Vacuum-sealed container for MnFePSi alloy fibers and vacuum sealing method

Abstract

The present disclosure relates to a MnFePSi alloy fiber vacuum sealing container and a vacuum sealing method, the MnFePSi alloy fiber vacuum sealing container is a closed quartz glass tube at both ends, and the quartz glass tube is filled with argon; a first tantalum foil sample tube is arranged in the quartz glass tube, titanium sheets are arranged on both sides of the first tantalum foil sample tube, and a second tantalum foil sample tube is arranged on one side of any one of the two titanium sheets; MnFePiSi alloy fibers are arranged in the first tantalum foil sample tube, and GdAlCo amorphous alloy fibers are arranged in the second tantalum foil sample tube. The MnFePSi alloy fiber vacuum sealing container and the vacuum sealing method provided by the present disclosure can prevent the problems that the MnFePSi alloy fibers are easily oxidized and contaminated during heat treatment.

Description

TECHNICAL FIELD

[0001] The present disclosure relates to the technical field of heat treatment, in particular to a MnFePSi alloy fiber vacuum sealing container and a vacuum sealing method. BACKGROUND

[0002] Melt-pulling MnFePSi room-temperature magnetic refrigeration micron-sized fiber magnetic refrigeration working medium needs to be heat treated at high temperature to obtain a higher main phase to achieve higher magnetic refrigeration performance and smaller thermal hysteresis. The heat treatment temperature is as high as 1100 degrees Celsius, and the heat treatment duration varies from 5 minutes to 2 days according to the alloy composition.

[0003] In the actual heat treatment process, the MnFePSi alloy fiber is extremely easy to oxidize, and after the heat treatment is completed, the broken glass tube debris is also easy to mix into the heat treated sample during the process of breaking the quartz glass tube to take out the sample, resulting in poor heat treatment effect. At present, there is still a lack of effective way to prevent the sample from being oxidized and contaminated during the vacuum heat treatment of the MnFePSi alloy fiber. SUMMARY

[0004] The present disclosure provides a MnFePSi alloy fiber vacuum sealing container and a vacuum sealing method, which can prevent the problem of easy oxidation and contamination of the MnFePSi alloy fiber during heat treatment.

[0005] According to a first aspect of the embodiments of the present disclosure, a MnFePSi alloy fiber vacuum sealing container is provided, which is a quartz glass tube with both ends closed, and the quartz glass tube is filled with argon; a first tantalum foil sample tube is arranged in the quartz glass tube, and titanium sheets are arranged on both sides of the first tantalum foil sample tube, and a second tantalum foil sample tube is arranged on one side of any one of the two titanium sheets; MnFePSi alloy fibers are arranged in the first tantalum foil sample tube, and GdAlCo amorphous alloy fibers are arranged in the second tantalum foil sample tube.

[0006] Preferably, the length of the quartz glass tube is 70 mm, the diameter is 6 mm, and the wall thickness is 1 mm.

[0007] Preferably, the length of the first tantalum foil sample tube and the second tantalum foil sample tube is 30 mm, and the wall thickness is 0.02 mm or 0.025 mm.

[0008] Preferably, the length of the titanium sheet is 30 mm, the thickness is 0.2 mm, and the width is 1 mm.

[0009] Preferably, the first tantalum foil sample tube and the second tantalum foil sample tube are in communication with the quartz glass tube.

[0010] According to a first aspect of the embodiments of the present disclosure, a vacuum sealing method is provided for preparing the MnFePSi alloy fiber vacuum sealing container of the first aspect, and the method comprises:

[0011] S1, placing the MnFePSi alloy fiber into a first tantalum foil sample tube, and placing the GdAlCo amorphous alloy fiber into a second tantalum foil sample tube;

[0012] S2, sequentially placing the second tantalum foil sample tube, a titanium sheet, the first tantalum foil sample tube, and a titanium sheet into a quartz glass tube with one end open;

[0013] S3, repeatedly performing vacuumizing and argon filling on the quartz glass tube until the quartz glass tube is in a vacuum state;

[0014] S4, performing heating treatment on the open end of the quartz glass tube in the vacuum state and sealing the open end to obtain the MnFePSi alloy fiber vacuum sealing container.

[0015] According to a third aspect of the embodiments of the present disclosure, a vacuum heat treatment method is provided, which first uses the vacuum sealing method of the second aspect to perform vacuum sealing treatment on the MnFePSi alloy fiber, and then performs heating treatment on the vacuum sealed MnFePSi alloy fiber.

[0016] The technical solutions provided by the embodiments of the present disclosure at least bring the following beneficial effects:

[0017] (1) The MnFePSi alloy fiber vacuum sealing container provided by the embodiments of the present disclosure has a simple structure, is easy to process and manufacture, and has low cost; the characteristics of the GdAlCo amorphous alloy fiber being easy to react with oxygen in the low temperature zone and the titanium sheet being easy to react with oxygen in the high temperature zone are utilized to remove residual oxygen in the double temperature zones to prevent the sample from being oxidized during heat treatment;

[0018] (2) The characteristics of high melting point and high stability of the tantalum material are utilized to isolate the contact between the MnFePSi alloy fiber and the oxygen-absorbing titanium sheet, the GdAlCo amorphous alloy fiber, and the quartz glass tube during heat treatment, to prevent the sample from being contaminated and to solve the problem of sample purity;

[0019] (3) The tantalum foil sample tube is very stable at low and high temperatures, does not react with the MnFePSi fiber material and the tube sealing quartz glass during heat treatment, does not contaminate the fiber sample, is easy to clean, and can be reused, further reducing the use cost.

[0020] It should be understood that the above general description and the following detailed description are only exemplary and explanatory, and cannot limit the present disclosure. BRIEF DESCRIPTION OF DRAWINGS

[0021] The accompanying drawings, which are incorporated into and constitute a part of the specification, illustrate embodiments consistent with the present disclosure and serve to explain the principles of the present disclosure, and do not constitute an improper limitation on the present disclosure.

[0022] Figure 1 is a structural schematic diagram of a MnFePSi alloy fiber vacuum sealed container according to an exemplary embodiment.

[0023] Figure 2 is a flow schematic diagram of a vacuum sealing method according to an exemplary embodiment.

[0024] Figure 3 is a structural schematic diagram of a ceramic round rod according to an exemplary embodiment.

[0025] Figure 4 is an application schematic diagram of a tantalum foil sample tube preparation method according to an exemplary embodiment.

[0026] Figure 5 is a structural schematic diagram of a quartz glass tube according to an exemplary embodiment.

[0027] Figure 6 is an application schematic diagram of a quartz tube glass tube sealing method according to an exemplary embodiment. DETAILED DESCRIPTION

[0028] In order for those skilled in the art to better understand the technical solutions of the present disclosure, the technical solutions in the embodiments of the present disclosure will be described clearly and completely below in conjunction with the drawings.

[0029] It should be noted that the terms "first", "second", and the like in the specification and claims of the present disclosure and the above-mentioned drawings are used to distinguish similar objects, and do not necessarily indicate a specific order or a chronological sequence. It should be understood that the data thus used can be interchanged under appropriate circumstances, so that the embodiments of the present disclosure described herein can be implemented in an order other than that illustrated or described herein. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present disclosure. Rather, they are merely examples of devices and methods consistent with some aspects of the present disclosure as detailed in the appended claims.

[0030] The embodiments of the present disclosure provide a MnFePSi alloy fiber vacuum sealed container, as shown in the figure, which comprises a quartz glass tube 1, a first tantalum foil sample tube 2, a titanium sheet 3 and a second tantalum foil sample tube 4, wherein the first tantalum foil sample tube 2 is provided with MnFePiSi alloy fibers, and the second tantalum foil sample tube 4 is provided with GdAlCo amorphous alloy fibers. Figure 1 The embodiments of the present disclosure provide a MnFePSi alloy fiber vacuum sealed container, as shown in the figure, which comprises a quartz glass tube 1, a first tantalum foil sample tube 2, a titanium sheet 3 and a second tantalum foil sample tube 4, wherein the first tantalum foil sample tube 2 is provided with MnFePiSi alloy fibers, and the second tantalum foil sample tube 4 is provided with GdAlCo amorphous alloy fibers.

[0031] In this embodiment, the MnFePSi alloy fiber vacuum sealed container is a quartz glass tube 1 sealed at both ends, and the quartz glass tube 1 is filled with argon gas; a first tantalum foil sample tube 2 is disposed inside the quartz glass tube 1, and titanium sheets 3 are disposed on both sides of the first tantalum foil sample tube 2, and a second tantalum foil sample tube 4 is disposed on one side of any one of the two titanium sheets 3.

[0032] In practical applications, the quartz glass tube 1 is 70 mm long, 6 mm in diameter, and 1 mm thick; the first tantalum foil sample tube 2 and the second tantalum foil sample tube 4 are 30 mm long and 0.02 mm or 0.025 mm thick; the titanium sheet 3 is 30 mm long, 0.2 mm thick, and 1 mm wide.

[0033] In an optional embodiment, both the first tantalum foil sample tube 2 and the second tantalum foil sample tube 4 are connected to the quartz glass tube 1, which can ensure that the vacuum level inside the first tantalum foil sample tube 2 and the second tantalum foil sample tube 4 is consistent with that inside the quartz glass tube 1.

[0034] This disclosure also provides a vacuum sealing method, such as... Figure 2 As shown, this method can be used to prepare the MnFePSi alloy fiber vacuum-sealed container in the above embodiments. Specifically, the method includes the following steps:

[0035] S1. Place MnFePSi alloy fibers into the first tantalum foil sample tube and place GdAlCo amorphous alloy fibers into the second tantalum foil sample tube.

[0036] In this embodiment, the first tantalum foil sample tube and the second tantalum foil sample tube can be made from tantalum foil as the raw material. Tantalum material has stable properties and a melting point as high as 2995 degrees Celsius. During high-temperature heat treatment, it does not react with MnFePSi alloy fibers and can protect MnFePSi, preventing titanium oxide generated by the oxygen absorber titanium during heat treatment from contaminating the MnFePSi alloy fibers.

[0037] In an optional embodiment, when fabricating the first tantalum foil sample tube and the second tantalum foil sample tube, tantalum foil with a thickness of 0.02 mm or 0.025 mm can be used as the raw material, and the tantalum foil can be cut into thin sheets 30 mm long and 12 mm wide (e.g., Figure 2 (As shown). Afterwards, a 3mm diameter can be used. Ceramic round rod (such as) Figure 3 As shown in the figure, tantalum foil is rolled into a cylinder on a cylindrical mold, and then one end is closed to prepare a tantalum foil sample tube. The preparation method of the tantalum foil sample tube is as follows: Figure 4 As shown. In this embodiment, the method for closing one end of the tantalum foil cylinder can be a closed fold-back.

[0038] In an optional embodiment, after the MnFePSi alloy fiber or the GdAlCo amorphous alloy fiber is placed into the tantalum foil sample tube, the opening end of the tantalum foil sample tube can also be closed. Since the mechanical closing method has certain gaps, the internal and external gases of the tantalum foil sample tube can be communicated.

[0039] S2, sequentially place the second tantalum foil sample tube, the titanium sheet, the first tantalum foil sample tube, and the titanium sheet into the quartz glass tube with one end open.

[0040] In this embodiment, first, the second tantalum foil sample tube wrapped with the GdAlCo amorphous alloy fiber is placed into the quartz glass tube with one end closed, and then a titanium sheet is placed. Subsequently, the first tantalum foil sample tube wrapped with the MnFePSi alloy fiber is placed into the quartz glass tube, and is closely arranged with the titanium sheet. Then, the same titanium sheet is placed (closely arranged with the first tantalum foil sample tube).

[0041] In actual application, the purity of the titanium sheet is 99.9%, the length is 30 mm, the thickness is 0.2 mm, and the width is 1 mm. The diameter of the MnFePSi alloy fiber is 40-80 μm, and the length is 5-20 mm.

[0042] In this embodiment, the quartz glass tube (as shown in Figure 5 The length of the quartz glass tube is 100 mm, the diameter is 6 mm, and the wall thickness is 1 mm.

[0043] S3, vacuumize the quartz glass tube and then fill it with argon, repeat multiple times, until the quartz glass tube is in a vacuum state.

[0044] In this embodiment, this step can be performed on a self-made or special quartz sealing tube equipment. The ultimate vacuum of the quartz sealing tube equipment can be 0.3 Pa. Specifically, first, the quartz glass tube is vacuumized to below 1 Pa by using a high vacuum mechanical pump, and then 10000 Pa of high-purity argon is filled by using a high-purity argon (99.98%) gas washing method. Repeat this process 3 times, and then fill 1000 Pa of high-purity argon into the quartz tube as a heat conduction medium to accelerate the sample heating rate during heat treatment and the cooling rate during quenching.

[0045] S4, heat and close the opening end of the quartz glass tube in a vacuum state to obtain a MnFePSi alloy fiber vacuum sealing container.

[0046] In this embodiment, the quartz tube can be sealed by using an acetylene flame. The sealing position is 70 mm away from the closed end of the quartz tube. After the sealing position is heated and softened, the quartz tube is automatically closed. Then, the softened area is pulled off. The closing method of the quartz tube is as shown in Figure 6The MnFePSi alloy fiber is vacuum sealed in the vacuum sealing container.

[0047] The embodiments of the present disclosure also provide a vacuum heat treatment method, which first uses the vacuum sealing method in the above embodiments to vacuum seal the MnFePSi alloy fiber, and then heats the vacuum sealed MnFePSi alloy fiber.

[0048] Based on the MnFePSi alloy fiber vacuum sealing container provided by the embodiments of the present disclosure, when residual oxygen does not react with the titanium sheet and the MnFePSi fiber sample in the low-temperature zone during heat treatment, the rare earth alloy is first used to react with the low-temperature oxygen-absorbing material GdAlCo amorphous alloy fiber due to the characteristic that the rare earth alloy is easy to react with oxygen at low temperature; in the high-temperature zone, the residual oxygen reacts with the titanium sheet to absorb the residual oxygen in the vacuum glass tube and protect the sample from being oxidized. In addition, the heat-treated MnFePSi fiber sample, the oxygen-absorbing titanium sheet, and the oxygen-absorbing GdAlCo amorphous alloy fiber are physically isolated by the tantalum foil sample tube: during the heat treatment process, the titanium sheet reacts with the oxygen in the quartz tube at high temperature to absorb oxygen, and the titanium sheet after absorbing oxygen becomes brittle; during the quenching process, the titanium sheet after absorbing oxygen is easily broken, and due to the existence of the tantalum foil sample tube, the internal fiber sample can be ensured not to be contaminated.

[0049] Other embodiments of the present disclosure will be apparent to those skilled in the art from consideration of the specification and practice of the aspects disclosed herein. The present disclosure is intended to cover any variations, uses or adaptations of the present disclosure following, in general, the principles of the present disclosure and including such

[0050] It should be understood that the present disclosure is not limited to the precise structures described and shown in the drawings, and that various modifications and changes can be made without departing from its scope. The scope of the present disclosure is limited only by the claims that follow.

Claims

1. A vacuum-sealed container made of MnFePSi alloy fiber, characterized in that, The MnFePSi alloy fiber vacuum-sealed container is a quartz glass tube sealed at both ends, and the quartz glass tube is filled with argon gas. A first tantalum foil sample tube is disposed inside the quartz glass tube, and titanium sheets are disposed on both sides of the first tantalum foil sample tube. A second tantalum foil sample tube is disposed on one side of either of the two titanium sheets. MnFePiSi alloy fibers are disposed in the first tantalum foil sample tube, and GdAlCo amorphous alloy fibers are disposed in the second tantalum foil sample tube. Both the first tantalum foil sample tube and the second tantalum foil sample tube are connected to the quartz glass tube.

2. The vacuum-sealed container according to claim 1, characterized in that, The quartz glass tube is 70mm long, 6mm in diameter, and 1mm thick.

3. The vacuum-sealed container according to claim 1, characterized in that, The first tantalum foil sample tube and the second tantalum foil sample tube are 30 mm long and have a wall thickness of 0.02 mm or 0.025 mm.

4. The vacuum-sealed container according to claim 1, characterized in that, The titanium sheet is 30mm long, 0.2mm thick, and 1mm wide.

5. A vacuum sealing method for preparing the MnFePSi alloy fiber vacuum-sealed container according to any one of claims 1-4, characterized in that, The method includes: S1. Place MnFePSi alloy fibers into the first tantalum foil sample tube and place GdAlCo amorphous alloy fibers into the second tantalum foil sample tube. S2. Place the second tantalum foil sample tube, the titanium sheet, the first tantalum foil sample tube, and the titanium sheet into a quartz glass tube that is open at one end in sequence. S3. First, evacuate the quartz glass tube and then fill it with argon gas, repeating this process multiple times until the quartz glass tube is in a vacuum state. S4. The open end of the quartz glass tube under vacuum is heated and then sealed to obtain the MnFePSi alloy fiber vacuum sealed container. Both the first tantalum foil sample tube and the second tantalum foil sample tube are connected to the quartz glass tube.

6. A vacuum heat treatment method, characterized in that, First, the MnFePSi alloy fiber is vacuum sealed using the vacuum sealing method described in claim 5, and then the vacuum-sealed MnFePSi alloy fiber is heat-treated.

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