CN113293343B

CN113293343B - Packaging method for heat treatment of powder sample

Info

Publication number: CN113293343B
Application number: CN202110525175.4A
Authority: CN
Inventors: 程宏辉; 胡帅成; 吴瑛; 朱云峰; 陈东雷; 刘晶晶; 严凯; 秦康生
Original assignee: Yangzhou University
Current assignee: Yangzhou University
Priority date: 2021-05-14
Filing date: 2021-05-14
Publication date: 2022-09-23
Anticipated expiration: 2041-05-14
Also published as: CN113293343A

Abstract

The invention discloses a packaging method for heat treatment of a powder sample, which comprises the steps of carrying out extrusion necking treatment on one end of a pipe fitting to form a necking part; a plugging piece is placed into the pipe from the other end of the pipe fitting to the position of the necking part; connecting one end of the necking treatment with an air pump, and sucking powder to be treated from the other end of the pipe fitting; a sealing element is arranged in the pipe from the other end of the pipe fitting to seal the opening of the pipe fitting; sealing both ends of the pipe. The invention has the advantages of simple and convenient operation, safety, reliability, high efficiency, easy realization, less material consumption, repeated recycling, low processing cost and use cost, and simultaneously can ensure that the sample obtains extremely high heating speed and cooling speed in the following heat treatment process.

Description

Packaging method for heat treatment of powder sample

Technical Field

The invention belongs to the technical field of powder sample heat treatment, and particularly relates to a packaging method for a heat-treated powder sample.

Background

The heat treatment is a processing technology which basically does not change the components and the shape and the size of the material, changes the internal structure or the surface components of the material through the heat action (sometimes accompanied by deformation action and chemical action), improves the performance of the material to meet the application requirements, and is widely used in the production and preparation processes of the material. In the development process of novel functional materials, heat treatment is often involved on some easily oxidized and easily hydrolyzed powder materials. For example, during the synthesis of high-performance magnesium-based nano hydrogen storage materials, rapid heating and cooling heat treatment is sometimes required. However, these materials are extremely reactive and can easily react with water vapor and oxygen in the air to cause failure, and therefore, they need to be protected during heat treatment. In the past, people used to seal a sample in a quartz tube, then the quartz tube was placed in a tube sealing machine, the tube was evacuated, protective argon gas was introduced, and the wall of the quartz tube was heated, so as to obtain a sealed quartz tube with two closed ends and containing the sample and argon atmosphere. Then, the quartz tube in which the sample is enclosed is subjected to heat treatment. Although the method can avoid the contact of the sample with water vapor and oxygen during the heat treatment, the quartz tube has poor heat conductivity and thick wall thickness, and is easy to crack during rapid heating and cooling to cause the sample to be damaged by being exposed to the air environment, so the method can be only used for general conventional heat treatment and cannot be used for the extreme heat treatment environment of rapid heating and cooling. Moreover, after the quartz tube is subjected to heat treatment and a sample is taken out, the quartz tube can be broken, the quartz tube can be used only once and cannot be used for multiple times, the sample is not convenient to operate and take out in the box body, and broken quartz tube fragments easily cut gloves to cause air leakage and damage of the box body. Therefore, there is a need to develop a new method for encapsulating a heat-treated powder sample, which can reliably ensure effective isolation between the sample and the air environment during the whole heat treatment process, significantly increase the heating and cooling speed during the heat treatment process, and reduce the use cost by recycling.

Disclosure of Invention

This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.

The present invention has been made keeping in mind the above problems and/or problems occurring in the prior art.

In order to solve the technical problems, the invention provides the following technical scheme: a packaging method for heat treating a powder sample, comprising,

carrying out extrusion necking treatment on one end of the pipe fitting to form a necking part;

a plugging piece is placed into the pipe from the other end of the pipe fitting to the position of the necking part;

connecting one end of the necking treatment with an air pump, and sucking powder to be treated from the other end of the pipe fitting;

a sealing element is arranged in the pipe from the other end of the pipe fitting to seal the opening of the pipe fitting;

sealing both ends of the pipe.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: and performing extrusion necking treatment, wherein the extrusion necking treatment is performed at the position with an axial distance from the end part of the pipe fitting.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: and sucking the powder to be treated in a box with argon-hydrogen mixed atmosphere.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: the argon-hydrogen mixed atmosphere in the box body consists of high-purity hydrogen and high-purity argon; wherein the volume concentration of the high-purity hydrogen is 15-25%.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: the blocking piece has a certain porosity, is high temperature resistant and has a low heat conductivity coefficient.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: the plugging piece is made of quartz wool.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: the filling length of the quartz wool in the pipe fitting is 5-20 mm, the filling mass of the quartz wool is 0.02-0.08 g, and the monofilament diameter of the quartz wool is 3-5 microns.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: the length of pipe fitting is 50~400mm, the material of pipe fitting includes one of stainless steel, aluminium, copper, the external diameter of pipe fitting is 0.4~6mm, the internal diameter of pipe fitting is 0.1~5.7mm, the wall thickness of pipe fitting is 0.15~1 mm.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: and sealing the two ends of the pipe fitting, flattening the two ends of the pipe fitting, and welding and sealing the flattened part.

As a preferable aspect of the encapsulating method for heat-treating a powder sample of the present invention, wherein: and performing cold welding operation on flattened positions at two ends of the pipe fitting in the box body by welding.

Compared with the prior art, the invention has the following beneficial effects:

the packaging method for the heat treatment powder sample is simple and convenient to operate, safe and reliable, high in efficiency, easy to implement, low in used material consumption, capable of being recycled for multiple times, low in processing cost and use cost, capable of reliably ensuring effective isolation of the sample from the air environment in the heat treatment process through the thin-wall pipe fitting and the argon-hydrogen mixed atmosphere, remarkably reducing the possibility of oxidation of the sample, and capable of ensuring that the sample obtains extremely high heating speed and cooling speed in the subsequent heat treatment process.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:

FIG. 1 is a process of powder sample encapsulation in example 1 of the present invention;

FIG. 2 shows four embodiments of the present invention for reducing pipe fittings;

fig. 3 is a schematic view of the connection between the suction pump and the pipe in embodiment 1 of the present invention.

Detailed Description

In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.

In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.

Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.

Example 1

As shown in fig. 1, a process of packaging the powder sample in this embodiment specifically includes:

(1) cutting a commercially available metal thin tube by using a tube cutter to obtain a tube 100 with the length of 200mm, wherein as shown in fig. 1(a), the selected commercially available metal thin tube is made of 304 stainless steel, the outer diameter of the commercially available metal thin tube is 3mm, the inner diameter of the commercially available metal thin tube is 2mm, the wall thickness of the commercially available metal thin tube is 0.5mm, the heat transfer efficiency of rapid heating and cooling in the heat treatment process of the powder 300 to be treated can be greatly improved by using the tube 100 with thin wall thickness and thin outer diameter and high heat conductivity coefficient, and the heat transfer efficiency can be improved by more than one order of magnitude compared with a quartz tube mode;

(2) flattening the pipe fitting 100, deburring, squeezing and necking one end of the pipe fitting 100, and then cleaning to obtain the pipe fitting 100 with a necking part 101 at one end, as shown in fig. 1 (b); the necking treatment can adopt the conventional technical means, as shown in fig. 2, four necking treatment embodiments are provided, as long as the inner diameter at the necking part 101 is smaller than the initial inner diameter of the pipe fitting 100; of course, those skilled in the art can also adopt other ways of necking treatment under the teaching of the present invention, and all of them are within the protection scope of the present invention;

(3) placing the plugging member 200 from the other end of the pipe member 100, i.e. the port not subjected to the necking treatment, to the necking part 101 to obtain the pipe member 100 with the plugging member 200, as shown in fig. 1 (c); preferably, the plugging member 200 is a material with a certain porosity, high temperature resistance and low thermal conductivity; the necking part 101 and the plugging piece 200 mainly play roles in blocking and filtering, so that the phenomenon that when powder is sucked later, the powder 300 to be processed escapes from the necking end of the plugging piece 200 and enters the air suction pump 500 to waste a sample and damage the air suction pump 500 is avoided; in addition, the blocking piece 200 with high temperature resistance and low heat conductivity coefficient can play a good heat insulation effect in the following welding operation, so that the samples are prevented from being in direct contact with welding seams, and uncontrollable influence on the properties of the samples due to overhigh arc temperature is avoided;

(4) placing the pipe fitting 100 with the plugging piece 200 into a box body, sleeving the end part of the necking part 101 with an air pipe 501 to obtain the pipe fitting 100 connected with the air pipe 501, wherein the air pipe 501 is made of silica gel or polyurethane, and the air pipe 501 and the pipe fitting 100 are well attached to ensure that the powder 300 to be processed has a good filling effect in the pipe fitting 100 when air is extracted from the rear;

(5) connecting the other end of the air pipe 501 with an air inlet of the air pump 500, as shown in fig. 3, obtaining a pipe fitting 100 connected with the air pump 500, wherein the air pump 500 can be a dual-purpose air pump or a one-way air pump;

(6) putting the powder 300 to be treated to be filled into a box body;

(7) placing the powder 300 to be treated on a clean flat plate 401, wherein the clean flat plate 401 can be a glass plate with a smooth surface, a metal plate with a smooth surface or a plastic plate with a smooth surface;

(8) starting the air pump 500 to suck the powder 300 to be processed through the open end of the pipe 100, as shown in fig. 1 (d);

(9) the gas pipe 501 is pulled out, and the sealing element 400 is plugged into the other end of the pipe fitting 100, i.e. the port which is not subjected to necking treatment, as shown in fig. 1(e), preferably, the sealing element 400 is made of a material with high temperature resistance and low thermal conductivity, and the sealing element 400 can play a role in heat insulation during subsequent welding, so that a sample is prevented from being in direct contact with a welding seam, and uncontrollable influence is generated on the sample property due to an excessively high arc temperature;

(10) cutting off the excess pipe 100 with the end of the pipe not filled with anything at the end of the reducing end by using a pipe cutter so that the plugging member 200 and the sealing member 400 are substantially flush with the end of the pipe 100, as shown in fig. 1 (f);

(11) flattening the two ends of the pipe fitting 100 by using an HY-12 type tablet press to change the original circular section into a straight seam, wherein the applied pressure is 10MPa as shown in figure 1 (g);

(12) both ends of the pipe 100 are welded and sealed in the case.

The packaging method for the heat treatment powder sample is simple and convenient to operate, safe, reliable, high in efficiency, easy to achieve, few in used material consumption, capable of being recycled for multiple times, low in processing cost and use cost, and capable of ensuring that the sample obtains extremely high heating speed and cooling speed in the following heat treatment process.

Example 2

This example 2 is substantially the same as the method of example 1 except that the block piece 200 and the sealing member 400 are both quartz wool.

The quartz wool is plugged into the other end of the pipe fitting 100, namely the port which is not subjected to necking treatment, and tests show that the plugged quartz wool is not too much, and the powder 300 to be treated cannot be sucked through the quartz wool due to too much plugged quartz wool; the quartz wool is not easy to be too little, and the quartz wool is too little, so that the powder 300 to be treated can escape from the necking end of the plugging member 200 and enter the air pump 500.

Tests show that quartz wool with the mass range of 0.02-0.08 g and the monofilament diameter range of 3-5 mu m is plugged into a port of the pipe fitting 100, which is not subjected to necking treatment, and the filling length of the quartz wool in the pipe fitting 100 is 5-20 mm, so that the purpose of better absorbing the powder 300 to be treated can be achieved. Preferably, 0.06g of quartz wool with a monofilament diameter of 3 μm is plugged, and the best effect is achieved when the filling length of the quartz wool in the pipe fitting 100 is 10 mm.

Example 3

The method of the embodiment 3 is basically the same as the method of the embodiment 1, except that the box is filled with argon-hydrogen mixed atmosphere, the argon-hydrogen mixed atmosphere is composed of high-purity hydrogen and high-purity argon, the packaged powder sample is ensured to be under a reducing protective atmosphere, the powder sample is prevented from being oxidized and damaged by oxygen possibly remaining in a tubule during heat treatment, wherein the argon is inert gas, the hydrogen is gas with optimal heat conductivity and reducing property, the argon-hydrogen mixed gas can be used for realizing effective protection of the sample, the subsequent welding operation is convenient, the argon-hydrogen mixed atmosphere can reliably ensure effective isolation of the sample from an air environment in the heat treatment process, and the possibility of oxidation of the sample is remarkably reduced;

however, the content of hydrogen is not too much, so that the operation safety is affected, and tests show that the concentration range of high-purity hydrogen in the box body is 15-25%, and the protection effect is good when the rest is high-purity argon; preferably, the protection effect is best when the concentration of the high-purity hydrogen in the box body is 20%.

Example 4

This example 4 is substantially the same as example 2 except that a cold welding machine was used to weld and seal both ends of the pipe 100 in a case, wherein the welding process was performed in a continuous mode with a pulse frequency of 1Hz, a cerium tungsten electrode having a diameter of 1.6mm was used as the electrode, and the end of the cerium tungsten electrode was ground into a cone of 70 degrees. The length of the cerium-tungsten electrode exposed out of the ceramic nozzle of the welding gun is 3mm, the welding is controlled by a foot switch arranged outside the box body during welding, the pulse voltage of the welding is 20V, the current is 150A, the pulse time is 15ms, and the distance between the cerium-tungsten electrode and a welding line is 0.3 mm. Adopt the cold welding machine to weld the both ends of pipe fitting 100 in the box of argon-hydrogen mixed atmosphere and seal, do not add the welding wire and just can weld, do not need the reentrant argon gas to carry out welding protection, can improve welding efficiency and welding seam quality greatly, but greatly reduced welding process's temperature, avoid producing uncontrollable influence to the nature of the inside powder sample of pipe fitting 100, can show the possibility that reduces the sample and oxidize, can promote the heat transfer efficiency that the later stage carries out rapid heating up and cooling heat treatment greatly.

It is important to note that the construction and arrangement of the present application as shown in the various exemplary embodiments is illustrative only. Although only a few embodiments have been described in detail in this disclosure, those skilled in the art who review this disclosure will readily appreciate that many modifications are possible (e.g., variations in sizes, dimensions, structures, shapes and proportions of the various elements, values of parameters (e.g., temperatures, pressures, etc.), mounting arrangements, use of materials, colors, orientations, etc.) without materially departing from the novel teachings and advantages of the subject matter recited in this application. For example, elements shown as integrally formed may be constructed of multiple parts or elements, the position of elements may be reversed or otherwise varied, and the nature or number of discrete elements or positions may be altered or varied. Accordingly, all such modifications are intended to be included within the scope of this invention. The order or sequence of any process or method steps may be varied or re-sequenced according to alternative embodiments. In the claims, any means-plus-function clause is intended to cover the structures described herein as performing the recited function and not only structural equivalents but also equivalent structures. Other substitutions, modifications, changes and omissions may be made in the design, operating conditions and arrangement of the exemplary embodiments without departing from the scope of the present inventions. Therefore, the present invention is not limited to a particular embodiment, but extends to various modifications that nevertheless fall within the scope of the appended claims.

Moreover, in an effort to provide a concise description of the exemplary embodiments, all features of an actual implementation may not have been described (i.e., those unrelated to the presently contemplated best mode of carrying out the invention, or those unrelated to enabling the invention).

It should be appreciated that in the development of any such actual implementation, as in any engineering or design project, numerous implementation-specific decisions may be made. Such a development effort might be complex and time consuming, but would nevertheless be a routine undertaking of design, fabrication, and manufacture for those of ordinary skill having the benefit of this disclosure, without undue experimentation.

It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims

1. A packaging method for heat treating a powder sample, characterized by: comprises the steps of (a) preparing a substrate,

carrying out extrusion necking treatment on one end of the pipe fitting (100) to form a necking part (101); the material of the pipe fitting (100) comprises one of stainless steel, aluminum and copper; the inner diameter of the pipe fitting (100) is 0.1-5.7 mm;

a plugging piece (200) is placed into the pipe from the other end of the pipe (100) to the position of the necking part (101); the blocking piece (200) has a certain porosity, is resistant to high temperature and has a low thermal conductivity coefficient;

connecting one end of the necking treatment with an air pump, and sucking powder (300) to be treated from the other end of the pipe fitting (100) in a box body with argon-hydrogen mixed atmosphere;

a sealing member (400) is arranged in the pipe from the other end of the pipe fitting (100) to seal the opening of the pipe fitting (100); the sealing element (400) is made of a high-temperature-resistant material with low heat conductivity coefficient;

flattening the two ends of the pipe fitting (100), and performing cold welding operation on the flattened parts of the two ends of the pipe fitting (100) to seal the two ends of the pipe fitting (100).

2. A packaging method for heat treating powder samples according to claim 1, characterized in that: and performing extrusion necking treatment, wherein the extrusion necking treatment is performed at a position with an axial distance from the end part of the pipe fitting (100).

3. A packaging method for heat-treating powder samples according to claim 1 or 2, characterized in that: the argon-hydrogen mixed atmosphere in the box body consists of high-purity hydrogen and high-purity argon; wherein the volume concentration of the high-purity hydrogen is 15-25%.

4. A packaging method for heat treating powder samples according to claim 3, characterized in that: the plugging piece (200) is made of quartz wool.

5. The packaging method for heat-treating powder samples according to claim 4, characterized in that: the filling length of the quartz wool in the pipe fitting (100) is 5-20 mm, the filling mass of the quartz wool is 0.02-0.08 g, and the monofilament diameter of the quartz wool is 3-5 microns.

6. A packaging method for heat-treating powder samples according to any one of claims 1, 2, 4, 5, characterized in that: the length of pipe fitting (100) is 50~400mm, the external diameter of pipe fitting (100) is 0.4~6mm, the wall thickness of pipe fitting (100) is 0.15~1 mm.