A method for measuring oxygen leakage during RTO of silicon-based materials and its application

By setting the temperature, pressure and inert atmosphere in the heat treatment device, combined with non-contact optical measurement and data processing, the measurement accuracy and speed of oxygen leakage during the RTO process are solved, and accurate measurement and sealing detection in high-temperature environments are achieved.

CN119381279BActive Publication Date: 2025-08-19ADVANCED MATERIALS TECH & ENG INC +1
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Patent Information

Application Number
CN202411513026.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-28
Publication Date
2025-08-19
Estimated Expiration
2044-10-28

AI Technical Summary

Technical Problem

Prior Art In the semiconductor manufacturing process, the measurement method of oxygen leakage during RTO process has problems such as insufficient accuracy, slow speed and inability to accurately measure in high temperature environments.

Method used

The silicon-based material is placed in a heat treatment device, the temperature is set to 800-900°C, the constant temperature time is 5-10 minutes, the cavity space pressure is 50-150kPa, and an inert atmosphere such as nitrogen, argon, helium, etc. is used to measure the thickness and uniformity of the oxide layer through a non-contact optical measurement device, and the parameters are adjusted in combination with the data processing system until no oxide layer appears.

Benefits of technology

It realizes accurate measurement of the oxygen leakage degree and uniformity of silicon-based materials under high temperature environments, improves measurement accuracy and efficiency, and can detect the sealing of the device cavity during RTO.

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Abstract

The present invention provides a method for measuring the degree of oxygen leakage during the RTO process of silicon-based materials and its application, which belongs to the field of semiconductor technology. The measurement method includes the following steps: placing the silicon-based material in a heat treatment device, then setting the temperature, constant temperature time and pressure of the inner cavity space of the heat treatment device, and making the atmosphere in the cavity space of the heat treatment device an inert atmosphere; measuring the thickness and uniformity of the oxide layer in the silicon-based material after heat treatment to determine the degree of oxygen leakage during the RTO process. The measurement method provided by the present invention is not only simple in process, can accurately measure the degree of oxygen leakage of silicon-based materials during the RTO process, and has high efficiency, but also can accurately measure the degree of oxygen leakage and uniformity of silicon-based materials in a high-temperature environment, and can realize the sealing detection of the cavity space in the device during the RTO process.
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Description

Technical Field

[0001] The present invention belongs to the field of semiconductor technology, and in particular relates to a method for measuring oxygen leakage during the RTO process of silicon-based materials and its application. Background Art

[0002] Rapid Thermal Oxidation (RTO) of silicon carbide and silicon-based materials is a critical step in semiconductor manufacturing, making the sealing of the heat treatment equipment used in this step crucial. However, traditional methods for measuring oxygen content (oxygen leakage) have several drawbacks, including insufficient measurement accuracy, slow measurement speed, and the inability to accurately measure in high-temperature environments.

[0003] Therefore, there is an urgent need to design a measurement method to improve the measurement accuracy and efficiency of oxygen leakage during the RTO process and achieve accurate measurement under high temperature conditions. Summary of the Invention

[0004] In response to the shortcomings of the prior art, the present invention aims to provide a method for measuring oxygen leakage during the RTO process of silicon-based materials and its application. The measurement method provided by the present invention is not only simple in process and can accurately measure the oxygen leakage level of silicon-based materials during the RTO process with high efficiency, but also can accurately measure the oxygen leakage level and uniformity of silicon-based materials in high-temperature environments, enabling the sealing of the cavity space within the device during the RTO process to be detected.

[0005] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0006] In a first aspect, the present invention provides a method for measuring oxygen leakage during the RTO process of a silicon-based material, the method comprising the following steps:

[0007] The silicon-based material is placed in a heat treatment device, and then the temperature, constant temperature time and pressure of the inner cavity space of the heat treatment device are set, and the atmosphere in the cavity space of the heat treatment device is made to be an inert atmosphere.

[0008] Measure the thickness and uniformity of the oxide layer in heat-treated silicon-based materials to determine the degree of oxygen leakage during the RTO process.

[0009] The measurement method provided by the present invention is not only simple in process and can accurately measure the degree of oxygen leakage of silicon-based materials during the RTO process with high efficiency, but also can accurately measure the degree and uniformity of oxygen leakage of silicon-based materials in a high-temperature environment, and can realize the sealing detection of the cavity space inside the device during the RTO process.

[0010] It should be noted that RTO stands for Rapid Thermal Oxidation. This process has some drawbacks, such as insufficient measurement accuracy, slow measurement speed, and inability to accurately measure in high-temperature environments.

[0011] As a preferred technical solution of the present invention, the silicon-based material includes any one of silicon carbide, porous silicon or microcrystalline silicon, or a combination of at least two of them.

[0012] As a preferred technical solution of the present invention, the temperature range of the heat treatment device is 800-900°C, for example, it can be 800°C, 850°C or 900°C.

[0013] The present invention performs an RTO process on a heat treatment device at a temperature of 800-900°C to determine the degree of oxygen leakage during the RTO process, which can fully realize thermal oxidation treatment of silicon-based materials. It is difficult to accurately determine the degree of oxygen leakage during the RTO process when the temperature is too low or too high.

[0014] As a preferred technical solution of the present invention, the constant temperature time of the heat treatment device is 5 to 10 minutes, for example, it can be 5 minutes, 7 minutes or 10 minutes.

[0015] As a preferred technical solution of the present invention, the pressure of the inner cavity space of the heat treatment device is 50-150 kPa, for example, it can be 50 kPa, 100 kPa or 150 kPa.

[0016] In the present invention, the pressure of the inner cavity space of the heat treatment device is limited to 50-150 kPa, which helps to more accurately determine the degree of oxygen leakage during the RTO process.

[0017] As a preferred technical solution of the present invention, the gas in the inert atmosphere includes an inert gas, and the inert gas includes any one of nitrogen, argon, helium, xenon, neon or krypton, or a combination of at least two of them.

[0018] In the present invention, the aforementioned inert gas is used instead of oxygen during the RTO process, which is a crucial condition for measuring the extent of oxygen leakage during the RTO process of silicon-based materials. This substitution indicates that if oxygen leakage occurs in the heat treatment apparatus during the RTO process, an oxide layer will inevitably form on the surface of the silicon-based material due to the infiltration of external oxygen.

[0019] Preferably, the concentration of the inert gas is greater than 99%, for example, it may be 99.2%, 99.4%, 99.6% or 99.9%.

[0020] As a preferred technical solution of the present invention, the equipment for measuring the thickness and uniformity of the oxide layer in the silicon-based material includes an optical measuring device, preferably a non-contact optical measuring device.

[0021] Preferably, the thickness measurement accuracy of the non-contact optical measuring device is -0.1 to 0.1 μm, for example, -0.1 μm, -0.05 μm, 0 μm, 0.05 μm or 0.1 μm.

[0022] The non-contact optical measuring device provided by the present invention has high precision and fast measuring speed and can perform accurate measurement in a high temperature environment.

[0023] As a preferred technical solution of the present invention, after determining the degree of oxygen leakage during the RTO process, steps of data processing and RTO parameter optimization are further performed.

[0024] As a preferred technical solution of the present invention, the measurement method includes the following steps:

[0025] (1) The silicon-based material is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 800-900° C., the constant temperature time is 5-10 minutes, the pressure of the inner cavity space is 50-150 kPa, and the atmosphere in the cavity space of the heat treatment device is a nitrogen atmosphere.

[0026] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0027] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0028] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0029] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0030] In a second aspect, the present invention provides an application of the measurement method described in the first aspect in the field of semiconductor manufacturing.

[0031] The numerical range described in the present invention includes not only the point values listed above, but also any point values between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values included in the range.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] The measurement method provided by the present invention is not only simple in process and can accurately measure the degree of oxygen leakage of silicon-based materials during the RTO process with high efficiency, but also can accurately measure the degree and uniformity of oxygen leakage of silicon-based materials in a high-temperature environment, and can realize the sealing detection of the cavity space inside the device during the RTO process. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is a flow chart for measuring the oxygen leakage level during the RTO process of silicon-based materials provided in Example 1 of the present invention. DETAILED DESCRIPTION

[0035] The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the embodiments are merely to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0036] Example 1

[0037] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials. The flow chart is as follows: Figure 1 As shown, the measurement method includes the following steps:

[0038] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 850° C., the constant temperature time is 7 minutes, the pressure of the inner cavity space is 100 kPa, and the atmosphere in the cavity space of the heat treatment device is a nitrogen atmosphere, and the concentration of the nitrogen is 99.9%.

[0039] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0040] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0041] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0042] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0043] Example 2

[0044] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0045] (1) Porous silicon is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 820°C, the constant temperature time is 8 minutes, the pressure of the inner cavity space is 80 kPa, and the atmosphere in the cavity space of the heat treatment device is an argon atmosphere with a concentration of 99.9%.

[0046] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0047] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0048] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0049] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0050] Example 3

[0051] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0052] (1) Microcrystalline silicon is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 870°C, the constant temperature time is 6 minutes, the pressure of the inner cavity space is 120 kPa, and the atmosphere in the cavity space of the heat treatment device is a helium atmosphere, and the concentration of the helium is 99.9%.

[0053] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0054] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0055] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0056] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0057] Example 4

[0058] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0059] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 800° C., the constant temperature time is 10 minutes, the pressure of the inner cavity space is 50 kPa, and the atmosphere in the cavity space of the heat treatment device is a nitrogen atmosphere with a nitrogen concentration of 99.9%.

[0060] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0061] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0062] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0063] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0064] Example 5

[0065] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0066] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 900° C., the constant temperature time is 5 minutes, the pressure of the inner cavity space is 150 kPa, and the atmosphere in the cavity space of the heat treatment device is a nitrogen atmosphere with a nitrogen concentration of 99.9%.

[0067] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0068] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0069] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0070] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0071] Example 6

[0072] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0073] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 600° C., the constant temperature time is 7 minutes, the pressure of the inner cavity space is 100 kPa, and the atmosphere in the cavity space of the heat treatment device is set to a nitrogen atmosphere.

[0074] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0075] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0076] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0077] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0078] Example 7

[0079] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0080] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 1000° C., the constant temperature time is 7 minutes, the pressure of the inner cavity space is 100 kPa, and the atmosphere in the cavity space of the heat treatment device is set to a nitrogen atmosphere.

[0081] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0082] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0083] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0084] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0085] Example 8

[0086] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0087] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 700°C, the constant temperature time is 3 minutes, the pressure of the inner cavity space is 100 kPa, and the atmosphere in the cavity space of the heat treatment device is set to a nitrogen atmosphere.

[0088] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0089] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0090] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0091] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0092] Example 9

[0093] This embodiment provides a method for measuring oxygen leakage during the RTO process of silicon-based materials, the method comprising the following steps:

[0094] (1) Silicon carbide is placed in a heat treatment device, and then the temperature of the heat treatment device is set to 700°C, the constant temperature time is 15 minutes, the pressure of the inner cavity space is 100 kPa, and the atmosphere in the cavity space of the heat treatment device is set to a nitrogen atmosphere.

[0095] (2) Starting a heat treatment device to perform heat treatment on the silicon-based material.

[0096] (3) Using a non-contact optical measuring device to measure the silicon-based material after heat treatment to measure whether there is an oxide layer on the surface of the silicon-based material and the uniformity of the oxide layer, which is used to determine the degree of oxygen leakage during the RTO process.

[0097] (4) Analyzing the data measured in step (3) using a data processing system to obtain a distribution diagram of the thickness and uniformity of the oxide layer, and then adjusting the setting parameters in the RTO process according to the distribution diagram, wherein the setting parameters include the temperature, constant temperature time and pressure of the heat treatment.

[0098] (5) Repeat steps (2) to (4) until no oxide layer is detected on the surface of the silicon-based material.

[0099] Comparative Example 1

[0100] The difference between this comparative example and Example 1 is that the atmosphere in the cavity space of the heat treatment device is a carbon dioxide atmosphere.

[0101] The rest of the preparation methods and parameters remained the same as in Example 1.

[0102] In summary, the measurement method provided by the present invention can accurately measure the oxygen leakage degree of silicon-based materials during the RTO process with high efficiency, and can accurately measure the oxygen leakage degree and uniformity of silicon-based materials in a high-temperature environment, and can realize the sealing detection of the cavity space inside the device during the RTO process.

[0103] It can be seen from Example 1 and Examples 6-7 that when setting the parameters of the heat treatment device, a temperature that is too low or too high will lead to insufficient measurement accuracy, slow measurement speed, and inability to obtain accurate measurement results.

[0104] It can be seen from Example 1 and Examples 8-9 that when setting the parameters of the heat treatment device, a constant temperature time that is too short or too long will lead to insufficient measurement accuracy and an inability to obtain accurate measurement results.

[0105] It can be seen from Example 1 and Comparative Example 1 that if the atmosphere in the chamber space of the heat treatment device is a carbon dioxide atmosphere, it is difficult to obtain accurate measurement results.

[0106] The applicant states that while the above-described embodiments illustrate the process of the present invention, the present invention is not limited to the above-described process steps, nor does it imply that the present invention must rely on the above-described process steps for implementation. Those skilled in the art will appreciate that any improvements to the present invention, equivalent substitutions for the raw materials used, additions of auxiliary components, and selection of specific methods, etc., fall within the scope of protection and disclosure of the present invention.

Claims

1. A method for measuring oxygen leakage during the RTO process of silicon-based materials, characterized in that: The measuring method comprises the following steps: Placing the silicon-based material in a heat treatment device, then setting the temperature, constant temperature time, and pressure of the inner cavity of the heat treatment device, and making the atmosphere in the cavity of the heat treatment device an inert atmosphere; the temperature range of the heat treatment device is 800-900° C.; the constant temperature time of the heat treatment device is 5-10 minutes; and the relative pressure of the inner cavity of the heat treatment device is 50-150 kPa; Starting a heat treatment device to perform heat treatment on the silicon-based material; Measuring the thickness and uniformity of the oxide layer in the heat-treated silicon-based material to determine the degree of oxygen leakage during the RTO process; the equipment for measuring the thickness and uniformity of the oxide layer in the silicon-based material is a non-contact optical measurement device; After determining the degree of oxygen leakage during the RTO process, steps of data processing and RTO parameter optimization are further performed.

2. The measurement method according to claim 1, wherein: The silicon-based material includes any one of silicon carbide, porous silicon or microcrystalline silicon, or a combination of at least two of them.

3. The measurement method according to claim 1, wherein: The gas in the inert atmosphere includes an inert gas, and the inert gas includes any one or a combination of at least two of nitrogen, argon, helium, xenon, neon or krypton; The concentration of the inert gas is greater than 99%.

4. The measurement method according to claim 1, wherein: The thickness measurement accuracy of the non-contact optical measuring device is -0.1~0.1μm.

5. Application of the measurement method according to any one of claims 1 to 4 in the field of semiconductor manufacturing.

Citation Information

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