CN116397328B - Component calibration method for molecular beam epitaxy low-aluminum component AlGaAs material - Google Patents
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 105
- 239000000463 material Substances 0.000 title claims abstract description 100
- 238000000034 method Methods 0.000 title claims abstract description 72
- 229910000980 Aluminium gallium arsenide Inorganic materials 0.000 title claims abstract description 64
- 238000001451 molecular beam epitaxy Methods 0.000 title claims abstract description 20
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 claims abstract description 159
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims abstract description 159
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 106
- MDPILPRLPQYEEN-UHFFFAOYSA-N aluminium arsenide Chemical compound [As]#[Al] MDPILPRLPQYEEN-UHFFFAOYSA-N 0.000 claims abstract description 89
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 87
- 239000002994 raw material Substances 0.000 claims abstract description 59
- 238000012360 testing method Methods 0.000 claims abstract description 44
- FTWRSWRBSVXQPI-UHFFFAOYSA-N alumanylidynearsane;gallanylidynearsane Chemical compound [As]#[Al].[As]#[Ga] FTWRSWRBSVXQPI-UHFFFAOYSA-N 0.000 claims description 43
- 238000013101 initial test Methods 0.000 claims description 19
- RNQKDQAVIXDKAG-UHFFFAOYSA-N aluminum gallium Chemical compound [Al].[Ga] RNQKDQAVIXDKAG-UHFFFAOYSA-N 0.000 claims description 14
- 229910052785 arsenic Inorganic materials 0.000 claims description 14
- 238000005259 measurement Methods 0.000 description 23
- 230000000737 periodic effect Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 1
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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
- C30B25/16—Controlling or regulating
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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
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D21/00—Measuring or testing not otherwise provided for
- G01D21/02—Measuring two or more variables by means not covered by a single other subclass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention relates to a component calibration method of a molecular beam epitaxy low-aluminum component AlGaAs material, wherein the component contents of aluminum element and gallium element meet the requirement of Al x Ga 1‑x As, wherein the content of the low aluminum component is 0.2% -10.0%, and the method comprises the following steps: s1, testing growth rate V of gallium arsenide in sample 1 The method comprises the steps of carrying out a first treatment on the surface of the S2, V is 1 Growth rate V of gallium arsenide in target product 0 Comparison is made when V 1 =V 0 At the time, the target gallium raw material temperature T is obtained 1 The method comprises the steps of carrying out a first treatment on the surface of the S3, through T 1 Determining the gallium feed temperature corresponding to one-h of the gallium arsenide growth rate in the sample to be approximately T 2 At a gallium raw material temperature of T 2 Correspondingly, the aluminum component content of AlGaAs in the sample is enlarged; s4, at T 2 Growth rate V of aluminum arsenide in test sample at temperature 3 The method comprises the steps of carrying out a first treatment on the surface of the S5, V is 3 Growth rate V of aluminum arsenide in target product 2 Comparison is made when V 3 =V 2 At the time, a target aluminum raw material temperature T is obtained 3 。
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a component calibration method of a molecular beam epitaxy low-aluminum component AlGaAs material.
Background
The aluminum gallium arsenic, also called aluminum gallium arsenide, is a commonly used semiconductor material, and is generally grown by adopting a molecular beam epitaxy method, in the growth process, the temperature of raw materials required by aluminum element and gallium element in the aluminum gallium arsenic is different, and the growth condition of each element can directly influence the content of corresponding components, so that in the actual processing process, different raw material temperatures are required for producing target aluminum gallium arsenic materials with different component contents.
At present, most of the raw material temperature is determined by adopting an X-ray diffractometer to reflect the growth thickness of each element in the product through satellite peaks of superlattice samples, but in the low-aluminum-component AlGaAs material, the accuracy of aluminum component measurement cannot be ensured even by adopting high-power ray diffraction, when the content of the aluminum component is extremely low, even the corresponding satellite peaks cannot be distinguished, so that the thickness and the component content cannot be calculated, and therefore, the raw material temperature most suitable for the growth of the product cannot be judged, and the prepared AlGaAs material often cannot reach the practical application standard.
Disclosure of Invention
Therefore, the invention aims to solve the technical problems that in the prior art, the accurate components of the low-aluminum-component AlGaAs material are difficult to test by an X-ray diffractometer, and the temperature of raw materials used for growth of the low-aluminum-component AlGaAs material is difficult to determine, and provides a component calibration method of the molecular beam epitaxy low-aluminum-component AlGaAs material.
In order to solve the technical problems, the invention provides a component calibration method of a molecular beam epitaxy low-aluminum component AlGaAs material, wherein the component contents of aluminum element and gallium element meet the requirement of Al x Ga 1-x As, the content of the aluminum element is lower than that of the gallium element, and the method comprises the following steps: s1, testing growth rate V of gallium arsenide in sample 1 The method comprises the steps of carrying out a first treatment on the surface of the S2, V is 1 Growth rate V of gallium arsenide in target product 0 Comparison was performed: when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample; when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample; when V is 1 =V 0 Obtaining the target gallium raw material temperature T during sample growth 1 The method comprises the steps of carrying out a first treatment on the surface of the S3, through T 1 Determining the temperature corresponding to the h-th fraction of the gallium arsenide growth rate in the sample as T 2 The method comprises the steps of carrying out a first treatment on the surface of the S4, at T 2 Growth rate V of aluminum arsenide in test sample at temperature 3 The method comprises the steps of carrying out a first treatment on the surface of the S5, V is 3 Growth rate V of aluminum arsenide in target product 2 Comparison was performed: when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth; when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth; when V is 3 =V 2 Obtaining the target aluminum raw material temperature T during sample growth 3 。
In one embodiment of the present invention, step S1 includes: s11 determining the initial test temperature T of the gallium by gallium vapor pressure curve 4 Determination of aluminum arsenide initial test temperature T with same growth rate of gallium arsenide material by aluminum vapor pressure curve 5 At a temperature T 4 Gallium arsenide is grown down for a second, thenTemperature T 5 Growing aluminum arsenide for b seconds, and obtaining a first set of gallium arsenide/aluminum arsenide superlattice materials after a plurality of cycles; s12 at temperature T 4 Gallium arsenide is grown for c seconds, then at temperature T 5 Growing aluminum arsenide for d seconds, and obtaining a second set of gallium arsenide/aluminum arsenide superlattice materials after a plurality of cycles, wherein a x d-b x c is not equal to 0; s13, respectively testing the thickness of each period of the first set of gallium arsenide/aluminum arsenide superlattice materials to be n-meter, and the thickness of each period of the second set of gallium arsenide/aluminum arsenide superlattice materials to be m-meter, and calculating the growth rate V of gallium arsenide 1 =(dn-bm)/(ad-bc)。
In one embodiment of the invention, the thickness of the first set of gallium arsenide/aluminum arsenide superlattice materials at each cycle is measured using an X-ray diffractometer.
In one embodiment of the invention, the thickness of the second set of gallium arsenide/aluminum arsenide superlattice materials at each cycle is measured using an X-ray diffractometer.
In one embodiment of the present invention, step S4 includes: s41 determination of its initial test temperature T by means of an aluminum vapor pressure curve 6 At T 2 Gallium arsenide a is grown first at temperature 1 Second, then at T 2 And T 6 Growth of AlGaAs b at temperature 1 Second, a first set of gallium arsenide/aluminum gallium arsenide superlattice materials are obtained after a plurality of cycles are circulated; s42 at T 2 Gallium arsenide c is grown first at temperature 1 Second, then at T 2 And T 6 Growth of AlGaAs d at temperature 1 Second, a second set of gallium arsenide/aluminum gallium arsenide superlattice materials is obtained after a plurality of cycles are circulated, and a is ensured at the same time 1 ×d 1 -b 1 ×c 1 Not equal to 0; s43, testing the thickness of each period of the first set of GaAs/AlGaAs superlattice material to be n 1 The thickness of each period of the Emi, second set of gallium arsenide/aluminum gallium arsenide superlattice materials is m 1 Emi, calculating the growth rate V of aluminum arsenide in the sample 3 =(a 1 m 1 -c 1 n 1 - d 1 n 1 +b 1 m 1 )/ (a 1 d 1 -b 1 c 1 )。
In one embodiment of the invention, the thickness of the first set of gallium arsenide/aluminum gallium arsenide superlattice materials at each cycle is measured using an X-ray diffractometer.
In one embodiment of the invention, the thickness of the second set of gallium arsenide/aluminum gallium arsenide superlattice materials at each cycle is measured using an X-ray diffractometer.
In one embodiment of the present invention, the content of the aluminum element component in the aluminum gallium arsenide material is in a range of 0.2% -10.0%.
Compared with the prior art, the technical scheme of the invention has the following advantages:
according to the component calibration method of the molecular beam epitaxy low-aluminum component AlGaAs material, provided by the invention, an experimenter can test the temperature of a raw material used for growing the AlGaAs material with relatively accurate low-aluminum component content only through an X-ray diffractometer, so that the testing process is simplified, the situation that the measurement result deviation is large and even cannot be measured due to the fact that the content of an aluminum element component is too low is avoided, and the yield of the AlGaAs material is greatly improved.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings.
FIG. 1 is a flow chart of a component calibration method for molecular beam epitaxy low aluminum component AlGaAs material in a preferred embodiment of the invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Referring to FIG. 1, the invention provides a component calibration method of a molecular beam epitaxy low-aluminum component AlGaAs material, wherein the component contents of aluminum element and gallium element satisfy Al x Ga 1-x As, and the content of the aluminum element is lower than that of the gallium element, comprising the following stepsThe steps are as follows:
s1, testing growth rate V of gallium arsenide in sample 1 ；
S2, V is 1 Growth rate V of gallium arsenide in target product 0 Comparison was performed: when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample; when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample; when V is 1 =V 0 Obtaining the target gallium raw material temperature T during sample growth 1 ；
S3, through T 1 Determining that the temperature corresponding to the h-th fraction of the gallium arsenide growth rate in the sample is approximately T 2 ；
S4, at T 2 Growth rate V of aluminum arsenide in test sample at temperature 3 ；
S5, V is 3 Growth rate V of aluminum arsenide in target product 2 Comparison was performed: when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth; when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth;
when V is 3 =V 2 Obtaining the target aluminum raw material temperature T during sample growth 3 。
According to the component calibration method for the molecular beam epitaxy low-aluminum component AlGaAs material, which is provided by the invention, the content component of gallium is reduced in the AlGaAs material to amplify the content component of aluminum, so that the situation that the XRD measurement result is overlarge and even cannot be measured due to the fact that the content of the component of aluminum is too low when the target component of the AlGaAs material is directly used for determining the temperature of the source material is avoided, and the temperature suitable for growth of the AlGaAs material is determined, and the AlGaAs material reaches the practical application standard.
Example 1
Referring to fig. 1, in this embodiment, an aluminum gallium arsenic material with an aluminum component of 1% needs to be obtained, wherein gallium arsenide accounts for 99% and aluminum arsenide accounts for 1%, in this embodiment, a gallium beam source furnace is used to change the temperature of the gallium raw material, and an aluminum beam source furnace is used to change the temperature of the aluminum raw material, and the specific implementation manner is as follows:
a) Growth rate of gallium arsenide in test sampleRate V 1 The method specifically comprises the following steps: firstly, determining that the initial testing temperature of gallium is 1147 ℃ according to a gallium vapor pressure curve, the temperature of the bottom is 917 ℃, and growing gallium arsenide for 5 seconds at the initial testing temperature of aluminum for gallium arsenide, which is the same as the growth rate of gallium arsenide materials, is 1169 ℃ according to an aluminum vapor pressure curve, the temperature of the bottom is 1169 ℃, and growing aluminum arsenide for 10 seconds at the initial testing temperature of aluminum for gallium, wherein the process is a growth period, and in the embodiment, 50 periods are selected for thickness measurement, so that a first set of gallium arsenide/aluminum arsenide superlattice materials is obtained.
And then growing a second gallium arsenide/aluminum arsenide superlattice, wherein gallium arsenide is grown for 15 seconds under the temperature condition that the temperature of the head of gallium is 1147 ℃ and the temperature of the bottom of gallium is 917 ℃, and then aluminum arsenide is grown for 20 seconds under the temperature of the head of aluminum is 1169 ℃ and the temperature of the bottom of aluminum is 1169 ℃, and the process is a growth period, and in the embodiment, 25 periods are selected for facilitating thickness measurement, so that the second gallium arsenide/aluminum arsenide superlattice material is obtained.
Finally, the first set of gallium arsenide/aluminum arsenide superlattice period thickness is measured to be 41.25 Emeter, the second set of gallium arsenide/aluminum arsenide superlattice period thickness is measured to be 96.25 Emeter, and the growth rate V of gallium arsenide is calculated according to the measured values 1 =2.75 emm/s. In this embodiment, the first set of gallium arsenide/aluminum arsenide superlattice is tested for each period thickness using an X-ray diffractometer, and the second set of gallium arsenide/aluminum arsenide superlattice is also tested for each period thickness using an X-ray diffractometer.
b) Will V 1 Growth rate V of gallium arsenide in target product 0 Comparison is performed =2.75 emm/s: in the present embodiment of the present invention,
when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample;
when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample;
when V is 1 =V 0 In this case, the target gallium raw material temperature at the time of sample growth was obtained, and in this example, the head temperature of gallium was 1147℃and the bottom temperature was 917 ℃.
c) By having a head temperature of 11Determining the corresponding temperature T when gallium arsenide growth rate in a sample is one tenth of that of gallium vapor pressure curve under the conditions of 47 ℃ and 917 ℃ bottom temperature 2 About: the temperature of the head is 1050 ℃ and the temperature of the bottom is 820 ℃, and the growth rate V of aluminum arsenide in the target AlGaAs is determined 2 =0.0278. In this embodiment, correspondingly, the content of aluminum element in aluminum gallium arsenic is calculated according to the formula: 10× (V 0 +V 2 ）/（V 0 +10×V 2 ) It was calculated to be about 9.2 times larger than before.
d) Testing the growth rate V of aluminum arsenide in the sample under the conditions that the temperature of the head part of gallium is 1050 ℃ and the temperature of the bottom part of gallium is 820 DEG C 3 The method specifically comprises the following steps: gallium arsenide is grown for 50 seconds under the conditions that the temperature of the head of gallium is 1050 ℃ and the temperature of the bottom is 820 ℃, the temperature of the head of target aluminum is 924 ℃ and the temperature of the bottom is 924 ℃ according to an aluminum vapor pressure curve, aluminum gallium arsenide is grown for 100 seconds at the temperature, and the process is a growth cycle, and in the embodiment, 50 cycles are selected for facilitating thickness measurement, so that the first gallium arsenide/aluminum gallium arsenide superlattice material is obtained.
And then growing a second set of gallium arsenide/aluminum gallium arsenide superlattice, wherein gallium arsenide is grown for 150 seconds under the temperature condition that the temperature of the head is 1050 ℃ and the temperature of the bottom is 820 ℃, and then aluminum gallium arsenide is grown for 200 seconds under the temperature of the head of 924 ℃ and the temperature of the bottom of 924 ℃ to obtain a second set of gallium arsenide/aluminum gallium arsenide superlattice material, and the process is a growth period, and in the embodiment, 20 periods are selected for thickness measurement to obtain the second set of gallium arsenide/aluminum gallium arsenide superlattice material.
Finally, the first set of GaAs/AlGaAs superlattice period thickness is 44.03 and the second set of GaAs/AlGaAs superlattice period thickness is 101.81, respectively, and the growth rate V of aluminum arsenide in the test sample is calculated according to the first set of GaAs/AlGaAs superlattice period thickness 3 =0.0278 emm/s. Further, the process uses an X-ray diffractometer to test a first set of gallium arsenide/aluminum gallium arsenide superlattice period thicknesses, and also uses an X-ray diffractometer to test a second set of gallium arsenide/aluminum gallium arsenide superlattice period thicknesses.
e) Will V 3 Growth rate V of aluminum arsenide in target product 2 Comparison =0.0278 emm/s: in the present embodiment of the present invention,
when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth;
when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth;
when V is 3 =V 2 When the sample was grown, the target aluminum was obtained at a head temperature of 924 ℃ and a bottom temperature of 924 ℃. To this end, the temperatures of the gallium and aluminum feedstock required for growth of the low aluminum composition AlGaAs material have been determined. In this example, the gallium arsenide substrate deoxidized thermocouple temperature was 580 ℃ and the growth thermocouple temperature was 580 ℃.
In sum, by the component calibration method of the molecular beam epitaxy low-aluminum component AlGaAs material, an experimenter can test the growth raw material temperature of the AlGaAs material with relatively accurate low-aluminum component content only by an X-ray diffractometer, so that the testing process is simplified, the situation that the measurement result deviation is large and even cannot be measured due to the too low content of the aluminum element component is avoided, and the yield of the AlGaAs material is greatly improved.
Example two
Referring to fig. 1, in this embodiment, an aluminum gallium arsenic material with an aluminum component of 0.2% needs to be obtained, wherein gallium arsenide accounts for 99.8% and aluminum arsenide accounts for 0.2%, in this embodiment, a gallium beam source furnace is used to change the temperature of the gallium raw material, and an aluminum beam source furnace is used to change the temperature of the aluminum raw material, and the specific implementation manner is as follows:
a) Growth rate V of gallium arsenide in test sample 1 The method specifically comprises the following steps: firstly, determining that the initial testing temperature of gallium is 1147 ℃ according to a gallium vapor pressure curve, the temperature of the bottom is 917.3 ℃, and growing gallium arsenide for 5 seconds at the initial testing temperature of aluminum for gallium arsenide, determining that the initial testing temperature of aluminum for aluminum arsenide, which has the same growth rate as that of gallium arsenide materials, is 1169 ℃ according to an aluminum vapor pressure curve, and growing aluminum arsenide for 10 seconds at the initial testing temperature of aluminum arsenide, wherein the process is a growth period, and in the embodiment, 50 periods are selected for thickness measurement, so that a first set of gallium arsenide/aluminum arsenide superlattice materials is obtained.
And then growing a second gallium arsenide/aluminum arsenide superlattice, wherein gallium arsenide is grown for 15 seconds under the temperature condition that the temperature of the head of gallium is 1147 ℃ and the temperature of the bottom of gallium is 917.3 ℃, and then aluminum arsenide is grown for 20 seconds under the temperature of the head of aluminum is 1169 ℃ and the temperature of the bottom of aluminum is 1169 ℃, and the process is a growth period, and in the embodiment, 25 periods are selected for facilitating thickness measurement, so that the second gallium arsenide/aluminum arsenide superlattice material is obtained.
Finally, the first set of gallium arsenide/aluminum arsenide superlattice period thickness is measured to be 41.58 Emeter, the second set of gallium arsenide/aluminum arsenide superlattice period thickness is measured to be 97.03 Emeter, and the growth rate V of gallium arsenide is calculated according to the measured values 1 =2.77 emm/s. In this embodiment, the first set of gallium arsenide/aluminum arsenide superlattice is tested for each period thickness using an X-ray diffractometer, and the second set of gallium arsenide/aluminum arsenide superlattice is also tested for each period thickness using an X-ray diffractometer.
b) Will V 1 Growth rate V of gallium arsenide in target product 0 Comparison is performed =2.77 emm/s: in the present embodiment of the present invention,
when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample;
when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample;
when V is 1 =V 0 In this case, the target gallium raw material temperature at the time of sample growth was obtained, and in this example, the head temperature of gallium was 1147℃and the bottom temperature was 917.3 ℃.
c) Determining the temperature T corresponding to one twentieth of gallium arsenide growth rate in a sample by a gallium vapor pressure curve at a head temperature of 1147 ℃ and a bottom temperature of 917.3 DEG C 2 About: the temperature of the head is 1021 ℃ and the temperature of the bottom is 791 ℃, and the growth rate V of aluminum arsenide in the target aluminum gallium arsenide is determined 2 =0.0056. In this example, the content of aluminum element in AlGaAs was correspondingly increased to 19.3 times.
d) Testing the growth rate V of aluminum arsenide in the sample under the conditions that the temperature of the head part of gallium is 1021 ℃ and the temperature of the bottom part of gallium is 791 DEG C 3 In particular, theThe method comprises the following steps: gallium arsenide is grown for 50 seconds under the conditions that the temperature of the head of gallium is 1021 ℃ and the temperature of the bottom is 791 ℃, the temperature of the head of aluminum is 839 ℃ and the temperature of the bottom is 839 ℃ according to the estimated aluminum vapor pressure curve, aluminum gallium arsenide is grown for 150 seconds at the temperature, and the process is a growth cycle, and in the embodiment, 70 cycles are selected for growth for thickness measurement, so that the first gallium arsenide/aluminum gallium arsenide superlattice material is obtained.
And then growing a second set of gallium arsenide/aluminum gallium arsenide superlattice, wherein gallium arsenide is grown for 150 seconds under the temperature condition that the temperature of the head is 1021 ℃ and the temperature of the bottom is 791 ℃, and then aluminum gallium arsenide is grown for 200 seconds under the temperature of the head of aluminum is 839 ℃ and the temperature of the bottom is 839 ℃ to obtain a second set of gallium arsenide/aluminum gallium arsenide superlattice material, and the process is a growth period, and in the embodiment, 40 periods are selected for thickness measurement and growth is facilitated, so that the second set of gallium arsenide/aluminum gallium arsenide superlattice material is obtained.
Finally, the first set of GaAs/AlGaAs superlattice period thickness is tested to be 28.56 Emeter, the second set of GaAs/AlGaAs superlattice period thickness is tested to be 49.63 Emeter, and the growth rate V of aluminum arsenide in the test sample is calculated according to the first set of GaAs/AlGaAs superlattice period thickness 3 =0.0056 emm/s. Further, the process uses an X-ray diffractometer to test a first set of gallium arsenide/aluminum gallium arsenide superlattice period thicknesses, and also uses an X-ray diffractometer to test a second set of gallium arsenide/aluminum gallium arsenide superlattice period thicknesses.
e) Will V 3 Growth rate V of aluminum arsenide in target product 2 Comparison is performed =0.0056 emm/s: in the present embodiment of the present invention,
when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth;
when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth;
when V is 3 =V 2 At this time, the temperature of the head of the target aluminum at 839℃and the temperature of the bottom at 839℃were obtained at the time of sample growth. To this end, the temperatures of the gallium and aluminum feedstock required for growth of the low aluminum composition AlGaAs material have been determined. In this example, the gallium arsenide substrate deoxidized thermocouple temperature was 580 ℃ and the thermocouple was grownThe temperature was 580 ℃.
In sum, by the component calibration method of the molecular beam epitaxy low-aluminum component AlGaAs material, an experimenter can test the growth raw material temperature of the AlGaAs material with relatively accurate low-aluminum component content only by an X-ray diffractometer, so that the testing process is simplified, the situation that the measurement result deviation is large and even cannot be measured due to the too low content of the aluminum element component is avoided, and the yield of the AlGaAs material is greatly improved.
Example III
Referring to fig. 1, in this embodiment, an aluminum gallium arsenic material with an aluminum component of 5% needs to be obtained, wherein gallium arsenide accounts for 95% and aluminum arsenide accounts for 5%, in this embodiment, a gallium beam source furnace is used to change the temperature of the gallium raw material, and an aluminum beam source furnace is used to change the temperature of the aluminum raw material, and the specific implementation manner is as follows:
a) Growth rate V of gallium arsenide in test sample 1 The method specifically comprises the following steps: firstly, determining that the initial testing temperature of gallium is 1145 ℃ according to a gallium vapor pressure curve, the temperature of the bottom is 915.2 ℃, and growing gallium arsenide for 5 seconds at the initial testing temperature of aluminum for gallium arsenide, determining that the initial testing temperature of aluminum for aluminum arsenide, which has the same growth rate as that of gallium arsenide materials, is 1166 ℃ according to an aluminum vapor pressure curve, and growing aluminum arsenide for 10 seconds at the initial testing temperature of aluminum arsenide, wherein the process is a growth period, and in the embodiment, 50 periods are selected for thickness measurement, so that a first set of gallium arsenide/aluminum arsenide superlattice materials is obtained.
And then growing a second gallium arsenide/aluminum arsenide superlattice, wherein gallium arsenide is grown for 15 seconds under the temperature condition that the temperature of the head of gallium is 1145 ℃ and the temperature of the bottom of gallium is 915.2 ℃, and then aluminum arsenide is grown for 20 seconds under the temperature of the head of aluminum is 1166 ℃ and the temperature of the bottom of aluminum is 1166 ℃, and the process is a growth period, and in the embodiment, 25 periods are selected for facilitating thickness measurement, so that the second gallium arsenide/aluminum arsenide superlattice material is obtained.
Finally, the periodic thickness of the first set of gallium arsenide/aluminum arsenide superlattice is measured to be 39.58 Emi, the periodic thickness of the second set of gallium arsenide/aluminum arsenide superlattice is measured to be 92.36 Emi, and the growth rate V of gallium arsenide is calculated according to the periodic thickness 1 =2.64 emm/s. In this embodiment, the first set of gallium arsenide/aluminum arsenide superlattice is tested for each period thickness using an X-ray diffractometer, and the second set of gallium arsenide/aluminum arsenide superlattice is also tested for each period thickness using an X-ray diffractometer.
b) Will V 1 Growth rate V of gallium arsenide in target product 0 Comparison is performed =2.64 emm/s: in the present embodiment of the present invention,
when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample;
when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample;
when V is 1 =V 0 In this case, the target gallium raw material temperature at the time of sample growth was obtained, and in this example, the head temperature of gallium was 1145℃and the bottom temperature was 915.2 ℃.
c) Determining the corresponding temperature T at one tenth of the gallium arsenide growth rate in the sample by a gallium vapor pressure curve under the conditions of a head temperature of 1145 ℃ and a bottom temperature of 915.2 DEG C 2 About: the temperature of the head is 1048 ℃ and the temperature of the bottom is 818 ℃, and the growth rate V of aluminum arsenide in the target AlGaAs is determined 2 = 0.1389. In this example, the content of aluminum element in AlGaAs was correspondingly increased to 6.9 times.
d) Testing the growth rate V of aluminum arsenide in the sample under the conditions that the temperature of the head of gallium is 1048 ℃ and the temperature of the bottom of gallium is 818 DEG C 3 The method specifically comprises the following steps: gallium arsenide is grown for 50 seconds under the conditions that the temperature of the head of gallium is 1048 ℃ and the temperature of the bottom of gallium is 818 ℃, the temperature of the head of aluminum is 1010 ℃ and the temperature of the bottom of aluminum is 1010 ℃ according to the estimated aluminum vapor pressure curve, aluminum gallium arsenide is grown for 100 seconds at the temperature, and the process is a growth cycle, and in the embodiment, 40 cycles are selected for growth for thickness measurement, so that the first gallium arsenide/aluminum gallium arsenide superlattice material is obtained.
And then growing a second set of gallium arsenide/aluminum gallium arsenide superlattice, wherein gallium arsenide is grown for 150 seconds under the temperature condition that the temperature of the head is 1048 ℃ and the temperature of the bottom is 818 ℃, and then aluminum gallium arsenide is grown for 200 seconds under the temperature of the head of aluminum is 1010 ℃ and the temperature of the bottom is 1010 ℃ to obtain a second set of gallium arsenide/aluminum gallium arsenide superlattice material, and the process is a growth period, and in the embodiment, 20 periods are selected for thickness measurement and growth is facilitated to obtain the second set of gallium arsenide/aluminum gallium arsenide superlattice material.
Finally, the first set of GaAs/AlGaAs superlattice period thickness is 53.47 and the second set of GaAs/AlGaAs superlattice period thickness is 120.14, respectively, and the growth rate V of aluminum arsenide in the test sample is calculated according to the first set of GaAs/AlGaAs superlattice period thickness 3 = 0.1389 emm/s. Further, the process uses an X-ray diffractometer to test a first set of gallium arsenide/aluminum gallium arsenide superlattice period thicknesses, and also uses an X-ray diffractometer to test a second set of gallium arsenide/aluminum gallium arsenide superlattice period thicknesses.
e) Will V 3 Growth rate V of aluminum arsenide in target product 2 Comparison is carried out = 0.1389 emm/s: in the present embodiment of the present invention,
when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth;
when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth;
when V is 3 =V 2 In this case, the temperature of the head of the target aluminum at 1010℃and the temperature of the bottom at 1010℃were obtained when the sample was grown. To this end, the temperatures of the gallium and aluminum feedstock required for growth of the low aluminum composition AlGaAs material have been determined. In this example, the gallium arsenide substrate deoxidized thermocouple temperature was 580 ℃ and the growth thermocouple temperature was 580 ℃.
In sum, by the component calibration method of the molecular beam epitaxy low-aluminum component AlGaAs material, an experimenter can test the growth raw material temperature of the AlGaAs material with relatively accurate low-aluminum component content only by an X-ray diffractometer, so that the testing process is simplified, the situation that the measurement result deviation is large and even cannot be measured due to the too low content of the aluminum element component is avoided, and the yield of the AlGaAs material is greatly improved.
Example IV
Referring to fig. 1, in this embodiment, an aluminum gallium arsenic material with an aluminum component of 10% needs to be obtained, wherein gallium arsenide accounts for 90% and aluminum arsenide accounts for 10%, in this embodiment, a gallium beam source furnace is used to change the temperature of the gallium raw material, and an aluminum beam source furnace is used to change the temperature of the aluminum raw material, and the specific implementation manner is as follows:
a) Growth rate V of gallium arsenide in test sample 1 The method specifically comprises the following steps: firstly, determining that the temperature of a gallium initial test temperature head is 1143 ℃ and the temperature of the bottom is 913 ℃ according to a gallium vapor pressure curve, and growing gallium arsenide for 5 seconds at the temperature, determining that the temperature of an aluminum initial test temperature head is 1164 ℃ and the temperature of the bottom is 1164 ℃ according to an aluminum vapor pressure curve, and growing aluminum arsenide for 10 seconds at the temperature, wherein in the embodiment, 55 periods are selected for thickness measurement, so as to obtain a first gallium arsenide/aluminum arsenide superlattice material.
And then growing a second gallium arsenide/aluminum arsenide superlattice, wherein gallium arsenide is grown for 15 seconds under the temperature condition that the temperature of the head of gallium is 1143 ℃ and the temperature of the bottom of gallium is 913 ℃, and aluminum arsenide is grown for 20 seconds under the temperature of the head of aluminum is 1164 ℃ and the temperature of the bottom of aluminum is 1164 ℃, and the process is a growth period, and in the embodiment, 25 periods are selected for facilitating thickness measurement, so that the second gallium arsenide/aluminum arsenide superlattice material is obtained.
Finally, the first set of gallium arsenide/aluminum arsenide superlattice period thickness is measured to be 37.5 Emeter, the second set of gallium arsenide/aluminum arsenide superlattice period thickness is measured to be 87.5 Emeter, and the growth rate V of gallium arsenide is calculated according to the first set of gallium arsenide/aluminum arsenide superlattice period thickness 1 =2.5 emm/s. In this embodiment, the first set of gallium arsenide/aluminum arsenide superlattice is tested for each period thickness using an X-ray diffractometer, and the second set of gallium arsenide/aluminum arsenide superlattice is also tested for each period thickness using an X-ray diffractometer.
b) Will V 1 Growth rate V of gallium arsenide in target product 0 Comparison is performed =2.5 emm/s: in the present embodiment of the present invention,
when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample;
when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample;
when V is 1 =V 0 In this example, the temperature of the gallium at the head of 1143℃and the temperature of the gallium at the bottom of 913.0 ℃were obtained as the target gallium raw material temperature for sample growth.
c) Determining the corresponding temperature T at one tenth of the gallium arsenide growth rate in the sample by a gallium vapor pressure curve under the conditions of a head temperature of 1143 ℃ and a bottom temperature of 913.0 DEG C 2 About: the temperature of the head is 1046 ℃ and the temperature of the bottom is 816 ℃, and the growth rate V of aluminum arsenide in the target AlGaAs is determined 2 = 0.2778. In this example, the content of aluminum element in AlGaAs was correspondingly increased by 5.3 times.
d) Testing the growth rate V of aluminum arsenide in the sample under the conditions that the temperature of the gallium head is 1046 ℃ and the temperature of the bottom is 816 DEG C 3 The method specifically comprises the following steps: gallium arsenide is grown for 50 seconds under the conditions that the temperature of the head of gallium is 1046 ℃ and the temperature of the bottom is 816 ℃, the temperature of the head of aluminum is 1047 ℃ and the temperature of the bottom is 1047 ℃ according to the estimated aluminum vapor pressure curve, aluminum gallium arsenide is grown for 100 seconds at the temperature, and the process is a growth cycle, and in the embodiment, 40 cycles are selected for growth for thickness measurement, so that the first gallium arsenide/aluminum gallium arsenide superlattice material is obtained.
And then growing a second set of gallium arsenide/aluminum gallium arsenide superlattice, wherein gallium arsenide is grown for 150 seconds under the temperature condition that the temperature of the head is 1046 ℃ and the temperature of the bottom is 816 ℃, and then aluminum gallium arsenide is grown for 200 seconds under the temperature of the head of 1047 ℃ and the temperature of the bottom of 1047 ℃ to obtain a second set of gallium arsenide/aluminum gallium arsenide superlattice material, and the process is a growth period, and in the embodiment, 20 periods are selected for thickness measurement and growth is facilitated to obtain the second set of gallium arsenide/aluminum gallium arsenide superlattice material.
Finally, the first set of GaAs/AlGaAs superlattice period thickness is 65.28 Emeter, the second set of GaAs/AlGaAs superlattice period thickness is 143.06 Emeter, and the growth rate V of aluminum arsenide in the test sample is calculated according to the first set of GaAs/AlGaAs superlattice period thickness 3 = 0.2778 emm/s. Further, the process uses an X-ray diffractometer to test the periodic thickness of the first set of GaAs/AlGaAs superlattice and also uses an X-ray diffractometer to test the second set of GaAs/AlGaAs superlatticeArsenic superlattice period thickness.
e) Will V 3 Growth rate V of aluminum arsenide in target product 2 Comparison is carried out = 0.2778 emm/s: in the present embodiment of the present invention,
when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth;
when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth;
when V is 3 =V 2 At this time, the head temperature of the target aluminum at the time of sample growth was 1047℃and the bottom temperature was 1047 ℃. To this end, the temperatures of the gallium and aluminum feedstock required for growth of the low aluminum composition AlGaAs material have been determined. In this example, the gallium arsenide substrate deoxidized thermocouple temperature was 580 ℃ and the growth thermocouple temperature was 580 ℃.
In sum, by the component calibration method of the molecular beam epitaxy low-aluminum component AlGaAs material, an experimenter can test the growth raw material temperature of the AlGaAs material with relatively accurate low-aluminum component content only by an X-ray diffractometer, so that the testing process is simplified, the situation that the measurement result deviation is large and even cannot be measured due to the too low content of the aluminum element component is avoided, and the yield of the AlGaAs material is greatly improved.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (5)
1. Component calibration method of molecular beam epitaxy low-aluminum component AlGaAs material, wherein the component contents of aluminum element and gallium element meet Al x Ga 1-x As, and the component content of the aluminum element is lower than that of the gallium element, and the aluminum gallium arsenic material is characterized in that the component content of the aluminum element in the aluminum gallium arsenic material is in the range of 0.2-10.0 percent, and specifically comprises the following steps:
s1, testing growth rate V of gallium arsenide in sample 1 The method specifically comprises the following steps:
s11 determining the initial test temperature T of the gallium by gallium vapor pressure curve 4 Determination of aluminum arsenide initial test temperature T with same growth rate of gallium arsenide material by aluminum vapor pressure curve 5 At a temperature T 4 Gallium arsenide is grown down for a second, then at temperature T 5 Growing aluminum arsenide for b seconds, and obtaining a first set of gallium arsenide/aluminum arsenide superlattice materials after a plurality of cycles;
s12 at temperature T 4 Gallium arsenide is grown for c seconds, then at temperature T 5 Growing aluminum arsenide for d seconds, and obtaining a second set of gallium arsenide/aluminum arsenide superlattice materials after a plurality of cycles, wherein a x d-b x c is not equal to 0;
s13 testing each cycle thickness of the first set of gallium arsenide/aluminum arsenide superlattice materials to n-meter and each cycle thickness of the second set of gallium arsenide/aluminum arsenide superlattice materials to m-meter,
calculating the growth rate V of gallium arsenide 1 ＝(dn-bm)/(ad-bc)；
S2, V is 1 Growth rate V of gallium arsenide in target product 0 Comparison was performed:
when V is 1 ＜V 0 In the process, the temperature of the gallium raw material is increased during the growth of the sample;
when V is 1 ＞V 0 Reducing the temperature of the gallium raw material during the growth of the sample;
when V is 1 ＝V 0 Obtaining the target gallium raw material temperature T during sample growth 1 ；
S3, through T 1 Determining the temperature corresponding to the h-th fraction of the gallium arsenide growth rate in the sample as T 2 ；
S4, at T 2 Growth rate V of aluminum arsenide in test sample at temperature 3 The method specifically comprises the following steps:
s41 determination of its initial test temperature T by means of an aluminum vapor pressure curve 6 At T 2 Gallium arsenide a is grown first at temperature 1 Second, then at T 2 And T 6 Growth of AlGaAs b at temperature 1 Second, a first set of gallium arsenide/aluminum gallium arsenide superlattice materials are obtained after a plurality of cycles are circulated;
s42 at T 2 Gallium arsenide c is grown first at temperature 1 Second, then at T 2 And T 6 Growth of AlGaAs d at temperature 1 Second, a second set of gallium arsenide/aluminum gallium arsenide superlattice materials is obtained after a plurality of cycles are circulated, and a is ensured at the same time 1 ×d 1 -b 1 ×c 1 ≠0；
S43, testing the thickness of each period of the first set of GaAs/AlGaAs superlattice material to be n 1 The thickness of each period of the Emi, second set of gallium arsenide/aluminum gallium arsenide superlattice materials is m 1 Emi, calculating the growth rate V of aluminum arsenide in the sample 3 ＝(a 1 m 1 -c 1 n 1 -d 1 n 1 +b 1 m 1 )/(a 1 d 1 -b 1 c 1 )；
S5, V is 3 Growth rate V of aluminum arsenide in target product 2 Comparison was performed:
when V is 3 ＜V 2 Raising the temperature of the aluminum raw material during sample growth;
when V is 3 ＞V 2 Reducing the temperature of the aluminum raw material during sample growth;
when V is 3 ＝V 2 Obtaining the target aluminum raw material temperature T during sample growth 3 。
2. The method for component calibration of molecular beam epitaxy low aluminum component aluminum gallium arsenic material according to claim 1, wherein: the thickness of the first set of gallium arsenide/aluminum arsenide superlattice materials at each cycle was measured using an X-ray diffractometer.
3. The method for component calibration of molecular beam epitaxy low aluminum component aluminum gallium arsenic material according to claim 1, wherein: the thickness of the second set of gallium arsenide/aluminum arsenide superlattice materials at each cycle was measured using an X-ray diffractometer.
4. The method for component calibration of molecular beam epitaxy low aluminum component aluminum gallium arsenic material according to claim 1, wherein: the thickness of the first set of gallium arsenide/aluminum gallium arsenide superlattice materials at each cycle was measured using an X-ray diffractometer.
5. The method for component calibration of molecular beam epitaxy low aluminum component aluminum gallium arsenic material according to claim 1, wherein: and testing the thickness of the second set of gallium arsenide/aluminum gallium arsenide superlattice materials in each period by adopting an X-ray diffractometer.
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| JPH01234390A (en) * | 1988-03-15 | 1989-09-19 | Fujitsu Ltd | Production of gallium arsenic layer and production of gallium arsenic-aluminum gallium arsenic laminate |
| CN101127432A (en) * | 2006-08-16 | 2008-02-20 | 中国科学院半导体研究所 | Ti Hz quanta cascaded semiconductor laser material and its growth method |
| WO2023035549A1 (en) * | 2021-09-07 | 2023-03-16 | 常州纵慧芯光半导体科技有限公司 | Vertical cavity surface emitting laser and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH01234390A (en) * | 1988-03-15 | 1989-09-19 | Fujitsu Ltd | Production of gallium arsenic layer and production of gallium arsenic-aluminum gallium arsenic laminate |
| CN101127432A (en) * | 2006-08-16 | 2008-02-20 | 中国科学院半导体研究所 | Ti Hz quanta cascaded semiconductor laser material and its growth method |
| WO2023035549A1 (en) * | 2021-09-07 | 2023-03-16 | 常州纵慧芯光半导体科技有限公司 | Vertical cavity surface emitting laser and preparation method therefor |
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