CN111270056A - Method for heat treatment of alloy containing volatile element in saturated steam environment of the element - Google Patents
Method for heat treatment of alloy containing volatile element in saturated steam environment of the element Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 32
- 229920006395 saturated elastomer Polymers 0.000 title claims abstract description 28
- 229910001325 element alloy Inorganic materials 0.000 claims description 4
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- 229910052748 manganese Inorganic materials 0.000 claims description 2
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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Abstract
本发明提供了一种含易挥发元素合金在该元素的饱和蒸气环境中热处理的方法。含有易挥发元素合金在高真空环境中热处理时，热处理温度越高，易挥发元素的挥发损失越严重。通过在含有易挥发元素合金的热处理环境中放置该元素单质，当易挥发元素单质熔融挥发时，快速形成该元素的饱和蒸气环境。同时饱和蒸气环境中易挥发元素渗透进入合金中，与合金中该元素的挥发形成动态平衡，从而减少合金中易挥发元素在热处理过程中的挥发损失，促进含易挥发元素合金在热处理过程中的固相反应，制备获得高纯度物相。本方法工艺简单、成本低廉，能避免含易挥发元素合金在热处理过程中易挥发元素的挥发损失，有助于制备获得成分均匀稳定、物相纯度高的合金。The present invention provides a method for heat-treating an alloy containing a volatile element in a saturated vapor environment of the element. When the alloy containing volatile elements is heat treated in a high vacuum environment, the higher the heat treatment temperature, the more serious the volatilization loss of the volatile elements. By placing the element in a heat treatment environment containing an alloy of volatile elements, when the volatile element is melted and volatilized, a saturated vapor environment of the element is rapidly formed. At the same time, the volatile elements in the saturated steam environment penetrate into the alloy, forming a dynamic balance with the volatilization of the elements in the alloy, thereby reducing the volatilization loss of the volatile elements in the alloy during the heat treatment process, and promoting the volatile element-containing alloy during the heat treatment process. Solid-phase reaction to prepare a high-purity phase. The method has simple process and low cost, can avoid the volatilization loss of the volatile element in the heat treatment process of the alloy containing the volatile element, and is helpful for preparing the alloy with uniform and stable composition and high phase purity.
Description
技术领域technical field
本发明属于合金制备技术领域，具体涉及一种含易挥发元素合金在该元素的饱和蒸气环境中热处理的方法热处理的方法，特别适用于含易挥发元素合金的热处理。The invention belongs to the technical field of alloy preparation, in particular to a heat treatment method for an alloy containing a volatile element in a saturated vapor environment of the element, and is particularly suitable for the heat treatment of an alloy containing a volatile element.
背景技术Background technique
热处理的目的是为了消除合金中的内应力、改善合金的组织结构，而含易挥发元素合金在热处理过程中会发生易挥发元素的挥发损失，造成合金中成分不均匀，降低合金在热处理过程中的固相反应，难以获得高纯度物相，进而影响合金的力学、热学、磁学、电学等宏观性能。The purpose of heat treatment is to eliminate the internal stress in the alloy and improve the structure of the alloy. However, the volatilization loss of volatile elements will occur in the alloy containing volatile elements during the heat treatment process, resulting in uneven composition in the alloy and reducing the alloy in the heat treatment process. It is difficult to obtain a high-purity phase, which in turn affects the mechanical, thermal, magnetic, electrical and other macroscopic properties of the alloy.
从目前的研究来看，为减少含易挥发元素合金在热处理过程中易挥发元素的挥发损失，采用将含易挥发元素合金在高真空环境中进行热处理的方法，但易挥发元素具有挥发度的物理特性，即使在高真空环境中进行热处理，易挥发元素仍然会发生不同程度的挥发损失。因此亟需一种方法避免含易挥发元素合金在热处理过程中易挥发元素的挥发损失。From the current research, in order to reduce the volatilization loss of volatile elements in the heat treatment process of alloys containing volatile elements, the method of heat treatment of alloys containing volatile elements in a high vacuum environment is adopted, but the volatile elements have high volatility. Physical properties, even if heat treatment is carried out in a high vacuum environment, volatile elements will still experience volatilization losses to varying degrees. Therefore, a method is urgently needed to avoid the volatilization loss of volatile elements during heat treatment of alloys containing volatile elements.
发明内容SUMMARY OF THE INVENTION
本发明要解决的技术问题是，针对目前含易挥发元素合金在热处理过程中发生易挥发元素的挥发损失问题，通过在含有易挥发元素合金的热处理环境中放置该元素单质，当易挥发元素单质熔融挥发时，快速形成该元素的饱和蒸气环境。同时饱和蒸气环境中易挥发元素渗透进入合金中，与合金中该元素的挥发形成动态平衡，从而减少合金中易挥发元素在热处理过程中的挥发损失，促进含易挥发元素合金在热处理过程中的固相反应，制备获得高纯度物相。The technical problem to be solved by the present invention is to solve the problem of volatilization loss of volatile elements during the heat treatment process of the alloys containing volatile elements. When melting and volatilizing, a saturated vapor environment of the element is rapidly formed. At the same time, the volatile elements in the saturated steam environment penetrate into the alloy, forming a dynamic balance with the volatilization of the elements in the alloy, thereby reducing the volatilization loss of the volatile elements in the alloy during the heat treatment process, and promoting the volatile element-containing alloy during the heat treatment process. Solid-phase reaction to prepare a high-purity phase.
为了解决上述技术问题，本发明提供一种含易挥发元素合金在该元素的饱和蒸气环境中热处理的方法，含有易挥发元素合金在放置于该易挥发元素的饱和蒸气环境中热处理后制备获得高纯度含有易挥发元素合金物相。In order to solve the above technical problems, the present invention provides a method for heat-treating an alloy containing a volatile element in a saturated vapor environment of the element. Purity contains volatile element alloy phases.
作为上述技术方案的优选，本发明提供的含易挥发元素合金在该元素的饱和蒸气环境中热处理的方法进一步包括下列技术特征的部分或全部：As a preference of the above-mentioned technical solutions, the method for heat-treating an alloy containing a volatile element in a saturated vapor environment of the element provided by the present invention further includes some or all of the following technical features:
作为上述技术方案的改进，含有易挥发元素合金在放置于该易挥发元素的饱和蒸气环境中热处理后制备获得高纯度含有易挥发元素合金物相具体方法如下：打磨除去各块体原料表面氧化层并按目标合金的化学计量比称量配制，在高纯度惰性气体环境中反复熔炼3-10次，熔炼后将易挥发元素合金放置于该易挥发元素的饱和蒸气环境中退火，获得高纯度含有易挥发元素合金物相。As an improvement of the above technical scheme, the alloy containing volatile elements is heat-treated in a saturated vapor environment of the volatile elements to obtain a high-purity alloy containing volatile elements. The specific method is as follows: grinding to remove the oxide layer on the surface of each bulk raw material And prepare according to the stoichiometric ratio of the target alloy, repeatedly smelting 3-10 times in a high-purity inert gas environment, after smelting, place the volatile element alloy in the saturated vapor environment of the volatile element for annealing to obtain high-purity alloy containing volatile elements. Volatile element alloy phase.
作为上述技术方案的改进，所述易挥发元素可包括：La、Eu、Mg、Mn、Sn、K、Zn、Bi、Ca、Na、Sr、I2、S、Se、Te、P、As中的任意一种元素。As an improvement of the above technical solution, the volatile elements may include: among La, Eu, Mg, Mn, Sn, K, Zn, Bi, Ca, Na, Sr, I 2 , S, Se, Te, P, As any element of .
作为上述技术方案的改进，所述易挥发元素的饱和蒸气环境可通过在热处理的环境中放置易挥发元素单质的方式实现。As an improvement of the above technical solution, the saturated vapor environment of the volatile element can be realized by placing the simple substance of the volatile element in the heat treatment environment.
作为上述技术方案的改进，所述易挥发元素单质需要避免与合金铸锭直接接触。As an improvement of the above technical solution, the volatile element needs to avoid direct contact with the alloy ingot.
作为上述技术方案的改进，在熔炼过程中，所述含有易挥发元素合金中按照化学计量比称量配置，并且使该易挥发元素单质在合金中的量过量1-10wt％。As an improvement of the above technical solution, in the smelting process, the volatile element-containing alloy is weighed and configured according to the stoichiometric ratio, and the amount of the volatile element in the alloy is excessive by 1-10 wt%.
含有易挥发元素合金在高真空环境中热处理时，热处理温度越高，易挥发元素的挥发损失越严重。通过在含有易挥发元素合金的热处理环境中放置该元素单质，当易挥发元素单质熔融挥发时，快速形成该元素的饱和蒸气环境。同时饱和蒸气环境中易挥发元素渗透进入合金中，与合金中该元素的挥发形成动态平衡，从而减少合金中易挥发元素在热处理过程中的挥发损失，促进含易挥发元素合金在热处理过程中的固相反应，制备获得高纯度物相。When the alloy containing volatile elements is heat treated in a high vacuum environment, the higher the heat treatment temperature, the more serious the volatilization loss of the volatile elements. By placing the element in a heat treatment environment containing an alloy of volatile elements, when the volatile element is melted and volatilized, a saturated vapor environment of the element is rapidly formed. At the same time, the volatile elements in the saturated steam environment penetrate into the alloy, forming a dynamic balance with the volatilization of the elements in the alloy, thereby reducing the volatilization loss of the volatile elements in the alloy during the heat treatment process, and promoting the volatile element-containing alloy during the heat treatment process. Solid-phase reaction to prepare a high-purity phase.
与现有技术相比，本发明的技术方案具有如下有益效果：本发明提供的一种含易挥发元素合金在该元素的饱和蒸气环境中热处理的方法热处理的方法。通过将含易挥发元素合金放置于该元素的饱和蒸气环境中进行热处理，可减少合金中易挥发元素在热处理过程中的挥发损失，保证合金成分的均匀稳定。饱和蒸气环境中的易挥发元素会渗透进入合金中，促进含易挥发元素合金在热处理过程中的固相反应，制备获得高纯度物相合金。本方法工艺简单、成本低廉，能避免含易挥发元素合金在热处理过程中易挥发元素的挥发损失，有助于制备获得成分均匀稳定、物相纯度高的合金。Compared with the prior art, the technical solution of the present invention has the following beneficial effects: the present invention provides a method for heat treating an alloy containing a volatile element in a saturated vapor environment of the element. By placing the volatile element-containing alloy in a saturated vapor environment of the element for heat treatment, the volatilization loss of the volatile element in the alloy during the heat treatment process can be reduced, and the uniformity and stability of the alloy composition can be ensured. The volatile elements in the saturated vapor environment will penetrate into the alloy, promote the solid-phase reaction of the alloy containing volatile elements during the heat treatment, and prepare a high-purity phase alloy. The method has simple process and low cost, can avoid the volatilization loss of the volatile element in the heat treatment process of the alloy containing the volatile element, and is helpful for preparing the alloy with uniform and stable composition and high phase purity.
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，而可依照说明书的内容予以实施，并且为了让本发明的上述和其他目的、特征和优点能够更明显易懂，以下结合优选实施例，详细说明如下。The above description is only an overview of the technical solutions of the present invention, in order to be able to understand the technical means of the present invention more clearly, it can be implemented according to the content of the description, and in order to make the above and other purposes, features and advantages of the present invention more obvious and easy to understand , in conjunction with the preferred embodiments, the detailed description is as follows.
附图说明Description of drawings
为了更清楚地说明本发明实施例的技术方案，下面将对实施例的附图作简单地介绍。In order to describe the technical solutions of the embodiments of the present invention more clearly, the accompanying drawings of the embodiments will be briefly introduced below.
图1是本发明中实施案例1和对比案例1所制备的LaFe11Co0.8Si1.2合金的XRD图谱。FIG. 1 is the XRD patterns of the LaFe 11 Co 0.8 Si 1.2 alloys prepared in Example 1 and Comparative Example 1 in the present invention.
具体实施方式Detailed ways
下面详细说明本发明的具体实施方式，其作为本说明书的一部分，通过实施例来说明本发明的原理，本发明的其他方面、特征及其优点通过该详细说明将会变得一目了然。The specific embodiments of the present invention will be described in detail below. As part of this specification, the principles of the present invention will be illustrated by examples. Other aspects, features and advantages of the present invention will become apparent from the detailed description.
实施案例1Implementation Case 1
将高纯度块体原料(99.5％La、99.99％Fe、99.99％Si、99.95％Co)打磨除去表面氧化层并按化学计量比LaFe11Co0.8Si1.2称量配制。为了弥补La在电弧熔炼过程中的挥发，添加过量5wt％。将配制好的单质原料放入高真空水冷式铜坩埚电弧熔炼炉中，在高纯度氩气环境中反复熔炼5次，以提高合金成分的均匀性，制备获得所需合金铸锭。在升温过程中，由于La块的熔融挥发，可在密闭容器中形成La饱和蒸气环境，因此将所得合金铸锭与La块密封于高真空石英管中。且需要避免La块与合金铸锭直接接触，防止在热处理过程中La块与合金铸锭互融。将装有合金铸锭和La块的高真空石英管放入马弗炉中进行退火，退火温度为1100℃，退火时间为9天，最后用冰水淬火，最终获得在La饱和蒸气环境中退火的LaFe11Co0.8Si1.2合金。The high-purity bulk raw material (99.5% La, 99.99% Fe, 99.99% Si, 99.95% Co) was polished to remove the surface oxide layer and prepared according to the stoichiometric ratio LaFe 11 Co 0.8 Si 1.2 . In order to make up for the volatilization of La during arc melting, an excess of 5 wt% was added. The prepared elemental raw materials are put into a high-vacuum water-cooled copper crucible arc smelting furnace, and smelted 5 times in a high-purity argon environment to improve the uniformity of the alloy composition and prepare the desired alloy ingot. During the heating process, due to the melting and volatilization of the La block, a La saturated vapor environment can be formed in the airtight container, so the obtained alloy ingot and the La block are sealed in a high-vacuum quartz tube. And it is necessary to avoid direct contact between the La block and the alloy ingot, and prevent the La block and the alloy ingot from melting each other during the heat treatment process. The high-vacuum quartz tube with alloy ingots and La blocks was put into a muffle furnace for annealing, the annealing temperature was 1100 °C, the annealing time was 9 days, and finally quenched with ice water, and finally the annealing in the La saturated steam environment was obtained. LaFe 11 Co 0.8 Si 1.2 alloy.
对比案例1Comparative case 1
以与实施案例1相同的方法熔炼制备LaFe11Co0.8Si1.2合金，将所得合金铸锭密封于高真空石英管中，并未在高真空石英管中添加La块，随后将高真空石英管放入马弗炉中进行退火，退火工艺与实施案例1相同，最终获得在高真空环境中退火的LaFe11Co0.8Si1.2合金。The LaFe 11 Co 0.8 Si 1.2 alloy was prepared by smelting in the same way as in Example 1, and the obtained alloy ingot was sealed in a high vacuum quartz tube without adding La blocks to the high vacuum quartz tube. It is annealed in a muffle furnace, and the annealing process is the same as that of Example 1, and finally a LaFe 11 Co 0.8 Si 1.2 alloy annealed in a high vacuum environment is obtained.
La(Fe,Si)13基合金的物相组成为：主相NaZn13型结构相(即1:13相)、杂相富La相和α-Fe相，其中主相NaZn13型结构相由富La相和α-Fe相在退火过程中通过包晶反应形成。而La(Fe,Si)13基合金中的稀土元素La属于易挥发元素，在热处理过程中，当温度高于La的挥发温度时，La会发生挥发损失，导致La(Fe,Si)13基合金中成分不均匀，且降低富La相的含量，影响其与α-Fe相在退火过程中的包晶反应，进而使NaZn13型结构相含量降低。The phase composition of the La(Fe,Si) 13 -based alloy is: the main phase NaZn 13 type structure phase (ie 1:13 phase), the impurity phase La-rich phase and the α-Fe phase, in which the main phase NaZn 13 type structure phase consists of La-rich phase and α-Fe phase are formed through peritectic reaction during annealing. The rare earth element La in the La(Fe,Si) 13 -based alloy is a volatile element. During the heat treatment process, when the temperature is higher than the volatilization temperature of La, La will be volatilized and lost, resulting in the La(Fe, Si) 13 -based alloy. The composition of the alloy is not uniform, and the content of the La-rich phase is reduced, which affects the peritectic reaction between it and the α-Fe phase during the annealing process, thereby reducing the content of the NaZn 13 -type structural phase.
表1本发明中通过K值法计算出XRD图谱中各样品的物相含量Table 1 Calculates the phase content of each sample in the XRD pattern by the K value method in the present invention
如图1所示，分别在高真空环境中退火和在La饱和蒸气环境中退火制备的LaFe11Co0.8Si1.2合金的XRD结果。由图可知，在高真空环境中退火制备的样品中除主相LaCo13相(NaZn13型结构相)外仍然含有非常明显的α-Fe杂相，而在La饱和蒸气环境中退火制备的样品中含有主相LaCo13相和极少量的α-Fe杂相。图中并未检测到富La相的特征衍射峰，这是由于富La相的含量低于XRD的检测极限(～1％)。如表1所示，利用K值法在Jade软件中计算出XRD图谱中各样品物相组成百分比。由表1可知，在La饱和蒸气环境中退火制备的样品中主相LaCo13相的含量达到95.37％，α-Fe杂相含量为4.63％，而在高真空环境中退火制备的样品中主相LaCo13相的含量为81.17％，α-Fe杂相含量却有18.83％。对比可知，在La饱和蒸气环境中退火制备的LaFe11Co0.8Si1.2合金中主相LaCo13相含量相对更高。As shown in Fig. 1, the XRD results of the LaFe 11 Co 0.8 Si 1.2 alloy prepared by annealing in high vacuum environment and annealing in La saturated vapor environment, respectively. It can be seen from the figure that in addition to the main phase LaCo 13 phase (NaZn 13 type structure phase), the samples prepared by annealing in high vacuum environment still contain very obvious α-Fe impurity phase, while the samples prepared by annealing in La saturated vapor environment It contains the main phase LaCo 13 phase and a very small amount of α-Fe impurity phase. The characteristic diffraction peaks of the La-rich phase are not detected in the figure because the content of the La-rich phase is below the detection limit of XRD (~1%). As shown in Table 1, the phase composition percentage of each sample in the XRD pattern was calculated in the Jade software using the K value method. It can be seen from Table 1 that the content of the main phase LaCo 13 phase in the samples prepared by annealing in La saturated vapor environment reaches 95.37%, and the content of α-Fe impurity phase is 4.63%, while the main phase in the samples prepared by annealing in high vacuum environment is 95.37%. The content of LaCo 13 phase is 81.17%, but the content of α-Fe impurity phase is 18.83%. The comparison shows that the LaFe 11 Co 0.8 Si 1.2 alloy prepared by annealing in the La saturated vapor environment has a relatively higher content of the main phase LaCo 13 phase.
本方法工艺简单、成本低廉，能避免含易挥发元素合金在热处理过程中易挥发元素的挥发损失，有助于制备获得成分均匀稳定、物相纯度高的合金。The method has simple process and low cost, can avoid the volatilization loss of the volatile element in the heat treatment process of the alloy containing the volatile element, and is helpful for preparing the alloy with uniform and stable composition and high phase purity.
以上所述是本发明的优选实施方式而已，当然不能以此来限定本发明之权利范围，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和变动，这些改进和变动也视为本发明的保护范围。The above descriptions are only the preferred embodiments of the present invention, of course, it cannot limit the scope of rights of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, Several improvements and changes are made, and these improvements and changes are also regarded as the protection scope of the present invention.
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| CN101671770A (en) * | 2009-09-15 | 2010-03-17 | 西部金属材料股份有限公司 | Heat treatment method of alloy containing volatile element |
| CN109136799A (en) * | 2018-09-18 | 2019-01-04 | 广东省稀有金属研究所 | A kind of heat treatment method of the volatile metal hydrogen storage alloy containing low melting point and application |
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| CN101671770A (en) * | 2009-09-15 | 2010-03-17 | 西部金属材料股份有限公司 | Heat treatment method of alloy containing volatile element |
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