CN104614283A - Analysis method for corresponding phase change in thermal treatment machining process of metal material - Google Patents
Analysis method for corresponding phase change in thermal treatment machining process of metal material Download PDFInfo
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Abstract
Description
技术领域 technical field
本发明涉及一种金属材料热处理加工过程中的所对应物相变化的分析方法，这些金属材料包括钢铁材料，铝合金，镁合金，钛合金等，该分析方法适用于一切具有相转变的金属材料。 The present invention relates to an analysis method for corresponding phase changes in the heat treatment process of metal materials, these metal materials include iron and steel materials, aluminum alloys, magnesium alloys, titanium alloys, etc., and the analysis method is applicable to all metal materials with phase transitions .
背景技术 Background technique
金属材料在加工过程中，将改变其物质结构状态，例如，一些钢铁及部分铝、镁合金材料可通过热处理来改变其相结构及相的组成，从而达到改变及提高材料性能的目的。金属材料的微观状态的改变，一般也将引起其尺寸及其他性能的变化，例如固体材料的一级相变，均伴随着其体积及尺寸的改变。因为此类变化一般很小，且测试及数据处理过程复杂，难以实用。例如，低碳钢淬火即发生马氏体相变时，其相对尺寸变化量仅为0.1% 数量级。另外，此处理过程将经过高温（如900℃左右）加热并水淬，此过程测量的影响因素多，如果对同一材料处理前、后的尺寸测量，很难得出可信的数据结果。然而，如果测量质量与体积的比值——密度，则可测量得出可靠的微小变化的数据。 Metal materials will change their material structure state during processing. For example, some steel and some aluminum and magnesium alloy materials can change their phase structure and phase composition through heat treatment, so as to achieve the purpose of changing and improving material properties. Changes in the microscopic state of metal materials will generally cause changes in their size and other properties, such as the first-order phase transition of solid materials, which are accompanied by changes in their volume and size. Because such changes are generally small, and the testing and data processing process is complicated, it is difficult to be practical. For example, when low carbon steel undergoes martensitic transformation after quenching, its relative dimensional change is only on the order of 0.1%. In addition, this treatment process will be heated at high temperature (such as about 900°C) and quenched in water. There are many influencing factors in the measurement of this process. It is difficult to obtain reliable data results if the dimensions of the same material before and after treatment are measured. However, if you measure density, which is the ratio of mass to volume, you can measure reliable small changes.
目前，测量金属材料物相状态有数种方法，例如有传统的金相观察法，及现代的检测手段如X射线衍射、热膨胀法、示差热分析法等，间接方法有硬度测量等。但是一些传统的金相观察法费时费人力，如显微镜下难以得出物相的定量含量；现代测试方法虽然可以直观地确定物质的物相，但是对于一些中、小企业，难以配备现代大型测试仪器，而需要求助外援来分析，而且仪器操作复杂，费用高；热膨胀分析需在线测量费时、费用高；硬度测量的精度较低，测量偶然误差大、影响因素多，实验数据重复性低等。 At present, there are several methods for measuring the phase state of metal materials, such as the traditional metallographic observation method, modern detection methods such as X-ray diffraction, thermal expansion method, differential thermal analysis, etc., and indirect methods such as hardness measurement. However, some traditional metallographic observation methods are time-consuming and labor-intensive. For example, it is difficult to obtain the quantitative content of the phase under a microscope; although modern testing methods can intuitively determine the phase of the substance, it is difficult for some small and medium-sized enterprises to be equipped with modern large-scale testing. Instruments need to be analyzed by foreign aid, and the operation of the instruments is complicated and expensive; thermal expansion analysis requires online measurement, which is time-consuming and expensive; the accuracy of hardness measurement is low, the measurement has large accidental errors, many influencing factors, and low repeatability of experimental data.
发明内容 Contents of the invention
本发明的目的，是为了解决金属材料的相变分析过程中，所存在定量测量分析技术复杂、测试费用高等技术问题而提供一种金属材料热处理加工过程中的所对应物相变化的分析方法。该方法通过测试分析待测金属材料相变的密度变化，来定量表征金属材料的相变状况。 The purpose of the present invention is to provide a method for analyzing the corresponding phase changes in the heat treatment process of metal materials in order to solve the technical problems of complex quantitative measurement and analysis technology and high testing costs in the phase change analysis process of metal materials. The method quantitatively characterizes the phase transition state of the metal material by testing and analyzing the density change of the phase transition of the metal material to be tested.
本发明的技术原理 Technical principle of the present invention
金属材料的一些相转变（如一级相变）必伴随着体积的改变，即也必伴随着密度的变化。另一方面，由于密度是固体材料的一个基本的性能，其可由二次称重法（阿基米德法），用精密天平来实现测量。密度的测量受到仪器精度及仪器操作方法限制，以前的旧式天平测量，采用人工加载砝码，光标读取测量数据，操作费时费工，重复性差，误差大。因此，旧式天平难以有效的实现本发明的精确测量。以前对金属材料相转变的分析，未引起足够的重视，此前无人提出用该方法来测量和分析金属材料的相转变。 Some phase transitions of metal materials (such as first-order phase transition) must be accompanied by changes in volume, that is, changes in density. On the other hand, since density is a basic property of solid materials, it can be measured with a precision balance by the double weighing method (Archimedes method). The measurement of density is limited by the accuracy of the instrument and the method of operation of the instrument. The old-style balance measurement in the past used manual loading of weights and cursor reading of measurement data. The operation was time-consuming and labor-intensive, with poor repeatability and large errors. Therefore, it is difficult for the old balance to effectively realize the accurate measurement of the present invention. The previous analysis of the phase transition of metal materials has not attracted enough attention, and no one has proposed to use this method to measure and analyze the phase transition of metal materials.
另一方面，随着电子技术的发展，精密的电子天平一改旧式天平的繁琐的测量加载和测量结果的读取方法，测量方便，精度得到很大的提高。本申请是利用目前测量仪器的进步，将二次称重法应用于金属材料相变的这一高精度测试和定量的分析领域。 On the other hand, with the development of electronic technology, precision electronic balances have changed the cumbersome measurement loading and reading methods of measurement results of old-style balances, and the measurement is convenient and the accuracy has been greatly improved. This application utilizes the progress of the current measuring instruments to apply the secondary weighing method to the field of high-precision testing and quantitative analysis of the phase transition of metal materials.
一种金属材料热处理加工过程中的所对应物相变化的分析方法，具体包括如下步骤： A method for analyzing corresponding phase changes in the heat treatment process of metal materials, specifically comprising the following steps:
（1）、首先建立待测金属材料的温度与密度关系 (1), first establish the relationship between the temperature and density of the metal material to be tested
先测量待测金属材料经不同的热处理状态下所对应的密度，然后以热处理温度为横坐标，待测金属材料的密度为纵坐标，建立待测金属材料的热处理温度与密度即物相变化的关系式，即工作曲线； First measure the corresponding density of the metal material to be tested under different heat treatment states, then take the heat treatment temperature as the abscissa, and the density of the metal material to be tested as the ordinate, and establish the heat treatment temperature and density of the metal material to be tested, that is, the phase change. Relational formula, that is, the working curve;
所述的待测金属材料为钢铁、铝、镁、钛或铝、镁和钛合金等； The metal material to be tested is steel, aluminum, magnesium, titanium or aluminum, magnesium and titanium alloy, etc.;
所述的待测金属材料经不同的热处理状态，包括各种钢的退火、淬火和回火，以及钢及铝、镁合金的固溶、时效等状态； The metal materials to be tested are subjected to different heat treatment states, including annealing, quenching and tempering of various steels, as well as solid solution and aging states of steel, aluminum and magnesium alloys;
上述待测金属材料经不同的热处理状态所对应的密度的测量是通过使用二次称重法即阿基米德法测量而得，此测量法的具体操作步骤如下： The measurement of the density corresponding to the above-mentioned metal materials to be tested under different heat treatment states is obtained by using the secondary weighing method, that is, the Archimedes method. The specific operation steps of this measurement method are as follows:
首先，测量某一热处理状态下待测金属材料在空气中的质量，记作m 1； First, measure the mass of the metal material to be tested in the air under a certain heat treatment state, denoted as m 1 ;
然后，将某一热处理状态下的待测金属材料放置在装有液体的容器中，测量待测金属材料浸没在密度为ρ 液的液体后的质量，记作m 2 ； Then, place the metal material to be tested under a certain heat treatment state in a container filled with liquid, measure the mass of the metal material to be tested immersed in the liquid with a density of ρ liquid , and record it as m 2 ;
最后，按如下公式计算，得到上述的某一热处理状态下的待测金属材料的密度ρ 物； Finally, calculate according to the following formula to obtain the density ρ of the metal material to be measured in the above-mentioned certain heat treatment state;
； ;
上述的经不同的热处理温度后待测金属材料的密度的测量方法，也适用于经不同的热处理温度后待测金属材料的比容的测量； The above-mentioned method for measuring the density of the metal material to be tested after different heat treatment temperatures is also applicable to the measurement of the specific volume of the metal material to be tested after different heat treatment temperatures;
（2）、通过步骤（1）中的工作曲线图，根据待测材料的密度数值在工作曲线图中的位置，或通过比较不同的热处理状态下的密度，定量判断得出待测金属材料在某一热处理状态下对应的物相状况。 (2) Through the working curve diagram in step (1), according to the position of the density value of the material to be tested in the working curve diagram, or by comparing the density under different heat treatment states, it can be quantitatively judged that the metal material to be tested is in The phase state corresponding to a certain heat treatment state.
上述的一种金属材料热处理加工过程中的所对应物相变化的分析方法，也适用于金属的焊接，轧制或锻造等过程中的物相分析。 The above-mentioned method for analyzing the corresponding phase changes in the heat treatment process of metal materials is also applicable to the phase analysis in the processes of metal welding, rolling or forging.
本发明的有益效果 Beneficial effects of the present invention
本发明的一种金属材料热处理加工过程中的所对应物相变化的分析方法，将密度法应用于金属材料的相变的定量分析和研究，该方法具有精度高，对金属材料状态变化敏感，相对密度测量的精确度可达0.01%及更高。 The present invention relates to an analysis method for corresponding phase changes in the heat treatment process of metal materials. The density method is applied to the quantitative analysis and research of the phase changes of metal materials. The method has high precision and is sensitive to state changes of metal materials. The accuracy of relative density measurement can reach 0.01% and better.
进一步，本发明的一种金属材料热处理加工过程中的所对应物相变化的分析方法，可直接反映待测金属材料的微观结构的变化，分析中所用仪器为天平，简单且通用，测量时仪器无需变温、真空等特殊环境；并且过程操作简单，对待测金属材料的制备要求不高，对待测金属材料无损，数据处理简单；分析过程速度快，耗能低，耗材少，即整个分析判断的过程不要求操作人员有很高的理论知识，减少了人力，物力，财力的消耗。 Further, the analysis method of the corresponding phase change in the heat treatment process of a metal material of the present invention can directly reflect the change of the microstructure of the metal material to be measured. The instrument used in the analysis is a balance, which is simple and universal. There is no need for special environments such as variable temperature and vacuum; and the process is simple to operate, the preparation of the metal material to be tested is not high, the metal material to be tested is non-destructive, and the data processing is simple; the analysis process is fast, with low energy consumption and less consumables, which is the key point of the entire analysis and judgment. The process does not require operators to have high theoretical knowledge, which reduces the consumption of manpower, material resources and financial resources.
附图说明 Description of drawings
图1、实施例1中待测金属材料的工作曲线。 The working curve of metal material to be tested in Fig. 1, embodiment 1.
具体实施方式 Detailed ways
下面通过具体实施例并结合附图对本发明进一步阐述，但并不限制本发明。 The present invention will be further described below through specific embodiments in conjunction with the accompanying drawings, but the present invention is not limited.
本发明实施例中质量测定所用的仪器为CP153型电子数字天平，感量为10-3g，对重量为10g物体相对测量精确度可达0.01%。 The instrument used for mass determination in the embodiment of the present invention is a CP153 electronic digital balance with a sensitivity of 10 -3 g and a relative measurement accuracy of 0.01% for an object weighing 10 g.
实施例1Example 1
一种金属材料热处理加工过程中的所对应物相变化的分析方法，具体包括如下步骤： A method for analyzing corresponding phase changes in the heat treatment process of metal materials, specifically comprising the following steps:
（1）、首先建立待测金属材料的温度与密度关系 (1), first establish the relationship between the temperature and density of the metal material to be tested
先测量3个待测金属材料经不同的热处理状态下所对应的密度，然后以处理温度为横坐标，密度为纵坐标，建立待测金属材料的温度与密度的关系式，即工作曲线； First measure the corresponding densities of the three metal materials to be tested under different heat treatment states, and then use the processing temperature as the abscissa and the density as the ordinate to establish the relationship between the temperature and density of the metal material to be tested, that is, the working curve;
待分析测试的材料是牌号为2XXX的铝合金，三个金属试样的尺寸约为 20′20′10mm，重量大于10g。先经过固溶处理，本测量是其时效效果的测量。三个试样编号分别为G1，G2和G3；其中G1为100℃时效；G2为165℃时效，并指定其为待测试样；G3为300℃时效，时效时间均为5h。 The material to be analyzed and tested is an aluminum alloy with a brand name of 2XXX. The size of the three metal samples is about 20′20′10mm, and the weight is more than 10 g . After solid solution treatment first, this measurement is the measurement of its aging effect. The numbers of the three samples are G 1 , G 2 and G 3 respectively; among them, G 1 is aging at 100°C; G 2 is aging at 165°C, and is designated as the sample to be tested; G 3 is aging at 300°C, and the aging time is uniform for 5h.
三个试样以二次称重法测量密度，得到的密度分别为ρ G1=2.8395（g/cm3），ρ G2=2.8347（g/cm3）和ρ G3=2.8273（g/cm3），测量的相对误差为±0.0003（g/cm3）。 The density of the three samples was measured by the double weighing method, and the obtained densities were ρ G1 =2.8395 (g/cm 3 ), ρ G2 =2.8347 (g/cm 3 ) and ρ G3 =2.8273 (g/cm 3 ) , The relative error of measurement is ±0.0003 (g/cm 3 ).
由上述结果，G1和G3的相对密度差约为0.43%。由G1，G3可建立待测金属材料的工作曲线，具体如图1所示的斜线，线左端点为G1、右端点为G3点； From the above results, the relative density difference between G 1 and G 3 is about 0.43%. From G1 and G3 , the working curve of the metal material to be tested can be established, specifically the oblique line shown in Figure 1, the left end point of the line is G1 , and the right end point is G3 point;
（2）、由步骤（1）所得的工作曲线，根据待测材料G2的密度数值在图1中的位置（即图1中的中间的点），即可判断出待材料对应的物相（165℃时效状态）；以判断其是否是预期的相转变； (2) From the working curve obtained in step (1), according to the position of the density value of the material G2 to be tested in Figure 1 (that is, the middle point in Figure 1), the corresponding phase of the material to be tested can be judged (165°C aging state); to judge whether it is the expected phase transition;
由步骤（1）的密度测定结果知，G2在图中的位置基本处于预期的线上（密度的相对偏差仅为0.03%，在测量范围内）。 According to the density measurement results in step (1), the position of G 2 in the figure is basically on the expected line (the relative deviation of the density is only 0.03%, within the measurement range).
由此表明：（1）此时效处理的密度变化可用线性变化来近似表达；（2）G2试样的处理工艺达到了预期的结果，其密度变化符合（线性）变化规律，偏差小、可忽略，即该工艺过程及实际处理结果达到了预期工艺要求；（3）该材料的密度的近似线性变化可由固溶体合金的Vegard定理给予理论说明，但在此不再赘述。 This shows that: (1) The density change of this aging treatment can be approximated by a linear change; (2) The treatment process of the G 2 sample has achieved the expected result, and its density change conforms to the (linear) change law, with small deviation and can be Neglect, that is, the process and the actual processing results meet the expected process requirements; (3) The approximate linear change of the density of the material can be theoretically explained by the Vegard theorem of solid solution alloys, but it will not be repeated here.
此例表明了本发明的分析方法的准确性、可靠性。 This example shows the accuracy and reliability of the analytical method of the present invention.
以上所述仅是本发明的实施方式的举例，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。 The foregoing is only an example of the embodiment of the present invention. It should be pointed out that for those of ordinary skill in the art, some improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and Modifications should also be regarded as the scope of protection of the present invention.
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| CN105371996A (en) * | 2015-10-16 | 2016-03-02 | 上海应用技术学院 | Method for measuring residual stress generated by metallic material pressure processing |
| CN105698746A (en) * | 2016-01-26 | 2016-06-22 | 上海应用技术学院 | A method for measuring strain in a metal material plastic working process |
| CN106896124A (en) * | 2017-04-24 | 2017-06-27 | 上海应用技术大学 | The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process |
| CN108303441A (en) * | 2018-01-22 | 2018-07-20 | 哈尔滨工业大学 | A method of it measuring white tin in tin and tin alloy sample and is changed into gray tin ratio |
| CN111855489A (en) * | 2020-07-22 | 2020-10-30 | 有研工程技术研究院有限公司 | Method for testing solid-liquid phase change volume change rate of material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105371996A (en) * | 2015-10-16 | 2016-03-02 | 上海应用技术学院 | Method for measuring residual stress generated by metallic material pressure processing |
| CN105698746A (en) * | 2016-01-26 | 2016-06-22 | 上海应用技术学院 | A method for measuring strain in a metal material plastic working process |
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| CN106896124A (en) * | 2017-04-24 | 2017-06-27 | 上海应用技术大学 | The assay method of corresponding residual austenite content in a kind of bearing steel material heat treatment process |
| CN108303441A (en) * | 2018-01-22 | 2018-07-20 | 哈尔滨工业大学 | A method of it measuring white tin in tin and tin alloy sample and is changed into gray tin ratio |
| CN108303441B (en) * | 2018-01-22 | 2020-11-10 | 哈尔滨工业大学 | Method for determining proportion of white tin converted into gray tin in tin and tin alloy samples |
| CN111855489A (en) * | 2020-07-22 | 2020-10-30 | 有研工程技术研究院有限公司 | Method for testing solid-liquid phase change volume change rate of material |
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