WO2017152397A1 - 一种铝合金相变点的测试方法 - Google Patents

一种铝合金相变点的测试方法 Download PDF

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WO2017152397A1
WO2017152397A1 PCT/CN2016/075988 CN2016075988W WO2017152397A1 WO 2017152397 A1 WO2017152397 A1 WO 2017152397A1 CN 2016075988 W CN2016075988 W CN 2016075988W WO 2017152397 A1 WO2017152397 A1 WO 2017152397A1
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tested
sample
resistivity
temperature
temperature curve
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French (fr)
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李红英
刘蛟蛟
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Central South University
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Central South University
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Priority to US16/079,207 priority patent/US10883946B2/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
    • G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20—Metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon

Definitions

  • the invention relates to the field of physical testing of metal materials, in particular to a test method for phase change points of aluminum alloys.
  • phase transition temperature In the heat treatment process of aluminum alloy, the solid phase transformation behavior during cooling has a great influence on the mechanical properties, corrosion resistance and processing properties of aluminum alloy. Therefore, accurate measurement of phase transition temperature has important theoretical and engineering value.
  • Temperature and time are the key factors determining the solid phase transformation of aluminum alloy.
  • the cooling curve (temperature-time curve) of aluminum alloy workpiece in actual production is nonlinear, and the corresponding phase transition process is very complicated; and the cooling involved in the heat treatment process of aluminum alloy
  • the rate range is wide.
  • the quenching cooling rate is usually above 1000 ° C / min.
  • Homogenization or annealing is usually performed by furnace cooling, and the cooling rate is very small.
  • the phase change volume fraction of the aluminum alloy is low, and the precipitation phase distribution is uneven and the size is small.
  • the commonly used differential calorimetry (DSC) method is only suitable for testing the phase transition behavior occurring under constant temperature or linear cooling conditions.
  • the measurable cooling rate range is narrow (about 5-475 ° C / min), and it is easy to form impurities.
  • the peak has low sensitivity to small volume fractional phase transition behavior and small size precipitation phase, and it is difficult to form a clear phase transition peak.
  • the main object of the present invention is to provide a test method for a phase change point of an aluminum alloy, which can realize a phase change behavior and a phase transition temperature under nonlinear cooling conditions, and has a wide cooling rate range, and can capture a phase with a small volume fraction. Variable behavior and small size precipitation phase information.
  • the second sample to be tested and the third sample to be tested are separately subjected to quenching treatment and annealing treatment to obtain a second sample to be tested in a quenched state and a third sample to be tested in a fully annealed state, and a second sample to be tested in the quenched state And heating the third sample to be fully annealed to obtain a second resistivity-temperature curve and a third resistivity-temperature curve;
  • ⁇ AQ (T) is the resistivity of the second sample to be tested in the quenched state obtained at the temperature T according to the second resistivity-temperature curve
  • ⁇ FA (T) is sufficient according to the third resistivity-temperature curve
  • the resistivity of the third sample to be tested in the annealed state at temperature T, ⁇ i (T) is the resistivity of the first sample to be tested at the temperature T during the heat treatment obtained according to the first resistivity-temperature curve;
  • a phase change onset temperature and a phase change termination temperature of the sample to be tested are determined according to the relative resistivity-temperature curve.
  • determining the phase change initiation temperature and the phase transition termination temperature of the sample to be tested according to the relative resistivity-temperature curve may include:
  • a temperature corresponding to an intersection of the straight line at which the extrapolation starting baseline is located and the relative resistivity-temperature curve is a phase transition starting temperature
  • the temperature corresponding to the intersection of the straight line at which the extrapolation termination baseline is located and the relative resistivity-temperature curve is the phase transition termination temperature.
  • the heat treatment is solid solution, homogenization, annealing or aging.
  • the method further comprises: obtaining a temperature-time curve of the first sample to be tested during heat treatment cooling.
  • the second sample to be tested and the third sample to be tested are respectively subjected to quenching treatment and annealing treatment, and obtaining the second sample to be tested in the quenched state and the third sample to be tested in the fully annealed state may include:
  • the second sample to be tested and the third sample to be tested are respectively heated and insulated, so that the soluble phase in the second sample to be tested and the third sample to be tested are sufficiently dissolved into the matrix, and are respectively cooled by water quenching. Obtaining a second sample to be tested in a quenched state and a third sample to be tested in a quenched state;
  • the third sample to be tested in the quenched state is annealed at a preset temperature to minimize the resistivity and hardness of the third sample to be tested, and a third sample to be tested in a sufficiently annealed state is obtained;
  • the resistivity of the second sample to be tested in the quenched state is a theoretical maximum; and the resistivity of the third sample to be fully annealed is a theoretical minimum.
  • the heating rate of the second sample to be tested in the quenched state and the third sample to be fully annealed is Above 1000 ° C / min, and the second test sample in the quenched state and the third test sample in the fully annealed state do not undergo phase change.
  • the first sample to be tested adopts a cooling method of aerosol cooling, high pressure gas cooling, air cooling, air cooling or furnace cooling.
  • the first sample to be tested is located at a predetermined distance from the heat source for cooling.
  • the average cooling rate of the first sample to be tested is between 2.58 and 1240 ° C / min.
  • the electrical resistivity of the aluminum alloy is composed of three parts: the electrical resistivity of the aluminum matrix, the electrical resistivity of the solid solution alloy element, and the resistivity of the precipitated second phase. Calculate formula based on relative resistivity It can be seen that the relative resistivity removes the electrical resistivity of the aluminum matrix and directly reflects the phase transition behavior of the aluminum alloy.
  • the invention provides a test method for a phase change point of an aluminum alloy, which comprises obtaining a resistivity-temperature curve of a first sample to be tested during heat treatment, a resistivity-temperature curve of a quenched state of a second sample to be tested, and a third
  • the resistivity-temperature curve of the sample to be tested is fully annealed, the relative resistivity-temperature curve is obtained according to the formula, and the phase transition initiation temperature and the phase transition termination temperature of the sample to be tested are obtained by the relative resistivity-temperature curve, and the measurement is accurate. It can test the phase transition behavior and phase transition temperature under nonlinear cooling conditions, and can test the phase transition behavior of aluminum alloy in a large cooling rate range, and can capture the phase change behavior of small volume fraction and small Size precipitation phase information.
  • FIG. 1 is a diagram showing relationship between resistivity and temperature according to Embodiment 1 of the present invention.
  • Embodiment 2 is a temperature-time curve provided by Embodiment 1 of the present invention.
  • FIG. 5 is a diagram showing relationship between resistivity and temperature according to Embodiment 2 of the present invention.
  • Figure 6 is a temperature-time curve provided by Embodiment 2 of the present invention.
  • FIG. 8 is a photomicrograph of a first sample to be tested after a phase change according to a second embodiment of the present invention.
  • FIG. 9 is a diagram showing relationship between resistivity and temperature according to Embodiment 3 of the present invention.
  • Figure 10 is a temperature-time curve provided by Embodiment 3 of the present invention.
  • FIG. 11 is a relative resistivity-temperature curve of a first sample to be tested according to Embodiment 3 of the present invention.
  • Figure 13 is a graph showing the relationship between resistivity and temperature according to Embodiment 4 of the present invention.
  • Figure 14 is a temperature-time curve provided by Embodiment 4 of the present invention.
  • FIG. 16 is a photomicrograph of a first sample to be tested after phase transformation according to Embodiment 4 of the present invention.
  • Table 1 is a chemical composition table of the aluminum alloy to be tested selected in the present embodiment.
  • the chemical composition of the aluminum alloy to be tested is shown in Table 1, wherein aluminum is the balance.
  • Step 1 Cutting the aluminum alloy material to be tested to obtain at least three samples to be tested, wherein the sample to be tested has a size of 200 ⁇ 5 ⁇ 1 mm and the precision is controlled within 0.02 mm.
  • Step 2 After the first sample to be tested is solid-liquidized at 535 ° C for 2 h, the first sample to be tested is placed at a distance of 30 cm from the furnace door of the furnace for cooling (the cooling of the first sample to be tested is subjected to heat radiation in the furnace) Affecting, and the first sample to be tested can be placed in another heat source for solution heat preservation), and the first resistivity-temperature curve of the first sample to be tested is obtained by a four-probe test method during cooling, and Obtaining a temperature-time curve (cooling curve) of the first sample to be tested, wherein FIG. 1 is a relationship between resistivity and temperature provided in the first embodiment, as shown in FIG.
  • 1 , 11 is a first resistivity-temperature curve; 2 is the temperature-time curve provided for the first embodiment. As shown in FIG. 2, the temperature-time curve is non-linear, and the average cooling rate can be calculated by the data corresponding to the curve to be 2.58 ° C / min.
  • the first sample to be tested can also be cooled at other distances from the furnace door of the furnace.
  • the resistivity is tested by making an ohmic connection between the four probes equidistant from the surface of the first sample to be tested, using a constant current source to pass two external probes with a smaller current, and measuring the inside with a precision voltmeter. A voltage between the two probes, and the temperature sensor is in contact with the first sample to be tested for acquiring a temperature signal of the first sample to be tested.
  • the voltage value obtained by the accurate voltmeter and the temperature signal obtained by the temperature sensor are input into the computer, and the resistivity of the first sample to be tested can be calculated by the voltage value and a preset formula, and the calculated resistivity data and temperature are calculated in the computer.
  • the data can plot the first resistivity-temperature curve, and the computer can record the time information for the temperature signal, so the temperature and time information can be used by the computer to automatically plot the temperature-time curve.
  • Step 3 quenching and annealing the second sample to be tested and the third sample to be tested, respectively, that is, the second sample to be tested and the third sample to be tested are respectively heated and insulated to respectively make the second sample to be tested and the first
  • the soluble phase in the three samples to be tested is fully dissolved in the aluminum matrix and cooled separately by water quenching.
  • the second sample to be tested in the quenched state and the third sample to be tested in the quenched state are obtained; the third sample to be tested in the quenched state is annealed at a preset temperature to make the resistivity of the third sample to be tested and The hardness is minimum, and a third sample to be tested in a sufficiently annealed state is obtained; then, the second sample to be tested in the quenched state and the third sample to be fully annealed are heated to 535 ° C at a rate of 1000 ° C / min, respectively.
  • the second resistivity-temperature curve and the third resistivity-temperature curve that is, the resistivity-temperature curve of the second sample to be tested in the quenched state and the resistivity-temperature curve of the third sample to be tested in the fully annealed state, as shown in FIG. 12 is the resistivity-temperature curve of the second sample to be tested, 13 is the resistivity-temperature curve of the third sample to be tested, wherein the resistivity-temperature curve of the second sample to be tested and the third to be tested
  • the solid line portion of the resistivity-temperature curve of the test sample was obtained by experimental tests.
  • the preset temperatures for quenching and annealing the samples to be tested of different compositions are different, and the preset temperature can be obtained according to the properties of the sample to be tested.
  • the resistivity of the second sample to be tested in the quenched state is the theoretical maximum; the resistivity of the third sample to be fully annealed is the theoretical minimum.
  • Step 4 Obtain the relative resistivity-temperature curve according to the following formula:
  • ⁇ AQ (T) is the resistivity of the second sample to be tested in the quenched state obtained at the temperature T according to the second resistivity-temperature curve
  • ⁇ FA (T) is sufficient according to the third resistivity-temperature curve
  • the resistivity of the third sample to be tested in the annealed state at temperature T, ⁇ i (T) is the resistivity of the first sample to be tested at the temperature T during the heat treatment obtained according to the first resistivity-temperature curve
  • the resistivity of the aluminum alloy is composed of three parts: the electrical resistivity of the aluminum matrix, the resistivity of the solid solution alloy element, and the resistivity of the precipitated second phase, according to the above formula for calculating the relative resistivity. It can be seen that the relative resistivity removes the electrical resistivity of the aluminum matrix and directly reflects the phase transition behavior of the aluminum alloy.
  • the data of the resistivity corresponding to the temperature T is ⁇ AQ (T)
  • the resistivity corresponding to the temperature T is ⁇ FA (T)
  • the temperature T corresponds to a resistivity ⁇ i (T). Since the temperature T is a variable, when the temperature T changes, a plurality of sets of ⁇ AQ (T), ⁇ FA (T), and ⁇ i (T) can be obtained, according to which ⁇ AQ (T), ⁇ FA (T), and ⁇ i are obtained.
  • FIG. 3 is a relative resistivity-temperature curve provided by the first embodiment.
  • the relative resistivity of the aluminum alloy (the first sample to be tested) changes with the change of temperature during the cooling process.
  • the relative resistivity and temperature are linear at the beginning; when the phase transition occurs, the relative resistivity-temperature curve deviates from the extrapolated starting baseline, and the deviation point is the phase transition starting temperature; the phase transition is completed.
  • the relative resistivity and temperature regression linear relationship the relative resistivity-temperature curve coincides with the extrapolated termination baseline, and the regression point is the phase transition termination temperature.
  • the extrapolation starting baseline is a linear portion where the slope between the starting point and the first phase transition peak does not change on the relative resistivity-temperature curve
  • the extrapolated termination baseline is the last phase transition on the relative resistivity-temperature curve. The linear portion of the slope between the peak and the end does not change.
  • the second phase also produces a significant resistance response signal.
  • the resistivity of the aluminum alloy increases as the size of the second phase increases, and the relative resistivity decreases, and the excited phase transition The peaks bulge upwards.
  • the aluminum alloy When the size of the second phase is equal to the mean free path of the electron, the aluminum alloy has the highest resistivity and the relative resistivity is the smallest. When the size of the second phase is greater than the mean free path of the electron, the resistivity of the aluminum alloy decreases as the size of the second phase increases, and the relative resistance The rate rises, so the excited phase transition peaks are recessed downward.
  • Step 5 Determine the phase change onset temperature and phase change termination temperature of the sample to be tested according to the relative resistivity-temperature curve.
  • the method for determining the phase transition initiation temperature and the phase transition termination temperature is specifically: determining an extrapolation starting baseline and an extrapolation termination baseline respectively on the relative resistivity-temperature curve, and extrapolating the straight line of the starting baseline
  • the temperature corresponding to the intersection of the relative resistivity-temperature curve is the phase transition onset temperature; the temperature corresponding to the intersection of the line at which the extinction termination of the baseline is located and the relative resistivity-temperature curve is the phase transition termination temperature.
  • phase transition onset temperature is 510 ° C
  • phase transition termination temperature is 106 ° C
  • three phase transition peaks appear on the relative resistivity-temperature curve, indicating that the first sample to be tested
  • 4 is a micrograph of the first sample to be tested after phase transformation according to the first embodiment.
  • there are three kinds of phases in the first sample to be tested which are ⁇ phase and ⁇ ' respectively.
  • Phase and ⁇ " phase wherein the three phase transition peaks on the relative resistivity-temperature curve in Fig. 3 correspond to the ⁇ phase, ⁇ ' phase and ⁇ " phase in Fig. 4, respectively.
  • the bulk particles which are coarse and have no phase relationship with the substrate are ⁇ phase, the acicular phase of 300 nm or more and parallel to the ⁇ 001 ⁇ A1 direction is ⁇ ' phase, and the acicular phase of 100-150 nm is ⁇ " Therefore, the phase change actually occurring in the first sample to be tested is the same as the phase change in the relative resistivity-temperature curve reaction, so the initial temperature of the phase transition and the termination of the phase change can be determined by the relative resistivity-temperature curve. temperature.
  • the difference between the second embodiment and the first embodiment is as follows: 1) the chemical composition of the aluminum alloy to be tested is different; Table 2 is the chemical composition table of the aluminum alloy to be tested selected in the embodiment; the chemical composition of the aluminum alloy to be tested As shown in table 2.
  • the dimensions of the aluminum alloy to be tested are different.
  • the sample to be tested is cut into a size of 150 ⁇ 5 ⁇ 0.8 mm, and the precision is controlled within 0.02 mm.
  • the first sample to be tested, the second sample to be tested and the third sample to be tested have the same size.
  • the first sample to be tested has different solid solution heat preservation conditions and cooling conditions.
  • the first sample to be tested is air-cooled at 470 ° C for 1 h, and then air-cooled to obtain a first resistivity-temperature curve and a temperature-time curve, wherein FIG. 5 is the resistivity and temperature provided in the second embodiment.
  • Diagram, 21 is the first resistivity-temperature curve.
  • FIG. 6 is a temperature-time curve provided by the second embodiment.
  • the average cooling rate of the first sample to be tested can be calculated by the temperature-time curve to be 41.3 ° C/min.
  • the second test sample in the quenched state and the third test sample in the fully annealed state have different heating conditions.
  • the second sample to be tested in the quenched state and the third sample to be in the fully annealed state are respectively heated to 470 ° C at a rate of 1200 ° C / min to obtain a second resistivity-temperature curve and a third resistivity.
  • a temperature curve, wherein the second resistivity-temperature curve and the third resistivity-temperature curve are as shown in FIG. 5, 22 is The second resistivity-temperature curve, 23 is the third resistivity-temperature curve, and both are linear.
  • Figure 7 is a graph showing the relative resistivity-temperature curve provided in the second embodiment.
  • the method for obtaining the relative resistivity-temperature curve and the method for obtaining the phase change onset temperature and the phase change termination temperature are the same as in the first embodiment.
  • the phase change onset temperature and the phase change termination temperature of the first sample to be tested are 440 ° C and 86 ° C, respectively, and a phase change peak appears in the relative resistivity-temperature curve, indicating that the first sample to be tested is cooled.
  • Two phase transitions occur during the process.
  • 8 is a micrograph of the first sample to be tested which undergoes a phase change after cooling according to the second embodiment; as shown in FIG.
  • the ⁇ phase is a coarse block phase
  • the ⁇ ' phase is small in size, which is 10 -30 nm
  • the two phase transition peaks in FIG. 7 correspond to the ⁇ phase and the ⁇ ′ phase of the first sample to be tested, respectively. Therefore, in practice, the phase change of the first sample to be tested is the same as the phase change of the relative resistivity-temperature curve reaction, so the phase transition initiation temperature and the phase transition termination temperature can be determined by the relative resistivity-temperature curve. .
  • the difference between the third embodiment and the first embodiment is as follows: 1) the chemical composition of the aluminum alloy to be tested is different; Table 3 is the chemical composition table of the aluminum alloy to be tested selected in the embodiment; the chemistry of the aluminum alloy to be tested The ingredients are shown in Table 3.
  • the first sample to be tested has different solid solution heat preservation conditions and cooling conditions.
  • the first sample to be tested is solid-liquidized at 470 ° C for 1 h, and then subjected to high-pressure gas cooling to obtain a first resistivity-temperature curve and a temperature-time curve, wherein FIG. 9 is the resistivity and the third embodiment provided in the third embodiment.
  • Temperature diagram, 31 is the first electricity Resistance rate - temperature curve.
  • FIG. 10 is a temperature-time curve provided by the third embodiment.
  • the average cooling rate of the first sample to be tested can be calculated by the temperature-time curve to be 768.8 ° C/min.
  • the second test sample in the quenched state and the third test sample in the fully annealed state have different heating conditions.
  • the second sample to be tested in the quenched state and the third sample to be fully annealed are respectively heated to 470 ° C at a rate of 1400 ° C / min to obtain a second resistivity-temperature curve and a third resistivity.
  • a temperature profile wherein the second resistivity-temperature curve and the third resistivity-temperature curve are as shown in FIG. 9, 32 is a second resistivity-temperature curve, and 33 is a third resistivity-temperature curve, and both are Linear relationship.
  • phase change onset temperature and the phase change termination temperature of the first sample to be tested are 402 ° C and 196 ° C, respectively, and a phase change peak appears in the relative resistivity-temperature curve, indicating that the first sample to be tested is cooled.
  • a phase change occurs during the process.
  • 12 is a micrograph of the first sample to be tested which undergoes phase change after cooling according to the third embodiment; as shown in FIG.
  • the ⁇ phase is nucleated on the Al 3 Zr particles, and the size is about 30-50 nm.
  • one phase change peak in FIG. 11 corresponds to the ⁇ phase of the sample to be tested in which the phase change occurs. Therefore, in practice, the phase change of the first sample to be tested is the same as the phase change of the relative resistivity-temperature curve reaction, so the phase transition initiation temperature and the phase transition termination temperature can be determined by the relative resistivity-temperature curve. .
  • the fourth embodiment differs from the third embodiment in that the first sample to be tested has different cooling conditions.
  • the first sample to be tested is solid-liquidized at 470 ° C for 1 h, and then subjected to a gas-cooled cooling mode to obtain a first resistivity-temperature curve and a temperature-time curve, wherein FIG. 13 is provided in the fourth embodiment.
  • the first resistivity-temperature curve, 41 is the first resistivity-temperature curve;
  • FIG. 14 is the temperature provided by the fourth embodiment -
  • the time curve, as shown in FIG. 14, can be calculated from the temperature-time curve, and the average cooling rate of the first sample to be tested is 1240 ° C / min.
  • the second sample to be tested and the third sample to be tested are processed in the same manner as in the third embodiment, the same second resistivity-temperature curve and third resistivity-temperature as in the third embodiment are obtained.
  • the temperature profile (shown in Figure 13, 42 is the second resistivity-temperature curve for this embodiment, 43 is the third resistivity-temperature curve for this example, and both are linear).
  • Figure 15 is a graph showing the relative resistivity-temperature curve of the first sample to be tested provided in the fourth embodiment. As shown in FIG. 15, since the cooling rate is fast, no phase transition peak appears on the relative resistivity-temperature curve, indicating that the first sample to be tested does not have a second phase precipitated during the cooling process.
  • Fig. 16 is a photomicrograph showing the first sample to be tested which undergoes phase change after cooling according to the fourth embodiment; as shown in Fig. 16, no precipitation of ⁇ phase was observed on the Al 3 Zr particles. Therefore, in practice, the phase change of the sample to be tested is the same as the phase change of the relative resistivity-temperature curve reaction.
  • the exemplary heat treatment method for the first sample to be tested is solid solution, but the embodiment of the present invention is not limited to the heat treatment method of solid solution for the first sample to be tested, and may also be the first
  • the sample to be tested is heat treated by homogenization, annealing or aging.
  • the embodiment of the present invention exemplarily uses a cooling method such as aerosol cooling, high pressure gas cooling, air cooling, etc. for the first sample to be tested, but the embodiment of the present invention is not limited to the above cooling method, and may also adopt air cooling and furnace cooling. Cooling method.

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Abstract

一种铝合金相变点的测试方法，包括将铝合金材料进行切割，获取至少三个待测样品；对第一待测样品进行热处理，获取第一电阻率-温度曲线；对第二待测样品和第三待测样品分别进行淬火处理和退火处理，获取淬火态的第二待测样品和充分退火态的第三待测样品，并对淬火态的第二待测样品和充分退火态的第三待测样品分别进行加热，以获取第二电阻率-温度曲线和第三电阻率-温度曲线；根据获取相对电阻率-温度曲线；根据相对电阻率-温度曲线确定待测样品的相变起始温度和相变终止温度。该方法能够实现对非线性冷却条件下发生的相变行为及相变温度的测试，可测试的冷却速率范围较宽，且能够捕捉小体积分数的相变行为及小尺寸的析出相信息。

Description

一种铝合金相变点的测试方法 技术领域
本发明涉及金属材料物理测试领域，尤其涉及一种铝合金相变点的测试方法。
背景技术
在铝合金的热处理工艺中，冷却过程中的固态相变行为对铝合金的力学性能、抗腐蚀性能和加工性能具有非常大的影响。因此，准确测量相变温度具有重要的理论意义和工程价值。
温度和时间是决定铝合金固态相变的关键因素，实际生产中铝合金工件的冷却曲线(温度-时间曲线)是非线性的，对应的相变过程非常复杂；并且铝合金热处理工艺中涉及的冷却速率范围较宽，如，淬火冷却速度通常达到1000℃/min以上，均匀化或退火通常采用炉冷，其冷却速率却非常小。在较快冷却条件下，铝合金的相变体积分数较低，并且析出相分布不均匀，且尺寸较小。目前常用的差示量热扫描法(DSC)仅适用于测试恒温或者线性冷却条件下发生的相变行为，可测的冷却速率范围较窄(约5-475℃/min)，且容易形成杂峰，对于小体积分数相变行为及小尺寸析出相的敏感度低，难以形成清晰的相变峰。
发明内容
本发明的主要目的在于提供一种铝合金相变点的测试方法，能够实现对非线性冷却条件下相变行为及相变温度的测试，且冷却速率范围较宽，能够捕捉小体积分数的相变行为及小尺寸的析出相信息。
本发明采用如下技术方案：
根据预设尺寸将待测的铝合金材料进行切割，获取至少三个待测样品；
对第一待测样品进行热处理，并获取第一待测样品在热处理冷却过程中的第一电阻率-温度曲线；
对第二待测样品和第三待测样品分别进行淬火处理和退火处理，获取淬火态的第二待测样品和充分退火态的第三待测样品，并对淬火态的第二待测样品和充分退火态的第三待测样品分别进行加热，以获取第二电阻率-温度曲线和第三电阻率-温度曲线；
根据如下的公式获取相对电阻率-温度曲线：
Figure PCTCN2016075988-appb-000001
其中，ρAQ(T)为根据第二电阻率-温度曲线获取的淬火态的第二待测样品在温度T的电阻率；ρFA(T)为根据第三电阻率-温度曲线获取的充分退火态第三待测样品在温度T的电阻率，ρi(T)为根据第一电阻率-温度曲线获取的热处理过程中的第一待测样品在温度T的电阻率；
根据所述相对电阻率-温度曲线确定待测样品的相变起始温度和相变终止温度。
进一步的，所述根据相对电阻率-温度曲线确定待测样品的相变起始温度和相变终止温度可包括：
在所述相对电阻率-温度曲线上分别确定外推起始基线和外推终止基线；
以所述外推起始基线所在的直线与所述相对电阻率-温度曲线的交点所对应的温度为相变起始温度；
以所述外推终止基线所在的直线与所述相对电阻率-温度曲线的交点所对应的温度为相变终止温度。
进一步的，所述热处理为固溶、均匀化、退火或时效。
进一步的，在所述对第一待测样品进行热处理之后，还包括：获取第一待测样品在热处理冷却过程中的温度-时间曲线。
进一步的，对第二待测样品和第三待测样品分别进行淬火处理和退火处理，获取淬火态的第二待测样品和充分退火态的第三待测样品可包括：
将第二待测样品和第三待测样品分别加热并保温，以使第二待测样品和第三待测样品中的可溶相充分溶解到基体中，并分别通过水淬的方式进行冷却，获得淬火态的第二待测样品和淬火态的第三待测样品；
将淬火态的第三待测样品在预设的温度下进行退火，以使第三待测样品的电阻率和硬度均最小，获得充分退火态的第三待测样品；
其中，淬火态的第二待测样品的电阻率为理论最大值；充分退火态的第三待测样品的电阻率为理论最小值。
进一步的，当对淬火态的第二待测样品和充分退火态的第三待测样品进行加热时，淬火态的第二待测样品和充分退火态的第三待测样品的加热速率均在1000℃/min以上，且淬火态的第二待测样品和充分退火态的第三待测样品均不发生相变。
进一步的，在热处理冷却过程中，第一待测样品采用气雾冷、高压气体冷、风冷、空冷或炉冷的冷却方式。
进一步的，在热处理冷却过程中，第一待测样品位于离热源预设的距离处进行冷却。
进一步的，在热处理冷却过程中，第一待测样品的平均冷却的速率在2.58-1240℃/min之间。
本技术方案的原理为：在本发明中，铝合金的电阻率由3个部分组成：铝基体的电阻率、固溶态合金元素产生的电阻率和析出的第二相的电阻率。根据 相对电阻率计算公式
Figure PCTCN2016075988-appb-000002
可知，相对电阻率去除了铝基体的电阻率，能够直接反应铝合金的相变行为。
本发明提供的一种铝合金相变点的测试方法，通过获取的第一待测样品在热处理过程中的电阻率-温度曲线、第二待测样品淬火态的电阻率-温度曲线以及第三待测样品充分退火态的电阻率-温度曲线，根据所述公式得到相对电阻率-温度曲线，通过相对电阻率-温度曲线获取待测样品的相变起始温度和相变终止温度，测量精确，能够实现对非线性冷却条件下发生的相变行为及相变温度的测试，且能够测试铝合金在较大冷却速率范围内的相变行为，且能够捕捉小体积分数的相变行为及小尺寸的析出相信息。
附图说明
为了更清楚地说明本发明的技术方案，下面将简单介绍实施例描述中所需使用的附图，当然，以下描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以对这些附图进行修改和替换。
图1为本发明实施例一提供的电阻率与温度关系图；
图2是本发明实施例一提供的温度-时间曲线；
图3是本发明实施例一提供的第一待测样品的相对电阻率-温度曲线；
图4是本发明实施例一提供的第一待测样品发生相变后的显微组织图片；
图5是本发明实施例二提供的电阻率与温度关系图；
图6是本发明实施例二提供的温度-时间曲线；
图7是本发明实施例二提供的第一待测样品的相对电阻率-温度曲线；
图8是本发明实施例二提供的第一待测样品发生相变后的显微组织图片；
图9是本发明实施例三提供的电阻率与温度关系图；
图10是本发明实施例三提供的温度-时间曲线；
图11是本发明实施例三提供的第一待测样品的相对电阻率-温度曲线；
图12是本发明实施例三提供的第一待测样品发生相变后的显微组织图片；
图13是本发明实施例四提供的电阻率与温度关系图；
图14是本发明实施例四提供的温度-时间曲线；
图15是本发明实施例四提供的第一待测样品的相对电阻率-温度曲线；
图16是本发明实施例四提供的第一待测样品发生相变后的显微组织图片。
具体实施方式
下面将结合附图对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例，是为了阐述本发明的原理，而不是要将本发明限制于这些具体的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一
表1为本实施例选用的待测铝合金的化学成分表，待测铝合金的化学成分如表1所示，其中铝为余量。
表1
Figure PCTCN2016075988-appb-000003
本实施例提供的铝合金相变点的测试方法步骤具体如下：
步骤一：将待测的铝合金材料进行切割，获取至少三个待测样品，其中待测样品的尺寸为200×5×1mm，精度控制在0.02mm以内。
步骤二：将第一待测样品在535℃固溶保温2h后，将第一待测样品放置于离加热炉的炉门30cm处进行冷却(第一待测样品的冷却受到加热炉内热辐射的影响，且还可以将第一待测样品放置在其他热源内进行固溶保温)，在冷却的过程中通过四探针测试的方法获取第一待测样品的第一电阻率-温度曲线，并获取第一待测样品的温度-时间曲线(冷却曲线)，其中图1为本实施例一提供的电阻率与温度关系图，如图1所示，11为第一电阻率-温度曲线；图2为本实施例一提供的温度-时间曲线，如图2所示，温度-时间曲线为非线性的，且通过该曲线对应的数据能够计算出平均冷却速率为2.58℃/min。
在本实施例中，第一待测样品还可以离加热炉的炉门其他距离进行冷却。电阻率的测试是通过将等距的四个探针与第一待测样品的表面形成欧姆连接，用恒流源给2个外探针通以较小的电流，并用精准电压表测量内侧的2个探针间的电压，并且温度传感器与第一待测样品接触，用于获取第一待测样品的温度信号。精准电压表得到的电压值以及温度传感器获取的温度信号输入到计算机中，通过电压值和预设的公式可以计算出第一待测样品的电阻率，在计算机中通过计算的电阻率数据和温度数据可以绘制第一电阻率-温度曲线，并且计算机能够记录获取温度信号的时间信息，因此，通过温度数据和时间信息，计算机可以自动绘制温度-时间曲线。
步骤三：对第二待测样品和第三待测样品分别进行淬火处理和退火处理，即将第二待测样品和第三待测样品分别加热并保温，以分别使第二待测样品和第三待测样品中的可溶相充分溶解到铝基体中，并分别通过水淬的方式进行冷 却，获得淬火态的第二待测样品和淬火态的第三待测样品；将淬火态的第三待测样品在预设的温度下进行退火，以使第三待测样品的电阻率和硬度均最小，获得充分退火态的第三待测样品；然后，对淬火态的第二待测样品和充分退火态的第三待测样品分别以1000℃/min的速率加热至535℃，获得第二电阻率-温度曲线和第三电阻率-温度曲线，即淬火态第二待测样品的电阻率-温度曲线和充分退火态第三待测样品的电阻率-温度曲线，如图1所示，图1中12为第二待测样品的电阻率-温度曲线，13为第三待测样品的电阻率-温度曲线，其中，第二待测样品的电阻率-温度曲线和第三待测样品的电阻率-温度曲线的实线部分均是通过实验测试进行获得的。
在本实施例中，不同成分的待测样品进行淬火和退火的预设温度是不同的，预设温度可以根据待测样品的性质获得。淬火态的第二待测样品的电阻率为理论最大值；充分退火态的第三待测样品的电阻率为理论最小值。
步骤四：根据如下的公式获取相对电阻率-温度曲线：
Figure PCTCN2016075988-appb-000004
其中，ρAQ(T)为根据第二电阻率-温度曲线获取的淬火态的第二待测样品在温度T的电阻率；ρFA(T)为根据第三电阻率-温度曲线获取的充分退火态第三待测样品在温度T的电阻率，ρi(T)为根据第一电阻率-温度曲线获取的热处理过程中的第一待测样品在温度T的电阻率；在本实施例中，铝合金的电阻率由3个部分组成：铝基体的电阻率、固溶态合金元素产生的电阻率和析出的第二相的电阻率，根据上述相对电阻率计算公式
Figure PCTCN2016075988-appb-000005
可知，相对电阻率去除了铝基体的电阻率，能够直接反应铝合金的相变行为。
在本实施例中，在第二电阻率-温度曲线上，温度为T对应的电阻率的数据 为ρAQ(T)，在第三电阻率-温度曲线上，温度T对应的电阻率为ρFA(T)；在第一电阻率-温度曲线上，温度T对应的电阻率为ρi(T)。因温度T是变量，当温度T改变时，可以获得多组ρAQ(T)、ρFA(T)和ρi(T)，根据获得ρAQ(T)、ρFA(T)和ρi(T)的数据，根据公式
Figure PCTCN2016075988-appb-000006
可以计算不同温度下的相对电阻率的数据，并以温度T为X轴，相对电阻率为Y轴，就可以绘制相对电阻率-温度曲线，绘制的相对电阻率-温度曲线无杂峰。图3为本实施例一提供的相对电阻率-温度曲线，如图3所示，铝合金(第一待测样品)在冷却过程中，相对电阻率随着温度的改变而发生变化。铝合金在冷却过程中，开始时，相对电阻率和温度呈线性关系；当发生相变时，相对电阻率-温度曲线偏离外推起始基线，偏离点为相变起始温度；相变完成后，相对电阻率和温度回归线性关系，相对电阻率-温度曲线与外推终止基线重合，回归点为相变终止温度。其中，外推起始基线为相对电阻率-温度曲线上起始处与第一相变峰之间的斜率不发生变化的线性部分，外推终止基线为相对电阻率-温度曲线上最后一个相变峰与终止处之间的斜率不发生变化的线性部分。
铝合金在冷却过程中，当析出的第二相的尺寸接近电子的平均自由程时，会对电子产生强烈的相干散射，导致铝合金的电阻率明显上升，因此在非线性的快速冷却条件下，当第二相的体积分数较小和/或第二相的尺寸较小时，第二相也会产生明显的电阻响应信号。如图3所示，开始时，当析出的第二相的尺寸小于电子平均自由程时，铝合金的电阻率随着第二相尺寸的增加而上升，而相对电阻率下降，激发的相变峰向上凸出。当第二相的尺寸等于电子的平均自由程时，铝合金的电阻率最大，而相对电阻率最小。当第二相的尺寸大于电子的平均自由程时，铝合金的电阻率随着第二相尺寸的增加而降低，而相对电阻 率上升，所以激发的相变峰向下凹陷。
步骤五：根据相对电阻率-温度曲线确定待测样品相变起始温度和相变终止温度。
在本实施中，确定相变起始温度和相变终止温度的方法具体为：在相对电阻率-温度曲线上分别确定外推起始基线和外推终止基线，以外推起始基线所在的直线与相对电阻率-温度曲线的交点所对应的温度为相变起始温度；以外推终止基线所在的直线与相对电阻率-温度曲线的交点所对应的温度为相变终止温度。
在本实施例中，如图3所示，相变起始温度为510℃，相变终止温度为106℃，相对电阻率-温度曲线上共出现3个相变峰，表明第一待测样品共发生了三种相变，析出了3种第二相。图4为本实施例一提供的第一待测样品发生相变后的显微组织图片，如图4所示，第一待测样品的组织中共有3种相，分别为θ相、θ’相和θ”相，其中图3中相对电阻率-温度曲线上的3个相变峰分别对应图4中的θ相、θ’相和θ”相。如图4所示，粗大且与基体无位相关系的块状粒子为θ相，300nm以上且平行于{001}A1方向的针状相为θ’相，100-150nm的针状相为θ”相。故第一待测样品实际发生的相变与相对电阻率-温度曲线反应的相变结果是相同的，因此通过相对电阻率-温度曲线可以确定相变的起始温度和相变的终止温度。
在上述实施例的基础上，当需要对待测铝合金进行多次相变测试时，需要将待测铝合金切割成的至少两个待测样品进行分别进行热处理，并且获得至少两个第一电阻率-温度曲线，但是淬火态的第二待测样品的电阻率-温度曲线和充分退火态的第三待测样品的电阻率-温度曲线将作为参比曲线，不需要进行重新获取即可；并与获得的至少两个第一电阻率-温度曲线，分别确定至少两个相 对电阻率-温度曲线，从而确定相变起始温度和相变终止温度。
实施例二
本实施二与实施例一的不同之处在于：1)选用的待测铝合金的化学成分不同；表2为本实施例选用的待测铝合金的化学成分表；待测铝合金的化学成分如表2所示。
表2
Figure PCTCN2016075988-appb-000007
2)将待测铝合金切割的尺寸不同。本实施例将待测铝合金切割成的样品的尺寸150×5×0.8mm，精度控制在0.02mm以内。其中，第一待测样品、第二待测样品和第三待测样品的尺寸均相同。
3)第一待测样品固溶保温以及冷却条件不同。本实施例中将第一待测样品在470℃固溶保温1h后进行空冷，获取第一电阻率-温度曲线和温度-时间曲线，其中图5为本实施例二提供的电阻率与温度的关系图，21为第一电阻率-温度曲线。图6为本实施例二提供的温度-时间曲线，通过温度-时间曲线可以计算出第一待测样品的平均冷却速率为41.3℃/min。
4)淬火态的第二待测样品和充分退火态的第三待测样品的加热条件不同。本实施例中分别将淬火态的第二待测样品和充分退火态的第三待测样品均以1200℃/min的速率加热至470℃，获得第二电阻率-温度曲线和第三电阻率-温度曲线，其中，第二电阻率-温度曲线和第三电阻率-温度曲线如图5所示，22为 第二电阻率-温度曲线，23为第三电阻率-温度曲线，且均为线性关系。
图7是本实施例二中提供的相对电阻率-温度曲线。其中相对电阻率-温度曲线的获得方法以及获取相变起始温度和相变终止温度的方法与实施例一相同。如图7所示，第一待测样品相变起始温度和相变终止温度分别为440℃和86℃，相对电阻率-温度曲线出现了2相变峰，表明第一待测样品在冷却过程中发生两次相变。图8为本实施例二提供的冷却后发生相变的第一待测样品的显微组织图片；如图8所示，η相为粗大的块状相，η’相尺寸较小，为10-30nm，且图7中的2个相变峰分别对应发生相变的第一待测样品的η相和η’相。因此，实际中第一待测样品发生相变情况与相对电阻率-温度曲线反应的相变结果是相同的，故可以通过相对电阻率-温度曲线确定的相变起始温度和相变终止温度。
实施例三
本实施例三与实施例一的不同之处在于：1)选用的待测铝合金的化学成分不同；表3为本实施例选用的待测铝合金的化学成分表；待测铝合金的化学成分如表3所示。
表3
Figure PCTCN2016075988-appb-000008
2)第一待测样品固溶保温以及冷却条件不同。本实施例中将第一待测样品在470℃固溶保温1h后进行高压气体冷却，获取第一电阻率-温度曲线和温度-时间曲线，其中图9为本实施例三提供的电阻率与温度的关系图，31为第一电 阻率-温度曲线。图10为本实施例三提供的温度-时间曲线，通过温度-时间曲线可以计算出第一待测样品的平均冷却速率为768.8℃/min。
3)淬火态的第二待测样品和充分退火态的第三待测样品的加热条件不同。本实施例中分别将淬火态的第二待测样品和充分退火态的第三待测样品均以1400℃/min的速率加热至470℃，获得第二电阻率-温度曲线和第三电阻率-温度曲线，其中，第二电阻率-温度曲线和第三电阻率-温度曲线如图9所示，32为第二电阻率-温度曲线，33为第三电阻率-温度曲线，且均为线性关系。
图11是本实施例三提供的第一待测样品的相对电阻率-温度曲线，其中相对电阻率-温度曲线的获得方法以及获取相变起始温度和相变终止温度的方法与实施例一相同。如图11所示，第一待测样品相变起始温度和相变终止温度分别为402℃和196℃，相对电阻率-温度曲线出现了1相变峰，表明第一待测样品在冷却过程中发生一次相变。图12为本实施例三提供的冷却后发生相变的第一待测样品的显微组织图片；如图12所示，η相在Al3Zr粒子上形核，尺寸约为30-50nm，且图11中的1个相变峰对应发生相变的待测样品的η相。因此，实际中第一待测样品发生相变情况与相对电阻率-温度曲线反应的相变结果是相同的，故通过相对电阻率-温度曲线可以确定的相变起始温度和相变终止温度。
实施例四
本实施例四与实施例三的不同之处在于：第一待测样品冷却条件不同。本实施例中将第一待测样品在470℃固溶保温1h后进行气雾冷的冷却方式，获取第一电阻率-温度曲线和温度-时间曲线，其中图13为本实施例四提供的第一电阻率-温度曲线，41为第一电阻率-温度曲线；图14为本实施例四提供的温度- 时间曲线，如图14所示，通过温度-时间曲线可以计算出第一待测样品的平均冷却速率为1240℃/min。
在本实施例中，因第二待测样品和第三待测样品的处理方式与实施例三中相同，故得到与实施例三相同的第二电阻率-温度曲线和第三电阻率-温度温度曲线(图13所示，42为本实施例的第二电阻率-温度曲线，43为本实施例的第三电阻率-温度曲线，且均为线性关系)。
图15是本实施例四提供的第一待测样品的相对电阻率-温度曲线。如图15所示，由于冷却速率较快，相对电阻率-温度曲线上没有出现相变峰，说明第一待测样品在冷却过程中没有第二相析出。图16为本实施例四提供的冷却后发生相变的第一待测样品的显微组织图片；如图16所示，Al3Zr粒子上没有发现η相析出。因此，实际中待测样品发生相变情况与相对电阻率-温度曲线反应的相变结果是相同的。
值得说明的是本发明示例性的对第一待测样品采用固溶的热处理方式，但是本发明实施例中并不局限于对第一待测样品采用固溶的热处理方式，还可以对第一待测样品采用均匀化、退火或者时效等热处理的方式。本发明实施例示例性的对第一待测样品采用了气雾冷、高压气体冷、空冷等冷却方式，但是本发明实施例并不局限与上述的冷却方式，还可以采用风冷、炉冷等冷却方式。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。

Claims (9)

  1. 一种铝合金相变点的测试方法，其特征在于，
    根据预设尺寸将待测的铝合金材料进行切割，获取至少3个待测样品；
    对第一待测样品进行热处理，并获取第一待测样品在热处理冷却过程中的第一电阻率-温度曲线；
    对第二待测样品和第三待测样品分别进行淬火处理和退火处理，获取淬火态的第二待测样品和充分退火态的第三待测样品，并对淬火态的第二待测样品和充分退火态的第三待测样品分别进行加热，以获取第二电阻率-温度曲线和第三电阻率-温度曲线；
    根据如下的公式获取相对电阻率-温度曲线：
    Figure PCTCN2016075988-appb-100001
    其中，ρAQ(T)为根据第二电阻率-温度曲线获取的淬火态的第二待测样品在温度T的电阻率；ρFA(T)为根据第三电阻率-温度曲线获取的充分退火态第三待测样品在温度T的电阻率，ρi(T)为根据第一电阻率-温度曲线获取的热处理过程中的第一待测样品在温度T的电阻率；
    根据所述相对电阻率-温度曲线确定待测样品的相变起始温度和相变终止温度。
  2. 根据权利要求1所述的方法，其特征在于：所述根据相对电阻率-温度曲线确定待测样品的相变起始温度和相变终止温度包括：
    在所述相对电阻率-温度曲线上分别确定外推起始基线和外推终止基线；
    以所述外推起始基线所在的直线与所述相对电阻率-温度曲线的交点所对应的温度为相变起始温度；
    以所述外推终止基线所在的直线与所述相对电阻率-温度曲线的交点所对应的温度为相变终止温度。
  3. 根据权利要求1所述的方法，其特征在于，在所述对第一待测样品进行热处理之后，还包括：获取第一待测样品在热处理冷却过程中的温度-时间曲线。
  4. 根据权利要求1所述的方法，其特征在于，对第二待测样品和第三待测样品分别进行淬火处理和退火处理，获取淬火态的第二待测样品和充分退火态的第三待测样品，包括：
    分别将第二待测样品和第三待测样品进行加热并保温，以使第二待测样品和第三待测样品中的可溶相充分溶解到基体中，并分别通过水淬的方式进行冷却，获得淬火态的第二待测样品和淬火态的第三待测样品；
    将淬火态的第三待测样品在预设的温度下进行退火，以使第三待测样品的电阻率和硬度均最小，获得充分退火态的第三待测样品；
    其中，淬火态的第二待测样品的电阻率为理论最大值；充分退火态的第三待测样品的电阻率为理论最小值。
  5. 根据权利要求1所述的方法，其特征在于，当对淬火态的第二待测样品和充分退火态的第三待测样品分别进行加热时，淬火态的第二待测样品和充分退火态的第三待测样品的加热速率均在1000℃/min以上，且淬火态的第二待测样品和充分退火态的第三待测样品均不发生相变。
  6. 根据权利要求1所述的方法，其特征在于，所述热处理为固溶、均匀化、退火或时效。
  7. 根据权利要求1所述的方法，其特征在于，在热处理冷却过程中，第一待测样品采用气雾冷、高压气体冷、风冷、空冷或炉冷的冷却方式。
  8. 根据权利要求1所述的方法，其特征在于，在热处理冷却过程中，第一待测样品位于离热源预设的距离处进行冷却。
  9. 根据权利要求7或8所述的方法，其特征在于，在热处理冷却过程中， 第一待测样品的平均冷却的速率在2.58-1240℃/min之间。
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