Special electrolyte compound for electrochemical property analysis of various semiconductor materials and application method thereof
By using a multi-system synergistic dedicated electrolyte compound and closed-loop system, the problems of etching thin films, rate and resolution matching, and safety in the electrochemical characteristic analysis of semiconductor materials have been solved, enabling accurate testing of materials such as GaAs, GaN, and SiC, and improving the reliability and efficiency of the test.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-14
- Publication Date
- 2026-04-03
AI Technical Summary
Existing methods for analyzing the electrochemical properties of semiconductor materials suffer from several problems, including the easy formation of thin films during etching, difficulty in matching etching rate and resolution, insufficient safety and equipment compatibility, and overly generalizable formulations. These issues lead to inaccurate test results and equipment damage.
It provides specialized electrolyte compounds with multi-system synergistic combinations, including basic, weakly basic, Tiron-based, and ammonium-based electrolytes. By constructing a three-dimensional mapping database and a closed-loop system, it can accurately match the electrochemical characteristics of different semiconductor materials and optimize etching stability, resolution, and safety.
It achieves precise compatibility with semiconductor materials such as GaAs, GaN, and SiC, solves the problem of synergistic effect between etching rate and resolution, reduces operational safety risks, extends equipment life, and improves the continuity of testing and data accuracy.
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Figure CN121784110A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of semiconductor material analysis technology, specifically to specialized electrolyte compounds for analyzing the electrochemical properties of various semiconductor materials and their application methods. Background Technology
[0002] Semiconductor materials are core foundational materials in fields such as electronics, information technology, and optoelectronics. The accurate analysis of their electrochemical properties directly determines the efficiency of material development and the reliability of device performance. Electrochemical capacitance-voltage analysis is one of the core technologies for detecting the electrochemical properties of semiconductor materials. Specialized electrolyte compounds, as key supporting materials for this analytical method, play a crucial role in selectively etching material surfaces and constructing a stable electrochemical testing environment. Currently, electrolyte systems based on components such as EDTA, Tiron, ammonium bifluoride, KOH, and NaOH have emerged in the industry. However, their applications are mostly concentrated on single materials or general scenarios. Precise adaptation solutions for different semiconductor material properties have not yet been formed, and the core focus is on meeting basic testing functions, with insufficient comprehensive optimization for testing resolution, continuity, and safety.
[0003] Existing electrolytes for electrochemical characterization of semiconductor materials have significant technical defects: First, they easily generate surface thin films during etching, especially when processing composite semiconductor materials such as AlGaAs. These films hinder charge transport and the continuous etching reaction, leading to test interruptions or data deviations, severely affecting the accuracy of analytical results. Second, etching rate and test resolution are difficult to match. For fine structures such as nanoscale pn junctions, existing formulations cannot simultaneously achieve efficient etching and high-resolution characterization, making it difficult to obtain accurate microstructural electrochemical data. Third, safety and equipment compatibility are poor. Some electrolytes rely on high-concentration strong acid components, which not only increases safety risks during operation but also easily corrodes test instrument components, reducing equipment lifespan. Fourth, the formulations are too general, lacking multi-system combination schemes with adjustable dilution, failing to meet the differentiated testing needs of different types of semiconductor materials such as GaAs, GaN, and SiC, thus limiting the application expansion of electrochemical characterization technology in multiple scenarios.
[0004] To address the aforementioned technical deficiencies, a solution is proposed. Summary of the Invention
[0005] The purpose of this invention is to provide a dedicated electrolyte compound for the electrochemical characterization of various semiconductor materials and its application method, in order to solve the problems mentioned above.
[0006] To achieve the above objectives, the present invention provides the following technical solution: a special electrolyte compound for the electrochemical characteristic analysis of various semiconductor materials, wherein the electrolyte compound is a multi-system synergistic combination system, comprising one of the following four series, and the components and concentrations of each series are adapted to meet the etching stability, resolution and safety requirements of electrochemical capacitance-voltage analysis of semiconductor materials;
[0007] a. Alkaline electrolyte series, including ethylenediamine, disodium ethylenediaminetetraacetate and deionized water, wherein the volume concentration of ethylenediamine is 4.0%-5.5% and the concentration of EDTA.2Na is 0.07M-0.13M. This series also includes at least two derivative formulations of the basic formulation diluted by a volume ratio of 1:5-1:25.
[0008] b. Weakly alkaline electrolyte series, with potassium hydroxide or sodium hydroxide as the active ingredient, and a concentration range of 0.001M-0.015M;
[0009] c. Tiron-based electrolyte, with the active ingredient being sodium 1,2-dihydroxybenzene-3,5-disulfonate (Tiron), at a concentration of 0.07M-0.13M;
[0010] d. Ammonium salt-based electrolyte, with ammonium hydrogen fluoride as the active ingredient, at a concentration of 0.07M-0.13M.
[0011] Furthermore, in the basic formulation of the alkaline electrolyte series, the volume concentration of ethylenediamine is preferably 4.76%-5.0%, and the concentration of EDTA.2Na is preferably 0.1M; the derived formulations include a low-speed high-resolution formulation and a high-speed low-resolution formulation. The low-speed high-resolution formulation is prepared by diluting the basic formulation with deionized water at a volume ratio of 1:15-1:25, and the high-speed low-resolution formulation is prepared by diluting the basic formulation with deionized water at a volume ratio of 1:8-1:12.
[0012] Furthermore, the weakly alkaline electrolyte series is divided into high-resolution, medium-resolution, and fast-etching types according to the concentration gradient. The high-resolution type has a concentration of 0.002M-0.0035M, the medium-resolution type has a concentration of 0.004M-0.0065M, and the fast-etching type has a concentration of 0.008M-0.012M.
[0013] Furthermore, the surfactant additive is Triton X-100, which is added to the electrolyte working solution on-site only before use. The addition amount is 4-8 drops per 110ml-140ml of working solution, and the additive is not pre-mixed into the storage mother liquor to ensure the long-term stability of the mother liquor.
[0014] Application methods for specialized electrolyte compounds used in the electrochemical property analysis of various semiconductor materials, including a core platform for application analysis of electrolyte compounds. The core platform includes a data acquisition module, a data analysis module, and a comprehensive judgment module with communication connections. The specific application process is as follows:
[0015] Step 1: The core platform receives the analysis task instruction and triggers the data acquisition module to start. The data acquisition module collects three types of key data through a combination of device sensing and manual data entry.
[0016] Step 2: The data acquisition module transmits the standardized raw data to the data analysis module. The data analysis module establishes a three-dimensional mapping database of material properties, electrolyte formulation, and etching pattern, and performs weighted analysis on the suitability of each candidate electrolyte formulation.
[0017] Step 3: The data analysis module transmits the compatibility analysis results to the comprehensive judgment module. The comprehensive judgment module filters the results using a preset compatibility threshold to determine the optimal electrolyte formula and matching etching parameters.
[0018] Step 4: The comprehensive judgment module generates operation instructions and a preliminary analysis report, which are transmitted to the core platform. The core platform then outputs instructions to guide the operators in performing ECV analysis and testing.
[0019] Step 5: During the test, the data acquisition module collects dynamic test data in real time and feeds it back to the data analysis module for dynamic optimization;
[0020] Step 6: After the test is completed, the comprehensive judgment module integrates the data from the entire process, generates the final analysis report, and feeds it back to the core platform for archiving, thus completing the closed-loop operation.
[0021] Furthermore, the collection process for the three types of key data in step 1 is as follows:
[0022] Based on the target material type, the data is manually entered through the material identification card. Whether it is easy to form a passivation film is determined by querying the material property database. The carrier concentration is obtained through previous Hall effect test experiments. The target analysis resolution is manually entered according to the user's R&D needs to construct the basic data of the semiconductor material to be tested.
[0023] The etching modes and process recipe options supported by the equipment are obtained by reading the parameter configuration file of the equipment control system. The equipment operating status data is collected in real time by the equipment's built-in status sensors to construct the ECV equipment operating parameters.
[0024] The component status and storage duration of candidate electrolyte formulations are queried through the laboratory reagent management system, and the expiration dates of additives are manually entered through reagent packaging labels, thus constructing electrolyte usage-related data.
[0025] Furthermore, the addition conditions and dosage calibration method for the additives in step 1 are as follows:
[0026] Addition conditions: Add electrolyte is only required when the contact angle between the working electrolyte and the test material is greater than 30°. The contact angle is detected in real time by an optical contact angle measuring instrument.
[0027] Dosage calibration: The basic dosage is 6 drops per 125ml of working solution. If the contact angle is greater than 45°, add 1 drop for every 5° increase, with a maximum addition of 8 drops. If the contact angle is less than 30°, no addition is required.
[0028] Furthermore, the dynamic optimization process of the fitness-weighted analysis in step 2 is as follows:
[0029] Acquire basic data of the semiconductor material to be tested, extract the core characteristics of material type, key chemical properties, carrier concentration, and application scenario, and compare them one by one with the preset formula-material matching rule library: if the formula matches the material type + core characteristics and does not trigger the mismatch conditions, it is judged as a match and assigned a value of 0.8-1.0 according to the degree of match; if the matching rules are not met or the mismatch conditions are triggered, it is judged as a mismatch and assigned a value of 0.5-0.7 according to the degree of mismatch, and it is marked as the material matching coefficient M.
[0030] Obtain the target resolution of the material to be tested, and combine it with the pre-stored standard resolution range of the formulation. Analyze the fit using interval overlap and deviation rate: when the target resolution is within the standard range, the fit = 1 - |target resolution - median of the standard range| / upper limit of the standard range; when the target resolution partially exceeds the standard range, the fit = length of the overlap interval between the standard range and the target resolution / length of the standard range; when the target resolution completely exceeds the standard range, the fit = 0. The obtained result is marked as the resolution matching coefficient R.
[0031] To obtain electrolyte usage data, a high-precision pH meter calibrated with standard buffer solutions of pH 4.00, 7.00, and 9.18 was first used to test the acidity and alkalinity of the formulation at room temperature (25°C) and normal pressure. The formulation was classified into three categories: weakly alkaline, neutral, and weakly acidic. Then, historical corrosion rates and data fluctuation data were queried from a pre-stored device model-formula compatibility database and compared one by one. The results were marked as the safety factor S.
[0032] Based on the formula F=w1×M+w2×R+w3×S, where F represents the fit degree, w1, w2, and w3 represent the weighting coefficients of the material matching coefficient M, the resolution matching coefficient R, and the safety coefficient S, and w1+w2+w3=1.
[0033] Furthermore, the method for verifying the dynamic test data in step 5 is as follows:
[0034] Etching rate verification: The etching depth is monitored in real time by the laser displacement sensor built into the ECV equipment. The etching rate is analyzed in combination with the test time and compared with the standard rate range of the formula. When the deviation exceeds ±10%, parameter adjustment is triggered.
[0035] Data continuity verification: The stability of current and voltage signals is monitored in real time by the data acquisition module. When the signal fluctuation exceeds ±5%, it is judged as a risk of test interruption. The data analysis module automatically adjusts the etching voltage or electrolyte flow rate.
[0036] Data deviation verification: The real-time collected carrier concentration data is compared with the standard data of the same type of material. If the deviation exceeds ±8%, a second etching verification is initiated.
[0037] The beneficial effects of this invention are:
[0038] 1. This invention achieves full coverage compatibility with mainstream semiconductor materials such as GaAs-based, GaN-based, and Si / SiC by constructing a multi-system synergistic dedicated electrolyte combination and precise adaptation scheme. Through three-dimensional mapping and compatibility analysis of formulation-material-etching mode, it accurately matches the chemical properties and resolution requirements of different materials, effectively solving the passivation film formation problem during etching of materials such as AlGaAs in the prior art. At the same time, it solves the problem of synergistic etching rate and resolution in the analysis of fine structures such as nanoscale pn junctions, ensuring test continuity and data accuracy.
[0039] 2. This invention optimizes the safety and equipment compatibility of electrolyte formulations. The formulation system, which is mainly weakly alkaline, avoids the use of high-concentration strong acids, reduces operational safety risks, minimizes equipment corrosion, and extends instrument lifespan. Relying on a closed-loop system of data acquisition, analysis, judgment, execution, and feedback, combined with dynamic data verification and weight optimization mechanisms, it clarifies operational guidelines such as additive usage conditions and etching parameters, significantly improving test repeatability and efficiency, shortening test preparation time, and providing efficient and reliable electrochemical characteristic analysis support for semiconductor material research and development. Attached Figure Description
[0040] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0041] Figure 1 This is a schematic diagram of four categories of electrolyte compounds of the present invention;
[0042] Figure 2 This is a flowchart of the method of the present invention. Detailed Implementation
[0043] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0044] Example 1: Please refer to Figure 1 - Figure 2 As shown, this embodiment describes a dedicated electrolyte compound and its application method for analyzing the electrochemical properties of various semiconductor materials. It includes in-depth electrochemical property analysis of three core semiconductor materials for device performance optimization. Specific materials and requirements are as follows:
[0045] Material 1: AlGaAs, a GaAs-based composite semiconductor. Previous characterization experiments showed that it readily forms a passivation film. Hall effect testing showed a carrier concentration of 3 × 10¹. 7 cm⁻³, with a target resolution of 2nm for user R&D needs, used for high-frequency device fabrication;
[0046] Material 2: GaN-based LED chip with a precision pn junction region; initial characterization showed a carrier concentration of 8 × 10¹. 7 cm⁻³, with a target resolution of 1 nm, is used to optimize luminous efficiency;
[0047] Material 3: 6H-SiC, a wide bandgap semiconductor with no risk of passivation film formation; Hall effect measurement shows a carrier concentration of 5 × 10¹. 6 cm⁻³, with a target resolution of 5nm, is used for power device research and development. The laboratory currently has two ECV devices from different brands. Option 1 supports conventional Faraday etching and pulsed anodizing etching; Option 2 supports pulsed anodizing etching and lamp-controlled etching. It is necessary to solve the problems of thin film formation, the contradiction between resolution and rate, narrow material applicability, insufficient safety and poor equipment compatibility in the existing technologies.
[0048] After receiving the analysis task submitted by the user, the core platform automatically triggers the data acquisition module to run. The specific acquisition process is as follows:
[0049] Materials basic data collection:
[0050] Material type and passivation film formation characteristics: determined by querying the company's material property database, which records the chemical properties and etching difficulties of various semiconductor materials. AlGaAs is marked as easy to form a passivation film, while GaN-based LED chips and SiC are marked as having no passivation film risk.
[0051] Carrier concentration: Retrieve previous Hall effect test reports. The test equipment was an HL5500 Hall effect analyzer, and the AlGaAs concentration was obtained as 3 × 10¹. 7 cm⁻³, GaN-based LED chip is 8×10¹ 7 cm⁻³, SiC is 5×10¹ 6 cm⁻³;
[0052] Target resolutions: manually entered by users through the core platform, namely 2nm, 1nm, and 5nm;
[0053] Equipment operating parameter collection:
[0054] Equipment Model and Supported Modes: By reading the parameter configuration files of the control systems of the two devices, it was determined that Option 1 supports conventional Faraday etching and pulsed anodizing etching, while Option 2 supports pulsed anodizing etching and lamp-controlled etching.
[0055] Process formulations: Option 1 includes FastGaN / LED and HRGaN / LED formulations; Option 2 includes standard GaN and high-resolution GaN formulations.
[0056] Equipment operating status: According to the temperature and voltage sensors built into the equipment, both devices are in normal condition;
[0057] Electrolyte correlation data acquisition:
[0058] Candidate formulation status: According to the laboratory reagent management system, the basic formulation of series A and its derivative formulations A1 and A2, the formulations of series B1, B2 and B3, formulation C and formulation D are all within their validity period;
[0059] Contact angle detection: The contact angles between the candidate electrolyte and the three materials were measured using an optical contact angle meter (model OCA20). The contact angle between AlGaAs and A2 formulation was 38°, the contact angle between GaN and B3 formulation was 32°, and the contact angle between SiC and D formulation was 28°.
[0060] The data acquisition module removes outliers from the three types of key data collected above, standardizes the data format, and then transmits the data to the data analysis module.
[0061] Establish a three-dimensional mapping database: Record the correspondence between material properties, electrolyte formulation, and etching mode into the database. Material properties are represented as type, carrier concentration, and passivation film risk. Electrolyte formulation is represented as components and concentration. Etching mode is represented as type and process formulation. For example, AlGaAs - easy to form passivation film - A2 formulation - pulsed anodic oxidation etching is a potential suitable combination.
[0062] Fit analysis: Initial weights were determined by scoring from 5 semiconductor analysis experts, with w1=0.4, w2=0.4, and w3=0.2.
[0063] AlGaAs candidate formulation a2: M=0.95, AlGaAs is compatible with formulation a2, R=0.98, formulation a2 can achieve 1-5nm resolution, with a 98% fit with the target 2nm, S=0.90, a2 is a weakly basic formulation, and the compatibility F=0.4×0.95+0.4×0.98+0.2×0.90=0.952;
[0064] Candidate formulation b3 for GaN-based LED chips: M=0.96, GaN is compatible with formulation b3, R=0.99, formulation b3 can achieve ≤1nm resolution, with a 99% fit with the target 1nm, S=0.92, b3 is a weakly alkaline formulation, and the compatibility F=0.4×0.96+0.4×0.99+0.2×0.92=0.964;
[0065] SiC candidate formulation D: M=0.97, SiC is compatible with formulation d, R=0.95, formulation d can achieve 3-5nm resolution, with a 95% fit with the target 5nm, S=0.88, d is a weakly acidic formulation with good equipment compatibility, and the compatibility F=0.4×0.97+0.4×0.95+0.2×0.88=0.944.
[0066] Example 2: Initial weights are determined by expert scoring. Material matching weight w1 = 0.35-0.45, resolution matching weight w2 = 0.35-0.45, and safety weight w3 = 0.15-0.25, with w1+w2+w3=1. After every 10 tests, the data analysis module adjusts the weights based on the test success rate: if a certain factor causes the test failure rate to exceed 5%, the weight of that factor increases by 0.02, and the weights of the other two factors decrease by 0.01 each, while the weight adjustment still satisfies w1+w2+w3=1.
[0067] The fit is calculated as F = w1 × M + w2 × R + w3 × S, where the material matching coefficient M represents the core characteristics extracted from the basic data of the semiconductor material under test, including material type, key chemical properties, carrier concentration, and application scenario. These core characteristics are compared one by one with a pre-defined formula-material fit rule library. Based on the formula's applicable scope, over 1000 sets of matching experimental data from the laboratory, and SEMI industry standards, formulas that meet the conditions of material type + core characteristics and do not trigger incompatibility conditions are considered fit, assigned a value of 0.8-1.0 based on the degree of fit. Completely matching all conditions is assigned a value of 0.95-1.0, and basically matching the core conditions is assigned a value of [missing value]. 0.8-0.94; If the fit rules are not met or the fit conditions are triggered, it is judged as misfit, and a value of 0.5-0.7 is assigned according to the degree of misfit, 0.6-0.7 for non-critical characteristics and 0.5-0.59 for core characteristics; The resolution matching coefficient R represents the target profile resolution of the material under test combined with the pre-stored standard resolution range of the formulation. The fit is analyzed by interval overlap + deviation rate: When the target resolution is within the standard range, the fit = 1 - |target resolution - median of standard range| / upper limit of standard range; When the target resolution partially exceeds the standard range, the fit = length of the overlap interval between the standard range and the target resolution. / Standard range length; when the target resolution completely exceeds the standard range, the fit = 0; assign values of 0.9-1.0 for fit ≥90%, 0.7-0.89 for 70%-89%, and 0.5-0.69 for <70%; the safety factor S represents the electrolyte usage correlation data. First, a high-precision pH meter calibrated with standard buffer solutions of pH 4.00, 7.00, and 9.18 is used to detect the acidity and alkalinity of the formula under normal pressure at room temperature (25℃) and normal pressure, classifying it into three categories: weakly alkaline (pH 7.5-9.0), neutral (pH 6.5-7.4), and weakly acidic (pH 4.0-6.4); then, through pre-stored equipment model-formula compatibility The database is used to query historical corrosion rates and data fluctuation data. For new equipment or new formulas, a small dose of 5ml is required for 10-minute etching verification. Compatibility is determined by corrosion rate ≤0.005mm / year and data fluctuation ≤±3%, and basic compatibility is determined by corrosion rate 0.005-0.01mm / year and data fluctuation 3%-5%. Finally, values are assigned based on both: weak alkaline + compatible 0.95-1.0, weak alkaline + basically compatible 0.9-0.94, neutral + compatible 0.90-0.95, neutral + basically compatible 0.85-0.89, weak acid + compatible 0.85-0.90, weak acid + basically compatible 0.8-0.84.
[0068] The comprehensive judgment module has a preset compatibility threshold of 0.88. This threshold is determined based on statistics from the enterprise's past 100 successful test data sets. When the compatibility is ≥0.88, the test success rate reaches over 95%.
[0069] The compatibility F of all three formulations is higher than the threshold, and the optimal solution is selected:
[0070] AlGaAs: Option 1 equipment + formula a2 + pulsed anodizing etching mode + add 7 drops of Triton X-100 per 125ml working solution. Because the contact angle is 38°, which exceeds the 30° baseline value, it needs to be added; if it exceeds 30° but does not reach 45°, add 6 drops + 1 drop = 7 drops.
[0071] GaN-based LED chip: Solution 1 equipment + formula b3 + pulsed anodizing etching mode + HRGaN / LED process formula + add 6 drops of TritonX-100 per 125ml working solution, contact angle 32°, add 6 drops of basic dosage;
[0072] SiC: Option 2 equipment + formula d + conventional Faraday etching mode + no need to add Triton X-100, contact angle 28°, less than 30°.
[0073] Equipment compatibility verification: Query the device model-formula compatibility comparison table stored in the core platform. Solution 1 is compatible with formulas a2 and b3, and Solution 2 is compatible with formula d. Since there are no new device models, small-dose testing is not required.
[0074] The comprehensive judgment module generates detailed operation instructions:
[0075] Recipe preparation instructions:
[0076] Formula a2: Take 50ml of EDTA alkaline base formula, ethylenediamine volume concentration 4.76%, EDTA.2Na 0.1M, dilute with deionized water to 1L, stir well and let stand for 30 minutes;
[0077] Formula b3: Take 25 ml of 0.1 MkOH standard solution (Sigma Aldrich, product number 35125-1L), dilute with deionized water to 1 L, and stir magnetically for 15 minutes;
[0078] Formula d: Weigh 5.7g of NH4F·HF reagent and slowly add it to 1L of deionized water, stirring until completely dissolved.
[0079] Additive addition instructions: Add TritonX-100 to the corresponding working solution 10 minutes before use, according to the dosage determined in step 3, and stir well.
[0080] Etching parameter instructions: Scheme 1 equipment pulse anodizing etching mode parameters, HRGaN / LED process formula parameters; Scheme 2 equipment conventional Faraday etching mode parameters; The core platform will output the operation instructions and preliminary analysis report, including the basis for formula selection and compatibility analysis results, to the laboratory operation terminal.
[0081] Operators execute tests according to instructions; the dynamic data acquisition and optimization process is as follows:
[0082] AlGaN test:
[0083] Etching rate verification: The laser displacement sensor monitors in real time. After 1 hour, the etching depth is 0.9 μm, and the etching rate is 0.9 μm / h. This is compared with the standard rate range of the a2 formula. The preset value of the standard rate range of the a2 formula is 0.8-1.0 μm / h, and the deviation is +1.1%, which meets the requirements.
[0084] Data continuity verification: Voltage signal fluctuation amplitude is 2.3%, less than ±5%, with no risk of interruption;
[0085] Data deviation verification: Real-time carrier concentration data is compared with industry standard data, with a deviation of 3.2%, which is less than ±8%, and no secondary etching is required.
[0086] GaN-based LED chip testing:
[0087] Etching rate verification: After 3 hours, the etching depth was 2.1 μm and the rate was 0.7 μm / h. Compared with the standard rate range of the b3 formulation, the preset value of the standard rate range of the b3 formulation is 0.6-0.8 μm / h, and the deviation is +1.4%, which meets the requirements.
[0088] Data continuity verification: Current signal fluctuation amplitude is 1.8%, stable;
[0089] Data deviation verification: The carrier concentration data deviation in the pn junction region is 2.7%, which meets the requirements.
[0090] SiC test:
[0091] Etching rate verification: After 2 hours, the etching depth was 1.8 μm and the rate was 0.9 μm / h. Compared with the standard rate range of formula D, the preset value of the standard rate range of formula D is 0.8-1.0 μm / h, with a deviation of 0, which meets the requirements.
[0092] Data continuity verification: Signal fluctuation amplitude 1.5%, stable;
[0093] Data deviation verification: The carrier concentration data deviation was 2.1%, which meets the requirements; no parameter adjustment was required during the test, and the test proceeded smoothly.
[0094] After the test is completed, the comprehensive judgment module integrates the following data to generate the final analysis report:
[0095] Static data: formula compatibility, basic material parameters, equipment model and parameters;
[0096] Dynamic data: etching rate, signal fluctuation amplitude, data deviation value;
[0097] Safety data: No safety incidents occurred during operation. Corrosion rate detection of equipment components was performed, and the corrosion rate of the equipment in Option 1 and the equipment data in Option 2 were displayed through corrosion sensors.
[0098] The above description is merely an example and illustration of the structure of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the structure of the invention or exceed the scope defined in the claims, all of which should fall within the protection scope of the present invention.
[0099] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0100] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to any specific implementation. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. A specialized electrolyte compound for analyzing the electrochemical properties of various semiconductor materials, characterized in that, The electrolyte compound is a multi-system synergistic combination system, which includes one of the following four series. The components and concentrations of each series are designed to meet the requirements of etching stability, resolution and safety for electrochemical capacitance-voltage analysis of semiconductor materials. a. Alkaline electrolyte series, including ethylenediamine, disodium ethylenediaminetetraacetate and deionized water. This series also includes at least two derivative formulations of the basic formulation diluted at a volume ratio of 1:5 to 1:
25. b. Weakly alkaline electrolyte series, with potassium hydroxide or sodium hydroxide as the active ingredient; c. Tiron-based electrolyte, with sodium 1,2-dihydroxybenzene-3,5-disulfonate as the active ingredient; d. Ammonium salt-based electrolyte, with ammonium hydrogen fluoride as the active ingredient.
2. The specialized electrolyte compound for electrochemical characterization of various semiconductor materials according to claim 1, characterized in that, In the basic formulation of the alkaline electrolyte series, the volume concentration of ethylenediamine is preferably 4.76%-5.0%, and the concentration of EDTA.2Na is preferably 0.1M. The derived formulations include a low-speed high-resolution formulation and a high-speed low-resolution formulation. The low-speed high-resolution formulation is prepared by diluting the basic formulation with deionized water at a volume ratio of 1:15-1:25, and the high-speed low-resolution formulation is prepared by diluting the basic formulation with deionized water at a volume ratio of 1:8-1:
12.
3. The specialized electrolyte compound for electrochemical characterization of various semiconductor materials according to claim 2, characterized in that, The weakly alkaline electrolyte series is classified into high-resolution, medium-resolution, and fast-etching types according to the concentration gradient.
4. The specialized electrolyte compound for electrochemical characterization of various semiconductor materials according to claim 3, characterized in that, The surfactant additive is Triton X-100, which is added to the electrolyte working solution on-site only before use. The addition amount is a few drops per 110ml-140ml of working solution, and the additive is not pre-mixed into the storage mother liquor to ensure the long-term stability of the mother liquor.
5. A method for using a specific electrolyte compound for analyzing the electrochemical properties of various semiconductor materials, comprising the specific electrolyte compound for analyzing the electrochemical properties of various semiconductor materials as described in any one of claims 1-4, characterized in that, It includes a core platform for the application analysis of electrolyte compounds. This core platform comprises a data acquisition module, a data analysis module, and a comprehensive judgment module connected via communication. The specific application process is as follows: Step 1: The core platform receives the analysis task instruction and triggers the data acquisition module to start. The data acquisition module collects three types of key data through a combination of device sensing and manual data entry. Step 2: The data acquisition module transmits the standardized raw data to the data analysis module. The data analysis module establishes a three-dimensional mapping database of material properties, electrolyte formulation, and etching pattern, and performs weighted analysis on the suitability of each candidate electrolyte formulation. Step 3: The data analysis module transmits the compatibility analysis results to the comprehensive judgment module. The comprehensive judgment module filters the results using a preset compatibility threshold to determine the optimal electrolyte formula and matching etching parameters. Step 4: The comprehensive judgment module generates operation instructions and a preliminary analysis report, which are transmitted to the core platform. The core platform then outputs instructions to guide the operators in performing ECV analysis and testing. Step 5: During the test, the data acquisition module collects dynamic test data in real time and feeds it back to the data analysis module for dynamic optimization; Step 6: After the test is completed, the comprehensive judgment module integrates the data from the entire process, generates the final analysis report, and feeds it back to the core platform for archiving, thus completing the closed-loop operation.
6. The application method of the special electrolyte compound for electrochemical characterization analysis of various semiconductor materials according to claim 5, characterized in that, The process for collecting the three types of key data in step 1 is as follows: Based on the target material type, the data is manually entered through the material identification card. Whether it is easy to form a passivation film is determined by querying the material property database. The carrier concentration is obtained through previous Hall effect test experiments. The target analysis resolution is manually entered according to the user's R&D needs to construct the basic data of the semiconductor material to be tested. The etching modes and process recipe options supported by the equipment are obtained by reading the parameter configuration file of the equipment control system. The equipment operating status data is collected in real time by the equipment's built-in status sensors to construct the ECV equipment operating parameters. The component status and storage duration of candidate electrolyte formulations are queried through the laboratory reagent management system, and the expiration dates of additives are manually entered through reagent packaging labels, thus constructing electrolyte usage-related data.
7. The application method of the special electrolyte compound for electrochemical characterization analysis of various semiconductor materials according to claim 6, characterized in that, The conditions for adding the additive and the method for calibrating the dosage in step 1 are as follows: Addition conditions: Add electrolyte is only required when the contact angle between the working electrolyte and the test material is greater than 30°. The contact angle is detected in real time by an optical contact angle measuring instrument. Dosage calibration: The basic dosage is 6 drops per 125ml of working solution. If the contact angle is greater than 45°, add 1 drop for every 5° increase, with a maximum addition of 8 drops. If the contact angle is less than 30°, no addition is required.
8. The application method of the special electrolyte compound for electrochemical characterization analysis of various semiconductor materials according to claim 7, characterized in that, The dynamic optimization process of the fitness-weighted analysis in step 2 is as follows: Acquire basic data of the semiconductor material to be tested, extract the core characteristics of material type, key chemical properties, carrier concentration, and application scenario, and compare them one by one with the preset formula-material matching rule library: if the formula matches the material type + core characteristics and does not trigger the mismatch conditions, it is judged as a match and assigned a value of 0.8-1.0 according to the degree of match; if the matching rules are not met or the mismatch conditions are triggered, it is judged as a mismatch and assigned a value of 0.5-0.7 according to the degree of mismatch, and it is marked as the material matching coefficient M. Obtain the target resolution of the material to be tested, and combine it with the pre-stored standard resolution range of the formulation. Analyze the fit using interval overlap and deviation rate: when the target resolution is within the standard range, the fit = 1 - |target resolution - median of the standard range| / upper limit of the standard range; when the target resolution partially exceeds the standard range, the fit = length of the overlap interval between the standard range and the target resolution / length of the standard range; when the target resolution completely exceeds the standard range, the fit = 0. The obtained result is marked as the resolution matching coefficient R. To obtain electrolyte usage data, a high-precision pH meter calibrated with standard buffer solutions of pH 4.00, 7.00, and 9.18 was first used to test the acidity and alkalinity of the formulation at room temperature (25°C) and normal pressure. The formulation was classified into three categories: weakly alkaline, neutral, and weakly acidic. Then, historical corrosion rates and data fluctuation data were queried from a pre-stored device model-formula compatibility database and compared one by one. The results were marked as the safety factor S. Based on the formula F=w1×M+w2×R+w3×S, where F represents the fit degree, w1, w2, and w3 represent the weighting coefficients of the material matching coefficient M, the resolution matching coefficient R, and the safety coefficient S, and w1+w2+w3=1.
9. The dedicated electrolyte compound for electrochemical characterization analysis of various semiconductor materials and its application method according to claim 8, characterized in that, The method for verifying the dynamic test data in step 5 is as follows: Etching rate verification: The etching depth is monitored in real time by the laser displacement sensor built into the ECV equipment. The etching rate is analyzed in combination with the test time and compared with the standard rate range of the formula. When the deviation exceeds ±10%, parameter adjustment is triggered. Data continuity verification: The stability of current and voltage signals is monitored in real time by the data acquisition module. When the signal fluctuation exceeds ±5%, it is judged as a risk of test interruption. The data analysis module automatically adjusts the etching voltage or electrolyte flow rate. Data deviation verification: The real-time collected carrier concentration data is compared with the standard data of the same type of material. If the deviation exceeds ±8%, a second etching verification is initiated.