CN114232085B - Method for epitaxial growth of InGaAs on InP substrate - Google Patents
Method for epitaxial growth of InGaAs on InP substrate Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 58
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000000407 epitaxy Methods 0.000 claims abstract description 23
- 238000003795 desorption Methods 0.000 claims abstract description 19
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 7
- 229910052738 indium Inorganic materials 0.000 claims abstract description 7
- 238000007872 degassing Methods 0.000 claims abstract description 5
- 238000007781 pre-processing Methods 0.000 claims abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 238000002128 reflection high energy electron diffraction Methods 0.000 claims description 4
- 238000005336 cracking Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 230000010287 polarization Effects 0.000 claims 1
- 230000001681 protective effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 22
- 229910002059 quaternary alloy Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000000969 carrier Substances 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 229910000673 Indium arsenide Inorganic materials 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000572 ellipsometry Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000603 solid-source molecular beam epitaxy Methods 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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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
- C30B25/16—Controlling or regulating
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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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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- 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 provides a method for epitaxially growing InGaAs on an InP substrate, which comprises the following steps: step 1, measuring the oxide film thickness of an InP substrate; step 2, determining growth rates of Ga and In; step 3, preprocessing and degassing the InP substrate; step 4, after the pretreatment in the step 3 is completed, the InP substrate is desorbed by an oxide film; step 5, carrying out InP buffer layer epitaxy after the desorption of the oxide film in the step 4 is completed; step 6, after the extension of the InP buffer layer in the step 5 is completed, the P valve is closed, and the As valve is opened to the required beam position; and 7, after the P/As beam switching in the step 6 is completed, carrying out InGaAs epitaxy. The method provided by the invention can avoid time deviation caused by observing the surface reconstruction of the substrate through the high-energy electron diffractometer, can effectively reduce the formation of quaternary alloy interfaces between the InP buffer layer and the InGaAs material, reduce impurity defects, reduce the concentration of InGaAs carriers and improve the mobility of the material.
Description
Technical Field
The invention belongs to the technical field of semiconductor material growth, and particularly relates to a method for epitaxially growing InGaAs on an InP substrate.
Background
The InGaAs material is composed of binary materials InAs and GaAs, the InAs and the GaAs are both direct band gap semiconductors and are both sphalerite structures, the composed InGaAs material is also a direct band gap semiconductor, and when In components are different, the forbidden band width of the InGaAs material is changed within 0.35-1.43 eV. When the In composition In the InGaAs material is 0.53, the InGaAs material and the InP substrate are lattice-matched, and the forbidden band width is 0.74eV.
InGaAs has many advantages over other materials, and using it as an absorber material allows for very fast response and operation detectors. The PIN detector made of InGaAs material plays an important role in optical fiber transmission, has higher internal quantum efficiency and lower dark current, and abandons the detector which needs refrigeration equipment to continuously work at room temperature in the past, so that the detector has good development prospect. High-speed photodetectors employing InGaAs material as the absorber layer have greatly evolved, and a number of different modes of operation have emerged, including InGaAs Avalanche Photodetectors (APDs), inGaAs PIN photodetectors, inGaAs metal-semiconductor-metal photodetectors (MSM-PD).
Therefore, the high mobility InGaAs material is obtained by using a solid source molecular beam epitaxy system through epitaxy, becomes an important research direction of the epitaxy of the InGaAs device material, and has important significance for the epitaxy production of the InGaAs photoelectric device and the micro-electric device material.
Disclosure of Invention
Based on the above problems, a main object of the present invention is to propose a method of epitaxially growing InGaAs on InP substrates.
The invention adopts the following technical scheme:
a method of epitaxially growing InGaAs on an InP substrate comprising the steps of:
step 1, measuring the oxide film thickness of an InP substrate;
step 2, determining growth rates of Ga and In;
step 3, preprocessing and degassing the InP substrate;
step 4, after the pretreatment in step 3 is completed, carrying out desorption of the oxide film on the InP substrate, wherein the desorption time of the oxide film is according to t= -2.3h 2 +8.4h+2.2 acknowledgementDetermining, wherein t is the desorption time of the oxide film, the unit is min, h is the thickness of the oxide film of the InP substrate obtained in the step 1, and the unit is nm;
step 5, carrying out InP buffer layer epitaxy after the desorption of the oxide film in the step 4 is completed;
step 6, after the extension of the InP buffer layer in the step 5 is completed, the P valve is closed, and the As valve is opened to the required beam position;
and 7, after the P/As beam switching in the step 6 is completed, carrying out InGaAs epitaxy.
Preferably, the InP substrate oxide film thickness is measured using an ellipsometer in step 1.
Preferably, the growth rate measurement of Ga and In step 2 uses a high energy electron diffractometer device.
Preferably, the temperature for preprocessing the InP substrate in the step 3 is 350-400 ℃, the preprocessing time is 1-2 hours, and the temperature and the cooling rate are 15-25 ℃/min.
Preferably, in step 4, the P beam is used as the substrate protecting gas, the substrate heater is heated until the RHEED pattern of the substrate appears x 4 reconstruction stripe, the temperature is Tc, and Tc is set as the reference temperature.
Preferably, in step 5, after the desorption of the oxide film is completed, the temperature of the substrate is reduced to 30 ℃ to 50 ℃ below Tc, and the InP buffer layer epitaxy is performed.
Preferably, in the step 5, an epitaxial growth of the InP buffer layer is performed using a solid-state phosphorus source pyrolysis furnace, wherein the V/III ratio of the P to In beam is 5-20.
Preferably, the duration of closing the P valve in step 6 is not more than 2 minutes; the As valve is opened to the desired beam position for no more than 2 minutes.
Preferably, in the step 7, the epitaxy temperature of InGaAs is 50 ℃ to 100 ℃ below Tc.
Preferably, in the step 7, the epitaxial V/III ratio of the InGaAs is 10-25.
The invention has the beneficial effects that:
the epitaxial method of the InGaAs high-mobility material has the following beneficial effects:
(1) The thickness of the InP substrate oxide film is obtained through ellipsometry, the desorption time of the substrate oxide film is set according to the thickness value and the empirical formula, the relation between the oxide film thickness and the desorption time can be effectively quantized, and the time deviation caused by the reconstruction of the substrate surface is avoided through observation of a high-energy electron diffractometer.
(2) The P/As beam switching process can effectively reduce the formation of quaternary alloy interfaces between the InP buffer layer and the InGaAs material, reduce impurity defects, reduce the concentration of InGaAs carriers and improve the mobility of the material.
(3) The invention can be popularized to the growth of other III-V arsenides and phosphide materials, can be used for the preparation of semiconductor devices with various system materials, and has good universality.
Drawings
Fig. 1 is a schematic diagram of the epitaxial structure of the method of the present invention for epitaxially growing InGaAs on an InP substrate.
Reference numerals illustrate: 101. an InP substrate; 102. an InP buffer layer; 103. an InGaAs epitaxial layer.
Detailed Description
The invention is further described below in connection with examples which are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the claims, as other alternatives will occur to those skilled in the art and are within the scope of the claims.
The invention provides a method for epitaxially growing InGaAs on an InP substrate, which comprises the following steps:
in step 1, the oxide film thickness of InP substrate 101 is measured, and the oxide film thickness of InP substrate 101 may be measured using an ellipsometer.
Step 2, the growth rates of Ga and In are measured, and can be measured using a high-energy electron diffractometer device.
And step 3, carrying out pretreatment and degassing on the InP substrate 101, wherein the pretreatment temperature is 350-400 ℃, the pretreatment time is 1-2 hours, and the heating and cooling rates are 15-25 ℃/min.
Step 4, after the pretreatment in step 3 is completed, the InP substrate 101 is desorbed with the oxide film, and the oxide film is desorbedThe interval is according to t= -2.3h 2 +8.4h+2.2, wherein t is the desorption time of the oxide film, the unit is min, and h is the thickness of the oxide film of the InP substrate obtained in the step 1, and the unit is nm; the P beam is used as a substrate shielding gas, the substrate heater is warmed up to the RHEED pattern where x 4 reconstruction fringes appear, at which point the temperature is Tc, and Tc is set as the reference temperature.
And 5, after the desorption of the oxide film In the step 4 is completed, the substrate temperature is reduced to 30-50 ℃ below Tc to carry out the epitaxy of the InP buffer layer 102, and a solid phosphorus source cracking furnace can be used for carrying out the epitaxy of the InP buffer layer 102, wherein the V/III ratio of P to In beam is 5-20.
And 6, after the InP buffer layer 102 is epitaxially finished in step 5, closing the P valve, opening the As valve to the required beam position, and controlling the closing time of the P valve to be not more than 2 minutes, and opening the As valve to the required beam position to be not more than 2 minutes.
And 7, after the P/As beam switching in the step 6 is completed, growing an InGaAs epitaxial layer 103, wherein the epitaxial temperature of the InGaAs is 50-100 ℃ below Tc, and the epitaxial V/III ratio of the InGaAs is 10-25.
The desorption time of the oxide film is set according to the thickness test value, so that time deviation caused by observing the surface reconstruction of the substrate in the traditional method is avoided, and a quaternary alloy interface between the InP buffer layer and the InGaAs material is avoided by adopting a P/As switching process after the growth of the InP buffer layer is completed. The process is simple and repeatable, and is suitable for mass production.
Example 1
Step 1, the oxide film thickness of the InP substrate was measured, and the oxide film thickness of the InP substrate was measured to be 0.8nm using an ellipsometer.
Step 2, the growth rates of Ga and In were determined using a high energy electron diffractometer apparatus, wherein the ratio of Ga growth rate to In growth rate was 47/53.
And step 3, carrying out pretreatment degassing on the InP substrate, wherein the pretreatment temperature is 350 ℃, the pretreatment time is 1h, and the heating and cooling rates are 25 ℃/min.
Step 4, after the pretreatment in step 3 is completed, the InP substrate is desorbed with the oxide film, and the oxide filmAccording to t= -2.3h 2 And (2) determining +8.4h+2.2, wherein t is the desorption time length of the oxide film, the unit is min, h is the thickness of the oxide film of the InP substrate obtained in the step (1), the unit is nm, the desorption time length of the oxide film is 7.26min, P beams are used as substrate protection gas, the substrate heater is heated until the RHEED pattern is in x 4 reconstruction stripes, the temperature is Tc, the Tc is 580 ℃, and the Tc is set as a reference temperature.
And 5, after the desorption of the oxide film In the step 4 is completed, the substrate temperature is reduced to 30 ℃ below Tc, namely 550 ℃ to carry out InP buffer layer epitaxy, and a solid phosphorus source cracking furnace can be used for carrying out InP buffer layer epitaxy, wherein the V/III ratio of P to In beam is 12.
Step 6, after the InP buffer layer epitaxy is completed in step 5, the P valve is reduced to 0% in step mode and maintained for 30s, and the as valve is opened to the desired beam position at 2%/s and maintained for 2min.
And 7, after the P/As beam switching in the step 6 is completed, carrying out InGaAs epitaxy, wherein the epitaxy temperature of the InGaAs is 50 ℃ below Tc, namely 530 ℃, and the epitaxy V/III ratio of the InGaAs is 17.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (5)
1. A method of epitaxially growing InGaAs on an InP substrate, comprising the steps of:
step 1, measuring the thickness of an oxide film of an InP substrate by using an elliptical polarization device;
step 2, determining growth rates of Ga and In;
step 3, preprocessing and degassing the InP substrate;
step 4, after the pretreatment in step 3 is completed, carrying out desorption of the oxide film on the InP substrate, wherein the desorption time of the oxide film is according to t= -2.3h 2 +8.4h+2.2, wherein t is the desorption time of the oxide film, the unit is min, and h is the thickness of the oxide film of the InP substrate obtained in the step 1, and the unit is nm; heating a substrate heater until the RHEED pattern of the substrate has x 4 reconstruction stripes by using P beam as substrate protective gas, wherein the temperature is Tc, and Tc is set as a reference temperature;
step 5, after the desorption of the oxide film In the step 4 is completed, carrying out InP buffer layer epitaxy, and carrying out InP buffer layer epitaxy by using a solid-state phosphorus source cracking furnace, wherein the V/III ratio of P to In beam is 5-20;
step 6, after the extension of the InP buffer layer in the step 5 is completed, the P valve is closed, the As valve is opened to the required beam position, and the closing time of the P valve is not longer than 2 minutes; the time for opening the As valve to the position of the required beam current is not more than 2 minutes;
and 7, after the P/As beam switching in the step 6 is completed, carrying out InGaAs epitaxy, wherein the epitaxy V/III ratio of the InGaAs is 10-25.
2. The method of epitaxial growth of InGaAs on an InP substrate according to claim 1, wherein the growth rate measurement of Ga and In step 2 uses a high-energy electron diffractometer device.
3. The method for epitaxial growth of InGaAs on an InP substrate according to claim 1, wherein the temperature of the InP substrate in step 3 is 350-400 ℃ and the pretreatment time is 1-2 hours, wherein the heating and cooling rates are 15-25 ℃/min.
4. The method of epitaxial growth of InGaAs on an InP substrate according to claim 1, wherein in step 5, after the oxide film desorption is completed, inP buffer layer epitaxy is performed by lowering the substrate temperature to 30 ℃ to 50 ℃ below Tc.
5. The method of epitaxial growth of InGaAs on an InP substrate according to claim 1, wherein in step 7, the InGaAs epitaxy temperature is 50 ℃ to 100 ℃ below Tc.
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