CN116106362A - Method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material - Google Patents
Method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material Download PDFInfo
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- CN116106362A CN116106362A CN202310167930.5A CN202310167930A CN116106362A CN 116106362 A CN116106362 A CN 116106362A CN 202310167930 A CN202310167930 A CN 202310167930A CN 116106362 A CN116106362 A CN 116106362A
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- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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Abstract
The invention discloses a method for measuring high-temperature specific heat capacity of a titanium alloy and a titanium-based composite material, which is characterized in that a differential scanning calorimeter segmentation method is utilized to carry out high-temperature specific heat capacity test, and a synchronous thermal analyzer is utilized to respectively obtain Differential Scanning Calorimeter (DSC) curves of a sapphire standard sample and a titanium metal material. According to the invention, the rhodium high-temperature furnace arranged on the synchronous thermal analyzer is used for carrying out sectional constant temperature rise and constant temperature test on the sample, so that DSC stability of the sample in a high-temperature section is ensured. Compared with the adiabatic calorimeter and the relaxation calorimeter, the invention has the advantages of wide measurement temperature range, small required sample amount and short test time, and can test various samples without limitation, such as films, powder, liquid and solid blocks. The sample in the invention is in argon atmosphere, so that the sample mass can be accurately weighed.
Description
Technical Field
The invention relates to the technical field of titanium alloy and titanium-based composite materials, in particular to a method for measuring the high-temperature specific heat capacity of the titanium alloy and the titanium-based composite materials.
Background
The titanium alloy and the titanium-based composite material have higher modulus, strength, wear resistance and excellent high-temperature comprehensive properties, such as oxidation resistance, creep resistance and the like, so that the titanium alloy and the titanium-based composite material have wide application prospects in the fields of aerospace, marine vessels, chemical engineering and the like. The thermophysical properties are critical to the structural design, fabrication and future applications of titanium alloys and their composites.
In the testing process of the existing method, the stability and repeatability of a high-temperature DSC curve cannot be realized, so that the inaccuracy of a high-temperature specific heat capacity testing result is caused.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: in the testing process of the existing method, the stability of a high-temperature DSC curve cannot be realized, so that the inaccuracy of a high-temperature specific heat capacity testing result is caused, and further the method for measuring the high-temperature specific heat capacity of the titanium alloy and the titanium-based composite material by using a differential scanning calorimetric segmentation method is provided.
The invention adopts the technical scheme for solving the technical problems that:
a method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material, which uses differential scanning calorimetric sectioning method to test high-temperature specific heat capacity, and uses synchronous thermal analyzer to obtain DSC curve of sapphire standard sample and titanium metal material, the specific measuring steps are as follows:
(1) Cleaning a sample, and then placing the sample at a sample end in a sample chamber of the synchronous thermal analyzer;
(2) Vacuumizing a sample chamber of the synchronous thermal analyzer, and then introducing inert gas to purify the sample chamber until the air pressure in the sample chamber reaches the atmospheric pressure;
(3) Weighing the mass of the sample in an inert gas atmosphere by using a balance in a sample chamber of the synchronous thermal analyzer;
(4) Heating to an initial temperature T at a certain heating rate by using a rhodium high-temperature furnace of a synchronous thermal analyzer, preserving heat, heating to T ' at a constant heating rate, preserving heat, heating to T ' at a constant heating rate by using T ' as the initial temperature, preserving heat, and circulating the processes until reaching a final target temperature, and recording a heat flow result of the sapphire standard sample in the heating process by using the synchronous thermal analyzer to obtain a DSC curve of the sapphire standard sample;
(5) The sample is tested by adopting the steps, and a heat flow result of the sample in the heating process is recorded by utilizing a synchronous thermal analyzer, so that a DSC curve of the sample is obtained;
(6) And (3) carrying out comparison calculation according to the heat flow result of the sapphire standard sample measured in the step (IV) and the heat flow result of the sample measured in the step (V) to obtain the specific heat capacity value of the sample.
Further, the inert gas is argon.
Further, the gas flow rate of the inert gas introduced into the sample chamber is 20-50 ml/min.
Furthermore, the sample end crucible in the sample chamber is a platinum rhodium and alumina combined crucible.
Further, the segmented temperature interval does not exceed 200 ℃.
Further, the heating rate is 20 ℃/min.
Further, the incubation time of the test initiation temperature T was 20min.
Further, the holding time of the end point temperature T' is 15min.
Further, the sample may be polygonal with a longest side of less than 4mm.
Further, the mass of the sample is selected from one of 12.5mg, 25mg, 37.5mg or 50 mg.
The invention has the beneficial effects that:
1. according to the invention, the rhodium high-temperature furnace arranged on the synchronous thermal analyzer is used for carrying out sectional constant temperature rise and constant temperature test on the sample, so that DSC stability of the sample in a high-temperature section is ensured.
2. Compared with the adiabatic calorimeter and the relaxation calorimeter, the invention has the advantages of wide measurement temperature range, small required sample amount and short test time, and can test various samples without limitation, such as films, powder, liquid and solid blocks.
3. The sample in the invention is in argon atmosphere, so that the sample mass can be accurately weighed.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate embodiments of the invention and together with the description serve to explain the invention, without limitation to the invention.
FIG. 1 is a DSC curve of a titanium alloy sample of example 1 of the present invention over a range of test temperatures;
FIG. 2 is a DSC curve of the titanium-based composite of example 1 of the present invention over a range of test temperatures.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
A method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material, which uses differential scanning calorimetric sectioning method to test high-temperature specific heat capacity, and uses synchronous thermal analyzer to obtain DSC curve of sapphire standard sample and titanium metal material, the specific measuring steps are as follows:
(1) Cleaning 52.5mg of sample, wherein the sample can be polygonal, the longest side is smaller than 4mm, and then placing the sample at a sample end in a sample chamber of the synchronous thermal analyzer, wherein a crucible at the sample end is a platinum-rhodium and alumina combined crucible;
(2) Vacuumizing a sample chamber of the synchronous thermal analyzer, and then introducing argon to purify the sample chamber until the air pressure in the sample chamber reaches the atmospheric pressure, wherein the air flow is 50 ml/min;
(3) Weighing the mass of the sample in an inert gas atmosphere by using a balance in a sample chamber of the synchronous thermal analyzer;
(4) Heating to an initial temperature T at a heating rate of 20 ℃/min by using a rhodium high-temperature furnace of a synchronous thermal analyzer, preserving heat for 20min, heating to T ' at a constant heating rate, preserving heat for 15min, heating to T ' at a constant heating rate by taking T ' as the initial temperature, preserving heat, circulating the above processes until reaching a final target temperature, recording a heat flow result of the sapphire standard sample in the heating process by using the synchronous thermal analyzer, and obtaining a DSC curve of the sapphire standard sample;
(5) The sample is tested by adopting the steps, and a heat flow result of the sample in the heating process is recorded by utilizing a synchronous thermal analyzer, so that a DSC curve of the sample is obtained;
(6) And (3) carrying out comparison calculation according to the heat flow result of the sapphire standard sample measured in the step (IV) and the heat flow result of the sample measured in the step (V) to obtain the specific heat capacity value of the sample. The specific results are shown in tables 1 and 2 and figures 1 and 2.
TABLE 1
| Temperature (. Degree. C.) | Specific heat capacity test value of |
| 100 | 0.584 |
| 300 | 0.615 |
| 500 | 0.636 |
| 700 | 0.732 |
| 900 | 0.790 |
TABLE 3 Table 3
| Temperature (. Degree. C.) | Specific heat capacity test value of titanium-based |
| 100 | 0.596 |
| 300 | 0.627 |
| 500 | 0.652 |
| 700 | 0.713 |
| 900 | 0.720 |
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. A method for determining the high temperature specific heat capacity of a titanium alloy and a titanium-based composite material, comprising:
(1) Cleaning a sample, and then placing the sample at a sample end in a sample chamber of the synchronous thermal analyzer;
(2) Vacuumizing a sample chamber of the synchronous thermal analyzer, and then introducing inert gas to purify the sample chamber until the air pressure in the sample chamber reaches the atmospheric pressure;
(3) Weighing the mass of the sample in an inert gas atmosphere by using a balance in a sample chamber of the synchronous thermal analyzer;
(4) Heating to an initial temperature T at a certain heating rate by using a rhodium high-temperature furnace of a synchronous thermal analyzer, preserving heat, heating to T ' at a constant heating rate, preserving heat, heating to T ' at a constant heating rate by using T ' as the initial temperature, preserving heat, and circulating the processes until reaching a final target temperature, and recording a heat flow result of the sapphire standard sample in the heating process by using the synchronous thermal analyzer to obtain a DSC curve of the sapphire standard sample;
(5) Testing the sample in the step (4), and recording a heat flow result of the sample in the heating process by using a synchronous thermal analyzer to obtain a DSC curve of the sample;
(6) And (3) carrying out comparison calculation according to the heat flow result of the standard sample measured in the step (4) and the heat flow result of the sample measured in the step (5) to obtain the specific heat capacity value of the sample.
2. The assay of claim 1, wherein:
the sample end crucible in the sample chamber in the step (1) is a platinum rhodium and alumina combined crucible.
3. The assay of claim 1, wherein:
the inert gas in the step (2) is argon; the gas flow of the inert gas introduced into the sample chamber is 20-50 ml/min.
4. The assay of claim 1, wherein:
the sectional temperature interval of the certain temperature rising rate in the step (4) is not more than 200 ℃.
5. The assay of claim 1, wherein:
and (3) the heating rate in the step (4) is 20 ℃/min.
6. The assay of claim 1, wherein:
and (3) the heat preservation time of the test starting temperature T in the step (4) is 20min.
7. The assay of claim 1, wherein:
and (3) the heat preservation time of the end temperature T' in the step (4) is 15min.
8. The assay of claim 1, wherein:
the longest edge of the sample in the step (1) is smaller than 4mm.
9. The assay of claim 1, wherein:
the mass of the sample in the step (3) is selected from one of 12.5mg, 25mg, 37.5mg or 50 mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310167930.5A CN116106362A (en) | 2023-02-27 | 2023-02-27 | Method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310167930.5A CN116106362A (en) | 2023-02-27 | 2023-02-27 | Method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material |
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| Publication Number | Publication Date |
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| CN116106362A true CN116106362A (en) | 2023-05-12 |
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| CN202310167930.5A Pending CN116106362A (en) | 2023-02-27 | 2023-02-27 | Method for measuring high-temperature specific heat capacity of titanium alloy and titanium-based composite material |
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- 2023-02-27 CN CN202310167930.5A patent/CN116106362A/en active Pending
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