Method for regulating and controlling evaporation rate of antimony source by controlling parameters of evaporation pipe

Abstract

The invention belongs to the technical field of evaporation source control in a material preparation process, particularly relates to a method for regulating and controlling the evaporation rate of an antimony source by controlling parameters of an evaporation pipe, and aims to solve the problems that in the existing traditional antimony source evaporation process, factors influencing the evaporation rate are insufficiently controlled, precise regulation and control cannot be realized, and the evaporation rate is not influenced in the evaporation process. In order to solve the problems that the evaporation rate is difficult to stabilize in a specific numerical range and large fluctuation is presented due to the fact that antimony contents in different areas of an image intensifier are different due to non-uniform distribution of an antimony source in an evaporation space, the following scheme is provided: the method comprises the following steps: S1, selecting an evaporation pipe, and controlling the size precision of the evaporation pipe; according to the antimony source evaporation pipe manufacturing method, fine regulation and control over the evaporation process are achieved by controlling the structure and the manufacturing technology of the antimony source evaporation pipe, the evaporation rate can be precisely regulated and controlled, the evaporation uniformity and stability are effectively improved, and the stability and repeatability of the technology are enhanced.

Description

Technical Field

[0001] The invention relates to the technical field of evaporation source control in a material preparation process, and in particular to a method for regulating the evaporation rate of an antimony source by controlling evaporation tube parameters. Background Art

[0002] As a key branch of modern optoelectronic technology, night vision technology uses optoelectronic imaging devices to achieve nighttime observation, greatly expanding human visual capabilities in low-light environments. It plays an irreplaceable role in many fields such as military, security, scientific research, and civil use. Its core principle is to convert weak optical images captured at night or under low illumination into enhanced optical images or electronic images through image intensifiers or camera devices, so that observers can clearly distinguish target objects.

[0003] As a typical representative product of night vision technology, low-light-level night vision devices cleverly use natural night sky lights such as weak moonlight, starlight, atmospheric glow, and Milky Way light as illumination sources. With the help of the core component of the image intensifier, it amplifies the weak photons reflected by the target and converts them into visible images, thereby realizing the function of night observation. In the military field, low-light-level night vision devices are widely used in key mission scenarios such as night aiming, night observation, and night tracking and identification. In the manufacturing process of low-light-level night vision devices, antimony source evaporation technology occupies an extremely critical position. The performance of the image intensifier depends to a large extent on the quality and stability of the antimony source evaporation.

[0004] In the prior art, in the traditional antimony source evaporation process, the factors affecting the evaporation rate are not adequately controlled, and precise regulation cannot be achieved. During the evaporation process, the antimony source is unevenly distributed in the evaporation space, resulting in differences in the antimony content in different areas of the image intensifier, which makes it difficult for the evaporation rate to stabilize within a specific numerical range and exhibits large fluctuations. For this reason, we propose a method for controlling the evaporation rate of the antimony source by controlling the evaporation tube parameters to solve the above problem. Summary of the invention

[0005] The purpose of the present invention is to solve the problem that in the traditional antimony source evaporation process in the prior art, the factors affecting the evaporation rate are not adequately controlled and precise regulation cannot be achieved. During the evaporation process, the antimony source is unevenly distributed in the evaporation space, resulting in differences in the antimony content in different areas of the image intensifier, which makes it difficult for the evaporation rate to be stabilized within a specific numerical range and presents a large fluctuation. A method for controlling the evaporation rate of the antimony source by controlling the evaporation tube parameters is proposed.

[0006] The present application provides a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube, which adopts the following technical solution:

[0007] A method for regulating the evaporation rate of antimony source by controlling the parameters of the evaporation tube, comprising the following steps:

[0008] S1: Select an evaporation tube and control the dimensional accuracy of the evaporation tube;

[0009] S2: Prepare antimony raw materials and pre-treat the antimony raw materials;

[0010] S3: Press the pre-treated antimony raw materials into antimony pellets;

[0011] S4: Place the antimony pellets in the evaporation tube;

[0012] S5: Select a mold and perform extrusion processing on the evaporation tube containing the antimony pellets;

[0013] S6: Evaporate the extrusion-processed evaporation tube.

[0014] Furthermore, in the step S1, a seamless solderless antimony source evaporation tube made of Ni80Cr20 alloy is selected, the thickness of the evaporation tube is 20 - 30 μm, the diameter of the evaporation tube is 2 - 3 mm, and the length is 20 - 30 mm.

[0015] Furthermore, in the step S1, a small hole is machined at the middle position of the evaporation tube by a drilling device, the diameter of the small hole is 1 - 2 mm, and the dimensional accuracy of the small hole is ±0.05 mm.

[0016] Furthermore, in the step S2, antimony raw materials with a purity of 7N are purchased. By placing the antimony raw materials in a specific chemical solution, impurities are dissolved through chemical reactions. An appropriate precipitant is added to the treated solution to precipitate antimony in the form of precipitation. The precipitated antimony is subjected to distillation treatment, and by controlling the temperature and pressure, antimony is separated from the mixture to obtain high-purity antimony.

[0017] Furthermore, in the step S2, the antimony raw materials are subjected to surface modification treatment by anionic, cationic or non-ionic surfactants, treated at 60 °C for 30 minutes, and the surfactant concentration is 0.5%.

[0018] Furthermore, in the step S2, the antimony raw materials are ball-milled by a ball mill, and the ball-milling time is 180 min;

[0019] Settings of ball-milling medium and parameters: The ball-milling tank is made of stainless steel, the inner liner is zirconia, the volume is 1000 mL, the grinding balls are made of zirconia, 200 grinding balls with a diameter of 6 mm are selected, 100 grinding balls with a diameter of 10 mm are selected, and 10 grinding balls with a diameter of 20 mm are selected. The total mass of the grinding balls is about 700 g;

[0020] Ball milling process: Coarse pure antimony metal blocks and grinding balls are placed in a ball milling jar and subjected to ball milling treatment in a ball mill. The antimony blocks are broken and refined into metallic antimony powder with the required particle size through the impact and friction of the grinding balls;

[0021] 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 stop for 2 min. Repeat this cycle 3 times, for a total of 192 min. Keep the inside of the ball milling jar under vacuum during the ball milling process;

[0022] The ball milled antimony powder is put into a vibrating sieve for screening. The mesh number of the sieve is 600 - 1200 meshes. After screening, a laser particle size analyzer is used to perform laser particle size analysis on the antimony powder to obtain the required particle size.

[0023] Further, in S3, the antimony powder is weighed by an analytical balance to ensure that the mass of each portion of the measured antimony powder is the same. Then, the forming die is assembled, the weighed powder is put into the four feeding ports of the die, the punch is put into the feeding port containing the antimony powder, and the antimony powder is pressed with uniform and stable pressure to form a hemispherical cylindrical antimony pellet. Finally, the upper and lower parts of the die are separated and the pressed antimony pellet is taken out.

[0024] Further, in S5, a round tube single - side flattening die is selected. The evaporation tube is placed in the die, and the small holes of the evaporation tube are aligned with the positioning protrusions on the die. Then, the upper and lower parts of the die are closed, and extrusion processing is carried out by a hydraulic press to slightly flatten one side of the evaporation tube wall.

[0025] Further, in S4 and S5, the antimony pellets are respectively put into the evaporation tube from both sides of the round tube. Then, the evaporation tube containing the antimony pellets is placed in the die, the small holes are also aligned with the positioning protrusions, and a positioning pin is used to push the antimony pellets to the designated positions. Then, the positioning pin is removed, the upper and lower parts of the die are closed, and it is pressed by a hydraulic press.

[0026] Further, in S6, the heating temperature of the evaporation furnace is set to 200 °C, 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 quartz crystal oscillator before and after evaporation, and the change of the evaporation rate is monitored in real - time by measuring the thin film deposition rate.

[0027] In summary, the present application includes at least one of the following beneficial technical effects:

[0028] 1. When this solution is actually applied to the antimony source evaporation system, it can accurately control the antimony source evaporation rate by adjusting the above - mentioned manufacturing process parameters under different production environments and process requirements, ensuring the stability of the production process. At the same time, the antimony source evaporation rate can be accurately controlled through this evaporation tube to meet the requirements of different coating thicknesses and optical properties;

[0029] 2. The materials of this solution have a controllable and stable evaporation rate, and are applicable to processes such as thin film deposition, optoelectronic material synthesis, semiconductor manufacturing, low-light level night vision image intensifier manufacturing, or other processes that require precise control of the evaporation rate of the antimony source. This antimony source evaporation material 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.

[0030] The present invention realizes the refined regulation of the evaporation process by controlling the structure and manufacturing process of the antimony source evaporation tube, can accurately regulate the evaporation rate, effectively improve the uniformity and stability of evaporation, and enhance the stability and repeatability of the process. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a flowchart of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0032] Figure 2 It is a flowchart of S1 of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0033] Figure 3 It is a flowchart of S2 of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0034] Figure 4 It is a flowchart of S4 and S5 of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0035] Figure 5 It is a diagram of the fabricated antimony source evaporation tube of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0036] Figure 6 It is a diagram of the fabricated antimony source evaporator of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0037] Figure 7 It is a curve diagram of the relationship between the thickness of the evaporation tube and the evaporation current of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0038] Figure 8 It is a curve diagram of the relationship between the length of the evaporation tube and the evaporation current of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0039] Figure 9 It is a curve diagram of the relationship between the diameter of the evaporation tube and the evaporation current of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention;

[0040] Figure 10 The curve graph showing the relationship between the small hole diameter of the evaporation tube and the evaporation current of a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed by the present invention. Specific implementation manners

[0041] 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.

[0042] Embodiment 1

[0043] Referring to Figures 1 - 10 , a method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube includes the following steps:

[0044] S1: Select an evaporation tube and control the dimensional accuracy of the evaporation tube;

[0045] S2: Prepare antimony raw materials and perform pretreatment on the antimony raw materials;

[0046] S3: Press the pretreated antimony raw materials into antimony pellets;

[0047] S4: Place the antimony pellets in the evaporation tube;

[0048] S5: Select a mold and perform extrusion processing on the evaporation tube containing the antimony pellets;

[0049] S6: Evaporate the extrusion-processed evaporation tube.

[0050] In this embodiment, in S1, a seamless and weld-free antimony source evaporation tube made of Ni80Cr20 alloy is selected to ensure that during the high-temperature evaporation process, the evaporation tube itself will not generate impurity pollution to the antimony source evaporation environment, and has sufficient structural strength and stability. The alkali source evaporation tube has the characteristics of being seamless and weld-free and being formed in one piece. Its function is to avoid weak links caused by welding points and prevent problems such as leakage and deformation in the high-temperature evaporation environment, ensuring the stability of the internal pressure of the evaporation tube, thereby providing a stable physical structure basis for accurately controlling the evaporation rate of the antimony source. At the same time, the one-piece forming process reduces the manufacturing process and the risk of introducing impurities due to multiple processing, which helps to maintain the consistency of the material properties of the evaporation tube. This alloy has good high-temperature resistance and a relatively high melting point. During the high-temperature evaporation process, its own structure is stable and it is not easy to deform or melt, which can ensure the structural integrity of the evaporation tube. At the same time, this alloy has a low vapor pressure, and in a high-temperature environment, the impurities generated by its own volatilization are extremely few and will not pollute the antimony source evaporation environment, and has sufficient structural strength and stability to meet the stringent requirements of the antimony source evaporation tube in the high-temperature evaporation process. The surface of the alkali source evaporation tube is specially treated, such as by using processes such as electrolytic polishing. The surface treatment can improve the surface performance of the evaporation tube, increase the surface smoothness, reduce the adhesion and residue of the antimony source on the surface of the evaporation tube, thereby improving the evaporation efficiency and the stability of the evaporation rate, enhancing the surface oxidation resistance and corrosion resistance, and extending the service life of the evaporation tube, ensuring that the control effect of the antimony source evaporation rate remains stable during long-term use, and further ensuring the accuracy of the control of the antimony source evaporation rate. The thickness of the evaporation tube is 20 - 30 μm, which ensures that the wall thickness can minimize the heat insulation of the material to the greatest extent on the basis of ensuring the structural strength, facilitating the rapid transfer of heat to the antimony source and thus accelerating the evaporation rate. The tube thickness not only affects the structural strength of the evaporation tube, but also has an impact on heat transfer and the evaporation environment of the internal antimony source. An appropriate tube thickness can ensure the stability and controllability of the evaporation process. The diameter of the evaporation tube is 2 - 3 mm and the length is 20 - 30 mm, which can ensure a sufficient antimony source loading capacity and maintain a stable evaporation for a certain period of time, while also ensuring the effective transfer of heat inside the tube. The diameter of the tube affects the loading capacity of the internal antimony source and the size of the evaporation space, and thus has a direct effect on the evaporation rate. The length of the tube determines the length of the evaporation path, affects the residence time of the antimony source in the evaporation tube and the evaporation uniformity, and has a significant impact on the overall evaporation rate. A small hole is processed in the middle position of the evaporation tube through a drilling device, and the antimony pellets are placed on both sides of the small hole. This can form a relatively symmetrical and stable gas flow distribution when the antimony source evaporates, which helps to improve the evaporation uniformity. The diameter of the small hole is 1 - 2 mm, and the dimensional accuracy of the small hole is ±0.05 mm, and the hole walls are smooth and free of burrs, ensuring the consistency and quality of the small holes. By precisely controlling the diameter of the small holes, the evaporation mode of the antimony source and the electron emission characteristics can be adjusted, thereby achieving precise control of the evaporation rate. The precise setting of the small hole diameter plays a crucial role in the evaporation rate of the antimony source. Different small hole diameters will result in different evaporation areas and gas escape rates, thereby directly affecting the evaporation efficiency of the antimony source. There is a clear positive correlation between the thickness of the evaporation tube, the diameter of the evaporation tube and the evaporation rate of the antimony source. There is a clear negative correlation between the diameter of the small hole in the evaporation tube, the length of the evaporation tube and the evaporation rate of the antimony source.

[0051] In this embodiment, in S2, antimony raw materials with a purity of 7N are purchased. By placing the antimony raw materials in a specific chemical solution, the impurities therein are dissolved through a chemical reaction. An appropriate precipitating agent is added to the treated solution to precipitate antimony in the form of a precipitate. The precipitated antimony is subjected to distillation treatment. By controlling the temperature and pressure, antimony is separated from the mixture to obtain high-purity antimony. The antimony raw materials are surface-modified with anionic, cationic or non-ionic surfactants and treated at 60 °C for 30 minutes, and the surfactant concentration is 0.5%. The antimony raw materials are ball-milled by a ball mill, the ball-milling time is 180 min, and the ball-milled antimony powder is put into a vibrating sieve for screening. The mesh number of the sieve is 600 - 1200 meshes. After the screening is completed, the antimony powder is subjected to laser particle size analysis using a laser particle size analyzer to obtain the required particle size;

[0052] Ball-milling medium and parameter settings: The ball-milling tank is made of stainless steel, the inner liner is zirconia, the volume is 1000 mL, the grinding balls are made of zirconia, 200 grinding balls with a diameter of 6 mm are selected, 100 grinding balls with a diameter of 10 mm are selected, and 10 grinding balls with a diameter of 20 mm are selected. The total mass of the grinding balls is about 700 g;

[0053] Ball-milling process: Coarse pure antimony metal blocks and grinding balls are put into the ball-milling tank and subjected to ball-milling treatment in a ball mill. The antimony blocks are broken and refined into metal antimony powder with a particle size meeting the requirements through the impact and friction of the grinding balls;

[0054] 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. This cycle is repeated 3 times, for a total of 192 min. The inside of the ball-milling tank is always kept under vacuum during the ball-milling process;

[0055] The ball-milled antimony powder is put into a vibrating sieve for screening. The mesh number of the sieve is 600–1200 meshes. After the screening is completed, the antimony powder is subjected to laser particle size analysis using a laser particle size analyzer to make the average particle diameter of the antimony powder reach about 17 μm, and the standard deviation of the particle size distribution does not exceed 20% of the average particle diameter;

[0056] Particle size detection: Use a laser particle size analyzer to detect the particle size of the antimony powder after screening, and determine whether the particle size meets the requirements. The particle size distribution of the antimony powder that meets the requirements is as follows: D50 is 17 (±1) μm, D10 > 5 μm, D90 < 34 μm; 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 1 kHz, light shielding rate between 10% and 20%, and take the average value of three measurements;

[0057] Particle size optimization: Select the antimony powder of the required particle size level for subsequent processing according to actual needs. If a narrower particle size distribution is required, further narrow the particle size distribution range by performing multiple screening processes.

[0058] In this embodiment, in S3, weigh the antimony powder with an analytical balance to ensure that the mass of each portion of the weighed antimony powder is the same. Then assemble the molding die, put the weighed powder into the four feeding ports of the die, put the punch into the feeding port containing the antimony powder, and press the antimony powder with a uniform and stable pressure to form a hemispherical cylindrical antimony pellet. Finally, separate the upper and lower parts of the die and take out the pressed antimony pellet. The entire operation process needs to keep the working environment clean and avoid impurities from mixing into the antimony powder.

[0059] In this embodiment, in S4 and S5, select a circular tube single-side flattening die, put the evaporation tube into the die, align the small hole of the evaporation tube with the positioning protrusion on the die, then close the upper and lower parts of the die, and perform extrusion processing through a hydraulic press to slightly flatten one side of the evaporation tube wall. The purpose is to prevent the antimony pellet from rolling to one side inside the evaporation tube and causing antimony leakage. Put the antimony pellets into the evaporation tube from both sides of the circular tube respectively, then put the evaporation tube containing the antimony pellets into the die, align the small hole with the positioning protrusion again, use a positioning pin to push the antimony pellet to the specified position, then remove the positioning pin, close the upper and lower parts of the die and press with a hydraulic press. After this pressing, both ends of the evaporation tube will be pressed into flat electrodes, and the evaporator is thus manufactured.

[0060] In this embodiment, in S6, the heating temperature of the evaporation furnace is set to 200°C, 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, and the change of the evaporation rate is monitored in real time by measuring the thin film deposition rate. When this evaporation tube is actually applied to the antimony source evaporation system, it can accurately control the antimony source evaporation rate by adjusting the above-mentioned manufacturing process parameters under different production environments and process requirements, ensuring the stability of the production process. At the same time, the antimony source evaporation rate can be accurately controlled by this evaporation tube to meet the requirements of different coating thicknesses and optical properties, and the material has a controllable and stable evaporation rate, which is applicable to processes such as thin film deposition, optoelectronic material synthesis, semiconductor manufacturing, low-light-level night vision image intensifier manufacturing, or other processes that require precise control of the antimony source evaporation rate. This antimony source evaporation material not only has excellent evaporation performance, but also has good stability and reliability, and can meet the needs of various high-performance material preparation and process applications.

[0061] Example Two

[0062] The difference between this embodiment and Example One lies in:

[0063] A method for regulating the antimony source evaporation rate by controlling the evaporation tube parameters, including the following steps:

[0064] S1: Select an evaporation tube and control the dimensional accuracy of the evaporation tube;

[0065] S2: Prepare antimony raw materials and perform pretreatment on the antimony raw materials;

[0066] S3: Press the pretreated antimony raw materials into antimony pellets;

[0067] S4: Place the antimony pellets in the evaporation tube;

[0068] S5: Select a mold, perform preheating treatment on the mold, and perform extrusion processing on the evaporation tube containing the antimony pellets;

[0069] S6: Evaporate the extrusion-processed evaporation tube.

[0070] In this embodiment, in S5, a round tube single-side flattening die is selected and the die is preheated to ensure the smooth progress of the extrusion process, improve the dimensional accuracy and surface quality of the evaporation tube after extrusion, enhance the mechanical strength and high-temperature resistance of the evaporation tube. The evaporation tube is placed in the die, and the small holes of the evaporation tube are aligned with the positioning protrusions on the die. Then, the upper and lower parts of the die are closed, and extrusion processing is carried out through a hydraulic press to slightly flatten one side of the evaporation tube wall. The purpose is to prevent the antimony pellets from rolling to one side inside the evaporation tube and causing antimony leakage. The antimony pellets are respectively placed into the evaporation tube from both sides of the round tube. Then, the evaporation tube containing the antimony pellets is placed into the die, and the small holes are also aligned with the positioning protrusions. A positioning pin is used to push the antimony pellets to the designated positions, and then the positioning pin is removed. The upper and lower parts of the die are closed and pressed with a hydraulic press. After this pressing, both ends of the evaporation tube will be pressed into flat electrodes, and the evaporator is thus fabricated.

[0071] Embodiment Three

[0072] The difference between this embodiment and Embodiment One lies in:

[0073] A method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube, comprising the following steps:

[0074] S1: Select an evaporation tube and control the dimensional accuracy of the evaporation tube;

[0075] S2: Prepare antimony raw materials and perform pretreatment on the antimony raw materials;

[0076] S3: Press the pretreated antimony raw materials into antimony pellets;

[0077] S4: Place the antimony pellets in the evaporation tube;

[0078] S5: Select a die, optimize the design of the die, and perform extrusion processing on the evaporation tube containing the antimony pellets;

[0079] S6: Evaporate the extrusion-processed evaporation tube.

[0080] In this embodiment, in S5, a round tube single-side flattening die is selected to optimize the die design. The shape and size of the die are accurately calculated using computer simulation technology to achieve the best extrusion effect, improve the geometric accuracy and performance of the evaporation tube after extrusion processing, reduce the difficulty and cost of subsequent processing. Place the evaporation tube into the die, align the small holes of the evaporation tube with the positioning protrusions on the die, then close the upper and lower parts of the die, and perform extrusion processing through a hydraulic press to slightly flatten one side of the evaporation tube wall. The purpose is to prevent the antimony pellets from rolling to one side inside the evaporation tube and causing antimony leakage. Put the antimony pellets into the evaporation tube from both sides of the round tube respectively, then place the evaporation tube with the antimony pellets into the die, align the small holes with the positioning protrusions as well, use a positioning pin to push the antimony pellets to the designated position, then remove the positioning pin, close the upper and lower parts of the die and press with a hydraulic press. After this pressing, both ends of the evaporation tube will be pressed into flat electrodes, and the evaporator is thus fabricated.

[0081] Example Four

[0082] The difference between this embodiment and Example One lies in:

[0083] A method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube, comprising the following steps:

[0084] S1: Select an evaporation tube and control the dimensional accuracy of the evaporation tube;

[0085] S2: Prepare antimony raw materials and perform pretreatment on the antimony raw materials;

[0086] S3: Press the pretreated antimony raw materials into antimony pellets;

[0087] S4: Place the antimony pellets inside the evaporation tube;

[0088] S5: Select a die, perform modification treatment on the material of the die, and perform extrusion processing on the evaporation tube containing the antimony pellets;

[0089] S6: Evaporate the extrusion-processed evaporation tube.

[0090] In this embodiment, in S5, a circular tube single-side flattening die is selected, and the material of the die is modified to improve its hardness, wear resistance and thermal stability to meet more stringent extrusion processing requirements, extend the service life of the die, reduce production costs, and at the same time improve the surface quality and dimensional accuracy of the evaporation tube after extrusion processing. The evaporation tube is placed in the die, the small holes of the evaporation tube are aligned with the positioning protrusions on the die, and then the upper and lower parts of the die are closed, and extrusion processing is carried out through a hydraulic press to slightly flatten one side of the evaporation tube wall. The purpose is to prevent the antimony pellets from rolling to one side inside the evaporation tube and causing antimony leakage. The antimony pellets are respectively put into the evaporation tube from both sides of the circular tube, and then the evaporation tube containing the antimony pellets is put into the die, and the small holes are also aligned with the positioning protrusions, and a positioning pin is used to push the antimony pellets to the designated positions, and then the positioning pin is removed, and the upper and lower parts of the die are closed and pressed with a hydraulic press. After this pressing, both ends of the evaporation tube will be pressed into flat electrodes, and the evaporator is thus manufactured.

[0091] Example Five

[0092] The difference between this embodiment and Example One is as follows:

[0093] A method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube includes the following steps:

[0094] S1: Select an evaporation tube and control the dimensional accuracy of the evaporation tube;

[0095] S2: Prepare antimony raw materials and preprocess the antimony raw materials;

[0096] S3: Press the preprocessed antimony raw materials into antimony pellets;

[0097] S4: Place the antimony pellets in the evaporation tube and support and position the antimony pellets;

[0098] S5: Select a die and carry out extrusion processing on the evaporation tube containing the antimony pellets;

[0099] S6: Evaporate the extrusion-processed evaporation tube.

[0100] In this embodiment, in S4, the antimony pellets are respectively put into the evaporation tube from both sides of the circular tube, and a special support structure or positioning device is adopted to ensure that the positions of the antimony pellets in the evaporation tube are accurate, avoid shaking and displacement, ensure the stability and consistency of the evaporation process, and improve the quality and repeatability of the coating.

[0101] Experimental Example

[0102] Through the schemes for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube proposed in Examples One to Five, compared with the conventional schemes for regulating the evaporation rate of the antimony source, the experimental data are as shown in the following table:

[0103]

[0104]

[0105] As described above, it is only the preferred specific implementation manner 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, making equivalent substitutions or changes should be covered within the protection scope of the present invention.

Claims

1. A method for regulating the evaporation rate of an antimony source by controlling the parameters of an evaporation tube, characterized in that: The following steps are involved: S1: Select the evaporation tube and control the size accuracy of the evaporation tube; S2: preparing antimony raw materials and pre-treating the antimony raw materials; S3: pressing the pretreated antimony raw material into antimony pellets; S4: Place the antimony pellets in the evaporation tube; S5: selecting a mold and performing extrusion processing on the evaporation tube with the antimony pellets placed thereon; S6: Evaporating the evaporation tube after the extrusion process.

2. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 1, characterized in that: In S1, a seamless, solder-free antimony source evaporator tube made of Ni80Cr20 alloy is selected, the thickness of the evaporator tube is 20-30 μm, the diameter of the evaporator tube is 2-3 mm, and the length is 20-30 mm.

3. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 2, characterized in that: In S1, a small hole is processed in the middle of the evaporation tube by a drilling device, the diameter of the small hole is 1-2 mm, and the size accuracy of the small hole is ±0.05 mm.

4. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 3, characterized in that: In S2, an antimony raw material with a purity of 7N is purchased, and the antimony raw material is placed in a specific chemical solution to dissolve impurities therein through a chemical reaction, and a suitable precipitant is added to the treated solution to precipitate the antimony. The precipitated antimony is distilled, and the antimony is separated from the mixture by controlling the temperature and pressure to obtain high-purity antimony.

5. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 4, characterized in that: In S2, the surface of the antimony raw material is modified by anionic, cationic or nonionic surfactants at 60° C. for 30 minutes, with a surfactant concentration of 0.5%.

6. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 5, characterized in that: In S2, the antimony raw material is ball-milled by a ball mill for 180 minutes; Ball milling media and parameter settings: The ball mill is made of stainless steel, the inner tank is made of zirconium oxide, the volume is 1000 mL, the grinding ball is made of zirconium oxide, 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 700 g. Ball milling process: put the coarser pure antimony metal block and grinding balls into a ball mill, and perform ball milling in a ball mill. The impact and friction of the grinding balls will break the antimony block and refine it into metal antimony powder with the required particle size. The ball milling process is: forward rotation at 160r / min for 30min and then stop for 2min, then reverse rotation at 160r / min for 30min and then stop for 2min, and repeat this process for 3 times, for a total of 192min. The vacuum in the ball milling tank is always maintained during the ball milling process. The ball-milled antimony powder is put into a vibrating screen for sieving, and the mesh number of the screen is 600-1200 mesh. After the sieving is completed, a laser particle size analyzer is used to perform laser particle size analysis on the antimony powder to obtain the required particle size.

7. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 6, characterized in that: In S3, the antimony powder is weighed by an analytical balance to ensure that the mass of each portion of antimony powder is consistent, then the molding mold is assembled, the weighed powder is put into the four feed ports of the mold, the punch is put into the feed port containing the antimony powder, and the antimony powder is pressed with uniform and stable pressure to form hemispherical cylindrical antimony pills, and finally the upper and lower parts of the mold are separated and the pressed antimony pills are taken out.

8. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 7, characterized in that: In S5, a round tube single-side flattening mold is selected, the evaporator tube is placed in the mold, the small hole of the evaporator tube is aligned with the positioning protrusion on the mold, and then the upper and lower parts of the mold are closed, and extrusion processing is performed by a hydraulic press to slightly flatten one side of the evaporator tube wall.

9. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 8, characterized in that: In S4 and S5, the antimony balls are placed into the evaporation tube from both sides of the round tube respectively, and then the evaporation tube with the antimony balls is placed into the mold, the small holes are also aligned with the positioning protrusions, and the antimony balls are pushed to the specified position using the positioning needles, and then the positioning needles are removed, and the upper and lower parts of the mold are closed and pressed with a hydraulic press.

10. The method for regulating the evaporation rate of the antimony source by controlling the parameters of the evaporation tube according to claim 9, characterized in that: In S6, the heating temperature of the evaporation furnace is set to 200°C, the vacuum degree is set to 10-7Pa, 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 film are obtained by measuring the frequency change of the crystal oscillator before and after evaporation, and the change of the evaporation rate is monitored in real time by measuring the film deposition rate.

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