A method for detecting carrier concentration of antimonide material

By growing antimony-containing compound material layers on conductive and semi-insulating substrates respectively, and combining electrochemical capacitance-voltage and Hall effect tests, the carrier concentration of each layer is corrected using a carrier concentration correction factor. This solves the problem of accurately measuring the carrier concentration of complex multilayer structures in existing technologies, and achieves efficient and accurate carrier concentration measurement and process optimization.

CN121275854BActive Publication Date: 2026-04-28SUZHOU KUNYUAN OPTOELECTRONICS CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
SUZHOU KUNYUAN OPTOELECTRONICS CO LTD
Filing Date
2025-12-08
Publication Date
2026-04-28

AI Technical Summary

Technical Problem

Existing technologies struggle to quickly and accurately obtain carrier concentration information for each layer in complex, multilayered antimony-containing compound materials, hindering the optimization of epitaxial processes for each layer of the device and thus restricting the research and industrialization of such materials.

Method used

Antimony-containing compound material layers were grown on conductive gallium antimonide substrates and semi-insulating gallium arsenide substrates, respectively. The carrier concentration values ​​were measured by electrochemical capacitance-voltage test and Hall effect test, respectively. The carrier concentration of each layer was corrected by a carrier concentration correction factor, and a carrier concentration correction factor bridge was constructed to achieve accurate measurement of the carrier concentration of each layer.

Benefits of technology

It enables accurate measurement of carrier concentration in each layer of a multilayer epitaxial structure, breaks through the limitations of substrate type, improves testing efficiency and applicability, and provides a powerful characterization tool for the design and process optimization of complex device structures.

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Abstract

The application belongs to the technical field of semiconductor material characterization, and relates to a carrier concentration detection method for antimonide materials, which comprises the following steps: growing a first antimonide compound material layer on a conductive gallium antimonide substrate; performing electrochemical capacitance-voltage testing on the first antimonide compound material layer to obtain a first carrier concentration value; growing a second antimonide compound material layer on a semi-insulating gallium arsenide substrate; performing Hall effect testing on the second antimonide compound material layer to obtain a second carrier concentration value; obtaining a carrier concentration correction factor based on the ratio of the second carrier concentration value to the first carrier concentration value; growing an antimonide compound material layer on the side, away from the substrate, of the first antimonide compound material layer and / or the second antimonide compound material layer; performing electrochemical capacitance-voltage testing on each antimonide compound material layer to obtain a corresponding carrier concentration value; and obtaining the carrier concentration of each antimonide compound material layer based on the carrier concentration value and the carrier concentration correction factor.
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Description

Technical Field

[0001] This invention relates to the field of semiconductor material characterization technology, and in particular to a method for detecting carrier concentration in antimony materials. Background Technology

[0002] Antimony-containing group III-V compound semiconductor materials (such as GaSb, InGaSb, AlGaAsSb, etc.) have wide applications in infrared photodetectors, lasers, and high-speed electronic devices. The performance of these devices is highly dependent on the precise control of the carrier concentration and conductivity type in the material. Therefore, rapid and accurate measurement of the carrier concentration in the device is crucial for material growth process development and product quality control.

[0003] Currently, the mainstream methods for measuring carrier concentration include electrochemical capacitance-voltage (ECV) testing and Hall effect testing. ECV testing uses a probe inserted into the test layer, forming a Schottky barrier between the test layer and the conductive substrate. The carrier concentration is obtained by measuring the capacitance response of the test layer. This method has the advantage of in-depth profiling, allowing for the individual detection of carrier concentration in each layer of a multilayer epitaxial structure. However, it can only detect the local carrier concentration at the probe tip and cannot accurately characterize the carrier concentration of the epitaxial layer. Hall effect testing applies a current and a perpendicular magnetic field to the semiconductor material. Utilizing the Lorentz force experienced by carriers in the magnetic field, a measurable Hall voltage is generated in the material perpendicular to the current and magnetic field directions, thus obtaining the carrier concentration value. This method can be directly applied to materials on semi-insulating substrates. However, its results reflect the average value of the entire epitaxial structure, making it difficult to perform independent and precise quantitative analysis of each layer in a multilayer structure.

[0004] In addition, in actual R&D and production, the ECV test method can test the carrier concentration of each epitaxial layer grown on a conductive or semi-insulating substrate, but the test results can only reflect the local carrier concentration at the probe tip, which deviates from the overall carrier concentration of the epitaxial layer. Hall test can only test epitaxial layers grown on semi-insulating substrates, and cannot perform rapid and accurate in-depth analysis of the carrier concentration of each epitaxial layer. That is, Hall test results cannot be accurately mapped to a specific layer, so it is impossible to optimize the growth process of each layer of the device based on the test results.

[0005] In summary, existing methods for detecting carrier concentration in antimony compound materials are insufficient to quickly and accurately obtain carrier concentration information for each layer in antimony-containing compound materials with complex multilayer structures. Consequently, it is impossible to optimize the epitaxial processes of each layer of the device based on the test results, which restricts the research and development and industrialization of such materials. Summary of the Invention

[0006] Therefore, the technical problem to be solved by the present invention is to overcome the difficulty of obtaining carrier concentration information of each layer in antimony compound materials with complex multilayer structures in the existing antimony material carrier concentration detection methods, which makes it impossible to optimize the epitaxial process of each layer of the device based on the test results, thus restricting the research and development and industrialization process of such materials.

[0007] To solve the above-mentioned technical problems, the present invention provides a method for detecting carrier concentration in antimony compound materials, comprising:

[0008] A first antimony-containing compound material layer is grown on a conductive gallium antimonide substrate; an electrochemical capacitance-voltage test is performed on the first antimony-containing compound material layer to obtain the first carrier concentration value;

[0009] A second antimony-containing compound material layer is grown on a semi-insulating gallium arsenide substrate; Hall effect tests are performed on the second antimony-containing compound material layer to obtain the second carrier concentration value;

[0010] Based on the ratio of the second carrier concentration value to the first carrier concentration value, a carrier concentration correction factor is obtained; N layers of antimony compound material are grown on the side of the first antimony compound material layer and / or the second antimony compound material layer away from the substrate.

[0011] Electrochemical capacitance-voltage tests were performed on each layer of antimony-containing compound material to obtain the corresponding carrier concentration value. The carrier concentration of each layer of antimony-containing compound material was obtained by multiplying the corresponding carrier concentration value of each layer of antimony-containing compound material with the carrier concentration correction factor.

[0012] In this application, antimony-containing compound material layers are epitaxially grown on conductive and semi-insulating substrates, respectively. The carrier concentration values ​​of the two epitaxial layers are then measured using two different methods to construct a carrier concentration correction factor between the two measurement methods. Subsequently, antimony-containing compound material layers are directly epitaxially grown on any substrate, and the carrier concentration of each antimony-containing compound material layer is directly measured using electrochemical capacitance-voltage (ECV) testing. The carrier concentration correction factor is then used to correct the concentration, thus obtaining the accurate actual carrier concentration of each antimony-containing compound material layer. This method can be applied to calibrate the carrier concentration of each layer in multilayer epitaxial structures, enabling the electrochemical capacitance-voltage (ECV) measurement technique to be effectively applied to the carrier concentration calibration analysis of materials grown on various substrates. This provides a powerful characterization tool for the design and process optimization of complex device structures.

[0013] Preferably, the antimony-containing compound material layer that continues to grow on the side of the first antimony-containing compound material layer and / or the second antimony-containing compound material layer away from the substrate has the same crystal orientation as the first antimony-containing compound material layer and the second antimony-containing compound material layer.

[0014] In this application, when using the carrier concentration correction factor for correction, it is necessary to consider the structural consistency between the newly grown antimony-containing compound material layer and the antimony-containing compound material layer grown in the comparative experiment, so as to ensure that the corrected carrier concentration is more consistent with the actual carrier concentration.

[0015] Preferably, the test solution ratio for electrochemical capacitance-voltage testing of each layer of antimony compound material is the same as the test solution ratio for electrochemical capacitance-voltage testing of the first layer of antimony compound material.

[0016] In this application, since the carrier concentration correction factor is the conversion factor between the electrochemical capacitance-voltage test value and the Hall effect test value, when converting the new electrochemical capacitance-voltage test result back to the Hall effect test result using the carrier concentration correction factor, it is necessary to ensure the consistency of the two electrochemical capacitance-voltage test conditions, so as to improve the accuracy of the conversion result.

[0017] Preferably, the growth process of the first antimony-containing compound material layer is the same as the growth process of the second antimony-containing compound material layer;

[0018] The composition of the first antimony-containing compound material layer is the same as that of the second antimony-containing compound material layer.

[0019] In this application, to accurately obtain the carrier concentration correction factor for a specific material and test environment through a single comparative experiment, it is necessary to ensure that all conditions are the same except for the substrate type and test method, i.e., to control the variables in the comparative experiment, thereby ensuring the accuracy of the carrier concentration correction factor.

[0020] Preferably, the growth rate of the first antimony-containing compound material layer and the second antimony-containing compound material layer is 0.1 Å / s to 3 Å / s.

[0021] In this application, by controlling the growth rate, the atomic migration and deposition efficiency during the epitaxial growth of the antimony-containing compound material layer can be balanced, ensuring that the composition and doped atom distribution of the first and second antimony-containing compound material layers are as consistent as possible, and avoiding intrinsic differences in carrier concentration due to compositional differences.

[0022] Preferably, both the first antimony-containing compound material layer and the second antimony-containing compound material layer are doped or intrinsic materials.

[0023] Preferably, the first antimony-containing compound material layer and the second antimony-containing compound material layer are doped materials, and the dopant is tellurium or beryllium.

[0024] Preferably, the conductive gallium antimonide substrate is an N-type tellurium-doped gallium antimonide substrate or a P-type undoped gallium antimonide substrate.

[0025] Preferably, the formula for calculating the carrier concentration correction factor is:

[0026] ,

[0027] in, This represents the carrier concentration correction factor; This indicates the second carrier concentration value; This represents the first carrier concentration value.

[0028] Preferably, the formula for calculating the carrier concentration of each antimony compound material layer is as follows:

[0029] ,

[0030] in, This indicates the carrier concentration of the antimony compound material layer; This represents the carrier concentration correction factor; This represents the carrier concentration value corresponding to the antimony-containing compound material layer.

[0031] The carrier concentration detection method for antimony compound materials provided in this application involves growing a first antimony-containing compound material layer on a conductive gallium antimony substrate; performing an electrochemical capacitance-voltage test on the first antimony-containing compound material layer to obtain a first carrier concentration value; growing a second antimony-containing compound material layer on a semi-insulating gallium arsenide substrate; performing a Hall effect test on the second antimony-containing compound material layer to obtain a second carrier concentration value; obtaining a carrier concentration correction factor based on the ratio of the second carrier concentration value to the first carrier concentration value; continuing to grow antimony-containing compound material layers on the side away from the substrate from the first and / or second antimony-containing compound material layers; performing an electrochemical capacitance-voltage test on each antimony-containing compound material layer to obtain a corresponding carrier concentration value; and obtaining the carrier concentration of each antimony-containing compound material layer based on the product of the corresponding carrier concentration value and the carrier concentration correction factor. This application provides a technical solution that combines the depth resolution capability of ECV with a testing method that does not require substrate conductivity, by epitaxially growing antimony-containing compound material layers on conductive and semi-insulating substrates respectively. The carrier concentration values ​​of the two epitaxial layers were then measured using two different methods to construct a carrier concentration correction factor between the two measurement methods. Since the Hall effect test results reflect the true carrier concentration of the entire antimony compound material layer when there is only one layer of antimony compound material on the substrate, while the electrochemical capacitance-voltage test results reflect the local carrier concentration, the carrier concentration correction factor can reflect the deviation between the local carrier concentration represented by the electrochemical capacitance-voltage test results and the true carrier concentration. Subsequently, antimony compound material layers were epitaxially grown on any substrate, and the carrier concentration of each antimony compound material layer was directly measured using electrochemical capacitance-voltage test. The carrier concentration correction factor was then used to correct the concentration, thus obtaining the accurate actual carrier concentration of each antimony compound material layer. This method can be applied to calibrate the carrier concentration of each layer in a multilayer epitaxial structure, enabling the electrochemical capacitance-voltage measurement technology to be effectively applied to the carrier concentration calibration analysis of materials grown on various semiconductor substrates, providing a powerful characterization tool for the design and process optimization of complex device structures. Attached Figure Description

[0032] To make the content of this invention easier to understand, the invention will be further described in detail below with reference to specific embodiments and accompanying drawings, wherein:

[0033] Figure 1 This is a flowchart of the carrier concentration detection method for antimony compound materials provided in this application;

[0034] Figure 2 This is a schematic diagram of the electrochemical capacitance-voltage test principle provided in this application;

[0035] Figure 3 A schematic diagram illustrating the testing principle for the carrier concentration values ​​of each antimony-containing compound material layer in the multilayer antimony-containing compound material layer provided in this application; wherein, Figure 3 (a) in the diagram is a schematic diagram of the carrier concentration test principle corresponding to the second layer of antimony-containing compound material. Figure 3 (b) in the diagram is a schematic diagram of the carrier concentration test principle corresponding to the third layer of antimony-containing compound material.

[0036] Explanation of reference numerals in the accompanying drawings: 1. Conductive gallium antimonide substrate; 11. First antimony-containing compound material layer; 2. Semi-insulating gallium arsenide substrate; 21. Second antimony-containing compound material layer; 22. Second antimony-containing compound material layer; 23. Third antimony-containing compound material layer; U. Probe. Detailed Implementation

[0037] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, so that those skilled in the art can better understand and implement the present invention. However, the embodiments described are not intended to limit the present invention.

[0038] Existing technologies provide two methods for detecting the carrier concentration of devices: electrochemical capacitance-voltage testing and Hall effect testing. Electrochemical capacitance-voltage testing uses a probe to penetrate the test layer, thereby applying a variable voltage to form a depletion layer and measuring the capacitance response of the test layer to infer the doping concentration distribution. However, the results obtained by this method only represent the local carrier concentration at the probe tip. Due to the influence of actual R&D and manufacturing processes, the local carrier concentration at different locations on the epitaxial layer may vary. Therefore, the test results of this method cannot accurately reflect the overall carrier concentration of the epitaxial layer. Hall effect testing, on the other hand, applies a current and a perpendicular magnetic field to the semiconductor material. Utilizing the Lorentz force experienced by carriers in the magnetic field, a measurable Hall voltage is generated in the material perpendicular to the current and magnetic field direction, thus obtaining the carrier concentration value of the material. This method can only detect epitaxial layers grown on semi-insulating substrates, and the measurement obtained is the average value of the entire epitaxial structure (multiple epitaxial layers). When the number of antimony-containing compound material layers on the substrate increases, it is impossible to measure the carrier concentration value of each epitaxial layer. Since it is impossible to accurately reflect the carrier concentration of each epitaxial layer, this poses certain limitations to device fabrication and performance optimization. This application is the first to discover this dilemma and propose a solution. By establishing a carrier concentration correction factor, it achieves rapid and accurate calibration of the carrier concentration of antimony-containing compound multilayer materials grown under arbitrary doping conditions, especially in vacuum epitaxial equipment. This overcomes the dependence of existing carrier concentration detection technologies on the substrate conductivity type and significantly improves testing efficiency and applicability.

[0039] Please see Figure 1 , Figure 1 The diagram shows a flowchart of the carrier concentration detection method for antimony compound materials provided in this application. The method specifically includes:

[0040] S10: Grow a first antimony-containing compound material layer on a conductive gallium antimonide substrate; perform an electrochemical capacitance-voltage test on the first antimony-containing compound material layer to obtain the first carrier concentration value.

[0041] Specifically, the conductive gallium antimonide substrate is either an N-type tellurium-doped gallium antimonide substrate or a P-type undoped gallium antimonide substrate.

[0042] S20: A second antimony-containing compound material layer is grown on a semi-insulating gallium arsenide substrate; Hall effect test is performed on the second antimony-containing compound material layer to obtain the second carrier concentration value.

[0043] S30: Based on the ratio of the second carrier concentration value to the first carrier concentration value, a carrier concentration correction factor is obtained; N layers of antimony compound material are grown on the side of the first and / or second antimony compound material layers away from the substrate. Wherein, N≥1.

[0044] S40: Perform electrochemical capacitance-voltage tests on each layer of antimony-containing compound material to obtain the corresponding carrier concentration value; based on the product of the carrier concentration value corresponding to each layer of antimony-containing compound material and the carrier concentration correction factor, obtain the carrier concentration of each layer of antimony-containing compound material.

[0045] Specifically, electrochemical capacitance-voltage testing uses a probe inserted into the test layer to apply a variable voltage to form a depletion layer, while simultaneously measuring the capacitance response of the test layer to infer its doping concentration distribution. Figure 2 As shown in the figure, a conductive gallium antimonide substrate 1 is used. By inserting a probe U into the first antimony-containing compound material layer 11, a Schottky barrier is formed between the first antimony-containing compound material layer 11 and the conductive gallium antimonide substrate 1, thereby detecting the carrier concentration value at the probe tip in the first antimony-containing compound material layer 11. The Hall effect test, on the other hand, applies a current and a perpendicular magnetic field to the semiconductor material. Utilizing the Lorentz force experienced by the carriers in the magnetic field, a measurable Hall voltage is generated in the material perpendicular to the current and magnetic field direction, thus obtaining the carrier concentration value of the material. When the number of antimony-containing compound material layers on the substrate increases, the measurement result reflects the average carrier concentration of all layers.

[0046] This application ingeniously combines electrochemical capacitance-voltage testing and Hall effect testing. By epitaxially growing antimony-containing compound material layers on conductive and semi-insulating substrates respectively, and then measuring the carrier concentration values ​​of the two epitaxial layers using two different methods, a carrier concentration correction factor is constructed between the two measurement methods. Since the Hall effect test reflects the true carrier concentration of the entire antimony-containing compound material layer when there is only one layer on the substrate, while the electrochemical capacitance-voltage test reflects the local carrier concentration, the carrier concentration correction factor can reflect the local concentration represented by the electrochemical capacitance-voltage test result. The deviation between the carrier concentration and the actual carrier concentration is determined by directly epitaxially growing antimony-containing compound material layers on any substrate. Simultaneously, the carrier concentration of each antimony-containing compound material layer is directly measured using electrochemical capacitance-voltage (ECV) testing. Then, a carrier concentration correction factor is used to correct the deviation, thus obtaining the accurate actual carrier concentration of each antimony-containing compound material layer. This method can be applied to calibrate the carrier concentration of each layer in multilayer epitaxial structures, enabling the electrochemical capacitance-voltage measurement technique to be effectively applied to the carrier concentration calibration analysis of materials grown on various semiconductor substrates. This provides a powerful characterization tool for the design and process optimization of complex device structures.

[0047] Specifically, the formula for calculating the carrier concentration correction factor is as follows:

[0048] ,

[0049] in, This represents the carrier concentration correction factor; This indicates the second carrier concentration value; This represents the first carrier concentration value.

[0050] The formula for calculating the carrier concentration of each layer of antimony compound material is as follows:

[0051] ,

[0052] in, This indicates the carrier concentration of the antimony compound material layer; This represents the carrier concentration correction factor; This represents the carrier concentration value corresponding to the antimony-containing compound material layer.

[0053] Furthermore, in order to accurately obtain the carrier concentration correction factor for a specific material and test environment through a comparative experiment, it is necessary to ensure that all conditions are the same except for the substrate type and test method, that is, to control the variables in the comparative experiment, thereby ensuring the accuracy of the carrier concentration correction factor.

[0054] Specifically, the growth process of the first antimony-containing compound material layer is the same as that of the second antimony-containing compound material layer; the composition of the first antimony-containing compound material layer is the same as that of the second antimony-containing compound material layer.

[0055] For example: the growth rate of the first antimony-containing compound material layer is equal to the growth rate of the second antimony-containing compound material layer; the growth temperature of the first antimony-containing compound material layer is equal to the growth temperature of the second antimony-containing compound material layer; the composition of the first antimony-containing compound material layer and the second antimony-containing compound material layer is the same.

[0056] Furthermore, the growth rate of the first antimony-containing compound material layer and the second antimony-containing compound material layer is 0.1 Å / s to 3 Å / s, for example, the growth rate can be 0.5 Å / s, 1 Å / s, 1.5 Å / s, 2 Å / s, 2.5 Å / s, or 3 Å / s.

[0057] By controlling the growth rate, the high atomic migration and deposition efficiency during the epitaxial growth of the antimony-containing compound material layer can be balanced, ensuring that the composition and doped atom distribution of the first and second antimony-containing compound material layers are as consistent as possible, and avoiding intrinsic differences in carrier concentration due to compositional differences.

[0058] Furthermore, both the first antimony-containing compound material layer and the second antimony-containing compound material layer are doped or intrinsic materials.

[0059] Furthermore, the first antimony-containing compound material layer and the second antimony-containing compound material layer are doped materials, and the dopant is tellurium or beryllium.

[0060] Furthermore, in addition to ensuring that the growth process and growth conditions of the first and second antimony-containing compound material layers are consistent when obtaining the carrier concentration correction factor, the structural consistency between the newly grown antimony-containing compound material layer and the antimony-containing compound material layer grown in the comparative experiment also needs to be considered when using the carrier concentration correction factor for correction. It is worth noting that, through research and analysis, this application found that the correction factor is determined only by the properties of the material itself (such as crystal orientation) and the test environment (such as the calibration status of the test instrument, the freshness of the electrolyte, and the contamination status), and is unrelated to the growth process parameters (such as dopant vapor pressure, growth temperature, and growth rate). Therefore, it is only necessary to control the crystal orientation of the antimony-containing compound material layer and the solution ratio during the test, without needing to ensure that the growth conditions of the newly grown antimony-containing compound material layer are consistent with those of the first antimony-containing compound material layer.

[0061] Specifically, the antimony-containing compound material layer that continues to grow on the side of the first antimony-containing compound material layer and / or the second antimony-containing compound material layer away from the semi-insulating gallium arsenide substrate has the same crystal orientation as the first antimony-containing compound material layer and the second antimony-containing compound material layer.

[0062] Specifically, the test solution ratio for each layer of antimony compound material is the same as that for the first layer of antimony compound material.

[0063] like Figure 3 The diagram shown illustrates the testing principle of the carrier concentration values ​​for each antimony-containing compound material layer in the multilayer antimony-containing compound material layer provided in this application; wherein, Figure 3 (a) in the diagram is a schematic diagram of the carrier concentration test principle corresponding to the second layer of antimony-containing compound material. Figure 3 (b) in the diagram is a schematic diagram of the carrier concentration test principle corresponding to the third layer of antimony compound material.

[0064] from Figure 3 As can be seen, after calculating the carrier concentration correction factor, a second antimony-containing compound material layer 22 and a third antimony-containing compound material layer 23 are further epitaxially grown on a conductive gallium antimonybide substrate 1 or a semi-insulating gallium arsenide substrate 2. Electrochemical capacitance-voltage tests are then performed on the second antimony-containing compound material layer 22 and the third antimony-containing compound material layer 23 to obtain their carrier concentration values.

[0065] Because the correction factor is universal, the electrochemical capacitance-voltage test results of the same material system grown on the same substrate under any other doping conditions can be converted using this correction factor. That is, for the carrier concentration value corresponding to each layer of antimony compound material, the calibrated and accurate carrier concentration can be obtained by calculating its product with the carrier concentration correction factor.

[0066] The above-mentioned method for detecting carrier concentration in antimony compounds is further explained and illustrated below through two specific examples:

[0067] Embodiment 1 of this application provides a method for detecting carrier concentration in antimony compound materials, which specifically includes:

[0068] Step 1 - Growth and testing on a conductive substrate: Using molecular beam epitaxy (MBE) technology, a Te-doped GaSb epitaxial layer with a thickness of 1 μm was grown on an N-type Te-doped GaSb substrate at a growth rate of 1 Å / s and a surface temperature of 520 °C.

[0069] Using a 0.1 mol / L NaOH solution as the electrolyte, the epitaxial layer was tested by ECV, and the carrier concentration N_ECV was measured to be [value missing]. .

[0070] Step 2 - Growth and testing on a semi-insulating substrate: Keeping all growth parameters exactly the same as in Step 1 (growth rate 1 Å / s, Te source temperature, substrate surface temperature 520 °C), grow a Te-doped GaSb epitaxial layer of the same thickness (1 μm) on a semi-insulating GaAs substrate.

[0071] The sample was subjected to a Van der Pauw method Hall effect test, and the carrier concentration N_Hall was measured to be [value missing]. .

[0072] Step 3 - Calculate the correction factor: Calculate the correction factor according to the formula. .

[0073] Step 4 - Application Calibration: In subsequent processes, multiple GaSb monolayer and multilayer samples are grown on arbitrary substrates under different Te source vapor pressures. ECV tests are performed directly on these samples to obtain a series of apparent carrier concentration values ​​(N_ECV_measured).

[0074] Using the correction factor K=0.8 determined in step 3, the actual carrier concentration after calibration, which is comparable to the accuracy of Hall's test, can be obtained by calculating using the formula N_calibrated=0.8×N_ECV_measured.

[0075] Embodiment 2 of this application provides a method for detecting carrier concentration in antimony compound materials, which specifically includes:

[0076] Step 1 - Growth and testing on a conductive substrate: Using molecular beam epitaxy (MBE) technology, a Te-doped GaSb epitaxial layer with a thickness of 1 μm was grown on an N-type Te-doped GaSb substrate at a growth rate of 1 Å / s and a surface temperature of 520 °C.

[0077] Using a 0.1 mol / L NaOH solution as the electrolyte, the epitaxial layer was tested by ECV, and the carrier concentration N_ECV was measured to be [value missing]. .

[0078] Step 2 - Growth and testing on a semi-insulating substrate: Keeping all growth parameters exactly the same as in Step 1 (growth rate 1 Å / s, Te source temperature, substrate surface temperature 520 °C), grow a Te-doped GaSb epitaxial layer of the same thickness (1 μm) on a semi-insulating GaAs substrate.

[0079] The sample was subjected to a Van der Pauw method Hall effect test, and the carrier concentration N_Hall was measured to be [value missing]. .

[0080] Step 3 - Calculate the correction factor: Calculate the correction factor according to the formula. .

[0081] Step 4 - Application Calibration: In subsequent processes, multiple GaSb monolayer and multilayer samples are grown on arbitrary substrates under different Te source vapor pressures. ECV tests are performed directly on these samples to obtain a series of apparent carrier concentration values ​​(N_ECV_measured).

[0082] Using the correction factor K=1.67 determined in step 3, the actual carrier concentration after calibration, which is comparable to the accuracy of the Hall test, can be calculated using the formula N_calibrated=1.67×N_ECV_measured. For example, if the apparent carrier concentration obtained from the ECV test is... The corrected actual carrier concentration is .

[0083] The carrier concentration detection method for antimony compounds provided in this application has the following advantages: 1. It overcomes substrate limitations by cleverly combining ECV testing with Hall testing, establishing a bridge through a correction factor, enabling ECV technology to be effectively applied to the carrier concentration calibration analysis of materials grown on various substrates; 2. It offers high calibration accuracy and strong versatility. The obtained correction factor K is only related to the intrinsic properties of the material and the testing environment, and is independent of variable production process parameters, ensuring the accuracy and repeatability of the calibration results, and is applicable to different process batches under the same material system; 3. It is efficient and convenient. Once the K factor for a specific material and testing environment is determined through a comparative experiment, subsequent routine ECV testing can quickly calculate the accurate actual carrier concentration, eliminating the need for multiple preparations of single-layer materials and complex Hall test sample preparation and measurement, greatly improving testing efficiency, and is particularly suitable for production process monitoring and large-scale production; 4. It is applicable to complex structures. This method can be applied to calibrate the carrier concentration of each layer in a multilayer epitaxial structure, providing a powerful characterization tool for the design and process optimization of complex device structures.

[0084] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for detecting carrier concentration in antimony compound materials, characterized in that, include: A first antimony-containing compound material layer is grown on a conductive gallium antimonide substrate; Electrochemical capacitance-voltage test was performed on the first antimony-containing compound material layer to obtain the first carrier concentration value; A second antimony-containing compound material layer is grown on a semi-insulating gallium arsenide substrate; Hall effect tests were performed on the second antimony-containing compound material layer to obtain the second carrier concentration value; wherein, the growth process of the first antimony-containing compound material layer is the same as that of the second antimony-containing compound material layer; the composition of the first antimony-containing compound material layer is the same as that of the second antimony-containing compound material layer; Based on the ratio of the second carrier concentration value to the first carrier concentration value, a carrier concentration correction factor is obtained; N layers of antimony compound material are further grown on the side of the first and / or second antimony compound material layers away from the substrate; wherein, the N layers of antimony compound material layers further grown on the side of the first and / or second antimony compound material layers away from the substrate have the same crystal orientation as the first and second antimony compound material layers; Electrochemical capacitance-voltage tests were performed on each layer of antimony-containing compound material to obtain the corresponding carrier concentration value. The carrier concentration of each layer of antimony-containing compound material was obtained by multiplying the corresponding carrier concentration value of each layer of antimony-containing compound material with the carrier concentration correction factor. The test solution ratio for electrochemical capacitance-voltage tests on each layer of antimony-containing compound material was the same as that for the first layer of antimony-containing compound material.

2. The method for detecting carrier concentration in antimony compound materials according to claim 1, characterized in that, The growth rates of the first and second antimony-containing compound material layers are 0.1 Å / s to 3 Å / s.

3. The method for detecting carrier concentration in antimony compound materials according to claim 1, characterized in that, Both the first and second antimony-containing compound material layers are doped or intrinsic materials.

4. The method for detecting carrier concentration in antimony compound materials according to claim 1, characterized in that, The first and second antimony-containing compound material layers are doped materials, with tellurium or beryllium as the dopant.

5. The method for detecting carrier concentration in antimony compound materials according to claim 1, characterized in that, The conductive gallium antimonide substrate is either an N-type tellurium-doped gallium antimonide substrate or a P-type undoped gallium antimonide substrate.

6. The method for detecting carrier concentration in antimony compound materials according to claim 1, characterized in that, The formula for calculating the carrier concentration correction factor is: , in, This represents the carrier concentration correction factor; This indicates the second carrier concentration value; This represents the first carrier concentration value.

7. The method for detecting carrier concentration in antimony compound materials according to claim 1, characterized in that, The formula for calculating the carrier concentration of each layer of antimony compound material is as follows: , in, This indicates the carrier concentration of the antimony compound material layer; This represents the carrier concentration correction factor; This represents the carrier concentration value corresponding to the antimony-containing compound material layer.

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