CN109521040A - A kind of high temperature thermal shock resistance energy detection method of composite material - Google Patents

A kind of high temperature thermal shock resistance energy detection method of composite material Download PDF

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Publication number
CN109521040A
CN109521040A CN201811405253.1A CN201811405253A CN109521040A CN 109521040 A CN109521040 A CN 109521040A CN 201811405253 A CN201811405253 A CN 201811405253A CN 109521040 A CN109521040 A CN 109521040A
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sample
test
heating apparatus
induction heating
composite material
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王鹏
于新民
王宇
于艺
金鑫
霍鹏飞
宋环君
张宝鹏
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Aerospace Research Institute of Materials and Processing Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N3/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N3/08Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
    • G01N3/18Performing tests at high or low temperatures
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2203/00Investigating strength properties of solid materials by application of mechanical stress
    • G01N2203/0014Type of force applied
    • G01N2203/0016Tensile or compressive
    • G01N2203/0017Tensile

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

The present invention relates to a kind of high temperature thermal shock resistance energy test methods of composite material, step includes: that test is fixed in the induction coil area defined of HF induction heating apparatus by (1) with sample, guarantees that sample testing region is located at the center of induction coil area defined;(2) by infrared radiation thermometer sensing point registration coupon test zone center, and infrared radiation thermometer and pcs signal acquisition system are attached, utilize the temperature change of pcs signal acquisition system record sample;(3) HF induction heating apparatus is opened, it is to be regulated to being kept the temperature after required temperature, HF induction heating apparatus is closed after heat preservation and cooled down by the surface temperature of the power governor adjusting sample of HF induction heating apparatus;(4) step (3) are repeated according to testing requirement, the high temperature thermal shock resistance for completing composite material can be tested.This method can quickly heat up to 1500 DEG C or more, and device therefor is simple, and wire examination method is simple, low in cost.

Description

A kind of high temperature thermal shock resistance energy detection method of composite material
Technical field
The present invention relates to material properties test technical fields more particularly to a kind of high temperature thermal shock resistance of composite material to examine Survey method.
Background technique
Carbon fiber-reinforced ceramic matric composite (such as C/SiC, C/ZrC and multicomponent ceramic matrix) has low thermal expansion system The characteristics such as several, moderate elasticity modulus, therefore there is excellent thermal shock resistance, it is mainly used in the high temperature of aerospace field Thermal structure material.
Mainly there are oxy-acetylene flame ablation, plasma to the wire examination method of the high-temperature oxidation resistance of such material at present Arcing erosion and combustion wind tunnel can use above-mentioned three kinds of methods to carry out material screening and performance comparison.Wherein oxy-acetylene flame Ablation the basic principle is that: be heat source (temperature of oxy-acetylene flame stream is up to 3500 DEG C or so) with oxy-acetylene flame stream, will The flame flow washes away specimen surface with 90 ° of angles, carries out ablation to material, and the change of sample thickness and quality after ablation is measured after test Change, calculates the linear ablative rate and mass ablative rate of sample.Plasma arc ablation argon gas is ionized using high voltage to be formed etc. from Plasma arc is washed away specimen surface with 90 ° of angles by subarc, to material carry out ablation, after test measure ablation after sample thickness and The variation of quality calculates the linear ablative rate and mass ablative rate of sample.Combustion wind tunnel is the high temperature generated using fuel combustion Gas simulates high temperature flow field as the test gas of wind-tunnel.
Above-mentioned three kinds of wire examination method higher costs, periods are longer, and realize that thermal shock resistance examination difficulty is big.In view of This, the present invention is specifically proposed.
Summary of the invention
It is an object of the invention to overcome existing wire examination method insufficient, a kind of quick, low cost is provided and suitable high temperature is anti- The test method of thermal shock performance examination.
To achieve the goals above, the present invention provides the following technical scheme that
1, the high temperature thermal shock resistance energy test method of a kind of composite material, includes the following steps:
(1) test is fixed in the induction coil area defined of HF induction heating apparatus with sample, guarantees examination Sample test zone is located at the center of induction coil area defined;
(2) by infrared radiation thermometer sensing point registration coupon test zone center, and infrared radiation thermometer and computer are believed Number acquisition system is attached, and the temperature change of the sample is recorded using pcs signal acquisition system;
(3) HF induction heating apparatus is opened, the sample is adjusted by the power governor of HF induction heating apparatus Surface temperature, it is to be regulated to being kept the temperature after required temperature, HF induction heating apparatus is closed after heat preservation and carried out cold But;
(4) step (3) are repeated according to testing requirement, the high temperature thermal shock resistance for completing composite material can be tested.
2, test method according to technical solution 1, the length of test sample are the 2 of induction coil total height ~5 times.
3, test method according to technical solution 1, the heat preservation carry out 10~60 minutes.
4, test method according to technical solution 1, using natural cooling, air is cooling, water cooling or oil it is cold by the way of Sample is cooled down.
5, test method according to technical solution 1, by calculating the weight-loss ratio of the composite material to composite material High temperature thermal shock resistance can be carried out examination.
6, test method according to technical solution 1 will include the sample, infrared radiation thermometer, pcs signal acquisition The test system of system and HF induction heating apparatus be placed in closing constant temperature space in, it is ensured that test in the case where closing temperature constant state into Row.
7, according to the described in any item test methods of technical solution 1 to 6, the composite material is carbon fiber-reinforced ceramic base Composite material.
8, test method according to technical solution 1 further includes following steps: specimen enclosure is existed in step (1) In salable device, sealing obtains test sample;Preferably, it is described can vacuum sealing device be quartz ampoule.
9, the test method according to technical solution 8, the salable device are vitreosil pipe.
10, the test method according to technical solution 8 or 9, the composite material are oxidizable material, it is preferable that institute Stating oxidizable material is carbon-based material.
Beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
(1) present invention heats tested sample using HF induction heating apparatus, it can be achieved that quickly heating up to 1500 DEG C or more;
(2) equipment of the invention is simple, and wire examination method is simple, and examination is low in cost, mentions for material screening and performance comparison More convenient method is supplied;
(3) present invention can carry out vacuum high-temperature Performance Assessment, be suitable for oxidizable material by installing vitreosil pipe additional The performance test of (such as carbon-based material);
(4) present invention can be used for mechanical behavior under high temperature test, and such as at sample both ends, high temperature tensile properties are can be realized in load Test;
(5) present invention is used in the thermal shock performance test of material, and reduces heating, cooling cycle period.
(6) present invention is suitable for carbon fiber-reinforced ceramic matric composite (such as C/SiC, C/ZrC and multicomponent ceramic base Body), it is equally applicable to the performance test of other conductive materials.
Detailed description of the invention
Fig. 1 is the flow diagram of test method provided by the invention;
Fig. 2 is to carry out the schematic diagram that high temperature thermal shock resistance can be examined using test method provided by the invention;
Fig. 3 is the test result of each embodiment.
In figure: 1: HF induction heating apparatus;2: induction coil;3: infrared radiation thermometer;4: pcs signal acquisition system;5: Sample is used in test.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of high temperature thermal shock resistance energy test methods of composite material, using HF induction heating apparatus Tested sample is quickly heated, since carbon fiber-reinforced ceramic matric composite sheet can be acted on as conductor in high frequency magnetic field Lower fever, and heating temperature is adjustable, sample need to be suspended from magnetic induction loop in heating process.Sample is measured by infrared radiation thermometer Surface temperature, and temperature variation curve is recorded by computer acquisition system.Specifically, as depicted in figs. 1 and 2, the test method Include the following steps:
(1) test sample 5 is fixed in 2 area defined of induction coil of HF induction heating apparatus 1, is guaranteed Sample testing region is located at the center of 2 area defined of induction coil;
Setup test sample 5 before test, the length of the sample are preferably 2~5 times of 2 height of induction coil, can Any number (comprising endpoint value) within the scope of this is thought, for example, can be 2 times, 2.5 times, 3 times, 3.5 times, 4 times, 4.5 times, 5 Times, the too long or too short charge and discharge operations for being all not easy to sample 5.
Since sample 5 is placed in induction coil 2, so 5 width of sample or diameter are not more than 2 internal diameter of induction coil.
(2) by 3 sensing point registration coupon test zone center of infrared radiation thermometer, and by infrared radiation thermometer 3 and computer Signal acquiring system 4 is attached, and the temperature change of the sample 5 is recorded using pcs signal acquisition system 4;
(3) HF induction heating apparatus 1 is opened, the examination is adjusted by the power governor of HF induction heating apparatus 1 The surface temperature of sample 5, different materials feed back difference to the response of high-frequency induction heating, can realize temperature indirectly by power regulation The adjusting of degree, to be regulated to being kept the temperature after required temperature, soaking time is preferably 10~60 minutes, can be within the scope of this Any number (including endpoint value), for example, can be 10 minutes, 15 minutes, 20 minutes, 25 minutes, 30 minutes, 35 minutes, 40 Minute, 45 minutes, 50 minutes, 55 minutes, 60 minutes close HF induction heating apparatus 1 and carry out to sample 5 after heat preservation Cooling, cooling means can be cold using natural cooling, air cooling, water cooling or oil;
(4) step (3) are repeated according to testing requirement, the high temperature thermal shock resistance for completing composite material can be tested.It, can when repeating Not change test temperature, the repeated experiment at a temperature of certain is carried out, also can change test temperature, it is compound after carrying out alternating temperature The high temperature thermal shock resistance of material can be tested.
It, can be by recording the mistake before and after the composite material test when carrying out high temperature thermal shock resistance to material can examine Weight, calculates the weight-loss ratio of composite material, can be carried out examination using high temperature thermal shock resistance of this index to composite material.
It in some embodiments, will include the sample 5, infrared radiation thermometer 3, pcs signal acquisition system 4 and high frequency sense The test system of heating equipment 1 is answered to be placed in closing constant temperature space, it is ensured that test is carried out in the case where closing temperature constant state, avoids air Convection current and indoor temperature change generated in case impact test result.
Carbon fiber-reinforced ceramic matric composite can be tested using test method provided by the invention, certainly The performance of other conductive materials can be tested.Composite material used can be made using existing preparation method, this Invention is not specifically limited in this embodiment.
It in some embodiments, further include following steps in step (1): by specimen enclosure in salable device (such as stone English pipe) in, sealing obtains test sample 5.Can vacuumize vacuumize in salable device (can use true Empty salable device can also use antivacuum salable device), vacuumize then can sample vacuum high-temperature performance, do not take out very It is empty then can oxidation behavior of the sample under atmospheric environment.But it regardless of whether being vacuumized, is encapsulated and is tried using salable device Sample can reduce the sample strong convection that nearby air generates under high temperature.Certainly, in face of oxidizable material (such as carbon-based material) When performance test, vacuumize process can be carried out, it can be packaged to sample using vitreosil pipe.
It in addition to this, in some embodiments, can also be by loading universal testing machine at the both ends of sample 5, to test High temperature tensile properties test is carried out, the mechanical behavior under high temperature of composite material is tested.Specifically, the test method includes following step It is rapid:
(1) test sample 5 is fixed in 2 area defined of induction coil of HF induction heating apparatus 1, is guaranteed Sample testing region is located at the center of 2 area defined of induction coil, and loads omnipotent examination at the both ends of the sample 5 Test machine;
(2) by 3 sensing point registration coupon test zone center of infrared radiation thermometer, and by infrared radiation thermometer 3 and computer Signal acquiring system 4 is attached, and the temperature change of the sample 5 is recorded using pcs signal acquisition system 4;
(3) HF induction heating apparatus 1 is opened, the examination is adjusted by the power governor of HF induction heating apparatus 1 The surface temperature of sample 5, it is to be regulated to being kept the temperature after required temperature, utilize universal testing machine to carry out tensile property at this temperature Test is closed HF induction heating apparatus 1 and is cooled down after test;
(4) step (3) can be repeated according to testing requirement, carry out the reperformance test under same temperature or changes test temperature Degree, the high temperature tensile properties of the composite material after testing alternating temperature.
It is the embodiment that the present invention enumerates below.
Embodiment 1
Test sample:
C/SiC composite material with antioxidant coating, the preparation method of the composite material are the prior art, the present invention couple This is no longer described in detail, and is processed into test bars as test sample.
Test method includes the following steps:
(1) test is fixed in the induction coil area defined of HF induction heating apparatus with sample, guarantees examination Sample test zone is located at the center of induction coil area defined;
Setup test sample before test, the length of the sample are 5 times of induction coil height, and specimen width is little In induction coil internal diameter.
(2) by infrared radiation thermometer sensing point registration coupon test zone center, and infrared radiation thermometer and computer are believed Number acquisition system is attached, and the temperature change of the sample is recorded using pcs signal acquisition system;
(3) HF induction heating apparatus is opened, the sample is adjusted by the power governor of HF induction heating apparatus Surface temperature to 1600 DEG C, it is to be regulated to being kept the temperature after required temperature, soaking time 30 minutes, closed after heat preservation high Frequency induction heating equipment simultaneously cools down the sample, and cooling means is natural cooling;
(4) it repeats step (3) 9 times, measures the weight-loss ratio after the composite material is repeated 10 times altogether at 1600 DEG C, complete multiple The high temperature thermal shock resistance of condensation material can be tested.
It should be noted that test process in, will include the sample, infrared radiation thermometer, pcs signal acquisition system and The test system of HF induction heating apparatus is placed in closing constant temperature space, it is ensured that test is carried out in the case where closing temperature constant state, is kept away Exempt from cross-ventilation and indoor temperature change generated in case impacts test result.
Embodiment 2
Test sample:
The preparation method of C/SiC composite material, the composite material is the prior art, this is no longer described in detail in the present invention, will It is processed into test bars as test sample.
Test method is the same as embodiment 1.
Embodiment 3
Test sample:
The preparation method of C/C composite material, the composite material is the prior art, this is no longer described in detail in the present invention, by it Test bars are processed into as test sample.
Test method includes the following steps:
(1) by specimen enclosure in vacuum sealing device (such as vitreosil pipe), vacuum sealing obtains test sample, Then test is fixed in the induction coil area defined of HF induction heating apparatus with sample, guarantees sample testing area Domain is located at the center of induction coil area defined;The length of setup test sample before test, the sample is 5 times of induction coil height, specimen width are not more than induction coil internal diameter.
(2) by infrared radiation thermometer sensing point registration coupon test zone center, and infrared radiation thermometer and computer are believed Number acquisition system is attached, and the temperature change of the sample is recorded using pcs signal acquisition system;
(3) HF induction heating apparatus is opened, the sample is adjusted by the power governor of HF induction heating apparatus Surface temperature to 1600 DEG C, it is to be regulated to being kept the temperature after required temperature, soaking time 30 minutes, closed after heat preservation high Frequency induction heating equipment simultaneously cools down the sample, and cooling means is natural cooling;
(4) it repeats step (3) 9 times, measures the weight-loss ratio after the composite material is repeated 10 times altogether at 1600 DEG C, complete multiple The high temperature thermal shock resistance of condensation material can be tested.
It should be noted that test process in, will include the sample, infrared radiation thermometer, pcs signal acquisition system and The test system of HF induction heating apparatus is placed in closing constant temperature space, it is ensured that test is carried out in the case where closing temperature constant state, is kept away Exempt from cross-ventilation and indoor temperature change generated in case impacts test result.
The test result of embodiment 1, embodiment 2 and embodiment 3 is shown in Fig. 3.
In conclusion test method provided by the invention, which can be realized, quickly heats up to 1500 DEG C or more, and this method institute Equipment is simple, and wire examination method is simple, examine it is low in cost, for material screening with performance comparison provide it is more convenient Method.In addition, test method provided by the invention can carry out vacuum high-temperature Performance Assessment, fit by installing vitreosil pipe additional Performance test for oxidizable material (such as carbon-based material).
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features; And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and Range.

Claims (10)

1. a kind of high temperature thermal shock resistance energy test method of composite material, characterized by the following steps:
(1) test is fixed in the induction coil area defined of HF induction heating apparatus with sample, guarantees that sample is surveyed Examination region is located at the center of induction coil area defined;
(2) by infrared radiation thermometer sensing point registration coupon test zone center, and infrared radiation thermometer and pcs signal are adopted Collecting system is attached, and the temperature change of the sample is recorded using pcs signal acquisition system;
(3) HF induction heating apparatus is opened, the table of the sample is adjusted by the power governor of HF induction heating apparatus Face temperature, it is to be regulated to being kept the temperature after required temperature, HF induction heating apparatus is closed after heat preservation and to the sample It is cooled down;
(4) step (3) are repeated according to testing requirement, the high temperature thermal shock resistance for completing composite material can be tested.
2. test method according to claim 1, it is characterised in that: the length of test sample is that induction coil is total 2~5 times of height.
3. test method according to claim 1, it is characterised in that: the heat preservation carries out 10~60 minutes.
4. test method according to claim 1, it is characterised in that: cold using natural cooling, air cooling, water cooling or oil Mode the sample is cooled down.
5. test method according to claim 1, it is characterised in that: by calculating the weight-loss ratio of the composite material to multiple The high temperature thermal shock resistance of condensation material can be carried out examination.
6. test method according to claim 1, it is characterised in that: will include the sample, infrared radiation thermometer, computer letter The test system of number acquisition system and HF induction heating apparatus is placed in closing constant temperature space, it is ensured that test is in closing constant temperature shape It is carried out under state.
7. test method according to any one of claims 1 to 6, it is characterised in that: the composite material is carbon fiber increasing Tough ceramic matric composite.
8. test method according to claim 1, it is characterised in that: further include following steps in step (1): will try Sample is encapsulated in salable device, and sealing obtains test sample;Preferably, it is described can vacuum sealing device be quartz ampoule.
9. test method according to claim 8, it is characterised in that: the salable device is vitreosil pipe.
10. test method according to claim 8 or claim 9, it is characterised in that: the composite material is oxidizable material, excellent Selection of land, the oxidizable material are carbon-based material.
CN201811405253.1A 2018-11-23 2018-11-23 A kind of high temperature thermal shock resistance energy detection method of composite material Pending CN109521040A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN111024746A (en) * 2019-11-27 2020-04-17 中山市海明润超硬材料有限公司 Method and device for testing heat resistance of diamond compact
CN113049402A (en) * 2021-04-30 2021-06-29 西南交通大学 Conductive ceramic thermal shock test equipment
CN115235934A (en) * 2022-07-18 2022-10-25 衡阳凯新特种材料科技有限公司 Method and equipment for detecting thermal shock resistance of silicon nitride ceramic material

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CN115235934A (en) * 2022-07-18 2022-10-25 衡阳凯新特种材料科技有限公司 Method and equipment for detecting thermal shock resistance of silicon nitride ceramic material

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