CN104593772B - A kind of heteroepitaxial growth antimonide method for semiconductor in Macrolattice mismatch substrate - Google Patents
A kind of heteroepitaxial growth antimonide method for semiconductor in Macrolattice mismatch substrate Download PDFInfo
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- CN104593772B CN104593772B CN201410843205.6A CN201410843205A CN104593772B CN 104593772 B CN104593772 B CN 104593772B CN 201410843205 A CN201410843205 A CN 201410843205A CN 104593772 B CN104593772 B CN 104593772B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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Abstract
A kind of heteroepitaxial growth antimonide method for semiconductor in Macrolattice mismatch substrate, belongs to technical field of semiconductor material preparation.The present invention is before growth antimonide quasiconductor, with other physical depositions (such as magnetron sputtering) film preparing technology deposition of aluminum the most on a silicon substrate (or AlSb) thin layer.Sample is carried in epitaxial growth in MOCVD system again.Growth is only passed through the organic source of Sb before starting, and anneals the most in place, makes aluminum (or AlSb) thin layer antimony, forms stable AlSb buffer layer structure.When antimonide growth starts, the AlSb buffer layer structure existed will promote antimonide semiconductor layer coverage.Whole growth course do not introduces organo-aluminium source in MOCVD system, it is to avoid the aluminum pollution of equipment.The method is possible not only to promote antimonide surface coverage on Macrolattice mismatch substrate, and can avoid aluminum source memory effect in a device.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, it is a kind of heavy with Metallo-Organic Chemical Vapor to be specifically related to
Long-pending (MOCVD) technology heteroepitaxial growth antimonide method for semiconductor in Macrolattice mismatch substrate.
Background technology
Iii-v antimonide is the low energy gap compound semiconductor materials that a class is important, and majority has direct band gap.
Its good electric conductivity makes this kind of material have important application in mid-infrared field with unique photoelectric characteristic, and such as the
Three generations's ultrahigh speed ultra low power integrated circuit, thermophotovoltaic, infrared laser, Infrared Detectors etc..Permitted
Such material is monolithically integrated in existing conventional substrate technology by many companies and the most autotelic research of research institution
On platform.The advantage integrated with conventional substrate is, substrate quality is high, price is low, technology maturation, Ke Yishi
Now single-chip integration and light with more devices are electrically integrated, and meet current integrated chip urgent needs.
At present, during with MOCVD technology epitaxial growth antimonide heterojunction structure, the antimonide layer of substrate surface
Coverage is relatively low, prepares related device difficulty.Its reason be between antimonide quasiconductor and conventional substrate (as silicon,
GaAs etc.) there is Macrolattice mismatch.One improved method is, before antimonide semiconductor growth layer starts,
Antimonide will be effectively promoted as cushion, the introducing of AlSb layer in advance at Grown AlSb micro-nano structure
Semiconductor layer coverage.But aluminum source exists memory effect in MOCVD system, easily cause equipment
Pollute, cause this equipment to form impurity or component deviation when growing other semiconductor lamellas, cause under device quality
Fall.
Summary of the invention
In order to overcome, existing MOCVD technology growth antimonide layer coverage is low, MOCVD system aluminum source dirty
The problem of dye, the present invention provides a kind of new growing method, and the method is possible not only to promote antimonide at big lattice
Surface coverage in mismatch substrate, and aluminum source memory effect in a device can be avoided.
The technical solution adopted for the present invention to solve the technical problems is: before growth antimonide quasiconductor, with it
His physical deposition (such as magnetron sputtering) film preparing technology deposition of aluminum the most on a silicon substrate (or AlSb) is thin
Layer.Sample is carried in epitaxial growth in MOCVD system again.Growth is only passed through the organic source of Sb before starting,
Anneal the most in place, make aluminum (or AlSb) thin layer antimony, form stable AlSb buffer layer structure.Work as antimony
When compound growth starts, the AlSb buffer layer structure existed will promote antimonide semiconductor layer coverage.
Whole growth course do not introduces organo-aluminium source in MOCVD system, it is to avoid the aluminum pollution of equipment.
By DC magnetron sputtering process in the upper step preparing GaSb of Macrolattice mismatch substrate (as a example by Si)
As follows:
(1) with 800～1000w magnetically controlled DC sputtering power, sputtering 30～60nm is thick on a si substrate
Aluminium lamination or aluminium antimonide layer, after having sputtered cool down substrate to room temperature；
(2) the Si substrate of sputtered aluminum layer is loaded in MOCVD reative cell, 200～300mbar,
Under conditions of 500～600 DEG C, it is passed through antimony triethyl (TESb (C2H5)3Sb)) organic source
30～60s (with hydrogen as carrier gas, its flow velocity is 1000～1200sccm (milliliters every point),
The intake of TESb is 0.5 × 10-6～1.5 × 10-6Mol/min), make aluminium lamination antimony, obtain
Aluminium antimonide layer；
(3) in MOCVD reative cell, in-situ annealing 2～3 minutes under the conditions of 650～800 DEG C, make
Aluminium antimonide layer that step (2) obtains or the aluminium antimonide layer that step (1) directly obtains are formed stable
Island (island a diameter of 80～200nm, height be 100～200nm) aluminium antimonide buffering knot
Structure (annealing process can significantly reduce the ratio that in aluminium antimonide, dephasign exists)；Annealing process is held
Continue and be passed through TESb, to suppress antimony in the volatilization of substrate surface；
(4) in MOCVD reative cell, under the conditions of 500～600 DEG C, 200～300mbar, simultaneously
The organic source of TESb of input gas phase and the organic source of trimethyl gallium (TMGa (CH3)3Ga))
20～30min (with hydrogen as carrier gas, its flow velocity is 1000～1200sccm, and TESb is organic
The intake in source is 0.5 × 10-6～1.5 × 10-6The intake in the organic source of mol/min, TMGa
It is 2.5 × 10-7～7.5 × 10-7Mol/min, and the intake in the organic source of V group element TESb
For 2 to 5 times of group-III element TMGa organic source intake, thus delay at island aluminium antimonide
The surface rushing structure obtains the GaSb thin layer that thickness is 0.3～0.7 micron.
The invention has the beneficial effects as follows, promote the covering at Macrolattice mismatch substrate surface of the antimonide quasiconductor
Degree, prepares the antimonide thin film of highly crystalline quality, avoids using aluminum source to make in MOCVD system simultaneously
The equipment pollution become, method is simple, cost-effective.
Accompanying drawing explanation
The sample surfaces stereoscan photograph of Fig. 1: comparative example 1 preparation；
The sample surfaces stereoscan photograph of preparation in Fig. 2: embodiment 2；
Fig. 3: routine techniques is at Si substrate Epitaxial growth antimonide method for semiconductor schematic diagram；
Fig. 4: the present invention is an embodiment schematic diagram of extension antimonide semiconductor approach in Si substrate；
Fig. 5: the present invention is another embodiment schematic diagram of extension antimonide semiconductor approach in Si substrate；
As it can be seen, each several part is entitled: substrate 1, GaSb layer 2, AlSb thin layer 3, AlSb island is tied
Structure 4, Al thin layer 5, the Sb layer 6 that organic source is decomposed to form.
Detailed description of the invention
Comparative example 1:
The Si substrate 1 of cleaning is loaded in MOCVD reative cell, abstraction reaction chamber pressure to 1mbar
Hereinafter, being passed through carrier gas (hydrogen 1200sccm), substrate, under 200mbar, is added by control reative cell pressure
Heat is to 600 DEG C, and being simultaneously entered gas phase V/III is 2 (V group element and the molar ratios in group-III element MO source
Be 2) TESb source and (with hydrogen as carrier gas, its flow velocity is 1200sccm, TESb source in TMGa source
Intake be 1 × 10-6The intake of mol/min, TMGa is 5 × 10-7Mol/min), extension is carried out raw
Long half an hour, thus on Macrolattice mismatch Si substrate 1, directly grow antimonide quasiconductor GaSb layer 2,
But its surface coverage is low, as shown in Figure 1.
Embodiment 1:
First the silicon substrate 1 of cleaning is loaded into magnetic control platform, loads aluminium antimonide sputtering target material, adjust target-substrate distance
80mm.System vacuum is evacuated to 10-5Pa magnitude, is filled with argon, and input flow rate is about 100sccm,
Adjustment sputtering pressure is 1Pa.Adjustment sputtering power is to 800W, and sputtering time is 10 minutes, at Si substrate table
Face obtains the aluminium antimonide thin layer 3 of about 0.1 μ m-thick；Stop sputtering, recover reative cell pressure to normal pressure (about
1000mbar), after substrate is cooled to room temperature, open magnetic control platform, rapidly substrate is loaded into
MOCVD reative cell.
By MOCVD reative cell extracting vacuum to below 1mbar, use hydrogen as carrier gas, recover reative cell
Pressure is to 200mbar；It is warming up to 700 DEG C anneal 2 minutes, forms stable AlSb island structure 4；Finally
At 550 DEG C, the intake being passed through TESb and TMGa, TESb is 1 × 10-6Mol/min, TMGa's
Intake is 5 × 10-7Mol/min, above substrate, hydrogen flow rate is 1200sccm, epitaxial growth GaSb layer
2, growth time is half an hour.Comparative example 1 shown in this flow process comparison diagram 1 improves substrate surface GaSb layer 2
Coverage.
Embodiment 2:
The silicon substrate 1 of cleaning is loaded into magnetic control platform, loads aluminum target, adjust target-substrate distance 80mm.By system
Vacuum is evacuated to 10-5Pa magnitude, is filled with argon, and input flow rate is about 100sccm, adjusts sputtering pressure and is
1Pa.Adjustment sputtering power is to 800W, and sputtering time is 5 minutes, obtains about 30nm at Si substrate surface thick
Aluminum thin layer 5.Stop sputtering, recover reative cell pressure, after substrate is cooled to room temperature, open magnetron sputtering
Platform, is loaded into rapidly MOCVD reative cell by substrate.
By MOCVD reative cell extracting vacuum to below 1mbar, use hydrogen as carrier gas, recover reative cell
Pressure is to 200mbar；It is warming up to 550 DEG C, using hydrogen as carrier gas, is passed through TESb growth, its input quantity
It is 1 × 10-6Mol/min, growth time is 1 minute, forms the Sb thin layer 6 of about 10nm on Al layer surface；
Then in MOCVD system, it is warming up to 700 DEG C of in-situ annealing 1 minute, keeps the input flow rate of TESb to press down
The surface volatilization of Sb processed, forms stable AlSb structure 4；Last at 550 DEG C, it is passed through TESb simultaneously
(1×10-6Mol/min) with TMGa (5 × 10-7Mol/min), above substrate, hydrogen flow rate is
1200sccm, epitaxial growth GaSb layer 2, growth time is half an hour.Contrast shown in this flow process comparison diagram 1
Example 1 improves the coverage of substrate surface GaSb layer 2, as shown in Figure 2.
Claims (5)
1. a heteroepitaxial growth antimonide method for semiconductor in Macrolattice mismatch substrate, its step is as follows:
(1) with 800～1000w magnetically controlled DC sputtering power, sputtering 30～60nm is thick on a si substrate
Aluminium lamination or aluminium antimonide layer, after having sputtered cool down substrate to room temperature；
(2) the Si substrate of sputtered aluminum layer is loaded in MOCVD reative cell, 200～300mbar,
Under conditions of 500～600 DEG C, with hydrogen as carrier gas, it is passed through the organic source of TESb 30～60s,
Make aluminium lamination antimony, obtain aluminium antimonide layer；
(3) in MOCVD reative cell, in-situ annealing 2～3 minutes under the conditions of 650～800 DEG C, make
Aluminium antimonide layer that step (2) obtains or the aluminium antimonide layer that step (1) directly obtains are formed stable
Island aluminium antimonide buffer structure；
(4) in MOCVD reative cell, under the conditions of 500～600 DEG C, 200～300mbar, with hydrogen
Gas is carrier gas, is simultaneously entered the organic source of TESb and the organic source of TMGa 20～30min of gas phase,
Thus obtain, on the surface of island aluminium antimonide buffer structure, the GaSb that thickness is 0.3～0.7 micron
Thin layer.
A kind of heteroepitaxial growth antimonide quasiconductor in Macrolattice mismatch substrate
Method, it is characterised in that: in step (2), the flow velocity of hydrogen is 1000～1200sccm, TESb's
Intake is 0.5 × 10-6～1.5 × 10-6mol/min。
A kind of heteroepitaxial growth antimonide quasiconductor in Macrolattice mismatch substrate
Method, it is characterised in that: the annealing process of step (3) is continually fed into TESb, to suppress antimony at substrate
The volatilization on surface.
A kind of heteroepitaxial growth antimonide quasiconductor in Macrolattice mismatch substrate
Method, it is characterised in that: in step (4), the flow velocity of hydrogen is 1000～1200sccm, and TESb has
The intake in machine source is 0.5 × 10-6～1.5 × 10-6The intake in the organic source of mol/min, TMGa is 2.5
×10-7～7.5 × 10-7mol/min。
A kind of heteroepitaxial growth antimonide quasiconductor in Macrolattice mismatch substrate
Method, it is characterised in that: the intake in the organic source of group Ⅴ element TESb is that III race's element T MGa is organic
2 to 5 times of source intake.
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| CN105696081B (en) * | 2016-03-23 | 2018-03-30 | 西北工业大学 | The preparation method of aluminium antimonide material |
| CN106702482B (en) * | 2016-12-23 | 2018-12-25 | 电子科技大学 | A method of growing indium stibide film on a silicon substrate |
| WO2020071025A1 (en) * | 2018-10-02 | 2020-04-09 | 国立研究開発法人科学技術振興機構 | Heteroepitaxial structure and method for producing same, metal layered product containing heteroepitaxial structure and method for producing same, and nanogap electrode and method for producing nanogap electrode |
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| CN101207022A (en) * | 2006-12-21 | 2008-06-25 | 中国科学院半导体研究所 | Method for epitaxial generation of gallium antimonide on gallium arsenide substrate |
| CN103915537A (en) * | 2013-01-09 | 2014-07-09 | 理想能源设备(上海)有限公司 | Growth method of compound semiconductor epitaxial layer on silicon substrate and device structure with epitaxial layer |
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| CN101207022A (en) * | 2006-12-21 | 2008-06-25 | 中国科学院半导体研究所 | Method for epitaxial generation of gallium antimonide on gallium arsenide substrate |
| CN103915537A (en) * | 2013-01-09 | 2014-07-09 | 理想能源设备(上海)有限公司 | Growth method of compound semiconductor epitaxial layer on silicon substrate and device structure with epitaxial layer |
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Effective date of registration: 20180212 Address after: 224500 extension section of the people south road of the industrial park of Yancheng City Binhai Economic Development Zone in Jiangsu Province Patentee after: BINHAI ZHIRUN ELECTRONIC CO., LTD. Address before: 130012 Changchun Qianjin Street, Jilin, No. 2699 Patentee before: Jilin University |