CN106483021B - Amorphous alloy thin strip stretching device used with nanoindenter and application method thereof - Google Patents
Amorphous alloy thin strip stretching device used with nanoindenter and application method thereof Download PDFInfo
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- G01N3/08—Investigating strength properties of solid materials by application of mechanical stress by applying steady tensile or compressive forces
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
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Abstract
The utility model provides a thin stretching device of amorphous alloy area that allies oneself with usefulness with nanometer indentation appearance, including the base, high accuracy worm wheel formula coarse and fine tuning differential head, the stationary mast, the adjustable fender, the fixed stop, including a motor, an end cap, a controller, and a cover plate, motor power, the gear, the sample support, anchor clamps and remote control unit, wherein high accuracy worm wheel formula coarse and fine tuning differential head is located between the stationary mast, its one end is connected with the adjustable fender, the adjustable fender is located base one end and is connected with base monolithic, the spring is by centre gripping between adjustable fender and adjustable fender, the sample support is arranged in on the base, be located between adjustable fender and adjustable fender, anchor clamps attach to the sample support, including a motor, motor power is fixed on the base, the transmission shaft of motor passes through the gear and is connected with high accuracy worm wheel formula coarse and fine tuning differential head. The device carries out micro-nano rheological mechanical behavior test, and deflection and strain are controllable and the precision is high. The device is particularly suitable for testing the micro-nano mechanical behavior of the film material in different tensile strain states in the tensile deformation process.
Description
Technical Field
The invention relates to a technology for researching structural evolution and related mechanical behavior of an amorphous alloy material by using a nano indenter, in particular to an amorphous alloy thin strip stretching device used with the nano indenter and a using method thereof.
Background
The amorphous alloy has unique mechanical properties of high elasticity, high strength and the like, has functions of soft magnetism, corrosion resistance and the like, and is a new material with wide application prospect. The amorphous alloy is an ideal model material for researching the deformation mechanism of the amorphous material, so that the structural mechanism of the amorphous alloy is always the focus and hot spot of people. The amorphous alloy has a nominal elastic zone of more than 2 percent, and researches show that the amorphous alloy shows many unique mechanical properties such as viscoelasticity, hysteresis elasticity, elastic rheological yield and the like in the nominal elastic zone, and the exploration of the amorphous alloy structure and deformation mechanism is particularly important in the zone. Researchers have proposed rheological cell models based on experiments and computational simulations to understand and interpret the physical and mechanical problems of amorphous materials. The model considers that there are some liquid-like regions on the nanometer scale in amorphous alloys. The liquid-like region exhibits lower atomic packing density, lower hardness and modulus, higher energy states, and susceptibility to shear deformation and flow than the surrounding region. The flowing units in the amorphous material are similar to the defects in the crystalline material, the distribution of the concentration, the size and the energy of the flowing units determines the mechanical properties, the aging and other properties of the amorphous alloy, and the mechanical properties and other properties of the amorphous alloy can be effectively improved by regulating and controlling the flowing units in the amorphous alloy. Although rheology-based elastic cell models and methods of internal dissipation, stress relaxation can characterize the rheological cell activation energy and size and distribution, these models have not been directly experimentally verified. Because a simple traditional experimental method generally analyzes the deformation mechanism of a material through the mechanical response of the material to an applied load, the method is difficult to detect the microscopic local flow behavior of the amorphous alloy in the deformation process, particularly in a nominal elastic section, and simultaneously lacks the evolution information of the structural details along with the load and the time in the corresponding deformation process, so that the deformation amount and the strain value of the material in the deformation process are difficult to accurately obtain, and the evolution information of the material structure in the deformation process under the action of an external force is the key for researching the deformation mechanism and the microscopic mechanism of the material. Meanwhile, due to the limitation of the size of the instrument and equipment, the size of the sample and the space size of the sample chamber, the traditional mechanical experimental equipment is difficult to be combined with an in-situ structure characterization experimental device. Although computational simulation provides many important deformation mechanisms at atomic or molecular scale, the simulation is usually based on extreme conditions that cannot be achieved at present, such as extremely high deformation rate, extremely low temperature or extremely small-scale samples, and the simulation result cannot be verified experimentally. Therefore, the experimental verification lack of the theoretical model limits further research and scientific understanding of the amorphous alloy deformation mechanism.
On the other hand, when the traditional macroscopic mechanics experimental equipment is used for researching micro-nano mechanical responses such as room-temperature visco-elastic behaviors and the like of materials with rate-related behaviors of amorphous alloys which are not as remarkable as those of certain polymer materials, defects in the aspects of equipment precision, data acquisition and the like are not beneficial to capturing details of rheological mechanical behaviors of the materials. Meanwhile, macro experiments require a large number of experimental samples, which raises the requirements for the material preparation process to a certain extent, and thus, discreteness of experimental results is difficult to avoid due to the process difference of sample preparation. A large number of researches prove that the research on the micro-nano mechanical behavior of the amorphous alloy by adopting a nano indenter is very suitable. The nano-indenter-based mechanical behavior characterization is particularly suitable for the rheological mechanical behavior research of materials such as amorphous alloys with limited size, room temperature brittleness and insignificant rate dependence due to the advantages of no damage, high precision and the like. By using the indenter nanoindentor, people can capture the rheological deformation details of the amorphous alloy, and the deformation details are the visual reflection of the microstructure of the material. However, the spatial size of the sample chamber of the nanoindenter is limited, and the test precision is very sensitive to the temperature change of the sample chamber during the test process, i.e. a slight temperature disturbance can also generate a remarkable temperature drift. Therefore, it is difficult to combine the conventional large-size mechanical experimental equipment with a nanoindenter to detect the micro-nano mechanical behavior evolution in the stress process. In addition, a nano-indenter is adopted to carry out micro-nano mechanical behavior test, particularly, the pressing depth is usually in a nano level under a low-load mode, so that the requirement on the flatness of the surface of a sample is very high, and the requirements on the surface of the sample by the general methods of mechanical polishing of the surface of a large-size sample and the like are difficult to achieve.
If the micro-nano mechanical response of the material can be characterized in real time in the deformation process of the material or in a constant strain state (namely in the stress relaxation process), and the structural evolution information of the material is analyzed based on the corresponding mechanical response, the method is an important breakthrough for researching the deformation mechanism of the amorphous material sensitive to the process and the speed. Therefore, the device which is ideally suitable for researching the structural evolution and related mechanical behavior of the amorphous alloy in the deformation process needs to realize controllable and high-precision deformation of the amorphous alloy, can be used together with a nanoindenter to research the micro-nano mechanical behavior change of the amorphous alloy in the deformation process or the stress relaxation process and explore the microstructure and the deformation mechanism of the amorphous alloy. The amorphous alloy thin strip stretching device used together with the nanoindenter can meet the requirements.
Disclosure of Invention
Aiming at the defects of the existing experimental device, the invention aims to provide an amorphous alloy thin strip stretching device combined with a nano-indenter and a using method thereof, wherein the device can be used for researching the micro-nano mechanical property change of amorphous alloy thin strip samples with different components in the stretching process and under different constant strain stretching states at different temperatures so as to reflect the structural evolution information of the materials in the deformation process.
According to a first embodiment of the present invention, an amorphous alloy ribbon stretching apparatus for use with a nanoindenter is provided.
The utility model provides a thin stretching device that takes of amorphous alloy with nanometer indentator allies oneself with usefulness, the device include base, high accuracy worm wheel formula coarse and fine tuning differential head, fixed upright, adjustable fender, fixed fender, motor power, sample support, two anchor clamps. Wherein: one end of the base is provided with a fixed baffle. The other end of the base is provided with a fixed upright post. The high-precision worm-gear type coarse and fine tuning differential head is arranged on the fixed upright post and is connected with the telescopic rod connecting piece on the movable baffle. The movable baffle is positioned between the fixed baffle and the fixed upright post. The sample support is placed on the base and located between the movable baffle and the fixed baffle. The top parts of the movable baffle and the fixed baffle are respectively provided with a clamp. The motor is connected with the high-precision worm-wheel type coarse and fine adjustment differential head and drives the high-precision worm-wheel type coarse and fine adjustment differential head. The motor power supply is connected with the motor; preferably, the motor power supply is electrically connected to the motor.
Preferably, the apparatus further comprises a control system. The control system comprises a receiving device and a remote control device. The control system is connected with and controls the motor power supply and/or the motor.
In the invention, the motor is connected with the high-precision worm-gear type coarse and fine adjustment differential head through a gear or a belt.
In the invention, the high-precision worm-gear type coarse and fine adjustment differential head comprises a fine adjustment button, a coarse and fine adjustment switching button and a telescopic rod. One end of the telescopic rod is fixedly connected with the telescopic rod connecting piece on the movable baffle plate. The fine adjustment button and the coarse adjustment button are both connected with the telescopic rod and control the extension or the shortening of the telescopic rod. Or the fine adjustment button and the coarse adjustment button control the movement of the telescopic rod. The coarse-fine adjustment switching button control motor is connected (or alternatively connected) with the fine adjustment button or the coarse adjustment button.
Preferably, the coarse-fine adjustment switch button is positioned at the end part of the high-precision worm-wheel type coarse-fine adjustment differential head, which is far away from one end of the movable baffle.
Preferably, the device further comprises a limit nut. Wherein, the high-precision worm-wheel type rough and fine adjustment differential head is fixed on the fixed upright post through a limit nut, and the telescopic rod passes through the fixed upright post and the limit nut to be connected with the telescopic rod connecting piece on the movable baffle.
In the invention, the upper part of the sample support is provided with a beam. The top of the beam is higher than the movable baffle and the fixed baffle. The difference in height between the cross beam and the flapper is 0.1 to 5mm, preferably 0.2 to 3mm, more preferably 0.5 to 2mm, for example 0.6mm,0.8mm.
In the present invention, the gap between the sample holder and the fixed baffle; the gap between the sample holder and the fixed barrier is 0.1-10mm, preferably 0.2-5mm, more preferably 0.5-3mm, e.g. 1mm,1.5mm.
In the present invention, the gap between the sample holder and the movable baffle; the gap between the sample holder and the flapper is 5mm to 20mm, preferably 2 to 10mm, more preferably 3 to 8mm, for example, 5mm,6mm.
Preferably, a spring is arranged between the movable baffle and the fixed baffle. The sample support surrounds in the periphery of spring, and the adjustable fender is connected to the one end of spring, and fixed stop is connected to the other end of spring.
In the present invention, the device has a length of 50 to 150mm, preferably 80 to 120mm, more preferably 90 to 110mm, for example 106mm. The width is 30-80mm, more preferably 40-70mm, preferably 50-65mm, e.g. 60mm. The height is 10-50mm, preferably 15-40mm, more preferably 20-30mm, e.g. 26mm.
Preferably, the displacement precision of the high-precision worm wheel type coarse and fine tuning differential head reaches 0.5 mu m, and the strain precision reaches 2.5 x 10 -5 。
According to a second embodiment of the invention, a method for using an amorphous alloy ribbon stretching device in combination with a nanoindenter is provided.
The use method of the amorphous alloy thin strip stretching device used with the nanoindenter comprises the following steps:
1) Pre-pressing: prepressing the spring through a fine adjusting button and a coarse adjusting button of the high-precision worm-wheel type coarse and fine adjusting differential head, and screwing the coarse and fine adjusting switching button;
2) Installation: processing an amorphous alloy thin strip sample into a preset size and then clamping the sample by a clamp;
3) Unloading: placing the amorphous alloy thin strip stretching device for clamping the thin strip sample into a working chamber of a nano indenter, and unloading the spring;
4) Micro-nano mechanical behavior test: the unloading rate of the spring is controlled by controlling the rotating speed of the motor, after the amorphous alloy thin strip sample stretches to reach a preset strain amount, the motor stops rotating, and the nano indentation meter performs micro-nano mechanical behavior test on the thin strip sample;
5) Continuously measuring micro-nano mechanical behavior: restarting the motor, repeating the step 4), and continuously measuring the micro-nano mechanical behavior of the thin strip sample in different tensile strain states;
6) Quantitative determination: after the motor is started to a preset stress relaxation initial strain value, the motor stops working, time is recorded, the nano indentation apparatus measures micro-nano mechanical behavior of the amorphous alloy at certain time intervals, and quantitative measurement of mechanical response change of the material in the stress relaxation process is achieved.
In the invention, the prepressing in the step 1) is realized by a high-precision worm-wheel type coarse and fine tuning differential head, a fine tuning button and a coarse tuning button of the high-precision worm-wheel type coarse and fine tuning differential head accurately control the compression displacement to a preset value, and after a spring is prepressed to a preset value, the coarse tuning button is fixed by the coarse and fine tuning switching button.
Preferably, the pre-pressure on the spring is exerted by the high-precision worm wheel type coarse and fine adjustment differential head jacking pressure, and the differential head jacking pressure can reach 39.2N.
In the invention, the specific operation of unloading the spring in the step 3) is as follows: and (3) putting the amorphous alloy thin strip stretching device into a working chamber of a nanoindenter integrally, after a temperature field is kept stable, starting a motor through a remote control device and a receiving device, driving a fine adjustment button of a high-precision worm wheel type coarse and fine adjustment differential head to rotate, and unloading the spring.
In the invention, the control of the deformation of the amorphous alloy thin strip stretching is realized by a fine adjusting button of a high-precision worm wheel type coarse fine adjusting differential head, the displacement precision reaches 0.5 mu m, and the strain precision reaches 2.5 x 10 -5 。
In the present invention, there is no particular requirement for the preparation of thin amorphous alloy strip samples, and known techniques are used. The material of the spring can be comprehensively selected according to the deformation, the strain requirement and the like of the stretched amorphous alloy.
In the invention, the device can realize the continuous stretching deformation of the amorphous alloy from zero strain and accurately control the strain, and the control of the stretching deformation of the amorphous alloy is realized by a fine adjustment button of a coarse fine adjustment micrometer head.
According to the method, the amorphous alloy is subjected to tensile deformation through the remote control device and the motor, so that the temperature of a working chamber can be kept stable during working, the height of a device in a sample testing area and the overall dimension of the device are small, the space requirement of the low-load mode working of the nanoindentor is met, the nanoindentor can be used together with the nanoindentor to test the change of micro-nano mechanical behaviors of the amorphous alloy, such as the hardness, the viscoelasticity response, the hysteresis elasticity response, the creep, the stress relaxation and the like in different tensile deformation states and stress relaxation processes. The apparatus and method are equally applicable to other materials than amorphous alloys that can be formed into a continuous ribbon having a smooth side surface.
In the invention, the fixed baffle is fixedly arranged at one end of the base. The fixed upright post is preferably a device with the lower end fixedly arranged on the base and the upper end divided into two upright posts, and the divided part is used for a telescopic rod of a high-precision worm gear type rough and fine adjustment differential head to penetrate through.
In the invention, one end of a telescopic rod of the high-precision worm-wheel type rough and fine adjustment differential head is connected with an adjusting device in the high-precision worm-wheel type rough and fine adjustment differential head, and the other end of the telescopic rod is connected with a telescopic rod connecting piece on the movable baffle. The telescopic rod can be a freely telescopic device or a device with a fixed length, and the coarse and fine adjustment switching button controls the motor to be connected with the fine adjustment button or the coarse adjustment button. The fine adjustment button and the coarse adjustment button are connected with the telescopic rod, the fine adjustment button and the coarse adjustment button control the extension or the shortening of the telescopic rod, or the fine adjustment button and the coarse adjustment button control the movement of the telescopic rod, so that the telescopic rod drives the movable baffle to be far away from or close to the fixed baffle, the adjustment of the distance between the movable baffle and the fixed baffle is realized, and the compression or the stretching of the spring is controlled.
In the present invention, the sample holder is placed on the base between the movable flap and the fixed flap. The sample support is used for supporting the amorphous alloy thin strip. The purpose that the top of the cross beam is higher than the movable baffle and the fixed baffle is that the amorphous alloy is in a stretched state on the thin belt stretching device, and when the amorphous alloy is used together with a nano-indenter, the amorphous alloy cannot generate large deformation, and the related performance can be measured more accurately. All there is the clearance between sample support and fixed stop and the adjustable fender, is to guarantee that the telescopic link drives the adjustable fender and removes to have abundant space, is convenient for survey the metallic glass in-process, can adjust the metallic glass thin area and be in different tensile state, survey various performances of metallic glass under the different states. Generally, the gap between the sample support and the fixed baffle is fixed and does not change; the gap between the sample support and the movable baffle is changed, the width of the gap is changed along with the movement of the movable baffle,
in the invention, the differential head pushes the spring to generate pre-pressure, and after a sample is loaded, the differential head is unloaded and the spring is recovered to drive the amorphous thin strip sample to stretch; the pre-pressure to the spring is applied by the high-precision worm wheel type coarse and fine adjustment differential head jacking pressure, and the differential head jacking pressure can reach 39.2 x 2N (namely 2 times of the original differential head jacking pressure). In addition, the purpose that is equipped with the spring between adjustable fender and the fixed stop: the inherent clearance of mechanical equipment and prefabrication bring inevitable errors; the high-precision worm-wheel type coarse and fine tuning differential head drives the movable baffle to move, and the error of the high-precision worm-wheel type coarse and fine tuning differential head is transferred to the test of the performance of the amorphous alloy; the spring is arranged, and has the functions of stretch resistance and compression resistance, so that the spring can act as force for movement in the moving process of the movable baffle plate, the movable baffle plate is constantly in a 'tightened' state, errors caused by driving the movable baffle plate by the high-precision worm-gear type coarse and fine tuning differential head are eliminated, the movement of the movable baffle plate can be controlled more accurately, and various performances of the amorphous alloy can be measured more accurately. The sample support surrounds the periphery of the spring; one end of the spring is fixedly connected with the fixed baffle, and the other end of the spring is fixedly connected with the movable baffle. That is, the spring passes through the interior of the sample holder and is free to compress or extend, unaffected by the sample holder.
In the invention, the selection of the motor has no special requirement, and because the device of the invention is smaller, a micro motor is generally selected.
In the invention, the control system comprises a receiving device and a remote control device, and the receiving device is in signal connection with the remote control device to realize the isolated control of the device.
In the invention, the limiting nut is used for fixing the high-precision worm wheel type coarse and fine tuning differential head on the fixed upright post. The telescopic link of the rough fine setting differential head of high accuracy worm wheel formula can freely remove.
In the invention, the differential head top pressure refers to the pressure generated by the pressing sheet on the spring in the advancing process when the differential head rotates the differential head coarse and fine adjusting buttons to enable the telescopic rod to advance.
In the present invention, the specification of the thin strip sample is not limited and is set according to the kind of the amorphous alloy and the property to be measured. Generally, the thickness of the ribbon sample is 20 μm to 100 μm, and the width of the ribbon sample is 100 μm to 1000 μm.
In the invention, the spring is unloaded, namely the differential head fine adjustment button is rotated to retract the telescopic rod, and the pressure applied to the spring by the pressing sheet is removed in the retracting process. Generally, the unloading speed is controlled by a remote control device to control the power supply of the motor and/or the motor, and the unloading speed can be selected between 5 mu m/s and 120 mu m/s according to the rotating speed of the motor. The fine tuning button of the differential head rotates for one circle, the corresponding telescopic rod moves for 5 mu m, the rotating speed of the motor of the electric motor is controllable at a constant speed in the embodiment, the rotating speed is 6-60 revolutions/minute (0.1-1 revolution/second), so the corresponding unloading speed can reach 0.5-5 mu m/s, and the unloading strain rate can reach 2.5-10 mu m/s by taking the initial length of the spring as an example, the initial length of the spring is 20mm -5 s -1 ～2.5*10 -4 s -1 )。
In the invention, the preset strain amount for stretching the amorphous alloy thin strip sample can reach 0-0.02. The strain 0.02 refers to the maximum tensile strain of the amorphous alloy thin strip which can be realized by the device, and actually, if the thickness and the width of the thin strip are small, larger tensile strain can be realized until the amorphous alloy is broken. In addition, 0.02 is the upper limit of elastic strain of most amorphous alloys, plastic deformation or fracture generally occurs when the strain value exceeds the upper limit, 0-0.02 is set according to needs, if the micro-nano mechanical behavior of the amorphous alloy in a stretching state with the strain of 0.01 needs to be known, the preset strain of the device is 0.01, which is a great characteristic of the device, after n strain values are selected between 0-0.02 to measure the micro-nano mechanical behavior, the strain values are taken as horizontal coordinates, the measured value of the micro-nano mechanical behavior is taken as vertical coordinates, and the evolution rule of the micro-nano mechanical behavior of the amorphous alloy in the stretching deformation process can be obtained.
In the invention, the time interval of the nano-indentation instrument on the micro-nano mechanical behavior of the amorphous alloy can be different according to the required micro-nano mechanical experiment. For example, in hardness, viscoelasticity and hysteresis elasticity tests, the time interval is generallyUnloading to thin strip to achieve the desired strain is designed by experimental protocols such as 0.002,0.006,0.01, etc. Different tensile strain states, according to the motor rotation speed, taking a motor with the rotation speed of 24 revolutions per minute as an example [ displacement rate of 2 μm/s, strain rate of 1 × 10 ] -4 s -1 ]Then the time interval is 20s,60s and 100s, and the test can be carried out after the temperature of the system is stable. For another example, during an experiment in the stress relaxation process, the amorphous alloy is unloaded to the required strain, the strain value can be any one of 0-0.02 through the design of an experimental scheme, and then the micro-nano mechanical behavior of the material is determined to be changed in the process that the constant strain of the amorphous alloy is increased along with the time at certain time intervals; for example, hardness, viscoelasticity, hysteretic elasticity and the like, stress relaxation refers to the phenomenon that stress is reduced along with time when a material is under constant strain, and the device can quantitatively measure the change of micro-nano mechanical behavior of the material along with time in the relaxation process, so that the structural evolution of the material in the process is indirectly reflected. In the relaxation process, the time interval of the nano indentation test in the initial stage is small, and according to the working mechanism of the nano indenter, the time interval of each nano indentation work in the relaxation process can be 10-180 s.
In the present invention, the preset value of the compression displacement amount refers to a preset value of the compression of the spring, and the value can reach 0.022 at most according to the maximum pressure that can be realized by the differential head, and the material, the outer diameter, the wire diameter and the elastic constant thereof of the spring.
In the present invention, the temperature of the nanoindenter, i.e., the operating temperature range of the nanoindenter, is set according to the ribbon sample. The temperature of the device can be directly set by the working temperature range of the nanoindenter and is not influenced by the device, the material quality of the spring is not influenced by temperature change when the temperature is not more than 300 ℃, and the range which can be reached by the working temperature of the nanoindenter is between room temperature and 350 ℃, so the recommended and applicable experimental temperature range of the device is between room temperature and 300 ℃. The material can show different characteristics in the process of tensile deformation at different temperatures, and the device can also be characterized by combining with a micro-nano mechanical experiment of a nano-indenter.
In the invention, the high-precision worm wheel type coarseThe displacement precision of the fine tuning differential head is calibrated by a differential head manufacturer, namely the displacement control precision can be realized by a fine tuning knob of the differential head; the strain precision is determined according to the displacement precision and the longitudinal length of the elastic substrate, and the strain precision reaches 0.5 mu m/20mm =0.000025, namely 2.5 x 10, because the displacement precision of the differential head reaches 0.5 mu m, and the longitudinal length of the spring in the device is 20mm in the embodiment -5 。
Besides being used with a nano-indenter, the device is also suitable for being used with other experimental equipment (such as a spectrum scanner) so as to observe or actually measure other physical quantity changes of the thin film or thin strip material in the stretching process.
Compared with the existing stretching device, the stretching device has the beneficial effects that:
1. the device has small overall dimension and convenient assembly and disassembly, and can be used together with a nanoindenter to perform hardness test and micro-nano rheological mechanical behavior tests such as viscoelasticity, hysteresis elasticity and the like;
2. the continuous stretching deformation of the amorphous alloy can be realized, the deformation and the strain are controllable, and the precision is high;
3. constant strain can be kept, and the stress relaxation process of the amorphous alloy is realized;
4. the method is suitable for different types of amorphous alloy materials, and the experimental temperature is controllable and the temperature field is stable;
5. the tested sample is an amorphous alloy thin strip prepared by a rotary quenching system, the surface of the thin strip attached to a roller is rough, the other surface of the thin strip is formed by a high-vacuum single-roller rotary quenching system through strip throwing, the surface of the thin strip is smooth and flat, and the testing precision is high.
Drawings
FIG. 1 is a schematic structural diagram of an amorphous alloy ribbon stretching device used in conjunction with a nanoindenter according to the present invention;
FIG. 2 is a front view of an amorphous alloy ribbon stretching apparatus used in conjunction with a nanoindenter of the present invention;
FIG. 3 is a top view of an amorphous alloy ribbon stretching apparatus used in conjunction with a nanoindenter of the present invention;
FIG. 4 is a left side view of an amorphous alloy ribbon stretching apparatus used in conjunction with a nanoindenter of the present invention;
FIG. 5 is a cross-sectional view of an amorphous alloy ribbon stretching apparatus of the present invention in use with a nanoindenter;
FIG. 6 is a schematic structural diagram of an experimental state of an amorphous alloy thin strip stretching device used in combination with a nanoindenter according to the present invention;
FIG. 7 is a front view of the experimental state of the amorphous alloy ribbon pulling apparatus used in conjunction with a nanoindenter of the present invention;
FIG. 8 is a top view of an experimental state of an amorphous alloy ribbon stretching apparatus used in conjunction with a nanoindenter of the present invention;
FIG. 9 is a left side view of an experimental state of an amorphous alloy ribbon stretching apparatus used in conjunction with a nanoindenter of the present invention;
FIG. 10 is a cross-sectional view of the amorphous alloy ribbon pulling apparatus of the present invention in an experimental state in combination with a nanoindenter;
FIG. 11 is a partial enlarged view of the experimental state M of the amorphous alloy thin strip stretching device used in combination with the nanoindenter of the present invention;
FIG. 12 is a schematic diagram of a control system according to the present invention.
Reference numerals: a: a nanoindenter; b: an amorphous alloy thin strip stretching device; 1: a base; 2: a high-precision worm wheel type coarse and fine adjustment differential head; 201: a fine adjustment button; 202: coarsely adjusting a button; 203: a coarse and fine adjustment switch button; 204: a telescopic rod; 3: fixing the upright post; 4: a movable baffle; 401: a telescopic rod connecting piece; 5: fixing a baffle plate; 6: a spring; 7: a motor; 8: a motor power supply; 9: a receiving device; 10: a gear; 11: a sample holder; 1101: a cross beam; 12: a clamp; 13: a remote control device; 14: a limit nut; 15: a thin strip sample; 16: a control system; d1: a gap between the sample support and the fixed baffle; d2: a gap between the sample holder and the movable baffle; h: the height difference between the cross beam and the movable baffle.
Detailed Description
According to a first embodiment of the present invention, an amorphous alloy ribbon stretching apparatus B for use with a nanoindenter a is provided.
The utility model provides a thin stretching device B of taking of amorphous alloy of alligator A antithetical couplet usefulness, the device B includes base 1, high accuracy worm-gear formula coarse and fine tuning differential head 2, fixed upright 3, adjustable fender 4, fixed baffle 5, motor 7, motor power 8, sample support 11, two anchor clamps 12. Wherein: one end of the base 1 is provided with a fixed baffle 5. The other end of the base 1 is provided with a fixed upright post 3. The high-precision worm-gear type coarse and fine adjustment differential head 2 is arranged on the fixed upright post 3 and is connected with a telescopic rod connecting piece 401 on the movable baffle 4. The movable baffle 4 is positioned between the fixed baffle 5 and the fixed upright 3. The sample holder 11 is placed on the base between the movable baffle 4 and the fixed baffle 5. The top of the movable baffle 4 and the fixed baffle 5 are respectively provided with a clamp 12. The motor 7 is connected with the high-precision worm-gear type coarse and fine adjustment differential head 2 and drives the high-precision worm-gear type coarse and fine adjustment differential head 2. The motor power supply 8 is connected with the motor 7; preferably, the motor power supply is electrically connected to the motor.
Preferably, the apparatus B further comprises a control system 16. The control system 16 comprises a receiving device 9 and a remote control device 13. The control system 16 is connected to and controls the motor power supply 8 and/or the motor 7.
In the invention, the motor 7 is connected with the high-precision worm-wheel type coarse and fine tuning differential head 2 through a gear 10 or a belt.
In the present invention, the high-precision worm-gear type coarse and fine adjustment head 2 includes a fine adjustment button 201, a coarse adjustment button 202, a coarse and fine adjustment switch button 203, and a telescopic rod 204. One end of the telescopic rod 204 is fixedly connected with a telescopic rod connecting piece 401 on the movable baffle plate 4. The fine adjustment button 201 and the coarse adjustment button 202 are both connected to the telescopic rod 204 and control the extension or contraction of the telescopic rod 204. Alternatively, the fine tuning knob 201 and the coarse tuning knob 202 control the movement of the telescopic rod 204. The coarse and fine adjustment switch button (203) controls the motor 7 to be connected with the fine adjustment button 201 or the coarse adjustment button 202 (or the coarse and fine adjustment switch button (203) controls the motor 7 to be alternately connected with the fine adjustment button 201 or the coarse adjustment button 202).
Preferably, the coarse-fine adjustment switch 203 is located at the end of the high-precision worm-wheel type coarse-fine adjustment head 2, which is far away from the movable baffle 4.
Preferably, the device B further comprises a limit nut 14. Wherein, the high-precision worm-gear type rough and fine adjustment differential head 2 is fixed on the fixed upright post 3 through the limit nut 14, and the telescopic rod 204 passes through the fixed upright post 3 and the limit nut 14 to be connected with the telescopic rod connecting piece 401 on the movable baffle 4.
In the present invention, the sample holder 11 is provided with a beam 1101 at the upper portion. The top of the beam 1101 is higher than the movable baffle 4 and the fixed baffle 5. The height difference h between the cross beam 1101 and the flapper 4 is 0.1-5mm, preferably 0.2-3mm, more preferably 0.5-2mm, such as 0.6mm,0.8mm.
In the present invention, the gap between the sample holder 11 and the fixed stop 5; the gap d1 between the sample holder 11 and the fixed stop 5 is 0.1-10mm, preferably 0.2-5mm, more preferably 0.5-3mm, e.g. 1mm,1.5mm.
In the present invention, the gap between the sample holder 11 and the flapper 4; the gap d2 between the sample holder 11 and the flapper 4 is 1-20mm, preferably 2-10mm, more preferably 3-8mm, for example, 5mm,6mm.
Preferably, a spring 6 is arranged between the movable baffle 4 and the fixed baffle 5. The sample support 11 surrounds the periphery of the spring 6, one end of the spring 6 is connected with the movable baffle 4, and the other end of the spring 6 is connected with the fixed baffle 5.
In the present invention, the device has a length of 50 to 150mm, preferably 80 to 120mm, more preferably 90 to 110mm, for example 106mm. The width is 30-80mm, more preferably 40-70mm, preferably 50-65mm, e.g. 60mm. The height is 10-50mm, preferably 15-40mm, more preferably 20-30mm, e.g. 26mm.
Preferably, the displacement precision of the high-precision worm-wheel type coarse and fine tuning differential head 2 reaches 0.5 mu m, and the strain precision reaches 2.5 x 10 -5 。
According to a second embodiment of the present invention, a method of using an amorphous alloy ribbon stretching apparatus in conjunction with a nanoindenter is provided.
A use method of an amorphous alloy thin strip stretching device B used together with a nano indenter A comprises the following steps:
1) Pre-pressing: prepressing the spring 6 through a fine tuning button 201 and a coarse tuning button 202 of the high-precision worm-wheel type coarse and fine tuning differential head 2;
2) Installation: processing an amorphous alloy thin strip sample 15 into a preset size and then clamping the sample by a clamp 12;
3) Unloading: placing the amorphous alloy thin strip stretching device B for clamping the thin strip sample 15 into a working chamber of a nano indenter A, and unloading the spring 6;
4) Micro-nano mechanical behavior test: the unloading rate of the spring 6 is controlled by controlling the rotating speed of the motor 7, after the amorphous alloy thin strip sample 15 is stretched to reach a preset strain amount, the motor 7 stops rotating, and the nano indentation apparatus A carries out micro-nano mechanical behavior test on the thin strip sample 15;
5) Continuously measuring micro-nano mechanical behavior: restarting the motor 7, repeating the step 4), and continuously measuring the micro-nano mechanical behavior of the thin strip sample 15 in different tensile strain states;
6) Quantitative determination: after the motor 7 is started to a preset stress relaxation initial strain value, the motor 7 stops working, time is recorded, the nano indentation apparatus A measures the micro-nano mechanical behavior of the amorphous alloy at a certain time interval, and quantitative measurement of mechanical response change of the material in the stress relaxation process is achieved.
In the invention, the pre-pressing in step 1) is realized by the high-precision worm-wheel type coarse and fine tuning differential head 2, the fine tuning button 201 and the coarse tuning button 202 of the high-precision worm-wheel type coarse and fine tuning differential head 2 precisely control the compression displacement to a preset value, and after the pre-pressing spring 6 reaches the preset value, the coarse and fine tuning switching button 203 fixes the coarse tuning button 202.
Preferably, the pre-pressure on the spring 6 is applied by pressing the high-precision worm wheel type coarse and fine adjustment head 2, and the pressure of the differential head can reach 39.2N.
In the present invention, the specific operations of unloading the spring 6 in step 3) are: and (3) putting the amorphous alloy thin belt stretching device B into a working chamber of the nanoindenter A, after the temperature field is kept stable, starting the motor 7 through the remote control device 13 and the receiving device 9, driving the fine tuning button 201 of the high-precision worm wheel type coarse and fine tuning differential head 2 to rotate, and unloading the spring 6.
In the invention, the control of the deformation of the amorphous alloy thin strip stretching is realized by the fine tuning knob 201 of the high-precision worm wheel type coarse and fine tuning differential head 2, the displacement precision reaches 0.5 mu m, and the strain precision reaches 2.5 x 10 -5 。
Example 1
Referring to fig. 1, an amorphous alloy thin strip stretching device B used in combination with a nanoindenter a comprises a base 1, a high-precision worm gear type rough and fine tuning differential head 2, a fixed upright column 3, a movable baffle 4, a fixed baffle 5, a motor 7, a motor power supply 8, a sample support 11 and two clamps 12. Wherein: one end of the base 1 is provided with a fixed baffle 5. The other end of the base 1 is provided with a fixed upright post 3. The high-precision worm-gear type rough and fine adjustment differential head 2 is arranged on the fixed upright post 3 and is connected with a telescopic rod connecting piece 401 on the movable baffle 4. The movable baffle 4 is positioned between the fixed baffle 5 and the fixed upright 3. The sample holder 11 is placed on the base between the movable baffle 4 and the fixed baffle 5. The top of the movable baffle 4 and the fixed baffle 5 are respectively provided with a clamp 12. The motor 7 is connected with the high-precision worm-gear type coarse and fine adjustment differential head 2 and drives the high-precision worm-gear type coarse and fine adjustment differential head 2. The motor power supply 8 is connected with the motor 7. The motor 7 is connected with the high-precision worm wheel type coarse and fine tuning differential head 2 through a gear 10. The high-precision worm-gear type coarse and fine adjustment head 2 comprises a fine adjustment button 201, a coarse adjustment button 202, a coarse and fine adjustment switching button 203 and a telescopic rod 204. One end of the telescopic rod 204 is fixedly connected with a telescopic rod connecting piece 401 on the movable baffle plate 4. The fine adjustment button 201 and the coarse adjustment button 202 are both connected to the telescopic rod 204 and control the extension or contraction of the telescopic rod 204. The coarse and fine adjustment switch button 203 controls the motor 7 to be connected with the fine adjustment button 201 or the coarse adjustment button 202. The coarse-fine adjustment switching button 203 is positioned at the end part of one end of the high-precision worm-wheel type coarse-fine adjustment differential head 2 departing from the movable baffle 4. The device B also comprises a limit nut 14. Wherein, the high-precision worm-gear type rough and fine adjustment differential head 2 is fixed on the fixed upright post 3 through the limit nut 14, and the telescopic rod 204 passes through the fixed upright post 3 and the limit nut 14 to be connected with the telescopic rod connecting piece 401 on the movable baffle 4. The sample holder 11 is provided with a beam 1101 at the upper part. The top of the beam 1101 is higher than the movable baffle 4 and the fixed baffle 5. The height difference h between the beam 1101 and the movable baffle 4 is 0.5mm. The gap between the sample holder 11 and the fixed baffle 5; the clearance d1 between the sample support 11 and the fixed baffle 5 is 1mm, and the clearance between the sample support 11 and the movable baffle 4 is provided; the gap d2 between the sample holder 11 and the flapper 4 is 5mm.
The length, width and height of the device are 106mm 60mm 26mm.
Example 2
Example 1 is repeated except that the apparatus B further comprises a control system 16. The control system 16 comprises a receiving device 9 and a remote control device 13. The control system 16 is connected to and controls the motor power supply 8 and the motor 7.
Example 3
Example 2 was repeated except that the motor 7 was connected to the high precision worm gear type coarse and fine tuning differential head 2 via a gear. The fine adjustment knob 201 and the coarse adjustment knob 202 control the movement of the telescopic rod 204.
Example 4
Example 2 was repeated except that the height difference h between the beam 1101 and the flapper 4 was 0.8mm. The gap between the sample holder 11 and the fixed baffle 5; the clearance d1 between the sample support 11 and the fixed baffle 5 is 2mm, and the clearance between the sample support 11 and the movable baffle 4 is larger than the clearance d1 between the sample support 11 and the fixed baffle 5; the gap d2 between the sample holder 11 and the flapper 4 was 6mm.
Example 5
Example 2 was repeated except that a spring 6 was provided between the movable shutter 4 and the fixed shutter 5. The sample support 11 surrounds the periphery of the spring 6, one end of the spring 6 is connected with the movable baffle 4, and the other end of the spring 6 is connected with the fixed baffle 5.
Example 6
The implementation 2 is repeated, and the base 1, the fixed upright post 3, the movable baffle 4 and the fixed baffle 5 are made of medium carbon steel. The high-precision worm-gear type coarse and fine tuning differential head 2 is WGP-13 produced by Sigma optical machine company of Japan, the stroke is 0-13mm, the rated static load is 39.2N, the minimum coarse tuning reading is 5 mu m, and the minimum fine tuning reading is 0.5 mu m. The nano-indenter A is a low-load mode nano-indenter module of a TriboInder micro-nano comprehensive mechanical testing system of Hysitron corporation in America. The spring 6 is made of alloy steel, the outer diameter is 10mm, the length is 20mm, the wire diameter is 2.5mm, and the room-temperature spring constant is 98N/mm through testing. Through calculation, the pre-pressing strain range which can be realized under the action of the rated static load of the high-precision worm-gear type coarse and fine adjustment differential head 2 is 0-2%.
Example 7
Referring to fig. 6, a method for using an amorphous alloy ribbon stretching apparatus in conjunction with a nanoindenter a, using the apparatus of example 2, pre-stresses a spring 6 by rotating a high-precision worm-gear type coarse and fine tuning differential head 2, and after the coarse and fine tuning scales of the high-precision worm-gear type coarse and fine tuning differential head 2 accurately control the compression displacement to a preset value of 0.4mm, the coarse tuning part is fixed by a coarse and fine tuning switch 203. An amorphous alloy thin strip sample 15 prepared by a high-vacuum single-roller rotary quenching system is processed into a tensile sample shape, and the end part of the sample is clamped by a clamp 12. The whole device is put into a working chamber of a nanoindenter A, after a temperature field is kept stable, the motor 7 is started through the remote control device 13 and the receiving device 9, the fine tuning button 201 of the high-precision worm-wheel type rough and fine tuning differential head 2 is driven to rotate, and the spring 6 is unloaded. The unloading speed of the spring 6 is controlled by accurately controlling the rotating speed of the motor 7, after the amorphous alloy thin belt stretches to reach the preset strain, the motor 7 stops rotating, and the nano indentation apparatus A performs micro-nano mechanical behavior test. And restarting the motor 7, repeating the previous step of operation, and continuously measuring the micro-nano mechanical behavior of the amorphous alloy in the state of the indefinite tensile strain. After the motor 7 is started to a preset stress relaxation initial strain value, the motor 7 stops working, time is recorded, the nano indentation apparatus A measures the micro-nano mechanical behavior of the amorphous alloy at a certain time interval, and quantitative measurement of mechanical response change of the material in the stress relaxation process is achieved.
Claims (12)
1. The use method of the amorphous alloy thin strip stretching device used with the nanoindenter comprises the following steps:
1) Pre-pressing: prepressing a spring (6) through a fine adjusting button (201) and a coarse adjusting button (202) of a high-precision worm-wheel type coarse and fine adjusting differential head (2), and screwing a coarse and fine adjusting switching button (203);
2) Installation: processing an amorphous alloy thin strip sample (15) into a preset size and then clamping the sample by a clamp (12);
3) Unloading: placing the amorphous alloy thin strip stretching device (B) for clamping the thin strip sample (15) into a working chamber of a nano indenter (A) and unloading the spring (6);
4) Micro-nano mechanical behavior test: the unloading rate of the spring (6) is controlled by controlling the rotating speed of the motor (7), after the amorphous alloy thin strip sample (15) is stretched to reach a preset strain amount, the motor (7) stops rotating, and the nano indentation apparatus (A) performs micro-nano mechanical behavior test on the thin strip sample (15);
5) Continuously measuring micro-nano mechanical behavior: restarting the motor (7), repeating the step 4), and continuously measuring the micro-nano mechanical behavior of the thin strip sample (15) in different tensile strain states;
6) Quantitative determination: after the motor (7) is started to reach a preset stress relaxation initial strain value, the motor (7) stops working, time is recorded, the nano indentation instrument (A) measures micro-nano mechanical behavior of the amorphous alloy at a certain time interval, and quantitative measurement of mechanical response change of the material in the stress relaxation process is achieved;
wherein: the device (B) comprises a base (1), a high-precision worm gear type coarse and fine tuning differential head (2), a fixed upright post (3), a movable baffle plate (4), a fixed baffle plate (5), a motor (7), a motor power supply (8), a sample support (11) and two clamps (12), wherein: one end of the base (1) is provided with a fixed baffle (5); the other end of the base (1) is provided with a fixed upright post (3); the high-precision worm-gear type rough and fine tuning differential head (2) is arranged on the fixed upright post (3) and is connected with the movable baffle (4); the movable baffle (4) is positioned between the fixed baffle (5) and the fixed upright post (3); the sample support (11) is placed on the base and positioned between the movable baffle (4) and the fixed baffle (5); the tops of the movable baffle (4) and the fixed baffle (5) are respectively provided with a clamp (12); the motor (7) is connected with the high-precision worm-wheel type coarse and fine adjustment differential head (2) and drives the high-precision worm-wheel type coarse and fine adjustment differential head (2); the motor power supply (8) is electrically connected with the motor (7); the high-precision worm-wheel type coarse and fine adjustment differential head (2) comprises a fine adjustment button (201), a coarse adjustment button (202), a coarse and fine adjustment switching button (203) and a telescopic rod (204), wherein one end of the telescopic rod (204) is fixedly connected with a telescopic rod connecting piece (401) on the movable baffle (4); the fine adjustment button (201) and the coarse adjustment button (202) are both connected with the telescopic rod (204) and control the extension or the shortening of the telescopic rod (204); or the fine adjustment button (201) and the coarse adjustment button (202) control the movement of the telescopic rod (204); the coarse and fine adjustment switching button (203) controls the motor (7) to be connected with the fine adjustment button (201) or the coarse adjustment button (202); a spring (6) is arranged between the movable baffle (4) and the fixed baffle (5), the sample support (11) surrounds the periphery of the spring (6), one end of the spring (6) is connected with the movable baffle (4), and the other end of the spring (6) is connected with the fixed baffle (5).
2. The method of claim 1, wherein: the prepressing in the step 1) is realized through a high-precision worm-wheel type coarse and fine adjustment differential head (2), a fine adjustment button (201) and a coarse adjustment button (202) of the high-precision worm-wheel type coarse and fine adjustment differential head (2) accurately control the compression displacement to reach a preset value, and after a pre-pressing spring (6) reaches the preset value, the coarse adjustment button (202) is fixed through a coarse and fine adjustment switching button (203).
3. The method of claim 2, wherein: the pre-pressure on the spring (6) is applied by the high-precision worm wheel type coarse and fine adjustment differential head (2) in a jacking mode, and the differential head jacking pressure can reach 39.2N.
4. The method according to any one of claims 1-3, wherein: the device (B) further comprises a control system (16), wherein the control system (16) comprises a receiving device (9) and a remote control device (13), and the control system (16) is connected with and controls the motor power supply (8) and/or the motor (7); the specific operation of unloading the spring (6) in the step 3) is as follows: the amorphous alloy thin belt stretching device (B) is integrally placed in a working chamber of a nano-indenter (A), after a temperature field is kept stable, a motor (7) is started through a remote control device (13) and a receiving device (9), a fine adjusting button (201) of a high-precision worm-wheel type coarse and fine adjusting differential head (2) is driven to rotate, and a spring (6) is unloaded.
5. The method according to any one of claims 1-3, wherein: wherein the control of the deformation of the amorphous alloy thin strip stretching is realized by a fine-tuning button (201) of a high-precision worm wheel type coarse and fine tuning differential head (2), the displacement precision reaches 0.5 mu m, and the strain precision reaches 2.5 x 10 -5 。
6. The method of claim 4, wherein: wherein the control of the deformation of the amorphous alloy thin strip stretching is realized by a fine-tuning button (201) of a high-precision worm wheel type coarse and fine tuning differential head (2), the displacement precision reaches 0.5 mu m, and the strain precision reaches 2.5 x 10 -5 。
7. The method of claim 4, wherein: the motor (7) is connected with the high-precision worm wheel type rough and fine adjustment differential head (2) through a gear (10) or a belt.
8. The method of claim 7, wherein: the coarse and fine adjustment switching button (203) is positioned at the end part of one end of the high-precision worm wheel type coarse and fine adjustment differential head (2) departing from the movable baffle (4).
9. The method of claim 8, wherein: the device (B) further comprises a limit nut (14), wherein the high-precision worm-wheel type coarse and fine adjustment differential head (2) is fixed on the fixed upright post (3) through the limit nut (14), and the telescopic rod (204) penetrates through the fixed upright post (3) and the limit nut (14) to be connected with a telescopic rod connecting piece (401) on the movable baffle (4); and/or
A cross beam (1101) is arranged at the upper part of the sample support (11); the top of the beam (1101) is higher than the movable baffle (4) and the fixed baffle (5), and the height difference (h) between the beam (1101) and the movable baffle (4) is 0.1-5mm; the clearance (d 1) between the sample support (11) and the fixed baffle (5) is 0.1-10mm;
the clearance (d 2) between the sample support (11) and the movable baffle (4) is 1-20mm.
10. The method of claim 9, wherein: the height difference (h) between the cross beam (1101) and the movable baffle (4) is 0.2-3mm; the clearance (d 1) between the sample bracket (11) and the fixed baffle (5) is 0.2-5mm;
the clearance (d 2) between the sample support (11) and the movable baffle (4) is 2-10mm.
11. The method according to any one of claims 7-10, wherein: the device has a length of 50-150mm and a width of 30-80mm.
12. The method of claim 11, wherein: the device has a length of 80-120mm, a width of 40-70mm and a height of 15-40mm.
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| CN110487628B (en) * | 2019-08-23 | 2022-04-19 | 杭州源位科技有限公司 | In-situ miniature mechanical test board |
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| CN112082939B (en) * | 2020-08-19 | 2021-08-13 | 上海交通大学 | Method for directly stretching and measuring film adhesion energy based on nano-indentation technology |
| CN112748099A (en) * | 2020-12-21 | 2021-05-04 | 湘潭大学 | Material micro-stretching device used with atomic force microscope and using method thereof |
| CN114791385A (en) * | 2021-01-26 | 2022-07-26 | 日立金属株式会社 | Method for evaluating embrittlement of amorphous alloy thin strip and test device for evaluating embrittlement of amorphous alloy thin strip |
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