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CN106783948A - Growth InN nano-pillar epitaxial wafers on a si substrate and preparation method thereof - Google Patents

Growth InN nano-pillar epitaxial wafers on a si substrate and preparation method thereof Download PDF

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CN106783948A
CN106783948A CN201611166965.3A CN201611166965A CN106783948A CN 106783948 A CN106783948 A CN 106783948A CN 201611166965 A CN201611166965 A CN 201611166965A CN 106783948 A CN106783948 A CN 106783948A
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nano
inn
growth
substrate
pillars
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CN106783948B (en
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李国强
高芳亮
温雷
张曙光
徐珍珠
韩晶磊
余粤锋
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South China University of Technology SCUT
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    • C30B29/10—Inorganic compounds or compositions
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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Abstract

The invention discloses growth InN nano-pillar epitaxial wafers on a si substrate, include Si substrates, In metal nanos microballoon layer and InN nano-pillars layer successively from the bottom to top.A diameter of 20 70nm of the In metal nano microballoons in the In metal nanos microballoon layer.A diameter of 40 80nm of InN nano-pillars in the InN nano-pillars layer.The invention also discloses the preparation method of growth InN nano-pillar epitaxial wafers on a si substrate.Nanometer column diameter of the invention is homogeneous, the technical barrier that InN produces a large amount of dislocations because existing between Si wherein compared with Macrolattice mismatch is solved simultaneously, greatly reduce the defect concentration of InN nano-pillar epitaxial layers, the favourable radiation recombination efficiency that improve carrier, can increase substantially the luminous efficiency of nitride device such as semiconductor laser, light emitting diode.

Description

Growth InN nano-pillar epitaxial wafers on a si substrate and preparation method thereof
Technical field
The present invention relates to InN nano-pillars epitaxial wafer and preparation method, InN nano-pillars on a si substrate are more particularly to grown Epitaxial wafer and preparation method thereof.
Background technology
III-V nitride is excellent due to stable physicochemical properties, thermal conductivity high and electron saturation velocities high etc. Point, is widely used in the aspects such as light emitting diode (LED), laser and opto-electronic device.In III-V nitride, nitridation Indium (InN) is more and more interested to researchers due to its own unique advantage.In III nitride semiconductor, InN Get over speed with minimum effective electron mass, highest carrier mobility and highest saturation, for Developing High-speed electronics Device is extremely advantageous.Moreover, InN has minimum direct band gap, and its energy gap is about 0.7eV, and this allows for nitridation The light emitting region of thing based light-emitting diode is widened near infrared region (0.7eV) from ultraviolet (6.2eV), in infrared laser, entirely Spectrum shows and the aspect such as high conversion efficiency solar cell illustrates great application prospect.With other III-V nitrides half Conductor material is compared, and in addition to above-mentioned advantage, its nano level material is in quantum effect, interfacial effect, volume effect for InN materials Should, the aspect such as dimensional effect also show more novel characteristics.
At present, III-V nitride semiconductor devices is mainly based upon Sapphire Substrate Epitaxial growth and preparation.So And, sapphire is low due to thermal conductivity, and the heat that the high power nitride semiconductor device with sapphire as substrate is produced cannot have Effect release, causes that heat is constantly accumulative to rise temperature, the deterioration of Accelerate nitriding thing semiconductor devices, exist device performance it is poor, The shortcomings of short life.By contrast, the thermal conductivity of Si is higher than sapphire, and cost is relatively low.High-performance, low is prepared on a si substrate The nitride compound semiconductor device of cost is inevitable development trend.However, growth diameter is homogeneous on a si substrate, order is high InN nano-pillars be prepare high-performance nitride semiconductor light electrical part first put forward condition.Due to the lattice mismatch between Si and InN It is big with thermal mismatching；Meanwhile, in early growth period, the difference of the In and N atom distribution proportions of substrate surface causes the InN of growth to receive Situations such as meter Zhu has height, path length is uneven, order is poor.
Most using direct growth InN nano-pillars on a si substrate at present, the nano-pillar that this growing method is obtained is straight Footpath heterogeneity, that is, the diameter of top and bottom is inconsistent, in the nano-pillar of the patterns such as inverted pyramid, softball bat.According to In, Ni, Au etc. carry out the growth of InN nano-pillars as catalyst, are deposited after growth as the metal such as In, Ni and Au of catalyst It is the top of InN, when element manufacturing is subsequently carried out, it is necessary to the metallic catalyst on top is removed, increased device technology Complexity.
The content of the invention
In order to overcome the disadvantages mentioned above and deficiency of prior art, Si substrates are grown in it is an object of the invention to provide one kind On InN nano-pillar epitaxial wafers, by the In metal nano microballoons on Si substrates, first, In metal nano microballoons are used as in InN In supplementary sources during nanocolumn growth, are conducive to forming core and the growth of the homogeneous InN nano-pillars of order high, diameter；Secondly, The technical barrier that InN produces a large amount of dislocations because existing between Si wherein compared with Macrolattice mismatch is solved, is greatly reduced The defect concentration of InN nano-pillar epitaxial layers, favorably improves the radiation recombination efficiency of carrier, can increase substantially nitride device The luminous efficiency of part such as semiconductor laser, light emitting diode.
Preparation side another object of the present invention is to provide above-mentioned growth InN nano-pillar epitaxial wafers on a si substrate Method, nano-pillar morphology controllable, preparation cost cheap advantage simple with growth technique.
The purpose of the present invention is achieved through the following technical solutions：
Growth InN nano-pillar epitaxial wafers on a si substrate, include Si substrates, In metal nano microballoons successively from the bottom to top Layer and InN nano-pillars layer.
A diameter of 20-70nm of the In metal nano microballoons in the In metal nanos microballoon layer.
The a diameter of 40-80nm of InN nano-pillars in the InN nano-pillars layer.
The preparation method of described growth InN nano-pillar epitaxial wafers on a si substrate, comprises the following steps：
(1) Si substrates cleaning；
(2) deposition In metal nanos microballoon layer：Using molecular beam epitaxial growth technique, underlayer temperature is controlled in 400-550 DEG C, it is 5.0~6.0 × 10 in the pressure of reative cell-10Under the conditions of Torr, In films are deposited on a si substrate, and annealed, obtain In metal nano microballoons；
(3) growth of InN nano-pillars layer：Using molecular beam epitaxial growth technique, underlayer temperature is controlled at 500~700 DEG C, It is 4.0~10.0 × 10 in the pressure of reative cell-5Torr, line than V/III values be 30~40 under the conditions of, obtained in step (2) In metal nano microballoons on the homogeneous InN nano-pillars of growth diameter.
The temperature of annealing is 400-550 DEG C in step (2), and annealing time is 50-300 seconds.
Step (1) the substrate cleaning, specially：
It is 1 that Si substrates are put into volume ratio:Ultrasound 1~2 minute in 20 HF and deionized water mixed solution, removal silicon lining Basal surface oxide and pickup particle, place into ultrasonic 1~2 minute, removal surface impurity in deionized water, use high-purity dry nitrogen Air-blowing is done.
A diameter of 20-70nm of the In metal nano microballoons in the In metal nanos microballoon layer.
The a diameter of 40-80nm of InN nano-pillars in the InN nano-pillars layer.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) growth of the invention InN nano-pillar epitaxial wafers on a si substrate, micro- by the In metal nanos on Si substrates Ball, solves the technical barrier that InN produces a large amount of dislocations because existing between Si wherein compared with Macrolattice mismatch, greatly reduces The defect concentration of InN nano-pillar epitaxial layers, favorably improves the radiation recombination efficiency of carrier, can increase substantially nitride The luminous efficiency of device such as semiconductor laser, light emitting diode.
(2) growth of the invention InN nano-pillar epitaxial wafers on a si substrate, using Si substrates, Si substrates have easy The advantage of removal, electrode is made on the InN nano-pillar semiconductor epitaxial wafers after Si substrates are removed, and is conducive to preparing vertical stratification Nitride compound semiconductor device.Si substrates have radioresistance, thermal conductivity high, high temperature resistant, chemical property relatively stable, intensity higher simultaneously The advantages of, with reliability very high, the InN nano-pillar epitaxial wafers based on Si substrates can be widely applied to high-temperature device.
(3) present invention uses Si as substrate, and In and shape of annealing first are deposited on a si substrate using molecular beam epitaxy technique Into In metal nano microballoons, pre-deposition In metal nanos microballoon on a si substrate is used as during InN nanocolumn growths In supplementary sources, it is to avoid InN nano-pillars in growth course because In sources deficiency causes to occur top diameter more than base diameter, directly The inhomogenous nano-pillar in footpath, is conducive to forming core and the growth of the homogeneous InN nano-pillars of order high, diameter, solves in Si substrates On be difficult to the technical barrier of the homogeneous InN nano-pillars of direct growth diameter.
(4) growth technique of the invention is unique and simple and easy to apply, with repeatability.
Brief description of the drawings
Fig. 1 is the structural representation of growth of the invention InN nano-pillar epitaxial wafers on a si substrate.
Fig. 2 is the electron scanning micrograph that embodiments of the invention 1 deposit In metal nano microballoons on a si substrate.
Fig. 3 is to deposit the InN nano-pillars for obtaining on the In metal nanos microballoon layer on a si substrate of embodiments of the invention 1 Electron scanning micrograph.
Fig. 4 is the cross sectional scanning electron microphotograph of direct growth InN nano-pillars on a si substrate.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
Fig. 1 is the structural representation of the growth InN nano-pillar epitaxial wafers on a silicon substrate of the present embodiment, from the bottom to top according to It is secondary including Si substrates 1, In metal nanos microballoon layer 2 and InN nano-pillars layer 3.
The preparation method of the growth of the present embodiment InN nano-pillar epitaxial wafers on a silicon substrate, comprises the following steps：
(1) selection of substrate and its crystal orientation：Using common Si substrates；
(2) substrate cleaning：It is 1 that Si substrates are put into volume ratio:2 points of ultrasound in 20 HF and deionized water mixed solution Clock, removes Si substrate surfaces oxide and pickup particle, places into ultrasonic 2 minutes, removal surface impurity, with height in deionized water Pure drying nitrogen drying；
(3) In metal nano microballoons are deposited：Using molecular beam epitaxial growth technique, underlayer temperature is controlled at 400 DEG C, anti- The pressure for answering room is 6.0 × 10-10Under the conditions of Torr, In films are deposited on a si substrate, and annealed 50 seconds in the original location, form straight Footpath is the In metal nano microballoons of 30-50nm.
(4) growth of the homogeneous InN nano-pillars of diameter：Using molecular beam epitaxial growth technique, underlayer temperature is controlled 600 DEG C, it is 6.0 × 10 in the pressure of reative cell-5Torr, line than V/III values be 30 under the conditions of, in the In metals that step (3) is obtained Diameter is homogeneous, the InN nano-pillars that diameter is distributed as 30-80nm for the Si Growns top and bottom of Nano microsphere.
As shown in Fig. 2 the present embodiment pre-deposition In metal nanos are micro- on a si substrate, the In of its a diameter of 30-50nm gold Category Nano microsphere electron scanning micrograph.
Fig. 3 is InN nanometer that embodiment 1 grows that order high, diameter be homogeneous, top remains without metal In on a si substrate Post electron scanning micrograph, shows the InN nano-pillar epitaxial wafer excellent performances of present invention preparation.And on a si substrate The cross sectional scanning electron microphotograph of direct growth InN nano-pillars is as shown in Figure 4, it is known that, using directly raw on a si substrate The nanometer column diameter heterogeneity that the growing method of InN nano-pillars long is obtained, that is, the diameter of top and bottom is inconsistent, is in The nano-pillar of the patterns such as inverted pyramid, softball bat.
Embodiment 2
The growth of the present embodiment InN nano-pillars epitaxial wafer on a silicon substrate includes Si substrates, In gold successively from the bottom to top Category Nano microsphere layer and InN nano-pillars layer.
The preparation method of the growth of the present embodiment GaN nano-pillar LEDs on a si substrate, comprises the following steps：
(1) selection of substrate and its crystal orientation：Using common Si substrates；
(2) substrate cleaning：It is 1 that Si substrates are put into volume ratio:2 points of ultrasound in 20 HF and deionized water mixed solution Clock, removes surface of silicon oxide and pickup particle, places into ultrasonic 1 minute, removal surface impurity, with height in deionized water Pure drying nitrogen drying；
(3) In metal nano microballoons are deposited：Using molecular beam epitaxial growth technique, underlayer temperature is controlled at 550 DEG C, anti- The pressure for answering room is 6.0 × 10-10Under the conditions of Torr, In films are deposited on a si substrate, and annealed 300 seconds in the original location, form straight Footpath is the In metal nano microballoons of 50-70nm.
(4) growth of the homogeneous InN nano-pillars of diameter：Using molecular beam epitaxial growth technique, underlayer temperature is controlled 700 DEG C, it is 6.0 × 10 in the pressure of reative cell-5Torr, line than V/III values be 40 under the conditions of, in the In metals that step (3) is obtained Diameter is homogeneous, the InN nano-pillars that diameter is distributed as 30-80nm for the Si Growns top and bottom of Nano microsphere.
InN nano-pillars epitaxial wafer on Si substrates manufactured in the present embodiment either in electrical properties, optical property, is gone back It is that all there is extraordinary performance in defect concentration, crystalline quality, test data is close with embodiment 1, will not be repeated here.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by the embodiment Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (8)

1. InN nano-pillar epitaxial wafers on a si substrate are grown, it is characterised in that include Si substrates, In gold successively from the bottom to top Category Nano microsphere layer and InN nano-pillars layer.
2. growth InN nano-pillar epitaxial wafers on a si substrate according to claim 1, it is characterised in that the In gold A diameter of 20-70nm of the In metal nano microballoons in category Nano microsphere layer.
3. growth InN nano-pillar epitaxial wafers on a si substrate according to claim 1, it is characterised in that the InN receives The a diameter of 40-80nm of InN nano-pillars in rice post layer.
4. the preparation method of the growth InN nano-pillar epitaxial wafers on a si substrate described in claim 1, it is characterised in that bag Include following steps：
(1) Si substrates cleaning；
(2) deposition In metal nanos microballoon layer：Using molecular beam epitaxial growth technique, underlayer temperature is controlled at 400-550 DEG C, The pressure of reative cell is 5.0~6.0 × 10-10Under the conditions of Torr, In films are deposited on a si substrate, and annealed, obtain In metals Nano microsphere；
(3) growth of InN nano-pillars layer：Using molecular beam epitaxial growth technique, underlayer temperature is controlled at 500~700 DEG C, anti- The pressure for answering room is 4.0~10.0 × 10-5Torr, line than V/III values be 30~40 under the conditions of, in the In that step (2) is obtained The homogeneous InN nano-pillars of growth diameter on metal nano microballoon.
5. the preparation method of growth InN nano-pillar epitaxial wafers on a si substrate according to claim 1, its feature exists In the temperature of annealing is 400-550 DEG C in step (2), and annealing time is 50-300 seconds.
6. the preparation method of growth InN nano-pillar epitaxial wafers on a si substrate according to claim 1, its feature exists In, step (1) the Si substrates cleaning, specially：
It is 1 that Si substrates are put into volume ratio:Ultrasound 1~2 minute in 20 HF and deionized water mixed solution, removes silicon substrate table Face oxide and pickup particle, place into ultrasonic 1~2 minute, removal surface impurity, with high-purity dry nitrogen air-blowing in deionized water It is dry.
7. the preparation method of growth InN nano-pillar epitaxial wafers on a si substrate according to claim 1, its feature exists In a diameter of 20-70nm of the In metal nano microballoons in the In metal nanos microballoon layer.
8. the preparation method of growth InN nano-pillar epitaxial wafers on a si substrate according to claim 1, its feature exists In a diameter of 40-80nm of InN nano-pillars in the InN nano-pillars layer.
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PCT/CN2017/090006 WO2018107713A1 (en) 2016-12-16 2017-06-26 Inn nanocolumn epitaxial wafer grown on si substrate and fabrication method for wafer

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Cited By (10)

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WO2018107713A1 (en) * 2016-12-16 2018-06-21 华南理工大学 Inn nanocolumn epitaxial wafer grown on si substrate and fabrication method for wafer
CN107731975A (en) * 2017-10-24 2018-02-23 江门市奥伦德光电有限公司 A kind of nanotube LED and preparation method thereof
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CN108231545A (en) * 2018-01-11 2018-06-29 华南理工大学 It is grown in InN nano-pillar epitaxial wafers on copper foil substrate and preparation method thereof
CN108206130B (en) * 2018-01-11 2023-10-10 华南理工大学 Indium nitride nano-pillar epitaxial wafer grown on aluminum foil substrate and preparation method thereof
CN108206130A (en) * 2018-01-11 2018-06-26 华南理工大学 It is grown in indium nitride nano-pillar epitaxial wafer in aluminum substrates and preparation method thereof
CN108735866A (en) * 2018-07-20 2018-11-02 华南理工大学 It is grown in InN nano-pillar epitaxial wafers and preparation method thereof in Si/ graphene compound substrates
CN110747506A (en) * 2019-10-22 2020-02-04 华南理工大学 Transition metal doped InxGa1-xN nano column and preparation method and application thereof
CN114657534A (en) * 2022-02-18 2022-06-24 华南理工大学 MoS-based2InN nano column on, preparation method and application thereof
CN114657641A (en) * 2022-02-22 2022-06-24 华南理工大学 Annealed Si-based InN nano-column heterojunction and preparation method and application thereof
CN114921804A (en) * 2022-04-26 2022-08-19 华南理工大学 Photoelectrode material based on InN/organic heterostructure and preparation method and application thereof
CN114921804B (en) * 2022-04-26 2023-06-20 华南理工大学 InN/organic heterostructure-based photoelectrode material and preparation method and application thereof
CN114875493A (en) * 2022-04-29 2022-08-09 华南理工大学 InN-VIA group heterojunction on Si substrate and preparation method and application thereof
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