Antimony bead evaporation source quantitative melting device and method

By using vacuum system and high-purity argon protection during the melting process of antimony bead evaporation source, combined with the nickel wire wrapping process, the problems of antimony bead oxidation and impurity pollution are solved, and the high purity and consistency of antimony beads are achieved, which improves the The performance and product yield of photomultiplier tubes.

CN119242932APending Publication Date: 2025-01-03NANJING SANLE GROUP
View PDF 0 Cites 2 Cited by

Patent Information

Application Number
CN202411241441.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-05
Publication Date
2025-01-03

AI Technical Summary

Technical Problem

The existing antimony bead evaporation sources are prone to oxidation and impurities contamination during the melting process, resulting in low cathode sensitivity, unstable performance and poor weight consistency of the photomultiplier tube, which affects the product yield.

Method used

A quantitative melting device for evaporation source of antimony beads was designed to remove impurity gases from the bell cover through a vacuum system, fill them with high-purity argon, and combine with nickel wire wrapping process to heat antimony powder in a vacuum state to ensure the antimony beads. High purity and consistency.

Benefits of technology

It significantly improves the purity and weight consistency of antimony beads, extends the life of the photomultiplier tube, and improves the yield and performance stability of the product.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119242932A_ABST
    Figure CN119242932A_ABST
Patent Text Reader

Abstract

The invention relates to the field of photomultiplier tube processing, and discloses an antimony bead evaporation source quantitative founding device and method, the antimony bead evaporation source quantitative founding device comprises a founding tool and a vacuum system connected with a bell jar above the device, the founding tool is provided with a groove for accommodating antimony powder, and quantitative founding of antimony beads of different specifications is realized by controlling the volume of the antimony powder groove; the melting tool is used for heating antimony powder through a heating part at the bottom of the melting tool; the exterior of the melting tool is evenly wound with a nickel wire, and the invention further discloses an antimony bead evaporation source quantitative melting method which comprises the following steps that S1, the nickel wire is wound and fixed, specifically, the purified nickel wire is evenly wound on the melting tool, and the nickel wire is fixed to the middle position of an antimony powder groove through a wire groove. The antimony powder is degassed and purified in a high-vacuum state, the antimony beads are molten in a high-purity argon atmosphere, the purity of an antimony bead evaporation source is guaranteed, in addition, the antimony powder quantitative loading tool is adopted, and the antimony beads are produced in batches with high specification consistency.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the field of photomultiplier tube processing, and in particular to a quantitative melting device and method for an antimony bead evaporation source. Background Art

[0002] Photomultiplier tubes are vacuum electronic devices that can convert weak light signals into electrical signals and amplify them. They have the characteristics of high gain and fast response, and are widely and importantly used in the fields of spectral analysis, biological detection, and radiation detection. The antimony-alkali photocathode formed by antimony metal and different alkali metals is the most commonly used cathode material for photomultiplier tubes, and the spectral response range can cover from the ultraviolet band to the near-infrared band. The antimony metal required for the preparation of the photocathode is usually heated and evaporated on the surface of the cathode light window by an antimony bead evaporation source.

[0003] At present, two heating methods are generally used for melting antimony bead evaporation sources. The first method is to use a hydrogen flame to heat the quartz boat or directly heat the antimony powder. The second method is to energize the metal evaporation boat or the heating wire to melt the antimony powder. Regardless of the heating method, nitrogen or argon protective gas is introduced under standard atmospheric pressure to melt the antimony powder and condense it into beads. The antimony bead evaporation source melted by this protection method often undergoes varying degrees of oxidation or contamination, resulting in low cathode sensitivity, or a decrease in electron extraction capacity under long-term light-exposed working conditions, resulting in a shortened life of the entire tube. In addition, the poor consistency of the antimony bead weight will result in a large distribution range of performance parameters during the batch preparation of the photocathode, which is not conducive to improving the product yield. Summary of the invention

[0004] In view of the shortcomings of the prior art, the present invention provides a quantitative melting device and method for an antimony bead evaporation source, which solves the problems of decreased purity, poor weight consistency, and unstable sensitivity and performance of the photomultiplier tube cathode caused by oxidation and impurity contamination during the melting process of antimony beads.

[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: a quantitative melting device for an antimony bead evaporation source, comprising a melting tool, and a vacuum system connected to a bell jar above the device, wherein a groove for accommodating antimony powder is provided on the melting tool, and quantitative melting of antimony beads of different specifications is achieved by controlling the volume of the antimony powder groove;

[0006] The melting tool heats the antimony powder through a heating component at the bottom thereof;

[0007] The outside of the melting tool is evenly wound with nickel wire, and the nickel wire is located in the middle part of the antimony powder groove. During the heating process, the nickel wire contacts the antimony powder and wraps the antimony powder after it melts to form an antimony bead.

[0008] The vacuum system is used to form a high vacuum environment by extracting impurity gases during the melting process to prevent the antimony powder from being oxidized or contaminated during the heating process.

[0009] Preferably, the heating component includes an electrode hole, which is arranged at the bottom of the melting tooling, and the electrode is connected to the electrode hole, and a heating circuit is provided through the electrode to heat the antimony powder under vacuum.

[0010] Preferably, the bell jar is connected with an argon valve for filling high-purity argon into the bell jar after gas purification to adjust the pressure in the bell jar, reduce the evaporation of antimony powder and maintain the purity of the melting environment.

[0011] Preferably, the bell jar is connected to a resistance gauge via an interface, which is used to monitor the vacuum degree in the bell jar in real time when the vacuum system is running.

[0012] Preferably, the bell jar is connected to an ionization gauge via an interface, which is used to accurately measure the low-pressure vacuum environment in the bell jar when the vacuum degree approaches the limit, and works in coordination with the vacuum system.

[0013] Preferably, the melting tool is made of metal molybdenum.

[0014] A quantitative melting method for an antimony bead evaporation source, used in conjunction with the above-mentioned quantitative melting device for an antimony bead evaporation source, comprises the following steps:

[0015] S1. Winding and fixing of nickel wire: Wind the purified nickel wire evenly on the melting tooling, and fix the nickel wire in the middle position of the antimony powder groove through the wire groove;

[0016] S2. Add antimony powder: Add high-purity antimony powder into the groove in the melting tooling, so that the antimony powder is flush with the surface of the tooling;

[0017] S3. Installing the melting tool: fixing the melting tool on the electrode of the antimony bead melting device through the electrode hole;

[0018] S4, install a plurality of melting tools in sequence according to steps S1 to S3;

[0019] S5, vacuuming and preliminary heating: lower the bell jar, start the vacuum system to vacuum, and after the vacuum in the bell jar reaches a certain degree, energize and heat the electrode with a current not exceeding 1.5A to degas and purify the antimony powder;

[0020] S6, filling with argon: close the vacuum system, fill the bell jar with high-purity argon, and adjust the vacuum degree in the bell jar to a suitable range;

[0021] S7, further heating and melting antimony beads: continue to increase the electrode current to 2.5A-3.0A, so that the antimony powder is completely melted and condensed into beads, and finally the molten antimony beads are wrapped around the nickel wire;

[0022] S8. Cooling and taking out the antimony beads: After the melting is completed, adjust the electrode current to 0A, and after cooling for a period of time, open the bell jar, take out the melted antimony beads, and store them properly for subsequent processes.

[0023] Preferably, the range of the certain vacuum degree reached in step S5 is 4×10 -4 Pa-6×10 -4 Pa, the S5 step needs to be powered on for heating for 25-35 minutes.

[0024] Preferably, the vacuum degree in step S6 is adjusted to a suitable range of 0.8×10 5 Pa-1.2×10 5 Pa.

[0025] Preferably, the cooling period in step S8 is 55-65 minutes.

[0026] The present invention provides a quantitative melting device and method for an antimony bead evaporation source, which has the following beneficial effects:

[0027] 1. The present invention designs a melting tool that accurately controls the loading amount of antimony powder, and can adjust the volume of the antimony powder groove according to the requirements of different specifications, thereby achieving quantitative melting of antimony beads and consistency of specifications, solving the problem of a large performance distribution range caused by inconsistent parameters in the existing photomultiplier tube cathode preparation process, and significantly improving the product yield.

[0028] 2. The present invention utilizes a high vacuum system to extract impurity gases in the bell jar, and fills in protective gases such as high-purity argon in a vacuum state, thereby ensuring that the antimony powder is not polluted by oxidation or other impurity gases during the melting process, thereby ensuring the high purity of the antimony beads.

[0029] 3. The present invention degasses and purifies the antimony powder under a high vacuum state and maintains a high-purity argon atmosphere in the bell jar during the subsequent heating process, thereby reducing the evaporation of antimony powder during the heating process and ensuring the molding quality of the antimony beads. This method is combined with a reasonably designed nickel wire wrapping process to improve the molding yield of the antimony beads, making it easier for the antimony beads to detach from the tooling, thereby ensuring the integrity and purity of the antimony beads. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a schematic diagram of the antimony bead evaporation source after melting in the present invention;

[0031] Figure 2 This is a schematic diagram of the antimony bead melting tooling of the present invention;

[0032] Figure 3 It is a schematic diagram of the antimony bead melting device of the present invention;

[0033] Figure 4 is a schematic diagram of antimony powder of the present invention;

[0034] Figure 5 Flow chart of the method of the present invention.

[0035] Among them, 1. vacuum system; 2. bell jar; 3. argon valve; 4. resistance gauge; 5. ionization gauge; 6. melting tool; 6-1. antimony powder; 6-2. nickel wire; 6-3. electrode hole; 7. electrode; 8. antimony bead. DETAILED DESCRIPTION

[0036] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] Example:

[0038] Please refer to the attached Figure 1 -Attached Figure 4 The embodiment of the present invention provides a quantitative melting device and method for an antimony bead evaporation source, comprising a melting tool 6, a vacuum system 1 connected to a bell jar 2 above the device, a groove for accommodating antimony powder 6-1 is provided on the melting tool 6, and quantitative melting of antimony beads 8 of different specifications is achieved by controlling the volume of the groove of the antimony powder 6-1;

[0039] The melting tool 6 heats the antimony powder 6-1 through the heating component at the bottom thereof;

[0040] The outside of the melting tool 6 is evenly wound with a nickel wire 6-2, and the nickel wire 6-2 is located in the middle part of the groove of the antimony powder 6-1. During the heating process, the nickel wire 6-2 contacts the antimony powder 6-1 and wraps the antimony powder 6-1 after it melts to form an antimony bead 8;

[0041] The vacuum system 1 is used to form a high vacuum environment by extracting impurity gases during the melting process to prevent the antimony powder 6 - 1 from being oxidized or contaminated during the heating process.

[0042] Specifically, the core structure of the device is a melting tool 6, which is provided with a groove for accurately controlling the loading amount of antimony powder 6-1. By adjusting the volume of the groove, quantitative melting of antimony beads 8 of different specifications can be achieved. Nickel wire 6-2 is evenly wound around the outside of the tool and contacts with the molten antimony powder 6-1 to ensure that the antimony beads 8 are well formed during the melting process.

[0043] In actual operation, the bell jar 2 is connected to the vacuum system 1, and a high vacuum environment is formed by removing the internal impurity gas. In this process, the oxidation and contamination of the antimony powder 6-1 during the heating process are avoided, ensuring the high purity of the antimony beads 8. Next, by filling with high-purity argon gas, the pressure in the bell jar 2 is further controlled to reduce the evaporation of the antimony powder 6-1 when heated.

[0044] During the melting process, the electrode 7 provides a stable heating current for the tooling, so that the antimony powder 6-1 is melted and condensed into beads under the dual environment of vacuum and argon protection. Finally, after cooling, high-purity and uniform weight antimony beads 8 are obtained. This method not only improves the quality of the antimony beads 8, but also effectively improves the overall performance of the photomultiplier tube.

[0045] Please refer to the attached Figure 2 The heating component includes an electrode hole 6-3, which is arranged at the bottom of the melting tool 6. The electrode hole 6-3 is connected to an electrode 7, and a heating circuit is provided through the electrode 7 to heat the antimony powder 6-1 under a vacuum state.

[0046] Specifically, under vacuum conditions, the electrode 7 gradually heats the antimony powder 6-1 by precisely controlling the current to reach the melting temperature. This design ensures that the antimony powder 6-1 is evenly heated in a high vacuum environment, avoiding interference and contamination from external gases. Through the stable heating circuit provided by the electrode 7, the antimony powder 6-1 can be gradually melted within the ideal temperature range, and finally form high-purity, uniform-weight antimony beads 8. The position design of the electrode hole 6-3 allows the current to be directly transmitted to the inside of the melting tool 6, thereby achieving an efficient heating process, effectively improving the melting efficiency and the quality of the antimony beads 8.

[0047] Please refer to the attached Figure 3 The bell jar 2 is connected with an argon valve 3, which is used to fill the bell jar 2 with high-purity argon after gas purification to adjust the pressure in the bell jar 2, reduce the evaporation amount of the antimony powder 6-1 and maintain the purity of the melting environment.

[0048] Specifically, the bell jar 2 is connected to the argon valve 3, and after the gas purification is completed, high-purity argon can be injected into the bell jar 2. In this way, the air pressure environment inside the bell jar 2 is adjusted, and the excessive evaporation of the antimony powder 6-1 that may occur during the heating process is reduced. At the same time, the introduction of high-purity argon ensures the purity of the melting environment, effectively prevents the mixing of impurities, and further ensures the high quality and consistency of the antimony beads 8 during the melting process.

[0049] Please refer to the attached Figure 3 The bell jar 2 is connected to a resistance gauge 4 via an interface, which is used to monitor the vacuum degree in the bell jar in real time when the vacuum system 1 is running.

[0050] The bell jar 2 is connected to an ionization gauge 5 via an interface, which is used to accurately measure the low-pressure vacuum environment in the bell jar 2 when the vacuum degree approaches the limit, and works in coordination with the vacuum system 1.

[0051] Specifically, the bell jar 2 is connected to the resistance gauge 4 and the ionization gauge 5 through interfaces, forming an all-round monitoring system for the vacuum environment. During the operation of the vacuum system 1, the resistance gauge 4 monitors the vacuum degree in the bell jar in real time, and feeds back the current vacuum level by measuring the change in air pressure. This monitoring mechanism can adjust the working state of the vacuum system 1 in time to ensure that the preset vacuum degree standard is reached before the antimony powder 6-1 is heated, thereby providing a stable low-pressure environment for the melting process.

[0052] When the vacuum degree approaches the limit state, the ionization gauge 5 takes over the monitoring function of the resistance gauge 4. The ionization gauge 5 can measure the vacuum degree in the bell jar more accurately under extremely low pressure. It uses the weak current generated by the ionized gas to measure the vacuum degree. This method has high accuracy under extremely low pressure environment. The ionization gauge 5 works in conjunction with the vacuum system 1 to further optimize the stability and purity of the vacuum environment during the melting process through precise monitoring and feedback. The entire system ensures that the antimony powder 6-1 is melted under high vacuum conditions through the coordinated use of the resistance gauge 4 and the ionization gauge 5, effectively preventing oxidation and contamination, and improving the final quality of the antimony beads 8.

[0053] The melting tool 6 is made of metal molybdenum.

[0054] Specifically, molybdenum has a relatively high melting point and poor wettability with antimony, making it easy to form the antimony beads 8 .

[0055] Please refer to the attached Figure 5 A quantitative melting method for an antimony bead evaporation source, used in conjunction with the above-mentioned quantitative melting device for an antimony bead evaporation source, comprises the following steps:

[0056] S1, nickel wire winding and fixing: the purified nickel wire 6-2 is evenly wound on the melting tool 6, and the nickel wire 6-2 is fixed in the middle position of the groove of the antimony powder 6-1 through the wire groove;

[0057] S2. Add antimony powder: Add high-purity antimony powder 6-1 into the groove in the melting tool 6, so that the antimony powder 6-1 is flush with the surface of the tool;

[0058] S3, installing the melting tool 6: fixing the melting tool 6 on the electrode 7 of the antimony bead 8 melting device through the electrode hole 6-3;

[0059] S4, install a plurality of melting tools 6 in sequence according to steps S1 to S3;

[0060] S5, evacuate and preliminarily heat: lower the bell jar 2, start the vacuum system 1 to evacuate, and after the vacuum in the bell jar 2 reaches a certain degree, energize and heat the electrode 7, with the current not exceeding 1.5A, to degas and purify the antimony powder 6-1;

[0061] S6, filling with argon: close the vacuum system 1, fill the bell jar 2 with high-purity argon, and adjust the vacuum degree in the bell jar 2 to a suitable range;

[0062] S7, further heating and melting the antimony beads 8: continue to increase the current of the electrode 7 to 2.5A-3.0A, so that the antimony powder 6-1 is completely melted and condensed into beads, and finally the molten antimony beads 8 are wrapped around the nickel wire 6-2;

[0063] S8, cooling and taking out the antimony beads 8: After the melting is completed, the current of the electrode 7 is adjusted to 0A, and after cooling for a period of time, the bell jar 2 is opened, the melted antimony beads 8 are taken out, and properly stored for subsequent processes.

[0064] The range of vacuum degree reached in step S5 is 4×10 -4 Pa-6×10 -4 Pa, in step S5, electric heating is required for 25-35 minutes.

[0065] In step S6, the vacuum degree is adjusted to a suitable range of 0.8×105Pa-1.2×105Pa.

[0066] The cooling period in step S8 is 55-65 minutes.

[0067] Based on the above embodiments, the present invention further provides a preferred embodiment: a quantitative melting method for an antimony bead evaporation source, comprising the following steps:

[0068] S1, winding and fixing the nickel wire 6-2: winding the purified nickel wire 6-2 evenly on the melting tool 6, and fixing the nickel wire 6-2 in the middle position of the groove of the antimony powder 6-1 through the wire groove;

[0069] S2, adding antimony powder 6-1: adding high-purity antimony powder 6-1 into the groove in the melting tool 6, so that the antimony powder 6-1 is flush with the surface of the tool;

[0070] S3, installing the melting tool: fixing the melting tool 6 on the electrode 7 of the antimony bead 8 melting device through the electrode hole 6-3;

[0071] S4, installing multiple melting tools: installing multiple melting tools 6 in sequence according to S1 to S3;

[0072] S5, vacuuming and preliminary heating: lower the bell jar 2, start the vacuum system 1 to vacuumize, and wait until the vacuum degree in the bell jar 2 reaches 5×10 -4After Pa, the electrode 7 is energized and heated for 30 minutes, with the current not exceeding 1.5A, to degas and purify the antimony powder 6-1;

[0073] S6, filling with argon: close the vacuum system 1, fill the bell jar 2 with high-purity argon, and adjust the vacuum degree in the bell jar 2 to 1×10 5 Pa;

[0074] S7, further heating and melting the antimony beads 8: continue to increase the current of the electrode 7 to 2.5A-3.0A, so that the antimony powder 6-1 is completely melted and condensed into beads, and finally the molten antimony beads 8 are wrapped around the nickel wire 6-2;

[0075] S8, cooling and taking out the antimony beads 8: After the melting is completed, the current of the electrode 7 is adjusted to 0A, and after cooling for 60 minutes, the bell jar 2 is opened, the melted antimony beads 8 are taken out, and properly stored for subsequent processes.

[0076] Experiment 1: Reflectivity Test

[0077] Purpose: To evaluate and compare the surface reflectivity of reflective photocathodes prepared by the method of the present invention and conventional methods, in order to verify the effectiveness of the present invention in improving cathode reflectivity.

[0078] Experimental setup: Antimony bead weight consistency comparison

[0079] 1. Sample preparation:

[0080] Experimental group: 10 samples of the embodiments prepared by the method of the present invention.

[0081] Control group: samples prepared by traditional method. The traditional method uses hydrogen burner to heat antimony beads, does not include the step of using mold to control the weight of antimony powder, and is a process controlled only by operating experience.

[0082] 2. Test equipment:

[0083] The weight of 10 samples was weighed using an analytical balance with a precision of 0.01 mg.

[0084] Experimental procedures

[0085] 1. Prepare the test sample:

[0086] The experimental and control group samples were placed in a dust-free environment to ensure that there was no dust and contaminants on the sample surface.

[0087] 2.Weight measurement:

[0088] Place the analytical balance on a horizontal anti-vibration table to ensure the accuracy of the analytical balance test.

[0089] Zero the balance, place the first sample in the middle of the pan, and measure and record the sample weight.

[0090] Repeat the above steps for all experimental and control group samples.

[0091] The results are shown in Table 1:

[0092] Table 1 Weight test data of antimony bead samples

[0093] Sample No. Weight of experimental group (mg) Weight of control group (mg) 1 0.98 1.12 2 1.02 1.03 3 1.01 1.42 4 0.99 0.94 5 0.97 1.29 6 1.02 1.54 7 1.04 1.01 8 1.01 0.99 9 0.98 1.24 10 0.99 1.32 Standard Deviation 0.02 0.20

[0094] Summary: According to the test data of the antimony bead weight in Table 1, the present invention significantly improves the consistency of the antimony bead weight by controlling the weight of antimony powder using an antimony bead melting tool.

[0095] For the samples in the control group, the weight of antimony powder was controlled by relying on operating experience, and the weight discreteness of antimony beads increased. This verifies that the melting tooling has significant advantages in controlling the weight of antimony beads.

[0096] In summary, the present invention realizes the quantitative melting of antimony beads through the antimony bead melting tool, significantly improves the consistency of the antimony beads, and further improves the consistency of the photocathode preparation process.

[0097] Experiment 2: Purity comparison experiment

[0098] Purpose:

[0099] The purity of antimony beads prepared by the method of the present invention and the traditional method was evaluated and compared, and the oxygen (O) and carbon (C) contents in the antimony beads were tested to verify the effect of the present invention in reducing impurities.

[0100] Experimental groups:

[0101] Experimental group: antimony beads prepared using the quantitative melting device and method of the present invention.

[0102] Control group: antimony beads prepared using the traditional method (hydrogen burner heating).

[0103] Test indicators:

[0104] Oxygen content (O), unit: ppm (parts per million).

[0105] Carbon content (C), unit: ppm (parts per million).

[0106] Test method:

[0107] The oxygen and carbon contents in the antimony beads were measured using an oxygen and nitrogen analyzer and a carbon and sulfur analyzer, respectively. Ten antimony bead samples were taken from each group, and their oxygen and carbon contents were tested respectively, and the results were averaged.

[0108] Experimental steps:

[0109] Sample preparation:

[0110] Experimental group: According to the method of the present invention, 10 antimony bead samples were prepared using a quantitative melting device.

[0111] Control group: 10 antimony bead samples were prepared according to the traditional method (hydrogen burner heating).

[0112] Test equipment:

[0113] Oxygen and nitrogen analyzer: used to measure the oxygen content in antimony bead samples.

[0114] Carbon-Sulfur Analyzer: Used to measure the carbon content in antimony bead samples.

[0115] Testing process:

[0116] Place the antimony bead sample in a dust-free environment to ensure that the sample is not contaminated by the outside world.

[0117] Use an oxygen-nitrogen analyzer and a carbon-sulfur analyzer to test the oxygen content and carbon content of each sample, respectively, and record the test data of each sample.

[0118] Table design:

[0119] The table below is designed to record the test data of oxygen and carbon content. There are 10 samples in the experimental group and the control group. The table records the specific content of each sample and calculates the average and standard deviation.

[0120]

[0121] Summarize:

[0122] Oxygen content: The oxygen content in the antimony beads of the experimental group is expected to be significantly lower than that of the control group, because the vacuum system and argon protection in the method of the present invention effectively reduce the mixing of oxygen.

[0123] Carbon content: The carbon content in the antimony beads of the experimental group is also expected to be significantly lower than that of the control group, because the hydrogen flame used in the traditional method is easy to introduce carbon impurities, while the method of the present invention avoids carbon contamination through high vacuum and inert gas protection.

[0124] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A quantitative melting device for an antimony bead evaporation source, comprising a melting tool (6), a vacuum system (1) connected to a bell jar (2) above the device, characterized in that: The melting tool (6) is provided with a groove for accommodating antimony powder (6-1), and quantitative melting of antimony beads of different specifications is achieved by controlling the volume of the groove for the antimony powder (6-1); The melting tool (6) heats the antimony powder (6-1) through a heating component at the bottom thereof; The outside of the melting tool (6) is evenly wound with a nickel wire (6-2), and the nickel wire (6-2) is located in the middle part of the groove of the antimony powder (6-1). During the heating process, the nickel wire (6-2) contacts the antimony powder (6-1) and wraps the antimony powder (6-1) after it melts to form an antimony bead (8); The vacuum system is used to form a high vacuum environment by extracting impurity gases during the melting process, so as to prevent the antimony powder (6-1) from being oxidized or contaminated during the heating process.

2. The quantitative melting device of antimony bead evaporation source according to claim 1, characterized in that: The heating component comprises an electrode hole (6-3), the electrode hole (6-3) is arranged at the bottom of the melting tool (6), the electrode hole (6-3) is connected to an electrode (7), and a heating circuit is provided through the electrode (7) to heat the antimony powder (6-1) in a vacuum state.

3. The quantitative melting device of antimony bead evaporation source according to claim 1, characterized in that: The bell jar (2) is connected to an argon valve (3) for filling high-purity argon into the bell jar (2) after gas purification to adjust the pressure in the bell jar (2), reduce the evaporation amount of antimony powder (6-1) and maintain the purity of the melting environment.

4. The quantitative melting device of antimony bead evaporation source according to claim 1, characterized in that: The bell jar (2) is connected to a resistance gauge (4) via an interface, and the resistance gauge (4) is used to monitor the vacuum degree in the bell jar in real time when the vacuum system (1) is running.

5. The quantitative melting device of antimony bead evaporation source according to claim 1, characterized in that: The bell jar (2) is connected to an ionization gauge (5) via an interface, and is used to accurately measure the low-pressure vacuum environment in the bell jar (2) when the vacuum degree approaches a limit, and works in coordination with the vacuum system (1).

6. The device for quantitatively melting an antimony bead evaporation source according to claim 1, characterized in that: The melting tool (6) is made of metal molybdenum.

7. A quantitative melting method for antimony bead evaporation source, characterized in that: Used in conjunction with the quantitative melting device for antimony bead evaporation source according to any one of claims 1 to 6, the device comprises the following steps: S1, winding and fixing the nickel wire: winding the purified nickel wire (6-2) evenly on the melting tool (6), and fixing the nickel wire (6-2) in the middle position of the groove of the antimony powder (6-1) through the wire groove; S2, adding antimony powder: adding high-purity antimony powder (6-1) into the groove in the melting tool (6) so that the antimony powder (6-1) is flush with the surface of the tool; S3, installing the melting tool (6): fixing the melting tool (6) on the electrode (7) of the antimony bead (8) melting device through the electrode hole (6-3); S4, sequentially installing a plurality of melting tools (6) according to steps S1 to S3; S5, evacuating and preliminarily heating: lowering the bell jar (2), starting the vacuum system (1) to evacuate, and after the bell jar (2) reaches a certain vacuum degree, heating the electrode (7) with a current not exceeding 1.5A, so as to degas and purify the antimony powder (6-1); S6, filling with argon gas: closing the vacuum system (1), filling the bell jar (2) with high-purity argon gas, and adjusting the vacuum degree in the bell jar (2) to a suitable range; S7, further heating and melting the antimony beads (8): continue to increase the current of the electrode (7) to 2.5A-3.0A, so that the antimony powder (6-1) is completely melted and condensed into beads, and finally the molten antimony beads (8) are wrapped around the nickel wire (6-2); S8, cooling and taking out the antimony beads (8): After the melting is completed, the current of the electrode (7) is adjusted to 0A, and after cooling for a period of time, the bell jar (2) is opened, the melted antimony beads (8) are taken out, and properly stored for subsequent processes.

8. The quantitative melting method of antimony bead evaporation source according to claim 7, characterized in that: The range of the certain vacuum degree reached in step S5 is 4×10 -4 Pa-6×10 -4 Pa, the S5 step needs to be powered on for heating for 25-35 minutes.

9. The quantitative melting method of antimony bead evaporation source according to claim 7, characterized in that: In the step S6, the vacuum degree is adjusted to a suitable range of 0.8×10 5 Pa-1.2×10 5 Pa.

10. The quantitative melting method of antimony bead evaporation source according to claim 7, characterized in that: The cooling period in step S8 is 55-65 minutes.

Citation Information

Cited By

  • Preparation equipment and preparation process of extremely-small-size antimony ball with lead for dynode type photomultiplier evaporation source

    CN121624404A

  • Preparation equipment and preparation process for evaporating small-size lead-wired antimony ball of anode type photomultiplier tube

    CN121624404B