CN105632965B - The measuring method of As atoms highest Percentage bound during GaAs molecular beam epitaxial growths - Google Patents

The measuring method of As atoms highest Percentage bound during GaAs molecular beam epitaxial growths Download PDF

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CN105632965B
CN105632965B CN201610171321.7A CN201610171321A CN105632965B CN 105632965 B CN105632965 B CN 105632965B CN 201610171321 A CN201610171321 A CN 201610171321A CN 105632965 B CN105632965 B CN 105632965B
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gaas
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CN105632965A (en
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龚谦
王朋
曹春芳
丁彤彤
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Suzhou Kunyuan Photoelectric Co ltd
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Shanghai Institute of Microsystem and Information Technology of CAS
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/10Measuring as part of the manufacturing process
    • H01L22/12Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/30Structural arrangements specially adapted for testing or measuring during manufacture or treatment, or specially adapted for reliability measurements
    • H01L22/32Additional lead-in metallisation on a device or substrate, e.g. additional pads or pad portions, lines in the scribe line, sacrificed conductors

Abstract

The present invention provides a kind of measuring method of As atom highest Percentage bounds during GaAs molecular beam epitaxial growths, it is characterized in that make the surface that rich Ga and richness As are alternately present in GaAs growth courses using the change of Ga atom lines, and the recording surface time that structure changes again, the expression formula for atom total amount of having more than needed eventually through solution surface, obtains highest Percentage bound of the As atoms in growth course.The measuring method is characterized in that being alternately present by switching but being not limited to second Ga sources shutter richness Ga or richness As surfaces, and measured with RHEED methods, and final result is not related to actual atom total amount, so related to the line value of the final Ga directly measured and As of line rule.For the present invention for preparing material using MBE, particularly Enhanced mobility epitaxial growth (MEE) pattern has important meaning.

Description

Method for measuring highest As atom binding rate in GaAs molecular beam epitaxial growth process
Technical Field
The invention relates to a method for measuring the highest binding rate of As atoms in a GaAs molecular beam epitaxy growth process, in particular to a method for measuring and calculating the highest binding rate of As atoms in a GaAs growth process in a Molecular Beam Epitaxy (MBE) technology, belonging to the technical field of semiconductor materials and device processes.
Background
From the 20 th 70 s to the present, molecular Beam Epitaxy (MBE) technology has been developed as an important crystal material growth technology [1-3] . The material grown epitaxially by MBE is the most important group iii-v semiconductor material, gaAs. The success of arsenide materials depends on a key reason that excess group V As will desorb from the surface of the sample and eventually lead to stoichiometric growth. Thus, in most cases only a portion of the As atoms will be incorporated into the crystal lattice and the sample surface will remain As-rich during growthStatus. The binding rate of As atoms can be defined As the ratio of the amount of As atoms bound to the crystal lattice to the amount of As atoms in the total incident As beam current. First, as desorption is a thermally activated process, the rate of incorporation of As is temperature dependent. In addition, the amount of Ga atoms at a particular temperature also determines the amount of As incorporation, since it determines how many As atoms can be incorporated into the epitaxial lattice, with the remaining excess As atoms being desorbed from the surface.
Therefore, the binding rate of As in molecular beam epitaxial growth is determined by the epitaxial growth temperature of the material and the flow of Ga atoms. When the growth temperature of the material is determined, the combination rate of As is only determined by the Ga atom beam current, and a limit maximum value exists. Since the As atoms tend to be in an excess during the growth of a typical material, it is not particularly necessary to accurately measure the As incorporation ratio. However, it is important to accurately measure the highest binding rate of As in certain cases, such As a special growth mode in molecular beam epitaxy: mobility enhanced epitaxial growth (MEE) the problem of interfacial atomic interdiffusion that often occurs during the epitaxy of heterojunction materials results in the doping of the epitaxial layer ultimately affecting the performance of the device. In order to suppress the problem of interfacial atomic interdiffusion, a lower growth temperature is generally used during the initial growth phase, which, however, leads to a decrease in the mobility of atoms at the growth surface and affects the lattice quality. Finally, MEE epitaxial growth mode of periodic interval growth of III/V family atoms is adopted to solve the problems [4] . One of the keys of the MEE epitaxial growth technology of the GaAs material is to adjust the amount of the As beam current so that the binding rate of As is at the critical point of the maximum value. In addition, if the maximum binding rate of As can be measured, the use of too high As beam current can be avoided when setting growth parameters, so that not only can the waste of source materials be avoided, but also the optimal quality of epitaxial materials can be obtained.
GaAs is a crystal material, atoms in the specific material are positioned on lattice points, and the positions of the atoms on the surface of the crystal can deviate from the positions of the lattice points, and meanwhile, some new chemical bonds are generated, so that the energy of the whole system is reduced to the minimum. The above process is called a surface reconstruction process. For GaAs material, the surface atoms of the GaAs material are moved and bonded in a specific crystal direction, and the surface reconstruction is embodied in high-energy electron diffraction (RHEED) stripes. The RHEED technology is a very critical surface characteristic characterization technology in molecular beam epitaxy, and has an irreplaceable effect. The reconstruction will be different for As-rich or Ga-rich GaAs surfaces, showing (2 × 4) and (4 × 2) surface reconstructions, respectively, in RHEED diffraction fringes. By analyzing the epitaxial growth process of the GaAs material, the obtained result is that the combination rate of As fluctuates periodically around the maximum value by periodically adjusting the value of the Ga beam in the growth process. The present invention is intended to measure and calculate the maximum binding rate of As atoms by using the periodic growth parameter change and the record of reconstruction change of the growth surface by high energy electron beam diffraction (RHEED). The method plays an important role in increasing the control of MEE epitaxial growth process and the like.
The references referred to above are:
1.A.Y.Cho,Growth of Periodic Structures by the Molecular-Beam Method,Appl.Phys.Lett.,19(11),467-468(1971).
2.M.B.Panish,Molecular Beam Epitaxy,Science,208,916-922(1980).
3.E.H.C.Parker,The Technology and Physics of Molecular Beam Epitaxy,Plenum Press(New York),1985.
4.Y.Horikoshi,M.Kawashima and H.Yamaguchi,Migration-Enhanced Epitaxy of GaAs and AlGaAs,Japanse Journal of Applied Physics,27(2),169-179(1988).
disclosure of Invention
The invention aims to provide a method for measuring the highest As atom bonding rate in the GaAs molecular beam epitaxial growth process.
The method comprises the steps of enabling Ga-rich surfaces and As-rich surfaces to appear alternately in the GaAs growth process by utilizing the change of Ga atom beam current, recording the time of surface reconstruction change, and finally obtaining the highest binding rate of As atoms in the growth process by solving the expression of the total amount of surface surplus atoms.
The method specifically comprises the following three steps: 1) Opening a second Ga source in the GaAs growth process, pre-adjusting to enable the As atomic bonding rate to be in the highest value state, observing and recording the time interval of reconstruction of the growth surface from the (2X 4) surface reconstruction in the As-rich state to the (4X 2) surface reconstruction in the Ga-rich state through high-energy electron beam diffraction (RHEED); 2) Immediately switching off the second Ga source when (4X 2) surface reconstruction of the surface in a Ga-rich state occurs, and observing the time interval for changing the (4X 2) to (2X 4) surface reconstruction of the recording growth surface; 3) And measuring the beam equivalent air pressures of the two Ga sources and the As source by using a beam current meter (BFM) in advance, and finally solving to obtain the highest As binding rate according to an equation of the depletion of the surface surplus As atoms and the accumulation of the surface surplus Ga atoms in the two processes.
The alternating appearance of Ga-rich or/and As-rich surfaces during GaAs growth is achieved by switching the second Ga source during the measurement. The key point is that the first Ga source has a beam value which makes the combination rate of As lower than the maximum value, and the sum of the beam values of the two Ga sources makes the combination rate of As reach and exceed the critical point of the highest combination rate. In the calculation of the results, values that cannot be measured, such As the total amount of Ga or As atoms that are surplus on the surface, are eliminated. And the highest binding rate value of As finally obtained already contains the difference of the beam current gauge for different atomic responses.
The measuring method is characterized in that:
(1) The alternating Ga-rich and As-rich surfaces of the GaAs growth process during measurement are achieved by switching, but not limited to, the shutter of the second Ga source.
(2) The state of the Ga-rich and As-rich surfaces was measured by the high energy electron diffraction (RHEED) method.
(3) The alternating appearance of the Ga-rich and As-rich surfaces is achieved by, but not limited to, a shutter that switches the second Ga source on and off.
(4) The beam current value of the first Ga source is controlled so that the As atom bonding ratio is smaller than the highest bonding ratio. When both Ga sources are turned on simultaneously, the total Ga beam value is such that the binding rate of As atoms is maximized while the growth surface is switched to the Ga-rich state.
(5) The parameters representing the total amount of the surplus Ga atoms and As atoms on the GaAs surface are eliminated in the process of solving the equation, and the residual required parameters are all measurable values.
(6) The calculated highest As atom binding rate already includes the difference of the response of the beam gauge for measuring the beam current value to different atoms.
The invention provides a method for measuring the highest As atom binding rate, which has the advantages that: 1) The in-situ measurement is accurate and reliable; 2) The operation is simple, and no additional measurement means is needed: the measurement of the required data can be completed by using a measuring device RHEED and a beam flow meter which are arranged on the MBE device; 3) The calculation accuracy can be improved by increasing the number of measurement cycles; 4) The calculation results already include the differences in the response of the beam gauge to different elements. The final result does not relate to the actual atomic population and is therefore related to the beam current values of Ga and As which are finally directly measured by the beam gauge.
Drawings
Fig. 1 is a graph showing the variation of the As bonding rate when the Ga beam is varied at a specific growth temperature and As beam value during MBE growth of GaAs.
FIG. 2 shows the procedure for measuring the parameters required to calculate the highest As binding rate.
Detailed Description
The invention aims to provide a method for measuring the highest As atom bonding rate in the GaAs molecular beam epitaxial growth process.
Firstly, the relevant phenomena in the GaAs molecular beam epitaxial growth process are described in a targeted way. Fig. 1 shows the binding rate of As a function of Ga beam current at a certain temperature and As beam current value. In the first part of the curve, an increase in Ga beam current decreases the amount of As atoms desorbed from the surface, resulting in an increase in the As incorporation efficiency. The binding rate of As then reaches a maximum and remains unchanged. The highest binding rate of As depends on the substrate temperature at the time of growth. The growth rate of GaAs depends on the size of the Ga beam before the combination rate of As reaches the maximum value, and the combination rate of As increases linearly with the Ga beam. As of the growth surface is in an excessive state, and the surface can observe (2X 4) surface reconstruction of the surface in an As-rich state through RHEED. When the Ga beam current is increased to enable the As combination rate to exceed the maximum critical point, the As beam current is not enough to match the Ga beam current so that Ga atoms on the growth surface are gathered, and the surface is observed to be in a Ga-rich state through RHEED and presents (4 multiplied by 2) surface reconstruction. The key of the measurement process is that the first Ga source beam is controlled to enable the As combination rate to be less than the maximum value, and the sum of the first Ga source beam and the second Ga source beam enables the As combination rate to reach and exceed the highest point.
When only the first Ga source is on, the As incorporation ratio does not reach a maximum. When both Ga sources are turned on simultaneously, the binding rate of As reaches a maximum while the growth surface is transformed into a Ga-rich state.
The measurement process needs to satisfy the following growth conditions. Because of the highest binding ratio eta of As atoms max Temperature T of substrate s In connection with, during the measurement T s Remain unchanged. Of course eta max The change rule along with the temperature of the substrate can be changed by changing T s The measurement was repeated. Actual beam current F of As in measuring process As Is also set at a fixed value so that the maximum atomic weight of As which can be incorporated into the crystal lattice at this time is η max ·F A . Two Ga beam sources are used for measurement, and the temperature of a source furnace is required to be adjusted to meet the condition mentioned in figure 1, namely F Ga1#max ·F A And F Ga1# +F Ga2#max ·F A (F is the beam value measured by the beam meter, and subscripts As, ga1#, ga2# denote As source and two Ga sources (1 # and 2 #), respectively). Note η discussed in this disclosure max The difference in the response sensitivity of the beam gauge to different atoms has been included.
At t 1 In the process, two Ga sources are simultaneously turned on, and t 2 Only the first Ga source is on in stage. When a (4 × 2) surface reconstruction of the Ga-rich state was observed for RHEED, the second Ga beam source was immediately turned off.
To further illustrate the method, the steps of the measurement calculation are described in detail below. Only the Ga1# beam source was turned on at the start of the test, when the growth table wasThe facets were in the As-rich state and showed (2X 4) surface reconstruction at RHEED. We set the total amount of As atoms remaining on the surface at this time to A. In the first step, the second Ga source, the Ga2# beam source, is turned on, when the As incorporation ratio reaches the maximum critical point. The surface-rich As atoms will be gradually consumed until depletion, followed by accumulation of Ga atoms at the growth surface. As shown in FIG. 2, a time t elapses after the Ga2# beam source is turned on 1 Thereafter, RHEED showed that the surface had a Ga-rich state (4 × 2) surface reconstruction. The total amount of Ga atoms remaining on the surface at this time is set to G. Second, when the (4 × 2) surface reconstruction just occurred, the Ga2# beam source was turned off. The surface-rich Ga atoms will be exhausted and have a gradual accumulation of As atoms, and the Ga2# beam source is turned off for a time t 2 The back surface exhibited (2 × 4) surface reconstruction (As-rich). I.e. at t 1 In the process, two Ga sources are simultaneously turned on, and t 2 Only the first Ga source is turned on during the phase and the second Ga beam source is immediately turned off when a (4 x 2) surface reconstruction of the Ga-rich state of RHEED is observed. The total excess As atomic weight of the surface at this point returns to the original value A. Third, we can conclude at t 1 +t 2 During the process that the sample surface in the whole time period is exhausted by surplus As atoms and is accumulated again, the binding rate of As is always at the maximum value eta max . At a first period of time t 1 In the process, the total amount a of excess As atoms on the surface is depleted, and excess Ga atoms in the total amount G are present. At a second period of time t 2 In the process, the total amount G of Ga atoms remaining on the surface is depleted, and then a total amount A of As atoms remaining. The above time can be obtained using a timer. So we can list the following equations for the two time periods, respectively:
(F Ga1# +F Ga2#max ·F As )·t 1 =A+G (1)
max ·F As -F Ga1# )·t 2 =A+G (2)
solving the above equation set, eliminating variables A and G to obtain eta max The expression of (a) is as follows:
in addition, the unit of the beam in the above expression may be directly solved using Beam Equivalent Pressure (BEP) substitution measured by a beam current meter (BFM). Meanwhile, the second Ga beam source can also be replaced by an Al beam source, because Al and Ga also belong to III-group elements and can also play a role in combining surface As atoms to enable the As combination rate to reach and exceed the highest critical point, and the flexibility of the measuring method is improved.

Claims (9)

1. A method for measuring the highest binding rate of As atoms in the GaAs molecular beam epitaxial growth process is characterized in that the variation of Ga atom beam current is utilized to enable surfaces rich in Ga and As to appear alternately in the GaAs growth process, the time of surface reconstruction variation is recorded, and finally the highest binding rate of As atoms in the growth process is obtained by solving the expression of the total amount of surface surplus atoms, and the method comprises the following specific steps:
(a) Opening the 2 nd Ga source in the GaAs growth process, pre-adjusting to enable the As atom bonding rate to reach the highest point, and then recording the time interval of converting the surface high-energy electron beam diffraction RHEED from As (2 multiplied by 4) to Ga (4 multiplied by 2);
(b) Immediately switching off the 2 nd Ga source when the surface has a (4X 2) surface reconstruction in a Ga-rich state, and recording the time interval for converting the surface from (4X 2) to (2X 4) surface reconstruction;
(c) And (3) listing equations of the total amount of the surface surplus atoms in the two processes according to the time obtained by measurement by utilizing the two Ga source and As source beams which are measured in advance, and finally solving to obtain the highest binding rate of As atoms.
2. A method As claimed in claim 1, characterized in that the alternating Ga-rich and/or As-rich surfaces during GaAs growth are realized by switching the shutter of the second Ga source.
3. The method of claim 1 wherein when only the first Ga source is on, the rate of As incorporation is below but not at a maximum; when both Ga sources are turned on simultaneously, the binding rate of As reaches a maximum while the growth surface is transformed into a Ga-rich state.
4. The method of claim 1, wherein the maximum binding ratio η of As atoms max Depending on the substrate temperature Ts, ts remains constant during the measurement.
5. A method As claimed in claim 2 or 4, characterized in that the highest binding rate of As atoms is
In the formula, F Ga1# Is the first Ga source beam value, F Ga2# Is the second Ga source beam value; f AS As source beam value, t 1 Time elapsed for reconstruction of the surface to appear in a Ga-rich state (4X 2) after the second Ga source is turned on, t 2 Time for (2 × 4) surface reconstruction to occur on the surface after the second Ga source is turned off, rich in As.
6. The method of claim 5, wherein at t 1 In the process, two Ga sources are simultaneously turned on, and t 2 Only the first Ga source is turned on during the phase and the second Ga source is immediately turned off when a (4 x 2) surface reconstruction of the Ga-rich state of RHEED is observed.
7. A method according to claim 5, wherein the second Ga source is replaced by an Al beam source which acts to bind surface As atoms.
8. The method of claim 6, wherein said units of beam current are directly solved by substituting the equivalent beam pressure (BEP) measured by a beam current meter (BFM).
9. The method of claim 5, wherein the calculated highest As atom incorporation rates are included in the corresponding differences of the beam gauge for measuring the beam current values for different atoms.
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US4876218A (en) * 1987-09-29 1989-10-24 Oy Nokia Ab Method of growing GaAs films on Si or GaAs substrates using ale

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