CN112649465B - Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology - Google Patents
Method for testing low-temperature thermal shrinkage coefficient of material by utilizing residual indentation morphology Download PDFInfo
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Abstract
The invention relates to a method for testing a low-temperature thermal shrinkage coefficient of a material by utilizing residual indentation morphology, belonging to the technical field of engineering testing. And (3) prefabricating marked indentations on the test surface of the test piece at different temperatures by using a nano indentation test instrument with an in-situ observation function, carrying out in-situ non-contact imaging and recording on the surface appearance of the test piece in real time, and measuring the thermal shrinkage coefficient of the material in a low-temperature environment in real time. Firstly, carrying out nano indentation tests on the surface of a material at different temperatures, and taking residual indentations as marking indentations; secondly, carrying out real-time in-situ imaging on the marked indentations at different temperatures, and extracting contrast imaging data; and finally, calculating the low-temperature thermal shrinkage coefficient of the material in different temperature intervals by using a formula. The method has the advantages that the required instruments and equipment are relatively simple to build, complex interference light paths/circuits are not required to build, the operation is simple and convenient, meanwhile, the method can qualitatively evaluate whether anisotropy exists in the low-temperature thermal shrinkage coefficient in the test plane, and a new method is provided for researching the low-temperature physical properties of the material.
Description
Technical Field
The invention relates to the technical field of engineering test, in particular to a method for testing a low-temperature thermal shrinkage coefficient of a material by utilizing the shape of a residual indentation, and provides a simple, convenient and quick technical means for testing the low-temperature physical properties of the material.
Background
With the continuous development and progress of low-temperature engineering technology, low-temperature materials are widely applied in the fields of aerospace science and technology, biology, life science and the like. In the period, various novel materials are produced and widely applied, so that the low-temperature physical property test of the material also plays a key role in the normal service reliability and the service performance of the material, particularly the low-temperature thermal shrinkage coefficient of the material and the like. For example, an aerospace vehicle such as the united states "challenger" exploded during 73 seconds of takeoff due to the rubber band acting as a seal that shrank poorly at low temperatures, causing hot gases to ignite the fuel in the outer fuel tank. Therefore, it is necessary to test the low temperature thermal shrinkage coefficient of the material.
At present, various methods can be adopted for detecting the thermal shrinkage coefficient of the low-temperature material, including capacitance dilatometer, interference dilatometer, laser speckle imaging technology, electronic speckle interference technology, X-ray and other testing technologies. These methods mainly utilize different sensitive signals (such as capacitance change, interference fringe number, etc.) to amplify and record the slight expansion/contraction amount of the material caused by the temperature influence. However, the above-mentioned method for measuring the thermal shrinkage coefficient of a material tends to have the following disadvantages: 1) the test instrument equipment is relatively complex, such as interference light path erection, no expansion support of a capacitor and the like; 2) the testing direction is single, and the testing parameters are less. Therefore, in the current research, a method for monitoring the low-temperature deformation behavior of the material in real time at the micro-nano level and simply and comprehensively characterizing the low-temperature physical properties and the mechanical properties of the material is lacked.
Disclosure of Invention
The invention aims to provide a method for testing the low-temperature thermal shrinkage coefficient of a material by utilizing the shape of a residual indentation, and solves the problems of complex instrument and equipment construction, single testing direction and the like in the prior testing technology. According to the invention, the low-temperature micro-nano indentation testing instrument is combined with an in-situ scanning electron microscope, a scanning tunnel microscope or other high-resolution microscopic imaging functional components, so that the real-time in-situ non-contact imaging and recording of the preformed mark indentation residual morphology on the surface of the material under a low-temperature environment are realized, and further, the low-temperature thermal shrinkage rate test of the material and the qualitative evaluation of the anisotropy of the low-temperature thermal shrinkage coefficient in a test plane are realized.
The above object of the present invention is achieved by the following technical solutions:
the method for testing the low-temperature thermal shrinkage coefficient of the material by utilizing the residual indentation morphology comprises the following steps of:
grinding and polishing an initial surface 6 of a test piece, adhering the initial surface to the surface of an objective table, carrying out indentation test on the surface of the test piece by using a nano indenter under a room temperature environment, selecting a sharp pyramid indenter 4 as the indenter, recording a characteristic angle as alpha, and recording residual indentation/pit on the surface of the test piece as a marked indentation A;
secondly, carrying out in-situ non-contact imaging on the marked indentation A by means of a microscopic imaging functional component and recording the shape information of the marked indentation A in a room temperature environment;
step three, selecting a reference temperature T within the temperature range from room temperature to 77K1Extracting the reference temperature T from the real-time topographic information of the marked indentation A1The length of a side a of the intersection line 7 of the lower marking impression A and the test cross sectioni(i-1, 2, … …, n), and obtaining the cross-sectional area A of the marking indentation A1Characteristic angle of alpha1(ii) a In a similar manner, at the target temperature T2Next, the side length of the intersection line 7 of the marking indentation A and the test cross section is bi(i ═ 1,2, … …, n), mark indentation a cross-sectional area a2；
Step four, the same as above, at the target temperature T2Next, the indentation tester is used to perform indentation test on the surface of the test pieceAt the moment, marking the residual indentation on the surface of the test piece as a mark indentation B; the edge length of the intersection 7 of the marking impression B and the test cross section is marked ci(i ═ 1,2, … …, n), mark indentation B cross-sectional area a3(ii) a Temperature change to a reference temperature T1Then, the side length d of the intersection line 7 of the marking impression B and the test cross section is extractedi(i-1, 2, … …, n), the cross-sectional area of marking indentation B at this time was derived as a4Characteristic angle of alpha2；
Step five, qualitatively judging whether the low-temperature thermal shrinkage coefficient of the material shows isotropy in a plane or not according to the ratio relation between the side length and the section area of the intersection line 7 of the marked indentation A, B and the test cross section in different temperature environments;
sixthly, before and after the temperature changing environment, as the axial shrinkage/expansion displacement delta L of the test piece is kept consistent, the contact surface distance between the mark indentation A and the mark indentation B is kept constant; using equation (1) to calculate the equation1To T2Axial shrinkage displacement amount Δ L of the test piece at temperature:
wherein n represents the number of faces of the selected pyramid pressure head 4;
step seven, substituting the formula (1) into the formula (2) to calculate the equation T1To T2Axial linear thermal shrinkage coefficient β of the test piece at temperature:
wherein L isTIs a reference temperature T1Axial dimension of lower specimen, from room temperature (i.e. T)0298K) specimen axial dimension L is iteratively extrapolated, which is not repeated here.
Compared with the prior art, the invention has the following advantages and prominent effects: by utilizing the nanoindentation testing instrument with the in-situ observation function to pre-mark the indentation on the testing surface of the test piece and carry out real-time in-situ non-contact imaging and recording on the surface appearance of the test piece, the measurement error caused by the temperature gradient between a scanning probe and the test piece in the traditional in-situ contact scanning imaging can be avoided, the low-temperature thermal shrinkage rate test of the material can be realized, the test precision can reach the nanometer level, meanwhile, whether anisotropy exists in the low-temperature thermal shrinkage coefficient in a test plane can be qualitatively evaluated, and a new method is provided for researching the low-temperature physical property of the material. In addition, the method has the advantages of relatively simple construction of required instruments and equipment, no need of complex interference light path/circuit construction and simple and convenient operation. The practicability is strong.
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 embodiment(s) of the invention and together with the description serve to explain the invention without limiting the invention.
FIG. 1 is a flow chart of a method for testing the low-temperature thermal shrinkage coefficient of a material by utilizing the residual indentation morphology according to the present invention;
FIG. 2 is a schematic cross-sectional view of a maximum indentation position of a prefabricated mark indentation of a test specimen according to the invention;
FIGS. 3 and 4 are schematic top views of two exemplary Boss residual indentation topographical features of the present invention;
FIGS. 5 and 6 are schematic top views of the low-temperature thermal shrinkage coefficient of the material of the present invention showing the glass residual indentation before and after the temperature change, which is isotropic and anisotropic (taking cubic symmetric crystals as an example), in the test plane;
FIG. 7 and FIG. 8 are graphs of marked indentations A and B for calculating low-temperature linear thermal shrinkage coefficient of material by utilizing residual indentation morphology change in variable temperature environment (i.e. reference temperature T)1And a target temperature T2) The next two representative cross-sectional schematic views; wherein FIG. 7 shows the marked indentation A of the present invention from a reference temperature T1Changing the temperature to a target temperature T2Typical section variation diagram (in this case, DeltaL ≧ S1) (ii) a FIG. 8 is a graph of mark indentation B of the present invention from a target temperature T2Changing the temperature to a reference temperature T1Typical cross-sectional variation diagram (in this case,. DELTA.L)<S2)；
FIG. 9 is a plot of indentation load versus depth for a single crystal copper Boss indenter marking at different temperatures in accordance with the present invention;
FIG. 10 is a plot of indentation load versus depth for a single crystal silicon Boss indenter marking at different temperatures in accordance with the present invention;
FIG. 11 is a plot of indentation load versus depth for a single crystal copper Vickers indenter mark at different temperatures in accordance with the present invention.
In the figure: 1. pressing into the deformed surface; 2. pile-up; 3. marking the intersection point of the indentation and the test cross section; 4. a pyramid indenter; 5. sink-in (sink); 6. an initial surface; 7. marking the intersection line of the indentation and the test cross section; 8. a glassy residual impression of the sink-in phenomenon; 9. glass-up phenomenon of residual indentations; 10. the shape of the residual indentation intersection line at the reference temperature; 11. and (4) the appearance of the residual indentation intersection line at the target temperature.
Detailed Description
The details of the present invention and its embodiments are further described below with reference to the accompanying drawings.
Referring to fig. 1 to 8, the method for testing the low-temperature thermal shrinkage coefficient of a material by using the residual indentation morphology of the present invention, in combination with a low-temperature generation system and matching with different in-situ observation means, can realize a low-temperature indentation process on a conventional nanoindentation instrument and can image a low-temperature residual indentation in real time, and the imaging precision can reach a nanometer level, so as to meet the test requirement of the thermal shrinkage coefficient of a general test material at a low temperature (especially in a normal cold temperature range). On the premise of not generating the conditions of phase change, thermal stress and the like in the low-temperature process of the material, firstly, carrying out nano indentation tests on the surface of the material at different temperatures, and taking residual indentations as marking indentations; secondly, carrying out real-time in-situ imaging on the marked indentations at different temperatures, and extracting contrast imaging data; and finally, calculating the low-temperature thermal shrinkage coefficient of the material in different temperature intervals by using a formula. The method has the advantages that the required instruments and equipment are relatively simple to build, complex interference light paths/circuits are not required to build, the operation is simple and convenient, meanwhile, the method can qualitatively evaluate whether anisotropy exists in the low-temperature thermal shrinkage coefficient in the test plane, and a new method is provided for researching the low-temperature physical properties of the material.
Referring to fig. 1, the method for testing the low-temperature shrinkage coefficient of the material by using the residual indentation morphology of the invention has a flow chart, and comprises the following specific operation steps:
the method comprises the following steps of firstly, grinding and polishing an initial surface 6 of a test piece to be tested to meet the requirements of a nano indentation test, adhering the test piece to the surface of an objective table by using low-temperature varnish, carrying out an indentation test on the surface of the test piece by using a nano indenter in a room-temperature environment, selecting a sharp pyramid indenter 4 (a characteristic angle is recorded as alpha) by using the indenter, and recording residual indentations/pits on the surface of the test piece as marked indentations A.
And secondly, carrying out in-situ non-contact imaging on the marked indentation A by means of a microscopic imaging functional component at room temperature and recording the shape information of the marked indentation A.
As shown in fig. 2, since the indentation deformation surface 1 may show a pile-up 2 behavior or a sink-in 5 behavior in the nanoindentation test process, the intersection point 3 of the marking indentation and the test cross section does not coincide with the contact point of the pyramid indenter 4, if a common glass indenter is taken as an example (the same below), a glass residual indentation 8 of the sink-in phenomenon and a glass residual indentation 9 of the pile-up phenomenon shown in fig. 3 and 4 appear, and data is recorded in the form of an intersection line 7 of the marking indentation and the test cross section;
step three, selecting any temperature as a reference temperature T1Extracting the side length a of the intersecting line 7 of the marked indentation A and the test cross section at the temperature from the real-time topography information of the marked indentation Ai(i is 1,2, … …, n), and then the cross-sectional area a of the marking indentation a is obtained1Characteristic angle of alpha1(ii) a In a similar manner, at the target temperature T2Next, the edge length of the intersection 7 of the marking mark A and the test cross section is denoted as bi(i ═ 1,2, … …, n), mark indentation a cross-sectional area a2(ii) a Wherein, the in-situ imaging picture in the test temperature interval is easily and directly processed from the reference temperature T1Acquiring data information from the lower residual indentation intersection line morphology 10 and the residual indentation intersection line morphology 11 at the target temperature;
step four, as above, at the target temperature T2Then, the indentation tester is used for carrying out indentation test on the surface of the test piece, and the residual indentation of the surface of the test piece is marked as a mark at the momentMarking an indentation B; the edge length of the intersection 7 of the marking impression B and the test cross section is marked ci(i ═ 1,2, … …, n), mark indentation B cross-sectional area a3(ii) a Temperature change to a reference temperature T1Then, the side length d of the intersection line 7 of the marking impression B and the test cross section is extractedi(i-1, 2, … …, n), the cross-sectional area of marking indentation B at this time was derived as a4Characteristic angle of alpha2；
Step five, referring to a relation shown in fig. 3, qualitatively judging whether the low-temperature thermal shrinkage coefficient of the material shows isotropy in a plane according to a ratio relation between the side length of the intersection line of the marked indentation and the cross-sectional area under different temperature environments, if the following expression (3) is met, testing that the low-temperature thermal shrinkage coefficient of the material shows isotropy in the plane, otherwise, testing that the low-temperature thermal shrinkage coefficient of the material shows isotropy;
step six, as shown in FIG. 7 and FIG. 8, no matter the material is in the state that the delta L is larger than or equal to S1Or Δ L<S2In which of the two typical thermal expansion/contraction behaviors, before and after the temperature changing environment, the axial contraction/expansion displacement amount delta L of the test piece is kept consistent, and the distance variation of the contact surface of the marking indentation A and the marking indentation B is kept constant, namely L2＝L'2(ii) a Using equation (1) to calculate the equation1To T2The axial shrinkage displacement delta L of the test piece at the temperature, wherein n represents the number of the surfaces of the selected pyramid indenter;
step seven, substituting the formula (1) into the formula (2) to calculate the equation T1To T2Axial linear thermal shrinkage coefficient β of the test material at temperature:
wherein L isTIs a reference temperature T1Axial dimension of lower specimen, from room temperature (i.e. T)0298K) specimen axial dimension L is iteratively extrapolated, which is not repeated here.
The calculation formula is derived as follows:
because the relationship between the axial low-temperature thermal shrinkage coefficient and the radial low-temperature thermal shrinkage coefficient of the tested material cannot be directly determined, the low-temperature linear thermal shrinkage coefficient of the material can be calculated by combining the two typical residual indentation morphology changes. Referring to fig. 5, 7 and 8, there are:
wherein S is1Indicating the radial heat shrinkage before and after the temperature change of the marked indentation A, S2And (4) showing the radial heat shrinkage before and after the temperature change of the marked indentation B. In addition, as shown in FIG. 7, although the half-angle of the residual indentation topography will change before and after the temperature change, i.e., λ ≠ α1However, according to the theorem of intersecting chords and the relationship between corresponding edges of similar triangles, there are:
|CF|·|FB|＝|AF|·|DF| (7)
L2＝△L·sinα1-s1·cosα1 (8)
similarly, referring to fig. 8, according to the theorem of intersecting chords and the relationship between corresponding edges of similar triangles, there are:
L'2＝△L·sinα2-s2·cosα2 (9)
and (8) and (9) are combined, so that the low-temperature axial thermal shrinkage delta L of the material can be calculated. Wherein the characteristic angle alpha at different temperatures1、α2Residual indentation depth h of indentation load-depth curve can be determined from marking indentation A, Bf1、hf2(see FIG. 9) and the mean value of the intersection length thereof are calculated as follows:
meanwhile, the derivation process can be simplified according to the inherent property characteristics of the tested material, if the tested material is in a cubic crystal structure, the radial low-temperature thermal shrinkage coefficient in the test plane is equal to the axial thermal shrinkage coefficient, namely alpha⊥β; if the test material is in a close-packed hexagonal crystal structure, the radial low-temperature thermal shrinkage coefficient and the axial thermal shrinkage coefficient in the test plane are different, and then the low-temperature thermal shrinkage coefficient alpha in the test plane is calculated⊥The expression is approximated as:
h0is the distance from the center of indentation to the perpendicular to the line of intersection.
Example 1:
in the example, the axial linear thermal shrinkage coefficient of the single crystal copper material at room temperature (298K) to 200K and the thickness of a test piece at room temperature of 2mm are tested by (100), and the specific test steps are as follows:
the method comprises the following steps: the surface of the (100) single crystal copper test specimen prepared by growth needs to be ensured to meet the requirements of a low-temperature nano indentation test on the surface quality, namely the nano indentation depth is not less than 20 times of the surface roughness Ra of the test specimen, and the surface roughness of the (100) single crystal copper test specimen is tested by an atomic force microscope at the moment to be 6.5 nm;
step two: pressing in a test on the surface of the test piece by using a glass indenter of a low-temperature nano indenter at room temperature (namely 298K, and recorded as reference temperature) to record as a marked indentation A, and obtaining a typical pressing-in load-depth curve, wherein the maximum pressing-in load is 250mN, the residual pressing-in depth reaches 3650nm, the hardness is 730MPa, and the elastic modulus is 91.6 GPa;
step three: the temperature of a test piece is controlled to be reduced from room temperature (namely 298K) to 200K (recorded as target temperature) through a cold finger integrated on the wall of a scanning electron microscope cavity, the single crystal copper test piece (100) generates thermal shrinkage deformation, and simultaneously, real-time in-situ imaging recording is carried out on a marked indentation A under 200K and 298K respectively;
step four: pressing in a test on the surface of the test piece by using a Bos indenter of an in-situ low-temperature nanoindenter at the temperature of 200K, and recording as a marked indentation B, and obtaining a typical indentation load-depth curve, wherein the maximum indentation load is 250mN, the residual indentation depth reaches 3250nm, the hardness is 900MPa, and the elastic modulus is 93.4 GPa;
step five: heating the temperature of the (100) single crystal copper test piece from 200K to room temperature (namely 298K) reversely by a heating element, reversely recovering the deformation of the material, and simultaneously carrying out real-time in-situ imaging recording on the marking indentation B under 200K and 298K respectively;
step six: extracting the cross-sectional area (169 μm) of the marked indentation from the real-time topographic information of the marked indentations A and B at 200K and room temperature (298K) respectively by using image processing software2，102μm2，165μm2，97μm2) And drawing and calculating the length of 3 intersecting lines of the marking indentation and the test cross section (19.755 μm,19.753 μm,19.757 μm; 15.347 μm,15.344 μm,15.346 μm; 19.521 μm,19.523 μm,19.524 μm; 14.966 μm,14.968 μm,14.965 μm);
step seven: referring to FIG. 9, room temperature marked indentation A has a residual indentation depth of 3.65 μm, and 200K marked indentation B has a residual indentation depth of 3.25 μm, when the length means of the intersection line of the marked indentation and the test cross-section are 19.755 μm and 14.966 μm, respectively. Then calculating according to the formula (9) to obtain the characteristic angle alpha1、α257.37 °, 53.04 °;
step eight: according to the formula (3), the area ratio of the marked indentation cross section at different temperatures is (A)1/A2,A3/A4) Squared ratio to average of intersecting line lengths ((a)i/bi)2,(ci/di)2I is approximately equal to 1,2,3), i.e. the system of anisotropic thermal contractionThe number is similar and is matched with the symmetry of the single crystal copper crystal;
step nine: substituting the cross-sectional areas and the intersection line lengths of the marked indentations A and B into the formula (1) for calculation to obtain the material low-temperature axial thermal shrinkage of 2.42 mu m in the temperature range from 200K to room temperature (namely 298K);
step ten: further, the axial linear thermal contraction coefficient in the temperature range is calculated by the formula (2) to be 1.30X 10-5K, according to the symmetry of the crystal, the low-temperature thermal shrinkage coefficients of the single-crystal copper material at the time are all 1.30 multiplied by 10-5/K。
Example 1 the low temperature thermal shrinkage and coefficient of thermal shrinkage of the material in the temperature range of 200K to room temperature were successfully calculated using the bosch residual indentation.
Example 2:
in the example, the axial linear thermal shrinkage coefficient of the monocrystalline silicon material (110) is tested from room temperature (298K) to 150K, the thickness of a test piece is 5mm at room temperature, and the specific test steps are as follows:
the method comprises the following steps: ensuring that the surface of the monocrystalline silicon test piece (110) meets the requirement of a low-temperature nanoindentation test on the surface quality, namely the nanoindentation indentation depth is not less than 20 times of the surface roughness Ra of the test piece, and testing the surface roughness of the monocrystalline silicon test piece (110) by an atomic force microscope at the moment to be 3.5 nm;
step two: pressing test is carried out on the surface of the test piece by using a glass indenter of a low-temperature nano indenter at room temperature (namely 298K, and recorded as reference temperature) to record a mark indentation A, a typical pressing load-depth curve is obtained, the maximum pressing load is 100mN, the residual pressing depth reaches 334nm, the hardness is 13.17GPa, and the elastic modulus is 186.5 GPa;
step three: the temperature of a test piece is controlled to be reduced from room temperature (namely 298K) to 150K (recorded as target temperature) through a cold finger integrated on the wall of a scanning electron microscope cavity, the monocrystalline silicon test piece (110) generates thermal shrinkage deformation, and simultaneously, real-time in-situ imaging recording is carried out on a marked indentation A under 150K and 298K respectively;
step four: pressing a test on the surface of the test piece by using a Bos indenter of an in-situ low-temperature nano indenter at the temperature of 150K, and recording as a marked indentation B, and obtaining a typical indentation load-depth curve, wherein the maximum indentation load is 100mN, the residual indentation depth reaches 237nm, the hardness is 13.8GPa, and the elastic modulus is 193.4 GPa;
step five: heating the temperature of the (110) monocrystalline silicon test piece from 150K to room temperature (namely 298K) reversely by a heating element, reversely recovering the deformation of the material, and simultaneously carrying out real-time in-situ imaging recording on the marking indentation B under 150K and 298K respectively;
step six: extracting the cross-sectional area (5.48 μm) of the marked indentation from the real-time topographic information of the marked indentations A and B at 150K and room temperature (i.e. 298K) respectively by using image processing software2，2.97μm2，4.63μm2，2.27μm2) And drawing and calculating the length of 3 intersecting lines of the marking indentation and the test cross section (3.568 μm,3.611 μm,3.495 μm; 2.482 μm,2.538 μm,2.574 μm; 3.270 μm,3.284 μm,3.267 μm; 2.314 μm,2.275 μm,2.284 μm);
step seven: referring to FIG. 10, room temperature marked indentation A has a residual indentation depth of 0.334 μm, and 150K marked indentation B has a residual indentation depth of 0.237 μm, when the length averages of the intersections of the marked indentations with the test cross-sections are 3.558 μm and 2.291 μm, respectively. Then calculating according to the formula (9) to obtain the characteristic angle alpha1、α271.99 degrees and 70.29 degrees;
step eight: substituting the cross-sectional areas and the intersection line lengths of the marked indentations A and B into the formula (1) for calculation to obtain the material low-temperature axial thermal shrinkage of 1.084 mu m in the temperature range from 150K to room temperature (298K);
step nine: further, the axial linear thermal contraction coefficient in the temperature range is calculated by the formula (2) to be 1.46X 10-6The low-temperature thermal shrinkage coefficient of the monocrystalline silicon material is 1.46 multiplied by 10 according to the crystal symmetry-6/K。
Example 2 the low temperature thermal shrinkage and coefficient of thermal shrinkage of the material in the temperature range of 150K to room temperature were successfully calculated using the bosch residual indentation.
Example 3:
in the test (100) of the example, the axial linear thermal shrinkage coefficient of the single-crystal copper material at room temperature (namely 300K) to 150K and the thickness of a test piece at room temperature is 2mm, and the difference between the example and the example 1 is that the measurement and calculation are carried out by utilizing the shape of Vickers residual indentation, and the specific test steps are as follows:
the method comprises the following steps: the same sample preparation process and surface quality as those in example 1 were used;
step two: pressing a test sample surface by using a Vickers indenter of a low-temperature nano indenter at room temperature (namely 300K, recorded as reference temperature) to record as a mark indentation A, and obtaining a typical pressing load-depth curve, wherein the maximum pressing load is 100mN, the residual pressing depth reaches 2610nm, the hardness is 750MPa, and the elastic modulus is 92.3 GPa;
step three: controlling the temperature of the test piece to be reduced from room temperature (namely 300K) to 150K (recorded as target temperature) by a cold finger integrated on the wall of the scanning electron microscope cavity, enabling the (100) single crystal copper test piece to generate thermal shrinkage deformation, and simultaneously carrying out real-time in-situ imaging recording on the marked indentation A under 150K and 300K respectively;
step four: pressing a test on the surface of the test piece by using a Vickers indenter of an in-situ low-temperature nano indenter at the temperature of 150K, and recording as a marked indentation B, and obtaining a typical indentation load-depth curve, wherein the maximum indentation load is 100mN, the residual indentation depth reaches 2240nm, the hardness is 1075MPa, and the elastic modulus is 95.7 GPa;
step five: heating the temperature of the (100) single crystal copper test piece from 150K to room temperature (namely 300K) reversely through a heating element, reversely recovering the deformation of the material, and simultaneously carrying out real-time in-situ imaging recording on the marked indentation B under 150K and 300K respectively;
step six: extracting the cross-sectional area (81 μm) of the marked indentation from the real-time topographic information of the marked indentations A and B at 150K and room temperature (namely 300K) by using image processing software2，60μm2，77μm2，55μm2) And drawing and calculating the lengths of 3 intersecting lines of the marking indentation and the test cross section (8.955 μm,9.014 μm,8.967 μm and 9.086 μm; 7.758 μm,7.724 μm,7.802 μm, 7.700 μm; 8.785 μm,8.697 μm,8.804 μm, 8.813 μm; 7.442 μm,7.398 μm,7.435 μm; 7.390 μm);
step seven: referring to FIG. 11, room temperature marked indentation A has a residual indentation depth of 2.610 μm, and 150K marked indentation B has a residual indentation depth of 2.240 μm, when the length averages of the intersection lines of the marked indentation and the test cross section are 9.106 μm and 7.416 μm, respectively. And then toCalculating according to the formula (9) to obtain the characteristic angle alpha1、α260.18 degrees and 58.86 degrees.
Step eight: substituting the cross-sectional areas and the intersection line lengths of the marked indentations A and B into the formula (1) for calculation to obtain the material low-temperature axial thermal shrinkage of 3.55 mu m in the temperature range from 150K to room temperature (namely 300K);
step nine: further, the axial linear thermal contraction coefficient in the temperature range is calculated by the formula (2) to be 1.18X 10-5K, the low-temperature thermal shrinkage coefficient of the single-crystal copper material is 1.18 multiplied by 10 at the moment according to the symmetry of the crystal-5/K。
Example 3 vickers residual indentation was successfully used to calculate the low temperature thermal shrinkage and coefficient of thermal shrinkage of the material in the temperature range of 150K to room temperature.
The above description is only a preferred example of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like of the present invention shall be included in the protection scope of the present invention.
Claims (2)
1. A method for testing the low-temperature thermal shrinkage coefficient of a material by utilizing the residual indentation morphology is characterized by comprising the following steps of: the method comprises the following steps:
grinding and polishing an initial surface (6) of a test piece, bonding the initial surface to the surface of an objective table, carrying out an indentation test on the surface of the test piece by using a nano indenter under a room temperature environment, selecting a sharp pyramid indenter (4) as the indenter, recording a characteristic angle as alpha, and recording a residual indentation/pit on the surface of the test piece as a marked indentation A;
secondly, carrying out in-situ non-contact imaging on the marked indentation A by means of a microscopic imaging functional component and recording the shape information of the marked indentation A in a room temperature environment;
step three, selecting a reference temperature T within the temperature range from room temperature to 77K1Extracting the reference temperature T from the real-time topographic information of the marked indentation A1The side length a of the intersection line (7) of the lower marking impression A and the test cross sectioni(i-1, 2, … …, n), and obtaining the cross-sectional area A of the marking indentation A1Characteristic angle of alpha1(ii) a In a similar manner, at the target temperature T2The side length of the intersection line (7) of the marking impression A and the test cross section is bi(i ═ 1,2, … …, n), mark indentation a cross-sectional area a2；
Step four, the same as above, at the target temperature T2Then, carrying out an indentation test on the surface of the test piece by using a nano indentation instrument, and recording the residual indentation of the surface of the test piece as a mark indentation B; the edge length of the intersection line (7) of the marking indentation B and the test cross section is recorded as ci(i ═ 1,2, … …, n), mark indentation B cross-sectional area a3(ii) a Temperature change to a reference temperature T1Then, the side length d of the intersection line (7) of the marking indentation B and the test cross section is extractedi(i-1, 2, … …, n), the cross-sectional area of marking indentation B at this time was derived as a4Characteristic angle of alpha2；
Step five, qualitatively judging whether the low-temperature thermal shrinkage coefficient of the material shows isotropy in the test cross section or not according to the ratio relation between the side length and the cross section area of the intersection line (7) of the marked indentation A, B and the test cross section in different temperature environments;
sixthly, before and after the temperature changing environment, as the axial shrinkage or expansion displacement delta L of the test piece is kept consistent, the contact surface distance between the mark indentation A and the mark indentation B is kept constant; using equation (1) to calculate the equation1To T2Axial shrinkage or expansion displacement amount Δ L of the test piece at temperature:
wherein n represents the number of faces of the selected pyramid pressure head (4);
step seven, substituting the formula (1) into the formula (2) to calculate the equation T1To T2Low-temperature thermal shrinkage coefficient β of the test piece at temperature:
wherein L isTIs a reference temperature T1Axial dimension of lower specimen from room temperature, i.e. T0298K, the specimen axial dimension L is iteratively extrapolated.
2. The method for testing the low-temperature thermal shrinkage coefficient of the material by utilizing the residual indentation morphology as claimed in claim 1, wherein: reference temperature T in the third and fourth steps1And a target temperature T2Preferably within the normal cold temperature range, i.e. 77K to room temperature.
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