano island structure of gallium nitride base nano column array prepared by conventional method is overlooked
Figure.
Fig. 2 b are that the SEM of the nickel metal nano island structure of gallium nitride base nano column array prepared by the method for the present invention bows
View.
Fig. 3 a are gallium nitride base nanometer column structure electron microscope prepared by conventional method
Fig. 3 b are gallium nitride base nanometer column structure electron microscope prepared by the method for the present invention.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
A kind of preparation method of gallium nitride base nano column array of the present invention, it comprises the following steps：
Step A：Aln layer, gallium nitride film layer are sequentially formed on substrate, the substrate is Sapphire Substrate.
Step B：The applying silicon oxide film layer on the gallium nitride film layer.
Step C：The layer gold of 0.5-1.5nm thickness is deposited in the silica membrane layer surface, the layer gold is profit
Gold is put into thermal evaporation coil with thermal evaporation coating machine, plus the electric current of 14-16 amperes, its distillation evaporation is arrived silica
On film.
Step D：Evaporation thickness is 10-20nm nickel dam on the layer gold surface, forms metallic nickel island structure；The nickel dam
It is to utilize thermal evaporation coating machine, under 18-22A electric current, its distillation is vaporized on the surface of the layer gold.The evaporation of different nickel
The average-size for the metallic island structure that thickness effect eventually forms, the thickness of nickel is bigger, and metallic island structure is bigger.
Step E：Use etching technics with metallic nickel island structure shape to gallium nitride film layer, silica membrane layer, gold
Layer and nickel dam perform etching, and form nanometer columnar arrays.
Embodiment 1, the preparation method for preparing gallium nitride base nano column array comprise the following steps：
Step A：Aln layer, gallium nitride film layer are sequentially formed on substrate, the substrate is Sapphire Substrate.
Step B：The applying silicon oxide film layer on the gallium nitride film layer.
Step C：The layer gold of 0.5-1.5nm thickness is deposited in the silica membrane layer surface, the layer gold is profit
Gold is put into thermal evaporation coil with thermal evaporation coating machine, plus 14 amperes of electric current, makes its distillation evaporation thin to silica
On film.
Step D：Evaporation thickness is 10-20nm nickel dam on the layer gold surface, forms metallic nickel island structure；The nickel dam
It is to utilize thermal evaporation coating machine, under 18-22A electric current, its distillation is vaporized on the surface of the layer gold.
Step E：Use etching technics with metallic nickel island structure shape to gallium nitride film layer, silica membrane layer, gold
Layer and nickel dam perform etching, and form nanometer columnar arrays.
Embodiment 2, the preparation method for preparing gallium nitride base nano column array comprise the following steps：
Step A：Aln layer, gallium nitride film layer are sequentially formed on substrate, the substrate is Sapphire Substrate.
Step B：The applying silicon oxide film layer on the gallium nitride film layer.
Step C：The layer gold of 1nm thickness is deposited in the silica membrane layer surface, the layer gold is steamed using heat
Gold is put into thermal evaporation coil by hair coating machine, plus 15 amperes of electric current, makes its distillation evaporation to silica membrane.
Step D：Evaporation thickness is 15nm nickel dam on the layer gold surface, forms metallic nickel island structure；The nickel dam is
Using thermal evaporation coating machine, under 20A electric current, its distillation is set to be vaporized on the surface of the layer gold.The evaporation thickness of different nickel
The average-size of metallic island structure eventually formed is influenceed, the thickness of nickel is bigger, and metallic island structure is bigger.
Step E：Use etching technics with metallic nickel island structure shape to gallium nitride film layer, silica membrane layer, gold
Layer and nickel dam perform etching, and form nanometer columnar arrays.
Above-described embodiment prepare gallium nitride base nano column array in, the aln layer include aln nucleation layer with
And it is formed at the pulse supplying high temperature aln layer on the aln nucleation layer.The formation of aln layer comprises the following steps：
Step 1：Utilize MOCVD one layer of 10-20nm of epitaxial growth on a sapphire substrate high-temperature ammonolysis aluminium nucleating layer, its formation condition
For 950-1100 DEG C of temperature, V/III molar flows ratio is 90-110, atmospheric pressure value 55-70Torr.The high-temperature ammonolysis aluminium of formation into
Stratum nucleare provides nucleation site for next growth pulse supplying high temperature aln layer；Step 2：Method is supplied in high-temperature ammonolysis with pulse
Extension forms pulse supplying high temperature aln layer on aluminium nucleating layer, and the thickness of pulse supplying high temperature aln layer is 75-85nm, its
Formation condition be temperature to 1150-1250 DEG C, V/III molar flows ratio is 1650-1750, atmospheric pressure value 225Torr.Formed
Pulse supplying high temperature aln layer improves the smooth degree of aln surface.
After the completion of prepared by aln layer, growth temperature is adjusted to 1110-1150 DEG C, V/III molar flows ratio is 1650-
1750, atmospheric pressure value 225Torr, on this condition, it is 0.8- that growth, which forms thickness, on pulse supplying high temperature aln layer
1.2um gallium nitride film layer.
Before nickel dam is deposited, one layer of about 0.5-1.5nm layer gold, then and then is first deposited on silica membrane
10-20nm nickel dam is deposited.When the thickness of the nickel of evaporation is blocked up, thickness the easy adhesion of island structure of formation, is not easy more than 20nm
Separation.
The gallium nitride base nano column array that the present invention is prepared with ni-au bimetallic as shown in Figure 3 b, its either shape,
Size, density, uniformity, repetitive rate etc. are all significantly better than the sample that conventional method is prepared.
Uniformity of the nanometer island structure that the present invention is prepared using the double film methods of nickel gold in shape, density and size
It is better than the nano island prepared using conventional method.It greatly improves the photoelectricity of the related photoelectric device using its preparation effect
Rate, when recycling gallium nitride nano-pillar realizes the growth of MOCVD secondary epitaxies, gallium nitride base nano column array can make gallium nitride
Quality is substantially improved, and then improves the luminous efficiency of the devices such as LED.The secondary of gallium nitride has been carried out to Fig. 3 a and Fig. 3 b sample
Extension, if Fig. 3 b nickel metal nano island XRD halfwidths are 400arc sec, and the XRD on Fig. 3 a nickel metal nano island half is high
Width is 550arc sec or so, and halfwidth is lower, and explanation crystal mass is better.The lifting of crystal mass can be substantially improved LED's
The efficiency of luminous efficiency and gallium nitride base photoelectric device.As shown in Figure 3 b, it is prepared using the double membrane technologies of ni-au of the present invention
The structural representation of the gallium nitride nano column array gone out, it can be seen that the gallium nitride base nanometer prepared using the present invention
Post array is significantly better than the nano column array that conventional method is prepared.The nano column array prepared using new method is to gallium nitride
Carry out MOCVD secondary laterally overgrown.Under identical MOCVD growth conditions, the crystal mass of gallium nitride has significantly
The lifting of degree.
The present invention is based on " self-organizing nano dot " principle, it is proposed that the new method for preparing gallium nitride base nano column array,
Gallium nitride base nano column array has more preferable uniformity, and preferably repeatability in size, shape, density etc..This
Shape, the size more rule of the gallium nitride base nano column array of invention, uniformity is more preferable, substantially increases its photoelectric device effect
The crystal mass of the gallium nitride of rate and secondary epitaxy.
Although above with general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (8)
- A kind of 1. preparation method of gallium nitride base nano column array, it is characterised in that the system of the gallium nitride base nano column array Preparation Method comprises the following steps：Step A：Aln layer, gallium nitride film layer are sequentially formed on substrate；Step B：The applying silicon oxide film layer on the gallium nitride film layer；Step C：The layer gold of 0.5-1.5nm thickness is deposited in the silica membrane layer surface；Step D：Evaporation thickness is 10-20nm nickel dam on the layer gold surface, forms metallic nickel island structure；Step E：Use etching technics with metallic nickel island structure shape to gallium nitride film layer, silica membrane layer, layer gold with And nickel dam performs etching, nanometer columnar arrays are formed.
- 2. the preparation method of gallium nitride base nano column array according to claim 1, it is characterised in thatThe aln layer includes aln nucleation layer and the pulse supplying high temperature nitrogen being formed on the aln nucleation layer Change aluminium lamination.
- 3. the preparation method of gallium nitride base nano column array according to claim 2, it is characterised in thatThe thickness of the aln nucleation layer is 10-20nm, and its growth temperature is 950-1100 DEG C, V/III molar flow flows Than for 90-110, atmospheric pressure value 55-70Torr.
- 4. the preparation method of gallium nitride base nano column array according to claim 3, it is characterised in thatThe thickness of the pulse supplying high temperature aln layer is 75-85nm, and its formation condition is that temperature is 1150-1250 DEG C, V/ III molar flows ratio is 1650-1750, atmospheric pressure value 220-230Torr.
- 5. the preparation method of gallium nitride base nano column array according to claim 1, it is characterised in thatThe thickness of the gallium nitride film layer is 0.8-1.2um.
- 6. the preparation method of gallium nitride base nano column array according to claim 1, it is characterised in thatThe layer gold is that gold is put into thermal evaporation coil using thermal evaporation coating machine, and it is added into the electric current of 14-16 amperes, made It, which distils, is deposited onto silica membrane.
- 7. the preparation method of gallium nitride base nano column array according to claim 1, it is characterised in thatThe nickel dam is to utilize thermal evaporation coating machine, under 18-22A electric current, its distillation is vaporized on the surface of the layer gold.
- 8. the preparation method of gallium nitride base nano column array according to claim 1, it is characterised in thatThe substrate is Sapphire Substrate.
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