Device, system and method for testing breakdown voltage of various non-ferrous metals

Through a multi-channel synchronous testing device and intelligent control system, the problems of low efficiency, low accuracy and environmental instability in the breakdown voltage test of tantalum, niobium and its oxide materials are solved, and efficient and accurate breakdown voltage measurement is achieved, which is suitable for batch detection and quality control of tantalum, niobium and its oxide materials.

CN120428046AActive Publication Date: 2025-08-05NINGXIA ORIENT TANTALUM INDUSTRY CO LTD

Patent Information

Application Number
CN202510593263.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-09
Publication Date
2025-08-05
Estimated Expiration
2045-05-09

AI Technical Summary

Technical Problem

In the prior art, the breakdown voltage test of tantalum, niobium and its oxide materials has problems such as low testing efficiency, insufficient environmental control, uneven electric field distribution and low breakdown determination accuracy, especially sensitive to temperature and liquid level fluctuations, resulting in systematic errors.

Method used

A multi-channel synchronous testing device is adopted, combined with temperature and humidity control system, symmetrical electrode layout, microsecond data acquisition and intelligent boost control, electric field uniformity is achieved through liquid turntable plate and liquid level adjustment, temperature stability is maintained using a PID controller, and a double threshold algorithm is used to determine breakdown events.

Benefits of technology

It significantly improves the testing efficiency and accuracy, reduces environmental interference, realizes high-precision breakdown voltage measurement, and improves the stability and consistency of the test results.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of electrical performance testing, and discloses a multi-class nonferrous metal breakdown voltage testing device, system and method. The testing device comprises a testing groove provided with a plurality of independent clamping grooves, a temperature and humidity regulation and control system, an electrode module, a power module and a data acquisition module, and high-precision breakdown voltage testing of multiple samples in a constant environment is achieved through multi-channel synchronous testing, temperature and liquid level dynamic control, symmetrical electrode layout and high-speed data acquisition. The system is integrated with a central control unit, the boosting rate is automatically set according to sample parameters, multiple channels independently boost and synchronously collect breakdown data, and a double-threshold algorithm is adopted to judge breakdown events in real time. The method comprises the whole process of solution preparation, sample installation, electric field optimization, boost control and data judgment. Compared with the prior art, the testing efficiency and the measuring precision are improved, the environmental interference is reduced, and the method is suitable for batch detection and quality control of tantalum, niobium and oxide materials of the tantalum, the niobium and the oxide materials of the tantalum and the niobium.
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Description

Technical Field

[0001] The present invention belongs to the technical field of electrical performance testing, and in particular relates to a high-precision breakdown voltage testing device, system and method for tantalum, niobium and their oxide materials. Background Art

[0002] Tantalum, niobium, and their oxides, due to their excellent dielectric properties and chemical stability, are widely used in capacitor manufacturing, semiconductor devices, energy storage, and other fields. Breakdown voltage, a key indicator for evaluating a material's electrical properties and quality stability, directly impacts its performance in high-reliability applications. Common existing breakdown voltage measurement methods include DC voltage boost, AC withstand voltage testing, and pulse breakdown. These methods still suffer from low test efficiency, inadequate environmental control, low detection accuracy, and uneven electric field distribution. In particular, the breakdown voltage of tantalum and niobium materials is extremely sensitive to ambient temperature, potentially decreasing by 5% to 8% for every 10°C increase in temperature. Furthermore, liquid level fluctuations and improper electrode layout can easily lead to uneven electric field strength, introducing systematic errors. Therefore, there is an urgent need to develop a breakdown test system that supports multi-channel simultaneous testing, features dynamic environmental control and high-speed data acquisition, and optimizes electric field uniformity. This system can improve measurement accuracy, stability, and test efficiency to meet the needs of electrical performance evaluation and quality control for nonferrous metal materials. Summary of the Invention

[0003] In response to the problems existing in the prior art such as low single-channel test efficiency, insufficient environmental parameter control, uneven electric field distribution, and low breakdown judgment accuracy, the present invention provides a new testing device and method that can significantly improve test efficiency, measurement accuracy, and test environment stability, and realize multi-sample synchronous testing and intelligent control.

[0004] To achieve the above object, the present invention adopts the following technical solutions:

[0005] A device for testing the breakdown voltage of various nonferrous metals, comprising a test tank, a temperature and humidity control system, an electrode module, a power supply module, and a data acquisition module, characterized in that:

[0006] The test slot is provided with a plurality of independent card slots, each card slot is used to fix a sample to be tested, and each card slot corresponds to a group of electrodes;

[0007] The electrode module includes a cathode plate disposed in each slot and arranged opposite to the sample to be tested, and an adjustable product steel bar for supporting the sample, wherein the cathode plate and the sample form a locally symmetrical electric field distribution, and the product steel bar is height-adjustable by adjusting the positioning screw and the product steel bar support to control the immersion depth of the sample to be tested;

[0008] The temperature and humidity control system includes a circulating liquid inlet pipe, a circulating liquid return pipe, a liquid turning plate and a liquid level regulating screw sleeve, and through the circulation flow and liquid level control, the test solution level is kept constant and the overflow is uniform;

[0009] The temperature control module includes a temperature measuring thermocouple and a heating element, and the temperature controller is used to maintain the test solution temperature fluctuation range within ±0.5°C;

[0010] The data acquisition module includes a voltage sensor and a current sensor with a response speed of microseconds, which synchronously collect the voltage drop and current mutation data at the moment of breakdown, and determine the breakdown event through a threshold comparison algorithm;

[0011] The power module automatically calculates the voltage boost rate according to the input sample parameters and independently applies voltage to each slot in a constant current mode until the sample breaks down.

[0012] The liquid turning plate is a structural component fixedly mounted on the inner wall of the test tank, and a serrated overflow tooth is provided on the top thereof to realize the natural overflow of the energizing liquid. The liquid level regulating screw sleeve is arranged on multiple supporting points outside the test tank, and the local lifting and lowering of the tank body is realized by rotating the screw sleeve to fine-tune the overall horizontality of the test tank. When the liquid level of the test solution rises to the top of the liquid turning plate, the liquid overflow speed at both ends of the liquid turning plate can be basically consistent, thereby maintaining the liquid level balance and ensuring the consistency of the electric field distribution and the repeatability of the test results. The product steel bar is made of stainless steel, and a plurality of equally spaced welding points are provided on the product steel bar for mounting multiple samples to be tested.

[0013] The temperature control module adopts a PID controller, which dynamically adjusts the power output of the heating element according to the difference between the real-time temperature feedback from the temperature measuring thermocouple and the set temperature, so that the temperature fluctuation of the test solution is controlled within ±0.5°C.

[0014] The data acquisition module further includes a noise filtering circuit, which uses a differential amplifier and a low-pass filter with a cut-off frequency of 10 kHz to eliminate high-frequency interference signals.

[0015] In the threshold comparison algorithm, the conditions for determining a breakdown event are: within 1 ms, the voltage value drops by more than 50% of the current value, and the current value rises to more than 10 times the initial value.

[0016] The water inlet direction of the circulating liquid inlet pipe is arranged perpendicular to the arrangement direction of the card slots in the test tank, and an independent water supply pipe is provided under each card slot. The flow rate is adjusted by a valve driven by a stepper motor to ensure a constant liquid level.

[0017] The product steel bar support is fixed on the top of the test slot, and the product steel bar is driven to move up and down by the adjusting positioning screw connected by the thread, and the adjustment range is 0 to 15 mm.

[0018] The calculation formula of the voltage boost rate (v) in the power module is:

[0019] v=k·I 密度 W 坯块 / S 接触面积

[0020] Where, v is the voltage increase rate (V / s), k is the material characteristic coefficient, I 密度 is the preset current density (A / m 2 ), W 坯块 is the mass of the block (g), S 接触面积 is the contact area between the electrode and the sample (m 2 ).

[0021] The product steel bars are made of stainless steel.

[0022] The top of the liquid turning plate is provided with serrated overflow teeth with a tooth height of 1 mm and a tooth spacing of 3 mm.

[0023] The breakdown event is determined by a dual-threshold strategy, where the voltage drops by ≥50% within 1ms and the current increases to more than 10 times the initial value.

[0024] The temperature control module adopts a PID controller, the proportional band is set between 0.8 and 1.2, and the integral time is 90 to 120 seconds.

[0025] The liquid inlet flow rate of the circulating liquid inlet pipe is controlled at 1.5±0.2L / min, and the valve opening is controlled by a stepper motor.

[0026] The test slot is provided with 10 to 20 independent card slots for synchronous testing.

[0027] The present invention also provides a multi-channel breakdown voltage test system, comprising the above-mentioned test device and a central control unit, which is used to automatically allocate test channels according to input sample parameters (including weight, material type and target current density) and generate independent voltage rise rate instructions for each channel;

[0028] A multi-channel data acquisition module, connected to the voltage / current sensor of the test device, for synchronously acquiring the voltage and current signals of each channel, with a sampling frequency of not less than 1 MHz;

[0029] The breakdown judgment module detects the voltage drop and current surge of each channel and determines the breakdown based on the threshold comparison algorithm;

[0030] The feedback control module is used to dynamically adjust the liquid level regulating screw sleeve and the flow rate of the circulating liquid inlet pipe according to the liquid level fluctuation detection results to ensure that the liquid level fluctuation amplitude is ≤±0.2mm.

[0031] The present invention also provides a method for testing the breakdown voltage of various non-ferrous metals, comprising the following steps:

[0032] (1) Solution configuration and temperature control initialization:

[0033] Prepare a test solution of ethylene glycol and nitric acid, and adjust the conductivity to 1.5-2.5 μS / cm. Pour the solution into the test tank and heat it to 30-80°C using the temperature control module, maintaining a temperature fluctuation of ≤±0.5°C.

[0034] (2) Sample installation and electric field adjustment:

[0035] Weld the sample to be tested to the product steel bar, control the sample immersion depth by 5-10mm by adjusting the positioning screw, and adjust the liquid level adjustment screw sleeve to control the overflow gap of the liquid turning plate so that the electric field uniformity deviation is ≤5%;

[0036] (3) Parameter self-tuning and voltage boost test:

[0037] Input the sample weight and preset current density. The central control unit calculates the parameters of each channel according to the boost rate formula. The power module applies boost in constant current mode with a boost rate range of 10 to 200 V / s.

[0038] (4) Breakdown event determination and recording:

[0039] The voltage and current signals of each channel are collected synchronously. When it is detected that the voltage drops by ≥50% and the current increases by ≥10 times within 1ms, a breakdown event is determined to have occurred, the breakdown voltage value is recorded, and a test report is generated.

[0040] Compared with the prior art, the present invention has the following significant advantages:

[0041] Significantly improved test efficiency: Supports simultaneous testing of multiple samples, with overall efficiency increased by 5 to 8 times compared to traditional single-channel devices;

[0042] The test environment is stable and reliable: temperature fluctuation ≤±0.5℃, liquid level fluctuation ≤±0.2mm, electric field uniformity deviation ≤5%, effectively reducing environmental interference;

[0043] Significantly improved measurement accuracy: microsecond-level transient signal acquisition and intelligent breakdown determination achieve breakdown voltage measurement error ≤±1.5%;

[0044] High degree of intelligent operation: parameter self-tuning and automatic boost control reduce human intervention, making the test process more efficient and stable;

[0045] Wide range of applications: Compatible with bulk and column samples of tantalum, niobium, and their oxide materials, suitable for R&D and quality inspection scenarios.

[0046] In summary, the present invention solves the key pain points in traditional breakdown voltage testing technology through structural innovation, control system optimization and improved data acquisition accuracy, and has significant application prospects and promotion value. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 : Schematic diagram of the test device structure of the present invention (side view).

[0048] Figure 2 : Schematic diagram of the test device structure of the present invention (front view).

[0049] The contents represented by the reference numerals in the figures are as follows:

[0050] 1—test tank; 2—adjustment seat; 3—product steel bar support; 4—product steel bar; 5—tested sample; 6—liquid level adjustment screw sleeve; 7—liquid turning plate; 8—cathode plate; 9—circulating liquid inlet pipe; 10—circulating liquid return pipe; 11—adjustment seat. DETAILED DESCRIPTION

[0051] The following describes the implementation process of the present invention in detail with reference to the accompanying drawings and embodiments to ensure the operability and repeatability of the technical solution.

[0052] Example 1: Tantalum block breakdown voltage test

[0053] This embodiment is based on the breakdown voltage testing device and system of the present invention, and performs high-precision breakdown voltage testing on tantalum block samples to verify the multi-channel synchronous testing efficiency and environmental stability control capabilities of the device.

[0054] 1. Test equipment construction

[0055] (1) Figure 1 and Figure 2 As shown, 10 independent card slots are set inside the test slot 1, each card slot is equipped with a set of cathode plates 8 and product steel bars 4, the product steel bars 4 are fixed to the top of the slot through the product steel bar support 3, the adjustment seat 11 is fixed to the side wall of the test slot, the adjustment positioning screw 2 is connected to the adjustment seat 11 through a thread and the vertical height of the product steel bar 4 is adjusted by the adjustment positioning screw 2 (adjustment range 0-15mm).

[0056] (2) The circulating liquid inlet pipe 9 and the circulating liquid return pipe 10 are connected to the energizing liquid storage device and the reflux device respectively. The liquid inlet flow rate is controlled at 1.5L / min and is precisely adjusted by the valve controlled by the stepping motor.

[0057] (3) Install the liquid turning plate 7, with serrated overflow teeth (tooth height 1mm, tooth pitch 3mm) on the top. By rotating the liquid level adjustment screw sleeves 6 set at the four corners of the test tank, the tank body level is fine-tuned to ensure that the liquid at both ends of the liquid turning plate overflows synchronously, preventing excessive overflow on one side or local distortion of the electric field, and improving test stability and repeatability. This structure does not require a complex mechanism. Based on this disclosure, technicians can directly achieve precise liquid level adjustment to ensure that the liquid level fluctuation is ≤±0.2mm.

[0058] (4) The cathode plate 8 is positioned opposite the sample 5 to be tested. The cathode plate is at least 30 mm larger than the tantalum block, ensuring a gap of approximately 15 mm between the tantalum block and the cathode wall in all directions. This creates a relatively uniform electric field distribution and prevents excessive local field strength at the edges of the tantalum block.

[0059] 2. Test solution configuration and temperature control initialization

[0060] (1) Prepare a test solution containing a mixture of ethylene glycol and nitric acid in a volume ratio of 3:1, and adjust the conductivity to 2.0 μS / cm at room temperature.

[0061] (2) The solution was injected into the test tank and heated to 50°C by the PID temperature control module, and the temperature fluctuation was maintained at ≤±0.5°C.

[0062] 3. Sample Installation and Electric Field Optimization

[0063] (1) Select 10 tantalum blocks with a size of 10 mm × 10 mm × 5 mm and a weight of 2.5 g ± 0.1 g as the test samples 5.

[0064] (2) The samples are spot welded to the product steel bar 4. The depth of each sample immersed in the solution is controlled within 8 mm, and the immersion depth error is ≤±0.1 mm.

[0065] (3) The liquid level is adjusted to a stable overflow state of the liquid turning plate, and the deviation of the detected electric field strength is ≤5%, ensuring that each sample is in a uniform electric field.

[0066] 4. Boost rate self-tuning and test execution

[0067] (1) Input sample parameters (weight 2.5g, preset current density 0.5A / m 2 ), using the boost rate formula:

[0068] v=k·I 密度 W 坯块 / S 接触面积

[0069] Among them, the material characteristic coefficient k = 0.12, the electrode contact area S = 0.001m 2 , the calculated boost rate v = 150V / s.

[0070] (2) Apply voltage to each channel independently in constant current mode and increase the voltage until the sample breaks down.

[0071] 5. Breakdown determination and data collection

[0072] (1) The data acquisition module monitors the voltage and current curves in real time at a sampling frequency of 1 MHz.

[0073] (2) When the voltage value drops by more than 50% within 1ms and the current value rises to more than 10 times the initial value, the system automatically determines a breakdown event.

[0074] (3) Record the voltage peak at the moment of breakdown as the breakdown voltage value, and generate a test report for each channel simultaneously.

[0075] 6. Experimental comparison and results

[0076] (1) 10 samples were tested under liquid level dynamic control conditions, and the average breakdown voltage was 1202V with a standard deviation of 1.1%.

[0077] (2) In the comparative test without using dynamic liquid level control, the standard deviation of the breakdown voltage increased to 4.5%.

[0078] (3) It shows that the liquid level dynamic control and electric field optimization design of the present invention can effectively improve the consistency and reliability of the test results.

[0079] Example 2: Breakdown voltage test of niobium oxide cylindrical blocks

[0080] 1. Test condition adjustment

[0081] Cathode plate spacing: For niobium oxide cylindrical blocks, adjust the cathode plate spacing to 15 mm.

[0082] Solution temperature: Set the temperature controller to 30°C, and adjust the PID parameters to a proportional band of 1.0, an integral time of 90 s, and a differential time of 15 s.

[0083] 2. Sample Installation

[0084] The niobium oxide cylindrical block (size Φ5mm×H5mm) is spot welded to the product steel bar (4) with an immersion depth of 5mm.

[0085] 3. Breakdown determination details

[0086] The voltage ramp rate was set at 10 V / s (calculated based on the weight of the niobium oxide cylinder, 0.50 g). At the breakdown instant, the voltage dropped from 450 V to 212 V (52.9%), and the current increased from 1 mA to 12 mA (12 times). The system locked the breakdown voltage at 450 V within 1 ms.

[0087] 4. Data Verification

[0088] The test was repeated three times, and the breakdown voltages were 450V, 448V, and 452V, respectively, with a standard deviation of 0.4%, verifying the high repeatability of the system (breakdown judgment accuracy ≥ 99%).

[0089] The present invention uses a liquid turnover plate, liquid level adjustment and dynamic temperature control system to ensure a highly stable test environment, effectively reducing data deviations caused by environmental fluctuations.

[0090] Adopting independent voltage boost and dual-threshold breakdown judgment, the breakdown moment is accurately captured, ensuring the authenticity and consistency of the breakdown voltage data;

[0091] The boost rate self-tuning mechanism automatically optimizes the test process according to different materials and sample sizes, improving the adaptability and intelligence of the system.

Claims

1. A device for testing the breakdown voltage of various nonferrous metals, comprising a test tank (1), a temperature and humidity control system, an electrode module, a power supply module, and a data acquisition module, characterized in that: The test slot (1) is provided with a plurality of independent slots, each slot is used to fix a sample (5) to be tested, and each slot corresponds to a group of electrodes; The electrode module comprises a cathode plate (8) disposed in each slot and arranged opposite to the sample (5) to be tested, and an adjustable product steel bar (4) for supporting the sample (5), wherein the cathode plate (8) and the sample (5) form a locally symmetrical electric field distribution, and the product steel bar (4) can be adjusted in height by adjusting a positioning screw (2) and a product steel bar support (3) to control the immersion depth of the sample (5) to be tested; The temperature and humidity control system comprises a circulating liquid inlet pipe (9), a circulating liquid return pipe (10), a liquid turning plate (7) and a liquid level regulating screw sleeve (6), and is configured to keep the test solution level constant and overflow uniform through circulating flow and liquid level control; The temperature control module includes a temperature measuring thermocouple and a heating element, and the temperature controller is used to maintain the test solution temperature fluctuation range within ±0.5°C; The data acquisition module includes a voltage sensor and a current sensor with a response speed of microseconds, which synchronously collect the voltage drop and current mutation data at the moment of breakdown, and determine the breakdown event through a threshold comparison algorithm; The power module automatically calculates the voltage boost rate according to the input sample parameters and independently applies voltage to each slot in a constant current mode until the sample breaks down.

2. The device according to claim 1, characterized in that: The top of the liquid turning plate (7) is provided with a sawtooth overflow structure, and the liquid level regulating screw sleeve (6) is used to adjust the overall level of the test tank (1) to achieve uniform overflow of the energizing liquid at both ends of the liquid turning plate, thereby ensuring liquid level stability and electric field consistency.

3. The device according to claim 1, characterized in that: The surface of the cathode plate (8) is provided with a platinum coating, and the distance between the cathode plate (8) and the side wall of the test slot (1) is 3 to 5 times the thickness of the sample (5) to be tested, so as to eliminate edge electric field distortion and maintain uniform electric field distribution.

4. The device according to claim 1, characterized in that: The product steel bar (4) is made of stainless steel, and its surface is covered with an aluminum oxide insulation layer with a thickness of 50 to 100 μm. The product steel bar (4) is provided with a plurality of equally spaced welding points for mounting a plurality of tested samples (5).

5. The device according to claim 1, characterized in that: The temperature control module adopts a PID controller, which dynamically adjusts the power output of the heating element according to the difference between the real-time temperature feedback from the temperature measuring thermocouple and the set temperature, so that the temperature fluctuation of the test solution is controlled within ±0.5°C.

6. The device according to claim 1, characterized in that: The data acquisition module further includes a noise filtering circuit, which uses a differential amplifier and a low-pass filter with a cut-off frequency of 10 kHz to eliminate high-frequency interference signals.

7. The device according to claim 1, characterized in that: In the threshold comparison algorithm, the conditions for determining a breakdown event are: within 1 ms, the voltage value drops by more than 50% of the current value, and the current value rises to more than 10 times the initial value.

8. The device according to claim 1, characterized in that: The water inlet direction of the circulating liquid inlet pipe (9) is arranged perpendicular to the arrangement direction of the slots in the test tank (1), and an independent water supply pipe is provided under each slot, and the flow rate is adjusted by driving the valve with a stepping motor to ensure a constant liquid level.

9. The device according to claim 1, characterized in that: The product steel bar support (3) is fixed to the top of the test slot (1), and is driven by a threaded adjustment positioning screw (1) to move the product steel bar (4) up and down, with an adjustment range of 0 to 15 mm.

10. The device according to claim 1, characterized in that: The calculation formula of the voltage boost rate (v) in the power module is: v=k·I 密度 ·W 坯块 / S 接触面积 Where, v is the voltage increase rate (V / s), k is the material characteristic coefficient, I 密度 is the preset current density (A / m 2 ), W 坯块 is the mass of the block (g), S 接触面积 is the contact area between the electrode and the sample (m 2 ).

11. A multi-type nonferrous metal breakdown voltage test system, characterized in that: include: The breakdown voltage testing device according to any one of claims 1 to 10; The central control unit is used to automatically allocate test channels based on input sample parameters (including weight, material type and target current density) and generate independent boost rate instructions for each channel; A multi-channel data acquisition module, connected to the voltage / current sensor of the test device, for synchronously acquiring the voltage and current signals of each channel, with a sampling frequency of not less than 1 MHz; The breakdown judgment module detects the voltage drop and current surge of each channel and determines the breakdown based on the threshold comparison algorithm; The feedback control module is used to dynamically adjust the liquid level regulating screw sleeve (6) and the flow rate of the circulating liquid inlet pipe (9) according to the liquid level fluctuation detection result to ensure that the liquid level fluctuation amplitude is ≤±0.2mm.

12. A method for testing the breakdown voltage of various nonferrous metals, characterized in that: The following steps are involved: (1) Solution configuration and temperature control initialization: Prepare a test solution of ethylene glycol and nitric acid mixture, and adjust the conductivity to 1.5-2.5 μS / cm; inject the solution into the test tank (1), and heat it to 30-80° C. through the temperature control module and maintain the temperature fluctuation ≤±0.5° C.; (2) Sample installation and electric field adjustment: The sample to be tested (5) is welded to the product steel bar (4), and the sample immersion depth is controlled by adjusting the positioning screw (2) to 5 to 10 mm. The liquid level regulating screw sleeve (6) is adjusted to control the overflow gap of the liquid turning plate (7) so that the electric field uniformity deviation is ≤5%; (3) Parameter self-tuning and voltage boost test: Input the sample weight and preset current density. The central control unit calculates the parameters of each channel according to the boost rate formula. The power module applies boost in constant current mode with a boost rate range of 10 to 200 V / s. (4) Breakdown event determination and recording: The voltage and current signals of each channel are collected synchronously. When it is detected that the voltage drops by ≥50% and the current increases by ≥10 times within 1ms, a breakdown event is determined to have occurred, the breakdown voltage value is recorded, and a test report is generated.

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