Method for regulating electrical properties of semiconductor material under high pressure-temperature coupling field

Abstract

The application discloses a kind of high pressure-temperature coupling field under the regulation and control method of electrical properties of semiconductor material, belongs to high pressure regulation and control technical field, including the following steps: S1, semiconductor material is cut, washed, and establishes "lattice orientation-initial electrical properties" individual archives;S2, build high pressure-temperature coupling field regulation and control device;S3, semiconductor sample is installed, and initial parameter dynamic correction calculation is carried out, and contact pressure is adaptively controlled;S4, temperature, pressure is increased to the initial temperature and initial pressure of correction, and electrical properties and contact pressure are detected in real time after stabilization, and the parameter is adjusted to reach standard and stabilize 30-60 minutes;S5, reduce pressure to normal pressure and record lattice orientation residual deviation angle θ', reduce temperature to room temperature, and the surface of sample is cleaned and electrical properties is rechecked.The application combines high pressure-temperature coupling field with real-time feedback, realizes the accurate, stable, non-damage regulation and control of electrical properties of semiconductor material.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high pressure regulation, in particular to a method for regulating the electrical properties of semiconductor materials under a high pressure-temperature coupling field. BACKGROUND

[0002] The electrical properties of semiconductor materials are the core factors determining the performance of semiconductor devices. Currently, the methods for regulating the electrical properties of semiconductor materials in the industry mainly include doping regulation, epitaxial growth regulation, ion implantation regulation, etc. Among them, doping regulation changes the carrier concentration by introducing impurity atoms into the semiconductor material, but it easily introduces lattice defects, resulting in a decrease in material stability; epitaxial growth regulation can achieve lattice matching, but the preparation process is complex, the cost is high, and it is difficult to adjust the electrical properties of the prepared semiconductor device later; ion implantation regulation has problems such as difficulty in accurately controlling the implantation depth and easy damage to the material structure during subsequent annealing treatment.

[0003] In recent years, high pressure regulation and temperature regulation have gradually attracted attention as emerging physical regulation methods. High pressure regulation can change the lattice spacing of semiconductor materials, adjust the atomic interaction, and thus affect the carrier transport characteristics; temperature regulation changes the thermal motion state of carriers to regulate the carrier concentration and mobility. However, in the existing technology, high pressure regulation and temperature regulation are used separately, and the synergistic coupling of the two is not achieved. When high pressure regulation is used alone, if the pressure is too high, it can easily cause material rupture, and the regulation range is limited; when temperature regulation is used alone, high temperature can easily cause material grain growth, damaging the material microstructure, and it is difficult to accurately intervene in the carrier transport path.

[0004] In addition, the existing regulation method has key defects in "sample installation and parameter initialization": first, the anisotropy of the semiconductor material lattice (such as the 20% difference in pressure response between silicon <100> and <111> orientations) is not considered, and the misalignment of the high pressure loading direction and the lattice orientation leads to poor regulation repeatability; second, the initial parameters are only set to a fixed range according to the material type, without dynamic adjustment based on the actual initial electrical properties of the sample after pretreatment (such as initial resistivity deviation), which can easily cause regulation "overshoot"; third, the contact between the probe and the sample relies on rigid pressing, and the fluctuation of the contact pressure (±0.2N) leads to unstable contact resistance (±0.3Ω), affecting the detection accuracy. At the same time, there is a lack of real-time monitoring feedback mechanism, resulting in low regulation accuracy and poor repeatability, which is difficult to meet the demand for high-performance semiconductor devices. SUMMARY

[0005] The purpose of the present application is to provide a method for regulating the electrical properties of semiconductor materials under a high pressure-temperature coupling field, which can achieve accurate, stable, and non-damaging regulation of the electrical properties of semiconductor materials by combining high pressure-temperature coupling fields and real-time feedback.

[0006] To achieve the above object, the application provides a method for regulating electrical properties of semiconductor materials under high-pressure-temperature coupling field, comprising the following steps:

[0007] S1, cutting and cleaning the semiconductor materials, and establishing an individual file of "lattice orientation-initial electrical properties";

[0008] S2, building a high-pressure-temperature coupling field regulating device;

[0009] S3, installing the semiconductor sample, and performing initial parameter dynamic correction calculation and self-adaptive control of the contact pressure;

[0010] S4, increasing the temperature and pressure to the corrected initial temperature and initial pressure, and after stabilization, detecting the electrical properties and contact pressure in real time, and adjusting the parameters to reach the standard and stabilize for 30-60 minutes;

[0011] S5, reducing the pressure to normal pressure and recording the residual deviation angle θ' of the lattice orientation, reducing the temperature to room temperature, and performing surface cleaning and electrical property re-inspection of the sample.

[0012] Preferably, in S1, the semiconductor materials to be regulated are selected, cut into sheet-shaped samples with a size of 5mm*5mm*0.1mm-20mm*20mm*1mm, and the sample surface is ensured to be defect-free; when the sample is cleaned, deionized water, ethanol and acetone are used for ultrasonic cleaning in sequence, and each cleaning time is 5-15 minutes to remove oil stains and impurities on the sample surface; after cleaning, the sample is placed in a vacuum drying box and dried at a temperature of 60-100℃ for 2-4 hours to avoid the influence of water on the subsequent regulation process.

[0013] The lattice orientation of the sample is detected by a polarized light microscope; the initial electrical properties at room temperature are detected by a Hall effect tester, and the initial resistivity ρ0 and initial carrier concentration n0 are recorded; and an individual file of "lattice orientation-initial electrical properties" is established.

[0014] Preferably, in S2, the high-pressure-temperature coupling field regulating device comprises a high-pressure generating module, a temperature control module, an electrical property detection module, a sample fixing module and a data processing and feedback module; the data processing and feedback module is electrically connected with the high-pressure generating module, the temperature control module, the electrical property detection module and the sample fixing module.

[0015] Preferably, the high-pressure generating module adopts a diamond anvil cell high-pressure device or a multi-anvil high-pressure device, and provides a controllable pressure of 0-10GPa, and the pressure control precision is ±0.01GPa.

[0016] The temperature control module adopts a surrounding resistance heating furnace or a laser heating system, the heating range is -196℃ to 800℃, the temperature control precision is ±1℃, and the uniformity error of the temperature field in the sample area is not more than ±2℃;

[0017] The electrical performance detection module adopts a four-probe tester or a Hall effect tester to detect the resistivity, carrier concentration and carrier mobility of the sample in real time; the probe end is integrated with a micro pressure sensor to monitor the contact pressure in real time.

[0018] The sample fixing module adopts high-temperature and high-pressure alumina ceramic material, integrates a micro displacement orientation adjustment assembly and a contact pressure buffer layer to realize lattice orientation alignment and stable contact pressure; the micro displacement orientation adjustment assembly includes an X / Y / Z three-axis adjustment platform matched with a corresponding rotary adjustment unit, and the contact pressure buffer layer is a 20-50μm thick nickel-based elastic film.

[0019] Preferably, in S3, the mounting of the semiconductor sample is specifically: placing the pretreated sample on the contact pressure buffer layer of the sample fixing module, starting the polarized light positioning system: calling the lattice orientation data from the sample individual file, comparing the pressure loading direction of the high-pressure generating module, calculating the initial deviation angle θ of the lattice orientation; if θ>0.5°, the data processing module drives the rotary adjustment unit of the micro displacement orientation adjustment assembly to fine-tune the sample position until θ≤0.5°; verifying the alignment effect by the Raman spectrometer to ensure that the pressure loading direction is consistent with the optimal carrier transport direction and eliminate the interference of lattice anisotropy.

[0020] Preferably, in S3, the initial parameter dynamic correction calculation is specifically: the data processing and feedback module imports the sample initial electrical performance individual file and the target performance parameters, and dynamically corrects the initial pressure P0 and the initial temperature T0 according to the following logic:

[0021] Calculate the initial performance deviation:

[0022] Δρ=(ρ0-ρ target ) / ρ target ×100%;

[0023] Δn=(n target -n0) / n target ×100%;

[0024] Wherein, Δρ is the initial resistivity deviation, ρ target is the target resistivity, Δn is the initial carrier concentration deviation, n target is the target carrier concentration.

[0025] Parameter correction rules:

[0026] If Δρ>15% and Δn>15%:

[0027] P0 = P base × (1 - Δρ × 0.02), T0 = T base × (1 + Δn × 0.03);

[0028] wherein, P base is the initial pressure of the material, T base is the initial temperature of the material;

[0029] If Δρ < -10% and Δn < -10%:

[0030] P0 = P base × (1 - Δρ × 0.01), T0 = T base × (1 + Δn × 0.02);

[0031] If Δρ, Δn are within ±10%:

[0032] P0 = P base , T0 = T base ;

[0033] Boundary check: ensure that P0≤80% of the ultimate compressive strength of the material, T0≤70% of the thermal decomposition temperature of the material, to avoid excessive initial parameters causing damage to the material.

[0034] Preferably, in S3, the contact pressure is adaptively controlled as follows: the probe position of the electrical property detection module is adjusted to make the probe contact the sample surface; the data processing module sets a contact pressure threshold, and the micro pressure sensor feeds back the contact pressure in real time; if the actual pressure is lower than the threshold, the sample fixing module is driven to increase the pressure; if it is higher than the threshold, it is adjusted in the opposite direction until the contact pressure is stabilized within the threshold range, and the contact resistance is <0.5Ω; after 3 minutes of continuous monitoring, it is ensured that the contact state is stable, and the next step of regulation is entered.

[0035] Preferably, in S4, it is specifically as follows:

[0036] Start the high-pressure generating module, slowly increase the pressure to the corrected initial pressure P0 at a rate of 0.01-0.1 GPa / min, and in the process, the data processing module receives the orientation data of the micro-displacement orientation adjustment assembly in real time; if θ > 1° due to pressure loading, automatically pause the pressure increase and fine-tune the sample angle to ensure alignment accuracy;

[0037] Start the temperature control module, and increase the temperature to the corrected initial temperature T0 at a rate of 5-20℃ / min; during the temperature increase process, the rate is optimized in combination with the initial resistivity ρ0: if ρ0>2ρ target , the temperature increase rate is increased to 15-20℃ / min to accelerate the carrier activation; if ρ0<0.8ρ targetThe heating rate was reduced to 5-10℃ / min to avoid over-excitation of charge carriers;

[0038] Once the pressure and temperature reach the initial set values, maintain the coupling field stable for 10-30 minutes to allow the internal structure of the sample to reach equilibrium.

[0039] The electrical performance parameters of the sample are detected in real time through the electrical performance detection module at a frequency of 1-5 minutes / time. At the same time, the miniature pressure sensor continuously monitors the contact pressure, and the detection data is transmitted to the data processing and feedback module in real time.

[0040] The data processing and feedback module compares the detected electrical performance parameters with the target parameters in real time.

[0041] Preferably, when comparing the real-time detected electrical performance parameters with the target parameters, if the real-time resistivity is higher than the target resistivity and the carrier concentration is lower than the target carrier concentration, the pressure is increased by 0.05-0.2 GPa or the temperature is increased by 10-30°C, provided that the pressure does not exceed the material's ultimate compressive strength and the temperature does not exceed the material's thermal decomposition temperature, until the resistivity and carrier concentration reach the target range. If the real-time carrier mobility is lower than the target mobility and the resistivity is higher than the target resistivity, the pressure is decreased by 0.05-0.1 GPa or the temperature is decreased by 5-15°C to reduce the lattice distortion's obstruction of carrier transport until the mobility and resistivity reach the target range. If the real-time electrical performance parameters fluctuate within the target range, the current pressure and temperature parameters are maintained, and monitoring continues for 30-60 minutes to ensure performance stability.

[0042] Preferably, in S5, specifically: after the electrical performance parameters of the sample have stabilized at the target value and remained stable for more than 30 minutes, the coupling field is stopped: first, the pressure is reduced to ambient pressure at a rate of 0.05-0.2 GPa / min, and the residual deviation angle θ' of the lattice orientation is recorded during the process; then, the temperature is reduced to room temperature at a rate of 10-30℃ / min.

[0043] After the temperature drops to room temperature, the sample is removed from the sample fixing module and the sample is cleaned and its electrical properties are re-inspected: the uniformity of electrical properties and lattice integrity are tested in the whole domain, and the repeatability error of the "orientation aligned group" and the "orientation misaligned group" is compared to ensure that the control effect meets the requirements.

[0044] Therefore, the beneficial effects of the above-mentioned method for controlling the electrical properties of semiconductor materials under a high-voltage-temperature coupled field are as follows:

[0045] (1) By precisely aligning (θ≤0.5°), the interference of lattice anisotropy is eliminated, and the repeatability error of electrical performance regulation of different samples of the same material is reduced from 5% to ≤3%, and the batch stability is significantly improved.

[0046] (2) Based on the parameter correction of the initial performance, the "overshoot" problem of traditional fixed range parameters is avoided. The single sample control cycle is shortened from 2-6 hours to 1.5-4 hours, and the efficiency is improved by 25%-30%.

[0047] (3) Adaptive control reduces contact resistance fluctuation from ±0.3Ω to ±0.05Ω and electrical performance detection deviation from ±3% to ±1%, providing a reliable data basis for precise control.

[0048] (4) Its innovative features can be adapted to various semiconductor materials such as silicon, gallium nitride, and silicon carbide. It does not require a separate initialization scheme, which expands the scope of application of the technology and makes it easier to meet the needs of industrial mass production.

[0049] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0050] Figure 1 This is a schematic diagram illustrating the steps of an embodiment of a method for controlling the electrical properties of semiconductor materials under a high-voltage-temperature coupled field according to the present invention.

[0051] Figure 2 This is a schematic diagram of the composition structure of an embodiment of the high-pressure-temperature coupled field control device of the present invention. Detailed Implementation

[0052] The technical solution of the present invention will be further described below with reference to the accompanying drawings and embodiments.

[0053] Unless otherwise defined, the technical or scientific terms used in this invention shall have the ordinary meaning understood by one of ordinary skill in the art to which this invention pertains. The terms "first," "second," and similar terms used in this invention do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed following the word and their equivalents, without excluding other elements or objects. Terms such as "connected" or "linked" are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. Terms such as "upper," "lower," "left," and "right" are used only to indicate relative positional relationships; when the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0054] Example 1

[0055] like Figure 1 As shown, this invention provides a method for controlling the electrical properties of semiconductor materials under a high-voltage-temperature coupled field, comprising the following steps:

[0056] S1. Cut and clean the semiconductor material, and establish an individual profile of "lattice orientation-initial electrical properties".

[0057] Select the semiconductor material to be controlled (such as single crystal silicon, gallium nitride single crystal, silicon carbide epitaxial wafer, etc.), cut it into sheet samples with a size of 5mm×5mm×0.1mm-20mm×20mm×1mm, and ensure that the sample surface is free of defects such as cracks and scratches.

[0058] The samples were cleaned sequentially using deionized water, ethanol, and acetone via ultrasonic cleaning, each time for 5-15 minutes, to remove oil and impurities from the sample surface. After cleaning, the samples were placed in a vacuum drying oven and dried at 60-100℃ for 2-4 hours to prevent moisture from affecting subsequent control processes.

[0059] The crystal orientation of the sample was detected using a polarizing microscope (resolution ≤ 0.1°). <100> Gallium nitride <0001> The initial electrical properties at room temperature were measured using a Hall effect tester, and the initial resistivity ρ0 (accuracy ±0.001 Ω·cm) and initial carrier concentration n0 (accuracy ±101) were recorded. 4 cm -3 Establish individual profiles for "lattice orientation-initial electrical properties".

[0060] In this implementation, the semiconductor material selected is an N-type single-crystal silicon wafer with a purity of 99.999%. <100> (Orientation), cut into 10mm×10mm×0.5mm samples, and ultrasonically cleaned with deionized water, ethanol and acetone for 10 minutes each, and vacuum dried at 80℃ for 3 hours.

[0061] Initial characterization: lattice orientation <100> , ρ0=2.8Ω·cm, n0=1.8×10 15 cm -3 Establish individual files.

[0062] S2. Construct a high-pressure-temperature coupled field control device.

[0063] like Figure 2 As shown, the high-voltage-temperature coupled field control device includes a high-voltage generation module, a temperature control module, an electrical performance testing module, a sample fixation module, and a data processing and feedback module.

[0064] The high-pressure generating module employs a diamond anvil high-pressure device or a multi-anvils high-pressure device, which can provide a controllable pressure of 0-10 GPa with a pressure control accuracy of ±0.01 GPa. In this embodiment, a diamond anvil high-pressure device (0-8 GPa) is used.

[0065] The temperature control module employs a surround-type resistance heating furnace or a laser heating system, with a heating range of -196℃ (liquid nitrogen cooling) to 800℃, a temperature control accuracy of ±1℃, and a temperature field uniformity error of no more than ±2℃ in the sample area. In this embodiment, a surround-type resistance heating furnace (25-600℃) is used.

[0066] The electrical performance testing module uses a four-probe tester or a Hall effect tester to detect the sample's resistivity (test accuracy ±0.001 Ω·cm) and carrier concentration (test accuracy ±10 Ω·cm) in real time. 14 cm -3 Carrier mobility (test accuracy ±1cm) 2 / (V·s)); The probe tip integrates a miniature pressure sensor (range 0-2N, accuracy ±0.01N) to monitor the contact pressure in real time. In this embodiment, a four-probe tester is used.

[0067] The sample fixation module has been innovatively upgraded: it adopts alumina ceramic material that is resistant to high temperature and high pressure, and integrates micro-displacement orientation adjustment components (including X / Y / Z three-axis adjustment platform with an accuracy of ±1μm; rotation adjustment unit with an accuracy of ±0.1°) and contact pressure buffer layer (20-50μm thick nickel-based elastic film, resistant to high temperature of 800℃) to achieve lattice orientation alignment and contact pressure stability.

[0068] The data processing and feedback module is electrically connected to the electrical performance testing module, high voltage generation module, temperature control module, pressure sensor, and micro-displacement orientation adjustment component. It can receive detection data, contact pressure data, and orientation data in real time and automatically adjust parameters.

[0069] S3. Install the semiconductor sample and perform dynamic correction calculations for initial parameters, and adaptively control the contact pressure.

[0070] S31. Sample mounting, precise alignment of lattice orientation and high-pressure loading direction.

[0071] The pretreated sample is placed on the contact pressure buffer layer of the sample fixing module, and the polarization positioning system is activated: the lattice orientation data is retrieved through the sample individual file, and the pressure loading direction of the high pressure generating module (such as the pressure axis of the diamond anvil cell) is compared to calculate the initial lattice orientation deviation angle θ; if θ > 0.5°, the data processing module drives the rotation unit of the micro-displacement orientation adjustment component to adjust the sample angle with an accuracy of 0.1° / step, and at the same time, the sample position is finely adjusted through the X / Y axis platform until θ ≤ 0.5°.

[0072] The alignment effect (e.g., silicon) was verified using Raman spectroscopy. <100> The offset difference between the orientation characteristic peak and the pressure axis is ≤0.2cm. -1 This ensures that the pressure loading direction is consistent with the optimal transport direction of charge carriers, thus eliminating interference from lattice anisotropy.

[0073] S32, Initial parameter dynamic correction calculation.

[0074] The data processing and feedback module imports the initial electrical performance profile and target performance parameters of the sample, and dynamically corrects the initial pressure P0 and initial temperature T0 according to the following logic:

[0075] Calculate the initial performance deviation:

[0076] Δρ=(ρ0-ρ target ) / ρ target ×100%

[0077] Δn=(n target -n0) / n target ×100%

[0078] Where Δρ is the initial resistivity deviation, ρtarget is the target resistivity, Δn is the initial carrier concentration deviation, and ntarget is the target carrier concentration;

[0079] Parameter correction rules:

[0080] If Δρ > 15% (initial resistivity is too high) and Δn > 15% (initial carrier concentration is too low):

[0081] P0 = P base ×(1-Δρ×0.02), T0=T base ×(1+Δn×0.03)

[0082] Among them, P base The initial pressure of the materials (silicon 0.5-3 GPa, gallium nitride 1-5 GPa, silicon carbide 2-6 GPa), T base The initial temperature of the material is (25-300℃ for silicon, 100-400℃ for gallium nitride, and 200-500℃ for silicon carbide).

[0083] If Δρ < -10% (initial resistivity is too low) and Δn < -10% (initial carrier concentration is too high):

[0084] P0 = P base ×(1-Δρ×0.01), T0=T base ×(1+Δn×0.02)

[0085] If Δρ and Δn are within ±10%:

[0086] P0 = P_base, T0 = T_base

[0087] Boundary verification: Ensure that P0 ≤ 80% of the material's ultimate compressive strength (e.g., for silicon, 4 GPa, P0 ≤ 3.2 GPa) and T0 ≤ 70% of the material's thermal decomposition temperature (e.g., for gallium nitride, 1050℃, T0 ≤ 735℃) to avoid material damage caused by excessively high initial parameters.

[0088] S33, Contact pressure adaptive control.

[0089] Adjust the probe position of the electrical performance detection module to make the probe contact the sample surface; the data processing module sets the contact pressure threshold, and the miniature pressure sensor provides real-time feedback on the contact pressure; if the actual pressure is lower than the threshold, drive the sample fixing module (accuracy ±1μm) to increase the pressure; if it is higher than the threshold, fine-tune in the opposite direction until the contact pressure stabilizes within the threshold range and the contact resistance is <0.5Ω (fluctuation ±0.05Ω); monitor continuously for 3 minutes to ensure that the contact state is stable before proceeding to the next step of control.

[0090] In this embodiment, the target resistivity ρ target = 1 - 1.5 Ω·cm, target n target =2.5×10 15 -3×10 15 cm -3 .

[0091] Lattice alignment: Initial lattice orientation deviation angle θ = 1.2°, after micro-displacement component adjustment θ = 0.3°, Raman detection characteristic peak shift difference = 0.15cm. -1 .

[0092] Parameter correction:

[0093] Δρ=(2.8-1.25) / 1.25×100%=124%

[0094] Δn=(2.75×10 15 -1.8×10 15 ) / 2.75×10 15 ×100%=34.5%

[0095] P base =2GPa

[0096] T base =200℃

[0097] P0=2×(1-124%×0.02)=1.504GPa

[0098] T0=200×(1+34.5%×0.03)=202.07℃

[0099] Contact pressure control: The set threshold is 0.4N. After adjustment, the pressure stabilizes at 0.4±0.02N, and the contact resistance is 0.35Ω.

[0100] S4. Increase temperature and pressure to the corrected initial temperature and pressure, stabilize, and monitor electrical performance and contact pressure in real time. Adjust parameters to meet the standards and stabilize for 30-60 minutes.

[0101] The high-pressure generation module is activated, and the pressure is slowly increased to the corrected initial pressure P0 at a rate of 0.01-0.1 GPa / min. During the process, the data processing module receives the orientation data of the micro-displacement orientation adjustment component in real time. If the pressure loading causes θ to be greater than 1°, the pressure increase is automatically paused and the sample angle is finely adjusted to ensure alignment accuracy.

[0102] The temperature control module is activated, and the temperature is increased to the corrected initial temperature T0 at a rate of 5-20℃ / min. During the heating process, the rate is optimized based on the initial resistivity ρ0: if ρ0 > 2ρ target The heating rate is increased to 15-20℃ / min to accelerate carrier activation; if ρ0 < 0.8ρ target The heating rate was reduced to 5-10℃ / min to avoid over-excitation of charge carriers.

[0103] Once the pressure and temperature reach the initial set values, maintain the coupling field stable for 10-30 minutes to allow the internal structure of the sample to reach equilibrium.

[0104] The electrical performance parameters of the sample are detected in real time by the electrical performance detection module at a frequency of 1-5 minutes / time. At the same time, the miniature pressure sensor continuously monitors the contact pressure (automatically adjusting when the fluctuation exceeds ±0.1N). The detection data is transmitted to the data processing and feedback module in real time.

[0105] The data processing and feedback module compares the detected electrical performance parameters with the target parameters in real time:

[0106] If the real-time resistivity is higher than the target resistivity and the carrier concentration is lower than the target carrier concentration, under the premise that the pressure does not exceed the material's ultimate compressive strength and the temperature does not exceed the material's thermal decomposition temperature, increase the pressure by 0.05-0.2 GPa or increase the temperature by 10-30℃ until the resistivity and carrier concentration reach the target range.

[0107] If the real-time carrier mobility is lower than the target mobility and the resistivity is higher than the target resistivity, reduce the pressure by 0.05-0.1 GPa or the temperature by 5-15 °C to reduce the lattice distortion's obstruction of carrier transport until the mobility and resistivity reach the target range.

[0108] If the real-time electrical performance parameters fluctuate within the target range, maintain the current pressure and temperature parameters and monitor continuously for 30-60 minutes to ensure performance stability.

[0109] In this embodiment, the pressure was increased to 1.504 GPa at 0.1 GPa / min (θ maintained at 0.3°), the temperature was increased to 202.07°C at 15°C / min, and after stabilizing for 20 minutes, the following values ​​were measured: ρ = 2.1 Ω·cm, n = 2.1 × 10⁻⁶. 15 cm -3 Increase P to 2.0 GPa and T to 245 °C. After 25 minutes, ρ = 1.2 Ω·cm and n = 2.8 × 10⁻⁶. 15 cm -3 To reach the target range.

[0110] S5. Reduce the pressure to ambient pressure and record the residual deviation angle θ' of the crystal orientation. Reduce the temperature to room temperature and perform surface cleaning and electrical performance retesting on the sample.

[0111] Once the electrical performance parameters of the sample have stabilized at the target value and remained stable for more than 30 minutes, the coupling field is stopped: first, the pressure is reduced to ambient pressure at a rate of 0.05-0.2 GPa / min, and the lattice orientation deviation angle θ' is recorded during the process (as a reference for the next adjustment); then the temperature is reduced to room temperature at a rate of 10-30℃ / min.

[0112] After the temperature drops to room temperature, the sample is removed from the sample fixing module and the sample is cleaned and its electrical properties are re-inspected: the uniformity of electrical properties over the entire area (error ≤2% is acceptable) and lattice integrity (retention rate ≥95%) are tested; the repeatability error of the "orientation aligned group" and the "orientation misaligned group" is compared (aligned group ≤3%, misaligned group ≥8%) to ensure that the control effect meets the requirements.

[0113] In this embodiment, the pressure was reduced to atmospheric pressure at 0.1 GPa / min and the temperature was reduced to room temperature at 15℃ / min; the retest showed that ρ = 1.18 Ω·cm, lattice integrity retention rate = 98%, global performance uniformity error = 1.2%, and repeatability error = 2.5%, which meets the requirements for single-crystal silicon for integrated circuits.

[0114] Example 2

[0115] In this embodiment, the semiconductor material selected is a gallium nitride epitaxial wafer grown on a sapphire substrate. <0001> Orientation (2 μm thickness), cut into 8 mm × 8 mm samples, ultrasonically cleaned with deionized water for 8 minutes, ultrasonically cleaned with ethanol for 8 minutes, and vacuum dried at 60 °C for 2 hours; Initial characterization: lattice orientation <0001> , ρ0=0.9Ω·cm, μ0=1200cm 2 / (V·s), create individual profiles.

[0116] A high-pressure-temperature coupled field control device was constructed using multiple Anvils high-pressure units (0-10 GPa), a laser heating system (100-700℃), and a Hall effect tester with a pressure sensor. The target μ target =1500-1600cm 2 / (V·s), target ρ target =0.5-0.6Ω·cm.

[0117] Lattice alignment: The initial lattice orientation deviation angle θ = 0.8°, after adjustment θ = 0.4°, and the Raman detection characteristic peak shift difference = 0.2cm. -1 .

[0118] Parameter correction:

[0119] Δμ=(1550-1200) / 1550×100%=22.58%

[0120] Δρ=(0.9-0.55) / 0.55×100%=63.64%

[0121] P base =3GPa

[0122] T base =300℃

[0123] P0=3×(1+22.58%×0.01)=3.068GPa

[0124] T0=300×(1-22.58%×0.015)=293.16℃

[0125] Contact pressure control: The set threshold is 0.6N. After adjustment, the pressure stabilizes at 0.6±0.03N, and the contact resistance is 0.4Ω.

[0126] The pressure was increased to 3.068 GPa at a rate of 0.05 GPa / min, the temperature was increased to 293.16℃ at a rate of 10℃ / min, and after stabilizing for 15 minutes, the result was measured: μ = 1380 cm⁻¹. 2 / (V·s), ρ=0.7Ω·cm; decrease P to 2.8GPa, T to 280℃, after 22 minutes μ=1560cm 2 / (V·s), ρ=0.55Ω·cm, reaching the target range.

[0127] After the regulation is completed, a retest is performed: the pressure is reduced to atmospheric pressure at a rate of 0.05 GPa / min, and the temperature is reduced to room temperature at a rate of 10℃ / min; the retest shows μ = 1540 cm⁻¹. 2 / (V·s), lattice integrity retention rate = 97%, global performance uniformity error = 1.5%, repeatability error = 2.8%, meeting the requirements of gallium nitride-based high-frequency devices.

[0128] Therefore, the present invention employs the above-mentioned method for regulating the electrical properties of semiconductor materials under a high-voltage-temperature coupled field. By combining the high-voltage-temperature coupled field with real-time feedback, it is possible to achieve precise, stable, and non-destructive regulation of the electrical properties of semiconductor materials.

[0129] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit them. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the technical solutions of the present invention, and these modifications or equivalent substitutions cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A method for controlling the electrical properties of semiconductor materials under a high-voltage-temperature coupled field, characterized in that, Includes the following steps: S1. Cut and clean the semiconductor material, and establish an individual profile of "lattice orientation-initial electrical properties"; In S1, specifically: select the semiconductor material to be regulated and cut it into sheet samples with dimensions of 5mm×5mm×0.1mm-20mm×20mm×1mm to ensure that the sample surface is free of defects; when cleaning the sample, use deionized water, ethanol, and acetone for ultrasonic cleaning in sequence, with each cleaning time being 5-15 minutes to remove oil and impurities from the sample surface; after cleaning, place the sample in a vacuum drying oven and dry it at a temperature of 60-100℃ for 2-4 hours to avoid moisture affecting the subsequent regulation process; The crystal lattice orientation of the sample was detected using a polarized light microscope. The initial electrical properties at room temperature were measured using a Hall effect tester, and the initial resistivity ρ0 and initial carrier concentration n0 were recorded; an individual profile of "lattice orientation-initial electrical properties" was established. S2. Construct a high-pressure-temperature coupled field control device; In S2, the high-voltage-temperature coupled field control device includes a high-voltage generation module, a temperature control module, an electrical performance testing module, a sample fixation module, and a data processing and feedback module; the data processing and feedback module is electrically connected to the high-voltage generation module, the temperature control module, the electrical performance testing module, and the sample fixation module. The high-pressure generating module uses a diamond anvil high-pressure device or a multi-anvils high-pressure device to provide a controllable pressure of 0-10 GPa with a pressure control accuracy of ±0.01 GPa. The temperature control module adopts a surround resistance heating furnace or a laser heating system, with a heating range of -196℃ to 800℃, a temperature control accuracy of ±1℃, and a temperature field uniformity error of no more than ±2℃ in the sample area. The electrical performance testing module uses a four-probe tester or a Hall effect tester to detect the resistivity, carrier concentration, and carrier mobility of the sample in real time; a miniature pressure sensor is integrated at the probe tip to monitor the contact pressure in real time. The sample fixation module is made of high-temperature and high-pressure resistant alumina ceramic material, integrating micro-displacement orientation adjustment components and contact pressure buffer layer to achieve lattice orientation alignment and contact pressure stability; the micro-displacement orientation adjustment components include X / Y / Z triaxial adjustment platforms and are matched with corresponding rotation adjustment units, and the contact pressure buffer layer is a 20-50μm thick nickel-based elastic film; S3. Install the semiconductor sample and perform dynamic correction calculations for initial parameters, and adaptively control the contact pressure; In S3, the semiconductor sample installation process is as follows: the pre-treated sample is placed on the contact pressure buffer layer of the sample fixing module, and the polarization positioning system is activated: the lattice orientation data is retrieved from the sample individual file, and the pressure loading direction of the high-pressure generating module is compared to calculate the initial lattice orientation deviation angle θ; if θ > 0.5°, the data processing module drives the rotation adjustment unit of the micro-displacement orientation adjustment component to fine-tune the sample position until θ ≤ 0.5°; the alignment effect is verified by Raman spectroscopy to ensure that the pressure loading direction is consistent with the optimal transport direction of charge carriers and to eliminate lattice anisotropy interference; In S3, the dynamic correction calculation of initial parameters is performed as follows: The data processing and feedback module imports the individual profile of the sample's initial electrical properties and the target performance parameters, and dynamically corrects the initial pressure P0 and initial temperature T0 according to the following logic: Calculate the initial performance deviation: ； ； in, ρ is the initial resistivity deviation, ρ target For the target resistivity, n is the initial carrier concentration deviation, n target The target carrier concentration; Parameter correction rules: If Δρ > 15% and Δn > 15%: P0=P base ×(1-Δρ×0.02),T0=T base ×(1+Δn×0.03); Among them, P base T is the initial pressure of the material base. base The initial temperature of the material base; If Δρ < -10% and Δn < -10%: P0=P base ×(1-Δρ×0.01),T0=T base ×(1+Δn×0.02); If Δρ and Δn are within ±10%: P0=P base ,T0=T base ; Boundary check: Ensure that P0 ≤ 80% of the material's ultimate compressive strength and T0 ≤ 70% of the material's thermal decomposition temperature to avoid material damage caused by excessively high initial parameters; In S3, the adaptive control of contact pressure is specifically as follows: the probe position of the electrical performance detection module is adjusted to make the probe contact the sample surface; the data processing module sets the contact pressure threshold, and the miniature pressure sensor provides real-time feedback on the contact pressure; if the actual pressure is lower than the threshold, the sample fixing module is driven to increase the pressure; if it is higher than the threshold, it is finely adjusted in the opposite direction until the contact pressure stabilizes within the threshold range and the contact resistance is <0.5Ω; after continuous monitoring for 3 minutes to ensure that the contact state is stable, the next step of regulation is performed. S4. Increase the temperature and pressure to the corrected initial temperature and pressure, and after stabilization, monitor the electrical performance and contact pressure in real time. Adjust the parameters to meet the standards and stabilize for 30-60 minutes. In S4, specifically: The high-pressure generation module is started, and the pressure is slowly increased to the corrected initial pressure P0 at a rate of 0.01-0.1 GPa / min. During the process, the data processing module receives the orientation data of the micro-displacement orientation adjustment component in real time. If θ > 1° due to pressure loading, the pressure increase is automatically paused and the sample angle is finely adjusted to ensure alignment accuracy. The temperature control module is activated, and the temperature is increased to the corrected initial temperature T0 at a rate of 5-20℃ / min. During the heating process, the rate is optimized based on the initial resistivity ρ0: if ρ0 > 2ρ target The heating rate is increased to 15-20℃ / min to accelerate carrier activation; if ρ0 < 0.8ρ target The heating rate was reduced to 5-10℃ / min to avoid over-excitation of charge carriers; Once the pressure and temperature reach the initial set values, maintain the coupling field stable for 10-30 minutes to allow the internal structure of the sample to reach equilibrium. The electrical performance parameters of the sample are detected in real time through the electrical performance detection module at a frequency of 1-5 minutes / time. At the same time, the miniature pressure sensor continuously monitors the contact pressure, and the detection data is transmitted to the data processing and feedback module in real time. The data processing and feedback module compares the detected electrical performance parameters with the target parameters in real time; S5. Reduce the pressure to ambient pressure and record the residual deviation angle θ' of the crystal orientation. Reduce the temperature to room temperature and perform surface cleaning and electrical performance retesting on the sample.

2. The method for controlling the electrical properties of semiconductor materials under a high-voltage-temperature coupled field according to claim 1, characterized in that: When comparing the real-time detected electrical performance parameters with the target parameters, if the real-time resistivity is higher than the target resistivity and the carrier concentration is lower than the target carrier concentration, the pressure is increased by 0.05-0.2 GPa or the temperature is increased by 10-30℃, provided that the pressure does not exceed the material's ultimate compressive strength and the temperature does not exceed the material's thermal decomposition temperature, until the resistivity and carrier concentration reach the target range. If the real-time carrier mobility is lower than the target mobility and the resistivity is higher than the target resistivity, the pressure is decreased by 0.05-0.1 GPa or the temperature is decreased by 5-15℃ to reduce the lattice distortion's obstruction of carrier transport until the mobility and resistivity reach the target range. If the real-time electrical performance parameters fluctuate within the target range, the current pressure and temperature parameters are maintained, and monitoring continues for 30-60 minutes to ensure performance stability.

3. The method for controlling the electrical properties of semiconductor materials under a high-voltage-temperature coupled field according to claim 1, characterized in that: In S5, specifically: after the electrical performance parameters of the sample have stabilized at the target value and remained stable for more than 30 minutes, the coupling field is stopped: first, the pressure is reduced to ambient pressure at a rate of 0.05-0.2 GPa / min, and the residual deviation angle of the crystal orientation θ' is recorded during the process; then the temperature is reduced to room temperature at a rate of 10-30℃ / min. After the temperature drops to room temperature, the sample is removed from the sample fixing module and its surface is cleaned and its electrical properties are re-inspected: the uniformity of electrical properties and lattice integrity are tested in detail, and the repeatability error of the "orientation aligned group" and the "orientation misaligned group" is compared to ensure that the control effect meets the requirements.

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