CN111650236A - Method for measuring titanium alloy beta transition temperature by adopting vertical tube furnace - Google Patents
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Abstract
The invention discloses a method for measuring the beta transition temperature of titanium alloy by adopting a vertical tube furnace, which comprises the following steps: step 1, arranging a thermocouple in a sample cavity; step 2, setting a detection temperature according to the detection standard and the temperature of the phase transformation point of the titanium alloy; step 3, when the thermocouple detects that the temperature in the sample cavity reaches the detection temperature set in the step 2, starting sample loading, carrying out heat treatment on the sample and then carrying out heat preservation; step 4, after the sample is insulated, cutting off the metal wire from the upper end, and smoothly discharging the sample out of the furnace under the traction of the heavy object block at the lower end to fall into a water tank right below the sample cavity; and 5, carrying out sample preparation corrosion on the sample treated in the step 4 according to a detection standard, and judging the obtained phase change point. The invention reduces the risk that the sample exceeds the range of the uniform area in the heat treatment process and improves the success rate of the experiment.
Description
Technical Field
The invention belongs to the technical field of titanium alloy material performance measurement, and relates to a method for measuring the beta transition temperature of a titanium alloy by adopting a vertical tube furnace.
Background
The beta transus temperature (hereinafter referred to as "transformation point") of a titanium alloy is defined as the lowest temperature at which the titanium alloy is completely transformed into a beta structure during heating. The measurement of the phase transformation point requires that the heat treatment furnace is a type I furnace, and the furnace temperature uniformity is not more than +/-3 ℃. After investigation, most physicochemical laboratories with the detection capability adopt a box-type furnace or a horizontal tubular furnace and other special phase change point furnaces. Most laboratories without dedicated ovens do not perform this test, and most of these laboratories have a number of endurance or high temperature tensile universal machines each with a vertical tube oven.
The vertical tube furnace with a general mechanical high-temperature testing machine (such as a high-temperature tensile testing machine, a endurance testing machine and the like) can also meet the requirement of +/-3 ℃, the hearth is large, but the radial uniform area of the hearth is small, generally phi 20-30 mm, and an obvious temperature gradient exists from the center to the furnace wall; in addition, the upper furnace plug and the lower furnace plug are provided with transition steps, when the transition steps are directly used for heat treatment of a phase change point, a sample can often fall on the steps during discharging water quenching, so that the sample can not be discharged from the furnace within 5 seconds, and the test fails.
Disclosure of Invention
The invention aims to provide a method for measuring the beta transition temperature of titanium alloy by adopting a vertical tube furnace, which reduces the risk that a sample exceeds the range of a uniform area in the heat treatment process and improves the success rate of experiments.
The invention adopts the technical scheme that a method for measuring the beta transition temperature of titanium alloy by adopting a vertical tube furnace specifically comprises the following steps:
step 4, after the sample is insulated, cutting off the metal wire from the upper end, and smoothly discharging the sample out of the furnace under the traction of the heavy object block at the lower end to fall into a water tank right below the sample cavity;
and 5, carrying out sample preparation corrosion on the sample treated in the step 4 according to a detection standard, and judging the obtained phase change point.
The present invention is also characterized in that,
the sample cavity in the step 1 is a high-temperature-resistant quartz tube with a turned-over edge at the upper part and a wall thickness of 1-3 mm.
The number of the thermocouples is three, and the three thermocouples are inserted into the quartz tube and distributed in the sample cavity.
The three thermocouples can be respectively inserted into one quartz tube and can also be simultaneously inserted into one quartz tube.
The heights of the three thermocouples in the quartz tube are sequentially reduced, and the height difference between the thermocouple with the highest height and the thermocouple with the lowest height is 150-200 mm.
Three thermocouples can be arranged in the sample cavity, and the thermocouples are positioned in the middle of the sample cavity with the height of 120-180 mm away from the top of the sample cavity.
And 3, stringing the titanium alloy sample on a metal wire, determining the furnace entering depth, marking the position on the metal wire, hanging a heavy object block at the lower end of the metal wire, then loading the titanium alloy sample into the sample cavity, ensuring that the heavy object is positioned outside the sample cavity, and fixing the upper end of the metal wire.
And (3) the heat treatment heat preservation time in the step 3 is 30-40 minutes.
In the step 4, the time from the sample outlet cavity to the water tank of the titanium alloy sample does not exceed 3 s.
The vertical tube furnace has the beneficial effects that the sample cavity suitable for discharging and charging phase change points is arranged in the vertical tube furnace, and the length of the sample cavity in the vertical height of the center is about 100-200 mm through reasonable thermocouple layout, so that the temperature requirement can be met; in addition, different from the discharging mode of a box-type furnace and a horizontal tube furnace, the sample is made to freely fall when discharged from the furnace by utilizing gravity and quickly enter water to finish water quenching, and the whole process can be controlled within about 3 seconds (the measurement standard requirement is less than 5 seconds).
Drawings
FIG. 1 is a schematic structural diagram of a sample chamber in a method for measuring the beta transus temperature of a titanium alloy by using a vertical tube furnace according to the present invention;
FIG. 2 is a top view of a quartz tube mounted in a sample chamber in a method of measuring the beta transus temperature of a titanium alloy using a vertical tube furnace according to the present invention;
FIG. 3 is a schematic structural view of a thermocouple installed in a sample chamber in a method for measuring a beta transus temperature of a titanium alloy using a vertical tube furnace according to the present invention;
FIG. 4 is a schematic view showing a state where a sample is placed in a sample chamber in a method for measuring a beta transus temperature of a titanium alloy using a vertical tube furnace according to the present invention;
FIG. 5 is a high power plot near the beta transus temperature of a TC18 titanium alloy coupon measured using a method of the present invention for titanium alloy beta transus temperature measurement using a vertical tube furnace;
fig. 6 is a high magnification picture of the vicinity of the β transus temperature of a TC21 titanium alloy sample measured for the β transus temperature using a method of the present invention for measuring the β transus temperature of a titanium alloy using a vertical tube furnace.
In the figure, 1 is a sample chamber, 2 is a quartz tube, 3 is a thermocouple, 4 is a metal wire, 5 is a titanium alloy sample, and 6 is a heavy object block.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a method for measuring the beta transition temperature of titanium alloy by adopting a vertical tube furnace, which comprises the following steps:
the structure of the sample cavity 1 is shown in figure 1, the internal dimension of the sample cavity 1 is designed to be between 40mm and 70mm (according to the dimension of a vertical tube furnace of a mechanical high-temperature tester in each laboratory); the shape is consistent about in the sample chamber 1 so that the sample business turn over, and sample chamber 1 adopts the high temperature resistant quartz capsule that upper portion area turn-ups and wall thickness are 1 ~ 3 mm. The quartz tube conducts heat quickly and is insulating. The quartz tube has good thermal conductivity and light transmittance, and can quickly conduct heat to the inside; in addition, the quartz tube is used as a heat radiation screen, and a good temperature equalizing effect is achieved.
As shown in fig. 2 and 3, the number of the thermocouples 3 is three, and three thermocouples 3 are inserted into the quartz tube 2 and arranged in the sample chamber 1.
Three thermocouples 3 can be inserted into one quartz tube 2 respectively or simultaneously into one quartz tube 2.
The center of the sample cavity is provided with a thermocouple (A), and the other two thermocouples (B, C) are respectively and symmetrically arranged at two opposite sides of the thermocouple (A);
the heights of the three thermocouples in the quartz tube are sequentially reduced, the height difference between the thermocouple with the highest height and the thermocouple with the lowest height is 150-200 mm, so that the uniform area can be ensured to be at least within the range of 120-180 mm, the thermocouple layout is shown in figure 3, and the temperature uniformity and the vertical height range from the center to the cavity wall in the sample cavity can be controlled within +/-2 ℃ through the temperature equalizing effect of the sample cavity, so that the standard +/-3 ℃ requirement is better.
Three thermocouples can be arranged in the sample cavity, the thermocouples are positioned in the middle of the sample cavity with the height of 120-180 mm away from the top of the sample cavity, and the three thermocouples can be used for detecting the temperature uniformity from the center of the sample cavity to the furnace wall.
the specific process of the step 3 is, referring to fig. 4, stringing a titanium alloy sample 5 on a metal wire 4, determining the furnace entering depth, marking the position on the metal wire 4, hanging a weight block 6 on the lower end of the metal wire 4, then loading the titanium alloy sample 5 into the sample cavity 1, ensuring that the weight block 6 is positioned outside the sample cavity 1, and fixing the upper end of the metal wire 4. The number of samples on the wire 4 does not exceed 5.
The heat treatment and heat preservation time is 30-40 minutes.
Step 4, after the sample is insulated, cutting off the metal wire from the upper end, and smoothly discharging the sample out of the furnace under the traction of the heavy object block at the lower end to fall into a water tank right below the sample cavity;
the time from the sample cavity to the water tank for the titanium alloy sample to fall into the water tank is not more than 3 s.
And 5, carrying out sample preparation corrosion on the sample treated in the step 4 according to a detection standard, and judging the obtained phase change point.
Example 1
1. Design of sample chamber
The sample cavity adopts a quartz tube with the inner diameter of 50mm, and 3 quartz tubes with the diameter of 10mm are fixed inside the sample cavity.
2. Thermocouple arrangement
Three temperature control thermocouples are respectively inserted into the three quartz tubes and are uniformly arranged in a region of 150mm in the middle of the furnace.
3. Sample discharging and charging furnace design
Fixing a sample by adopting a high-temperature-resistant nickel-chromium wire, wherein a heavy object block at the lower end of the nickel-chromium wire weighs 200 g; the upper end of the nickel-chromium wire is fixedly suspended; a cooling water tank is arranged right below the sample cavity.
4. Temperature measurement
The temperature measurement couple is arranged in the range of 150mm in the middle, the temperature uniformity measurement result meets +/-3 ℃ of the requirement of the detection standard, and the specific data are shown in the following table 1:
TABLE 1
5. Measuring
1) Charging furnace
The titanium alloy sample with the mark number of TC18 is strung and fixed by a nickel-chromium wire, the depth of the sample entering the furnace is determined, the position of the sample is marked on the nickel-chromium wire, and a weight is hung at the lower end of the sample, so that the weight block is ensured to be positioned outside the furnace after being charged. After the temperature of the furnace is respectively raised from low to high to 865 ℃, 870 ℃, 875 ℃, 880 ℃ and 890 ℃, the sample is loaded into the middle position of the sample cavity from the upper part of the furnace after each temperature point is stable, the upper end of the nickel-chromium wire is fixed, and a group of samples are processed at different heat treatment temperature points.
2) Thermal treatment
Carrying out heat treatment on a titanium alloy sample according to the GB/T23605 standard, wherein the heat preservation time is 30 minutes;
3) discharging from the furnace
After the heat preservation of the sample is finished, cutting off the metal wires from the upper end, smoothly discharging the sample out of the furnace under the traction of the heavy object block at the lower end, and dropping the sample into a lower water tank, wherein the whole discharging time is 2 s;
4) phase change point determination
And (3) sample preparation and corrosion are carried out on the sample treated in the step (4), the phase transformation point of the sample is judged according to the detection standard of the phase transformation point, and the obtained high-power picture with the temperature of the phase transformation point of 878 ℃ and the temperature near the beta transformation temperature (870 ℃, 875 ℃ and 880 ℃) is shown in figure 5.
When the beta transus temperature was measured for a titanium alloy sample having a trade mark TC21, according to the procedure of the measurement section in example 1, the distribution of the in-furnace temperature points was selected to be 960 deg.C, 965 deg.C, 970 deg.C, 975 deg.C, 980 deg.C, and the resulting phase transition point temperature was 968 deg.C, and a high-power picture around the beta transus temperature (960 deg.C, 965 deg.C, 970 deg.C) was shown in FIG. 6.
The method for measuring the beta transition temperature of the titanium alloy by adopting the vertical tubular furnace is characterized in that a uniform area of the furnace can be expanded to phi 50-70 mm by additionally arranging a sample cavity made of a specific material in a hearth of the vertical tubular furnace, the vertical height range of the central position in the sample cavity is 150-200 mm, the whole space from the center to the wall of the sample cavity can reach +/-3 ℃, and the range of the uniform area is greatly expanded. The risk of exceeding the range of the uniform area in the heat treatment process of the sample is reduced, and the success rate of the experiment is improved.
The invention is suitable for carrying out phase change point detection items in physicochemical experiments which have mechanical high-temperature testing machines and do not have special phase change point heat treatment furnaces. The invention can reach the standard requirement of phase change point measurement, and complete the phase change point measurement experiment.
The method for measuring the beta transition temperature of the titanium alloy by adopting the vertical tube furnace has the advantages that firstly, the defect that a physicochemical laboratory lacking a special phase transition point furnace cannot carry out a phase transition point detection experiment is overcome; secondly, when the productivity of the special phase change point furnace is insufficient, the productivity can be expanded by utilizing the heat treatment furnace of the mechanical high-temperature testing machine.
Claims (9)
1. A method for measuring the beta transition temperature of titanium alloy by adopting a vertical tube furnace is characterized by comprising the following steps: the method specifically comprises the following steps:
step 1, arranging a thermocouple in a sample cavity;
step 2, setting a detection temperature according to the detection standard and the temperature of the phase transformation point of the titanium alloy;
step 3, when the thermocouple detects that the temperature in the sample cavity reaches the detection temperature set in the step 2, starting sample loading, carrying out heat treatment on the sample and then carrying out heat preservation;
step 4, after the sample is insulated, cutting off the metal wire from the upper end, and smoothly discharging the sample out of the furnace under the traction of the heavy object block at the lower end to fall into a water tank right below the sample cavity;
and 5, carrying out sample preparation corrosion on the sample treated in the step 4 according to a detection standard, and judging the obtained phase change point.
2. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 1, wherein the method comprises the following steps: and the sample cavity in the step 1 is a high-temperature-resistant quartz tube with a turned-over edge at the upper part and a wall thickness of 1-3 mm.
3. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 2, wherein the method comprises the following steps: the number of the thermocouples is three, and the three thermocouples are inserted into the quartz tube and distributed in the sample cavity.
4. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 3, wherein the method comprises the following steps: the three thermocouples can be respectively inserted into one quartz tube and can also be simultaneously inserted into one quartz tube.
5. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 4, wherein the method comprises the following steps: the heights of the three thermocouples in the quartz tube are sequentially reduced, and the height difference between the thermocouple with the highest height and the thermocouple with the lowest height is 150-200 mm.
6. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 3, wherein the method comprises the following steps: three thermocouples can be further arranged in the sample cavity, and the thermocouples are located in the middle of the sample cavity, wherein the distance from the thermocouples to the top of the sample cavity is 120-180 mm.
7. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 5, wherein the method comprises the following steps: and 3, stringing the titanium alloy sample on a metal wire, determining the furnace entering depth, marking the position on the metal wire, hanging a heavy object block at the lower end of the metal wire, then loading the titanium alloy sample into the sample cavity, ensuring that the heavy object is positioned outside the sample cavity, and fixing the upper end of the metal wire.
8. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 7, wherein the method comprises the following steps: and the heat treatment heat preservation time in the step 3 is 30-40 minutes.
9. The method for measuring the beta transus temperature of the titanium alloy by using the vertical tube furnace according to claim 7, wherein the method comprises the following steps: in the step 4, the time from the sample cavity to the water tank for the titanium alloy sample to fall into the water tank is not more than 3 s.
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