Process for controlling evaporation rate of antimony source

Abstract

The invention belongs to the technical field of metal evaporators for night-vision devices, particularly relates to a process for controlling the evaporation rate of an antimony source, and aims to solve the problems that the quality of a final product is affected due to the fact that the antimony source is always unevenly distributed in the evaporation process in an existing traditional evaporation method, and the physical characteristics (such as granularity and distribution) of antimony powder are difficult to accurately regulate and control. In order to solve the problem that the stability and controllability of the evaporation rate are influenced by the fact that the heat conduction efficiency and the surface area in the evaporation process cannot reach the optimum due to the fact that the heat conduction efficiency and the surface area cannot reach the optimum in the prior art, the invention provides the following scheme: the method comprises the following steps: S1, selecting an antimony raw material, and pretreating the antimony raw material; s2, the pretreated antimony raw material is subjected to powder mixing, and the antimony powder distribution narrowness is optimized; s3, tungsten powder is added into the antimony powder, and mixing is conducted; according to the method, the evaporation rate can be accurately regulated and controlled, the tungsten powder diluent is innovatively introduced, the predictability and repeatability of the evaporation process are improved, and the film preparation quality and efficiency are improved.

Description

Technical Field

[0001] The invention relates to the technical field of metal evaporators for night vision devices, and in particular to a process for controlling the evaporation rate of an antimony source. Background Art

[0002] Night vision technology, as an optoelectronic technology that uses optoelectronic imaging devices to achieve nighttime observation, plays a vital role in modern security, scientific research and other fields. Its basic principle is to capture weak optical images at night or under low illumination, and convert these images into enhanced optical images or electronic images with the help of image intensifiers or camera devices, so as to achieve nighttime observation. Low-light-level night vision devices, as one of the important applications of night vision technology, use natural night sky light (such as weak moonlight, starlight, atmospheric glow, galaxy light, etc.) as the illumination source, and use image intensifiers to amplify and convert weak photons reflected from the target into visible images. In the manufacturing process of low-light-level night vision devices, antimony source evaporation technology occupies a pivotal position. However, the traditional antimony source evaporation process faces many challenges.

[0003] In the prior art, traditional evaporation methods often lead to uneven distribution of the antimony source during the evaporation process, thus affecting the quality of the final product. In addition, the physical properties of antimony powder (such as particle size, distribution, etc.) are difficult to precisely control, resulting in the failure to achieve optimal heat conduction efficiency and surface area during the evaporation process, which in turn affects the stability and controllability of the evaporation rate. To this end, we proposed a process for controlling the evaporation rate of the antimony source to solve the above problems. Summary of the invention

[0004] The purpose of the present invention is to solve the problems in the prior art that traditional evaporation methods often lead to uneven distribution of antimony source during the evaporation process, thereby affecting the quality of the final product, and the physical properties of antimony powder (such as particle size, distribution, etc.) are difficult to accurately control, resulting in the failure to achieve optimal heat conduction efficiency and surface area during the evaporation process, thereby affecting the stability and controllability of the evaporation rate, and a process for controlling the evaporation rate of the antimony source is proposed.

[0005] The present application provides a process for controlling the evaporation rate of an antimony source using the following technical solution:

[0006] A process for controlling the evaporation rate of an antimony source comprises the following steps:

[0007] S1: Selecting antimony raw materials and pre-treating the antimony raw materials;

[0008] S2: Powder adjustment of the pretreated antimony raw materials and optimization of the distribution narrowness of the antimony powder;

[0009] S3: adding tungsten powder to antimony powder and mixing;

[0010] S4: Make the processed antimony powder into antimony pellets;

[0011] S5: Select a mold and fabricate an evaporator;

[0012] S6: Treat the inner wall surface of the evaporator;

[0013] S7: Evaporate the antimony pellets inside the evaporation tube.

[0014] Further, in S1, purchase antimony raw materials with a purity of 7N, ball-mill the antimony raw materials using a ball mill for 180 minutes, keep the inside of the ball mill tank under vacuum throughout the ball-milling process, and perform laser particle size analysis on the obtained antimony powder after the ball-milling ends;

[0015] Particle size detection and adjustment: After the ball-milling is completed, use a laser particle size analyzer to detect the particle size of the antimony powder to ensure that the particle size of the antimony powder meets the predetermined requirements. The model of the laser particle size analyzer is Omec LS-609, and the test parameters are: automatic wet sampling, imported helium-argon laser, scanning frequency of 1 kHz, light obscuration rate between 10% and 20%, and take the average value of three measurements. If it does not meet the requirements, adjust the ball-milling parameters or perform re-ball-milling until the predetermined particle size is reached.

[0016] Further, in S2, put the ball-milled antimony powder into a vibrating sieve for screening treatment. The mesh number of the sieve is 650 - 1200 meshes, and through the filtering action of the sieve, the antimony powder is separated into powders of different particle size levels;

[0017] Particle size detection: After the screening ends, use a laser particle size analyzer to detect the particle size of the antimony powder to determine whether it meets the requirements. The model of the laser particle size analyzer is Omec LS-609, and the test parameters are: automatic wet sampling, imported helium-argon laser, scanning frequency of 1 kHz, light obscuration rate between 10% and 20%, and take the average value of three measurements. The particle size distribution of the antimony powder that meets the requirements is: D50 is 17 (±1) μm, D10 > 5 μm, D90 < 34 μm.

[0018] Further, in S2, perform laser particle size analysis on the antimony powder using a laser particle size analyzer to determine whether it reaches the particle size required for the subsequent evaporation process. If a narrower particle size distribution is needed, perform multiple screening and classification treatments.

[0019] Further, in S3, mix tungsten powder and antimony powder in a mass ratio of 3:97 to 5:95 through a three-dimensional motion mixer for about 90 minutes.

[0020] Further, in S4, the mixed powder of antimony and tungsten is weighed by an analytical balance, the molding die is assembled, the weighed powder is put into the feeding ports of the four dies, the punch is put into the feeding port containing the powder, and the powder is pressed with uniform and stable pressure to form hemispherical cylindrical antimony pellets. Finally, the upper and lower parts of the die are separated and the pressed antimony pellets are taken out.

[0021] Further, in S5, a circular tube single-side flattening die is selected, and the circular tube of the evaporator housing is put into the die. The round hole in the upper part of the evaporator is aligned with the positioning protrusion on the die, and then the upper and lower dies are closed and placed in a hydraulic press for extrusion processing, so that one side of the circular tube wall is slightly flattened.

[0022] Further, in S5, the antimony source is respectively put into the evaporator housing from both sides of the circular tube, then the evaporator is put into the die, the round hole is also aligned with the positioning protrusion, and the antimony source is pushed to the designated position by using a positioning pin. Then the positioning pin is removed, the upper and lower dies are closed and placed in a hydraulic press for pressing.

[0023] Further, in S6, the active particles in the plasma react with the inner wall surface of the evaporation tube to remove the grease and oxide layer pollutants on the surface. The inner wall of the evaporation tube is bombarded by a high-energy ion beam, and the parameters of the bombardment are precisely controlled to remove the surface impurities and defects and change the surface microstructure.

[0024] Further, in S7, the heating temperature of the evaporation furnace is set to 200 °C and the vacuum degree is 10-7 Pa. The temperature is controlled by current and the evaporation rate is controlled by temperature. During the evaporation process, the deposition thickness and deposition rate of the thin film are obtained by measuring the frequency change of the crystal oscillator before and after evaporation. The change of the evaporation rate can be monitored in real time by measuring the thin film deposition rate.

[0025] In summary, the present application includes at least one of the following beneficial technical effects:

[0026] 1. By adjusting the particle size distribution of the antimony powder and adding tungsten powder, this solution realizes the fine regulation of the evaporation rate, thereby improving the quality and efficiency of thin film preparation;

[0027] 2. The antimony source evaporation material of this solution not only has excellent evaporation performance, but also has good stability and reliability, and can meet the requirements of various high-performance material preparation and process applications.

[0028] The present invention can accurately control the evaporation rate, innovatively introduce tungsten powder diluent, improve the predictability and repeatability of the evaporation process, and improve the quality and efficiency of thin film preparation. Description of the Drawings

[0029] Figure 1 is a flowchart of a process for controlling the evaporation rate of an antimony source proposed by the present invention;

[0030] Figure 2 Flow chart of S2 of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0031] Figure 3 Flow chart of S4 of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0032] Figure 4 Flow chart of S5 of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0033] Figure 5 Flow chart of S6 of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0034] Figure 6 Particle size distribution diagram of the screened antimony powder of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0035] Figure 7 Particle size distribution diagram of the tungsten powder of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0036] Figure 8 Schematic diagram of the made antimony pellets of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0037] Figure 9 Schematic diagram of the made antimony source evaporator of a process for controlling the evaporation rate of antimony source proposed by the present invention;

[0038] Figure 10 Evaporation current comparison diagram of the pure antimony source evaporator and the antimony source evaporator added with tungsten of a process for controlling the evaporation rate of antimony source proposed by the present invention. Detailed implementation manners

[0039] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments.

[0040] Embodiment 1

[0041] Refer to Figures 1 - 10 , a process for controlling the evaporation rate of antimony source, comprising the following steps:

[0042] S1: Select antimony raw materials and perform pretreatment on the antimony raw materials;

[0043] S2: Adjust the powder of the pretreated antimony raw materials and optimize the narrowness of the antimony powder distribution;

[0044] S3: Add tungsten powder to the antimony powder and mix them;

[0045] S4: Make the processed antimony powder into antimony pellets.

[0046] S5: Select a mold and fabricate an evaporator.

[0047] S6: Treat the inner wall surface of the evaporator.

[0048] S7: Evaporate the antimony pellets in the evaporation tube.

[0049] In this embodiment, in S1, purchase antimony raw materials with a purity of 7N, ball-mill the antimony raw materials with a ball mill, the ball-milling time is 180 min, keep the inside of the ball mill tank vacuum during the ball-milling process, and perform laser particle size analysis on the obtained antimony powder after the ball-milling is completed, so as to obtain antimony powder that meets the particle size requirements for sieving powder. Select a high-efficiency and energy-saving ball mill as the ball-milling equipment to ensure the stability and uniformity during the ball-milling process.

[0050] Ball-milling medium and parameter settings: The ball mill tank is made of stainless steel, the inner liner is zirconia, with a volume of 1000 mL. The grinding balls are made of zirconia. Select 200 grinding balls with a diameter of 6 mm, 100 grinding balls with a diameter of 10 mm, and 10 grinding balls with a diameter of 20 mm. The total mass of the grinding balls is about 700 g.

[0051] Ball-milling process: Feed the coarser pure antimony metal blocks into the ball mill for ball-milling treatment. Through the impact and friction of the ball-milling medium, break and refine the antimony metal blocks into powders with a particle size that meets the requirements.

[0052] The ball-milling process is as follows: Rotate forward at a speed of 160 r / min for 30 min and then stop for 2 min, then rotate backward at a speed of 160 r / min for 30 min and then stop for 2 min. Repeat this cycle 3 times, for a total of 192 min. Keep the inside of the ball mill tank vacuum during the ball-milling process.

[0053] Particle size detection and adjustment: After the ball-milling is completed, use a laser particle size analyzer to detect the particle size of the antimony powder to ensure that the particle size of the antimony powder meets the predetermined requirements. The model of the laser particle size analyzer is Omec LS-609, and the test parameters are: automatic wet sample injection, imported helium-argon laser, scanning frequency 1 kHz, light obscuration rate between 10% and 20%, and take the average value of three measurements. If it does not meet the requirements, adjust the ball-milling parameters or perform re-ball-milling until the predetermined particle size is reached.

[0054] In this embodiment, in S2, the ball-milled antimony powder is put into a vibrating sieve for screening. The mesh number of the sieve is 650 - 1200 meshes. Through the filtering effect of the sieve, the antimony powder is separated into powders of different particle size grades. The antimony powder is subjected to laser particle size analysis by a laser particle size analyzer to judge whether it reaches the particle size required for the subsequent evaporation process. If a narrower particle size distribution is needed, through multiple screening and classification processes, the particle size distribution range is further narrowed. The particle size and the narrowness of the particle size distribution of the antimony powder are precisely adjusted to control the evaporation rate. This adjustment aims to ensure that the heat conduction efficiency and surface area during the evaporation process reach the optimum, so as to achieve precise control of the evaporation rate. According to the target evaporation rate, the particle size range of the antimony powder is selectively adjusted so that the median particle size of the antimony powder is about 17 microns. This step is achieved through the screening of the vibrating sieve and particle size analysis technology to ensure the consistency of the particle size of the antimony powder. An efficient and precise screening device, such as a vibrating sieve, is selected to ensure the stability and accuracy during the screening process;

[0055] Particle size detection: After screening, use a laser particle size analyzer to detect the particle size of the antimony powder to judge whether it meets the requirements. The model of the laser particle size analyzer is Omec LS-609. The test parameters are: automatic wet sampling, imported helium-argon laser, scanning frequency 1 kHz, light obscuration rate between 10% - 20%, and take the average value of three measurements. The particle size distribution of the antimony powder that meets the requirements is: D50 is 17(±1)μm, D10 > 5μm, D90 < 34μm.

[0056] In this embodiment, in S3, the tungsten powder is dried to remove the moisture and impurities in it. The tungsten powder and the antimony powder are mixed at a mass ratio of 3:97 to 5:95. The particle size of the tungsten powder is less than 50% of the particle size of the antimony powder. The mixture is processed by a three-dimensional motion mixer for about 90 minutes, so that the tungsten powder is evenly dispersed in the antimony powder. Due to its high thermal stability and chemical inertness, the tungsten powder can remain stable during the evaporation process. At the same time, its small particle size and uniform distribution can slow down the evaporation rate of the antimony powder, making the evaporation rate more stable. The addition of the tungsten powder not only improves the controllability of the evaporation rate, but also enhances the predictability and repeatability of the evaporation process. After mixing, the mixture is sampled and detected to ensure that the distribution of the tungsten powder in the antimony powder is uniform and the content meets the predetermined requirements.

[0057] In this embodiment, in S4, weigh the mixed powder of antimony and tungsten by an analytical balance, assemble the forming die, put the weighed powder into the feeding ports of the four dies, put the punch into the feeding port containing the powder, press the powder with uniform and stable pressure to form hemispherical cylindrical antimony pellets, and finally separate the upper and lower parts of the die and take out the pressed antimony pellets. The entire operation process needs to keep the working environment clean and avoid impurities from mixing into the mixed powder.

[0058] In this embodiment, in S5, a circular tube single-side flattening die is selected, and the circular tube of the evaporator housing is placed in the die. The round holes in the upper part of the evaporator are aligned with the positioning protrusions on the die. Then, the upper and lower dies are closed and placed in a hydraulic press for extrusion processing, so that one side of the circular tube wall is slightly flattened. The purpose is to reduce the movement of the antimony source inside the circular tube and prevent the antimony source from rolling to one side and causing antimony leakage. The antimony source is respectively placed into the evaporator housing from both sides of the circular tube, and then the evaporator is placed in the die. The round holes are also aligned with the positioning protrusions, and a positioning needle is used to push the antimony source to the designated position. Then, the positioning needle is removed, the upper and lower dies are closed and placed in the hydraulic press for pressing. After this pressing, both ends of the evaporator will be pressed into flat electrodes, and the evaporator is thus manufactured. This not only facilitates subsequent welding and use, but also improves the overall structural strength of the evaporator. The material of the evaporator is selected from metals or alloys with high melting points and high electrothermal efficiency, such as nickel-chromium alloy. The evaporator is formed by pressing a seamless tube with a thickness of 24 μm and a hole diameter of 1.8 mm. Its shape and size can be optimized according to the specific requirements of the evaporation equipment to improve the evaporation efficiency and product quality.

[0059] In this embodiment, in S6, the active particles in the plasma react with the inner wall surface of the evaporation tube to remove the grease and oxide layer pollutants on the surface and improve the surface activity.

[0060] The specific process of plasma cleaning is as follows:

[0061] Pretreatment: Place the evaporation tube in the vacuum chamber of the plasma cleaner to ensure that its surface is clean and there are no obvious pollutants.

[0062] Vacuum pumping: Start the vacuum pump to reduce the pressure in the chamber to the base pressure, generally set between 20 Pa and 60 Pa.

[0063] Filling process gas: Select a suitable process gas according to needs, such as argon (Ar) or oxygen (O2), and adjust the gas flow through a mass flow controller (MFC), usually in the range of 10 sccm to 100 sccm.

[0064] Exciting plasma: Turn on the radio frequency power supply and apply a certain voltage (generally between several hundred volts and several thousand volts) to ionize the gas in the chamber to form plasma.

[0065] Cleaning process: The high-energy particles (ions, electrons, free radicals, etc.) in the plasma react with the inner wall surface of the evaporation tube physically and chemically to remove the surface pollutants and microparticles. The cleaning time is generally between several minutes and dozens of minutes, and the specific time is determined according to the material and degree of pollution.

[0066] End of cleaning: Turn off the radio frequency power supply, stop the gas supply, and let the plasma extinguish naturally. Then, slowly release the vacuum in the chamber and take out the evaporation tube.

[0067] The inner wall of the evaporation tube is bombarded with a high-energy ion beam, and the parameters of the bombardment are precisely controlled to remove surface impurities and defects, change the surface microstructure, and improve its wettability and reactivity;

[0068] The specific process of ion beam bombardment is as follows:

[0069] Pretreatment: Fix the evaporation tube on the workpiece table of the ion beam bombardment equipment to ensure its accurate and stable position;

[0070] Vacuum pumping: Start the vacuum system to reduce the pressure in the vacuum chamber to 6×10 - 3 Pa or lower;

[0071] Adjust the gas flow rate: Fill in a certain proportion of argon (Ar) or other auxiliary gases (such as oxygen) as needed, and adjust the gas flow rate to keep the pressure in the vacuum chamber between 1×10 - 2 - 6×10 - 2 Pa;

[0072] Start the ion source: Turn on the various power supplies of the ion source to generate an ion beam with a certain energy and density;

[0073] Bombardment process: After the ion beam is neutralized by the electrons emitted by the neutralizer, it passes through the shutter and the aperture hole to bombard the inner wall surface of the evaporation tube, removing surface impurities and defects;

[0074] Control the bombardment time: Set an appropriate bombardment time according to the material and size of the evaporation tube, as well as the required surface treatment effect, generally between several minutes and dozens of minutes;

[0075] End the bombardment: Turn off the ion source and related power supplies, stop the gas supply, slowly release the vacuum in the vacuum chamber, and take out the evaporation tube.

[0076] In this embodiment, in S7, the heating temperature of the evaporation furnace is set to 200°C, the vacuum degree is 10-7 Pa, the temperature is controlled by current, and the evaporation rate is controlled by temperature. Before evaporation, the uniformly mixed antimony powder and tungsten powder are preheated to remove adsorbed moisture and gas, reduce pollution and fluctuations during evaporation. During evaporation, the deposition thickness and deposition rate of the thin film are obtained by measuring the frequency change of the crystal oscillator before and after evaporation. By measuring the thin film deposition rate, the change of the evaporation rate can be monitored in real time. In addition, the film thickness gauge can detect the deposition rate and thickness of the thin film in real time, ensuring the uniformity and consistency of evaporation, thereby judging the stability of the evaporation rate. If the evaporation rate does not meet the requirements, it is adjusted by adjusting the heating power, temperature control parameters, etc.

[0077] Example Two

[0078] The difference between this embodiment and the first embodiment is as follows:

[0079] A process for controlling the evaporation rate of the antimony source includes the following steps:

[0080] S1: Select the antimony raw material and perform pretreatment on the antimony raw material;

[0081] S2: Adjust the powder of the pretreated antimony raw material and optimize the narrowness of the antimony powder distribution;

[0082] S3: Add tungsten powder to the antimony powder and mix them;

[0083] S4: Make the treated antimony powder into antimony pellets;

[0084] S5: Select a mold and fabricate an evaporator;

[0085] S6: Treat the inner wall surface of the evaporator and modify the inner wall surface of the evaporator;

[0086] S7: Evaporate the antimony pellets in the evaporation tube.

[0087] In this embodiment, in S6, the active particles in the plasma react with the inner wall surface of the evaporation tube to remove the grease and oxide layer pollutants on the surface, improve the surface activity. The inner wall of the evaporation tube is bombarded by high-energy ion beams, and the parameters of the bombardment are precisely controlled to remove the surface impurities and defects, change the surface microstructure, improve its wettability and reactivity. After treating the inner wall surface of the evaporator, the inner wall of the evaporation tube is further subjected to surface modification treatment. A coating with specific functions is formed on the inner wall surface by electroless plating or physical vapor deposition (PVD) technology to enhance the high-temperature resistance, corrosion resistance or oxidation resistance of the inner wall, thereby extending the service life of the evaporation tube and improving the stability of the evaporation process and the product quality

[0088] Embodiment Three

[0089] The difference between this embodiment and the first embodiment is as follows:

[0090] A process for controlling the evaporation rate of the antimony source includes the following steps:

[0091] S1: Select the antimony raw material and perform pretreatment on the antimony raw material;

[0092] S2: Adjust the powder of the pretreated antimony raw material and optimize the narrowness of the antimony powder distribution;

[0093] S3: Add tungsten powder to the antimony powder and mix them;

[0094] S4: Make the treated antimony powder into antimony pellets;

[0095] S5: Select a mold and fabricate an evaporator;

[0096] S6: Treat the inner wall surface of the evaporator.

[0097] S7: Evaporate the antimony pellets in the evaporation tube and optimize the evaporation environment.

[0098] In this embodiment, in S7, the heating temperature of the evaporation furnace is set to 200 °C, and the vacuum degree is 10-7 Pa. The temperature is controlled by current, and the evaporation rate is controlled by temperature. Before evaporation, the uniformly mixed antimony powder and tungsten powder are preheated to remove adsorbed moisture and gas, reducing pollution and fluctuations during the evaporation process. During the evaporation process, the deposition thickness and deposition rate of the thin film are obtained by measuring the frequency change of the crystal oscillator before and after evaporation. By measuring the thin film deposition rate, the change of the evaporation rate can be monitored in real time. In addition, the film thickness gauge can detect the deposition rate and thickness of the thin film in real time, ensuring the uniformity and consistency of evaporation, thereby judging the stability of the evaporation rate. If the evaporation rate does not meet the requirements, it is adjusted by adjusting the heating power, temperature control parameters, etc. At the same time, combined with vacuum technology and gas control system, the evaporation environment is optimized, such as controlling the vacuum degree and introducing an inert gas atmosphere, to improve the stability of the evaporation process and product quality. By precisely controlling the gas composition and pressure in the evaporation environment, the risk of oxidation and pollution during the evaporation process can be reduced, and the purity and performance of the coating can be improved.

[0099] Example 4

[0100] The difference between this embodiment and Example 1 is as follows:

[0101] A process for controlling the evaporation rate of the antimony source includes the following steps:

[0102] S1: Select antimony raw materials and perform pretreatment on the antimony raw materials.

[0103] S2: Adjust the powder of the pretreated antimony raw materials and optimize the narrowness of the antimony powder distribution.

[0104] S3: Add tungsten powder to the antimony powder and mix them.

[0105] S4: Make the treated antimony powder into antimony pellets.

[0106] S5: Select a mold and make an evaporator.

[0107] S6: Treat the inner wall surface of the evaporator.

[0108] S7: Evaporate the antimony pellets in the evaporation tube and monitor the evaporation process.

[0109] In this embodiment, in step S7, set the heating temperature of the evaporation furnace to 200 °C and the vacuum degree to 10-7 Pa. Control the temperature through current and control the evaporation rate through temperature. Before evaporation, preheat the uniformly mixed antimony powder and tungsten powder to remove adsorbed moisture and gas, reducing pollution and fluctuations during the evaporation process. During the evaporation process, obtain the deposition thickness and deposition rate of the thin film by measuring the frequency change of the crystal oscillator before and after evaporation. By measuring the thin film deposition rate, the change of the evaporation rate can be monitored in real time. In addition, the film thickness gauge can detect the deposition rate and thickness of the thin film in real time, ensuring the uniformity and consistency of evaporation, thereby judging the stability of the evaporation rate. If the evaporation rate does not meet the requirements, adjust it by adjusting the heating power, temperature control parameters, etc. At the same time, by introducing a real-time monitoring and feedback control system, use sensors to monitor evaporation parameters such as temperature, pressure, and evaporation rate in real time, and automatically adjust the evaporation conditions according to the feedback information to achieve precise control of the evaporation rate of the antimony source, improving the automation and intelligence level of the production process, and ensuring the consistency and stability of product quality.

[0110] Example Five

[0111] The difference between this embodiment and Embodiment 1 is as follows:

[0112] A process for controlling the evaporation rate of an antimony source includes the following steps:

[0113] S1: Select antimony raw materials and perform pretreatment on the antimony raw materials;

[0114] S2: Adjust the powder of the pretreated antimony raw materials and optimize the narrowness of the antimony powder distribution;

[0115] S3: Add tungsten powder to the antimony powder and mix them;

[0116] S4: Make the treated antimony powder into antimony pellets;

[0117] S5: Select a mold and make an evaporator;

[0118] S6: Treat the inner wall surface of the evaporator;

[0119] S7: Evaporate the antimony pellets in the evaporation tube, perform post-treatment on the evaporated antimony source, and detect the product.

[0120] In this embodiment, in S7, the heating temperature of the evaporation furnace is set to 200 °C, and the vacuum degree is 10-7 Pa. The temperature is controlled by current, and the evaporation rate is controlled by temperature. Before evaporation, the uniformly mixed antimony powder and tungsten powder are preheated to remove the adsorbed moisture and gas, reducing the pollution and fluctuations during the evaporation process. During the evaporation process, the deposition thickness and deposition rate of the thin film are obtained by measuring the frequency change of the quartz crystal oscillator before and after evaporation. By measuring the thin film deposition rate, the change of the evaporation rate can be monitored in real time. In addition, the film thickness gauge can detect the deposition rate and thickness of the thin film in real time, ensuring the uniformity and consistency of evaporation, thereby judging the stability of the evaporation rate. If the evaporation rate does not meet the requirements, it is adjusted by adjusting the heating power, temperature control parameters, etc. After the evaporation process is completed, post-treatment is carried out on the evaporated antimony source, such as cooling, encapsulation, etc., and the product quality is comprehensively inspected. Advanced inspection equipment and technologies, such as spectral analysis, X-ray diffraction, etc., are used to accurately detect the composition, structure, thickness, etc. of the coating, ensuring that the product quality meets the standard requirements. At the same time, the quality inspection data is fed back to the previous process steps, providing a basis for process optimization and quality control, forming a closed-loop quality control system, and continuously improving the reliability of the entire process and the product quality.

[0121] Experimental Example

[0122] Through the schemes for controlling the evaporation rate of the antimony source proposed in Examples 1 to 5, compared with the conventional scheme for controlling the evaporation rate of the antimony source, the experimental data are as follows in the following table:

[0123]

[0124] As mentioned above, the above is only the preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention, according to the technical solution and inventive concept of the present invention, makes equivalent substitutions or changes, and all should be covered within the protection scope of the present invention.

Claims

1. A process for controlling the evaporation rate of an antimony source, characterized in that: The following steps are involved: S1: Selecting antimony raw materials and pre-treating the antimony raw materials; S2: Powder adjustment of the pretreated antimony raw materials and optimization of the distribution narrowness of the antimony powder; S3: adding tungsten powder to antimony powder and mixing; S4: preparing antimony pellets from the treated antimony powder; S5: Select a mold and make an evaporator; S6: treating the inner wall surface of the evaporator; S7: Evaporating the antimony pellets in the evaporation tube.

2. A process for controlling the evaporation rate of an antimony source according to claim 1, characterized in that: In S1, an antimony raw material with a purity of 7N is purchased, and the antimony raw material is ball-milled by a ball mill for 180 minutes. During the ball milling process, the vacuum in the ball milling tank is always maintained. After the ball milling is completed, the antimony powder obtained is subjected to laser particle size analysis; Particle size detection and adjustment: After ball milling, use a laser particle size analyzer to detect the particle size of the antimony powder to ensure that the particle size of the antimony powder meets the predetermined requirements. The test parameters are: automatic wet sampling, imported helium-argon laser, scanning frequency 1kHz, shading rate between 10%-20%, and take the average of three measurements. If it does not meet the requirements, adjust the ball milling parameters or perform ball milling again until the predetermined particle size is reached.

3. A process for controlling the evaporation rate of an antimony source according to claim 2, characterized in that: In S2, the antimony powder after ball milling is placed in a vibrating screen machine for screening, the mesh number of the screen is 650-1200 mesh, and the antimony powder is separated into powders of different particle sizes through the filtering effect of the screen; Particle size detection: After screening, use a laser particle size analyzer to detect the particle size of the antimony powder to determine whether it meets the requirements. The test parameters are: automatic wet sampling, imported helium-argon laser, scanning frequency 1kHz, shading rate between 10%-20%, and take the average of three measurements. The particle size distribution of antimony powder that meets the requirements is: D50 is 17 (±1) μm, D10>5μm, D90<34μm.

4. A process for controlling the evaporation rate of an antimony source according to claim 3, characterized in that: In S2, the antimony powder is subjected to laser particle size analysis by a laser particle size analyzer to determine whether the particle size required for the subsequent evaporation process is reached. If a narrower particle size distribution is required, multiple screening and grading processes are performed.

5. A process for controlling the evaporation rate of an antimony source according to claim 4, characterized in that: In S3, tungsten powder and antimony powder are mixed in a mass ratio of 3:97 to 5:95 by a three-dimensional motion mixer for about 90 minutes.

6. A process for controlling the evaporation rate of an antimony source according to claim 5, characterized in that: In S4, the mixed powder of antimony and tungsten is weighed by an analytical balance, the molding mold is assembled, the weighed powder is put into the feed ports of four molds, the punch is put into the feed port containing the powder, the powder is pressed with uniform and stable pressure to form a hemispherical cylindrical antimony pill, and finally the upper and lower parts of the mold are separated and the pressed antimony pill is taken out.

7. A process for controlling the evaporation rate of an antimony source according to claim 6, characterized in that: In S5, a round tube single-side flattening mold is selected, and the evaporator shell round tube is placed in the mold, the round hole on the upper part of the evaporator is aligned with the positioning protrusion on the mold, and then the upper and lower molds are closed and placed in a hydraulic press for extrusion processing, so that one side of the round tube wall is slightly flattened.

8. A process for controlling the evaporation rate of an antimony source according to claim 7, characterized in that: In S5, the antimony source is placed into the evaporator shell from both sides of the round tube, and then the evaporator is placed in the mold, the round hole is also aligned with the positioning protrusion, and the antimony source is pushed to the specified position using a positioning pin, and then the positioning pin is removed, the upper and lower molds are closed and placed in a hydraulic press for pressing.

9. A process for controlling the evaporation rate of an antimony source according to claim 8, characterized in that: In S6, active particles in the plasma react with the inner wall surface of the evaporation tube to remove grease and oxide layer pollutants on the surface, and high-energy ion beams are used to bombard the inner wall of the evaporation tube, and the bombardment parameters are precisely controlled to remove surface impurities and defects and change the surface microstructure.

10. A process for controlling the evaporation rate of an antimony source according to claim 9, characterized in that: In S7, the heating temperature of the evaporation furnace is set to 200° C. and the vacuum degree is set to 10-7 Pa. The temperature is controlled by current, and the evaporation rate is controlled by temperature. During the evaporation process, the deposition thickness and deposition rate of the thin film are obtained by measuring the frequency change of the crystal oscillator before and after evaporation. By measuring the film deposition rate, the change of the evaporation rate can be monitored in real time.

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