CN111257360B - Application of laser and method for detecting critical crystallization time of amorphous alloy - Google Patents
Application of laser and method for detecting critical crystallization time of amorphous alloy Download PDFInfo
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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Abstract
The invention provides application of laser in detecting the critical crystallization time of amorphous alloy. The invention also provides a method for detecting the critical crystallization time of the amorphous alloy. The laser processing sample has high speed, and can be processed on a small sample at high flux by changing experimental parameters. Conventional methods can only measure those components that have good glass forming ability, i.e., components that have a critical crystallization time on the order of milliseconds. The method of the present invention can measure not only components having good glass-forming ability but also components having poor glass-forming ability. The laser pulse width is short, the method is suitable for searching the critical crystallization time of the amorphous alloy with millisecond magnitude, and the time resolution is high. By the detection method, the structure from the amorphous state to the crystalline state is accurately judged. The detection method is simple and effective, and the amorphous alloy critical crystallization time detected by the method is high in precision and small in error.
Description
Technical Field
The invention belongs to the field of materials. In particular, the invention relates to application of laser and a method for detecting the critical crystallization time of amorphous alloy.
Background
Amorphous alloys have attracted much attention because of their excellent properties such as high strength, high hardness, high elasticity, and high wear resistance, and nearly thousands of components have been developed. The glass forming ability of an amorphous alloy is a critical factor that limits its dimensions. The critical crystallization time is the shortest crystallization time for an amorphous alloy below the melting point and above the glass transition temperature. The longer the critical crystallization time, the greater the glass forming ability. Currently, the main methods for measuring the critical crystallization time are measuring the minimum rapid cooling rate during cooling or the minimum uncrystallized critical heating rate during heating. However, the conventional experimental method is time-consuming and labor-consuming, requires repeated tests of a large number of samples, is harsh to the experimental environment, and is difficult to rapidly and accurately characterize the amorphous forming ability of a certain component, so that the direct measurement of the critical crystallization time of the amorphous alloy is a great challenge.
The conventional method is, for example, an electric levitation method, the precision of which is 1 s; differential thermal analysis with an accuracy of 0.1 s; flash differential thermal analysis with an accuracy of 0.1 ms. The conventional method is to measure under vacuum conditions with an accuracy of only up to 0.1ms at the most and only those components with good glass forming ability, i.e. components with a critical crystallization time in the order of milliseconds, can be measured.
Therefore, a new method for measuring the critical crystallization time of the amorphous alloy is urgently needed.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a novel method for measuring the critical crystallization time of the amorphous alloy. Specifically, the invention aims to provide a method which has high detection speed and simple and effective detection method and can directly detect the critical crystallization time of the amorphous alloy.
The purpose of the invention is realized by the following technical scheme:
the inventor finds that laser processing is an advanced technology, has the main advantage of high processing speed, and the interaction of the laser processing on materials is a process of repeatedly and rapidly heating and cooling for many times, so that the requirement of rapid detection is met, and high-throughput detection of the critical crystallization time of amorphous alloys of different systems can be realized by utilizing laser processing. The present inventors have also unexpectedly found that the laser treatment method under air conditions not only can achieve an accuracy of 0.01us, but also can measure both a component having a good glass-forming ability and a component having a poor glass-forming ability. The accuracy of the method of the present invention is not achievable by conventional methods.
In one aspect, the invention provides an application of laser in detecting the critical crystallization time of an amorphous alloy.
In another aspect, the present invention provides a method for detecting a critical crystallization time of an amorphous alloy, comprising the following steps:
(1) cleaning the amorphous alloy;
(2) after the cleaned amorphous alloy is fixed, processing the amorphous alloy by adopting laser under the air condition, and judging whether a laser processing area is crystallized by adopting an X-ray diffractometer; the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 800mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 400 kHz;
when the laser is adopted to process the amorphous alloy, the power and the spot diameter in the selected process parameters are unchanged, and the scanning speed v, the laser pulse width tau and the repetition frequency f are randomly changed; wherein, the step length delta f when the repetition frequency f is changed is less than or equal to 50 kHz; the step length of the scanning speed is that delta v is less than or equal to 20 mm/s;
(3) judging whether the laser processing area is crystallized or not by an X-ray diffractometer, finding out laser process conditions for enabling the amorphous alloy to be in an amorphous state or in a crystalline state, defining the corresponding laser process parameters when the amorphous alloy is crystallized as the critical crystallization laser process parameters of the amorphous alloy, and recording the corresponding repetition frequency as f0The scanning speed is denoted by v0Laser pulse width is recorded as τ0The spot diameter is recorded as D0；
Calculating the critical crystallization time t of the amorphous alloy by the following formula:
t＝D0f0τ0/v0wherein D is0＝0.05。
In the method, when the laser is used for processing the amorphous alloy, whether the area processed by the amorphous laser is obviously damaged by the laser is observed, if the area processed by the amorphous laser is obviously damaged, the parameter is stopped to be changed, then an X-ray diffractometer is used for judging whether the laser processing area generates the crystallization phenomenon, and the critical laser process parameter from the amorphous state to the crystalline state is found.
Fig. 1 of the present invention shows that the process of laser acting on the material is a complete process of heating and cooling the material, which is called a laser annealing process. If the critical time for keeping the amorphous state and the crystalline state of the amorphous alloy after laser annealing is found, namely the critical crystallization time of the amorphous alloy, the action time of the laser on the material is equal to the critical crystallization time of the amorphous alloy. So the critical crystallization time t ═ D of amorphous alloy can be calculated0f0τ0/v0Wherein the spot diameter D0Indicating the selected distance traveled by the laser on the materialScanning velocity v0Indicating the speed of laser operation, repetition frequency f0Indicates the number of laser pulses output by the laser in 1s and the laser pulse width tau0Representing the time a laser pulse is applied to the material; d0/v0Representing laser operation D0How many seconds the distance took; f. of0τ0Indicating how long the laser was on the material in 1 second. So D0f0τ0/v0For laser operation D0The total time of the laser acting on the material, namely the acting time t of the laser acting on the material.
Preferably, in the method of the present invention, the amorphous alloy is an iron-based, zirconium-based, lanthanum-based, or cerium-based amorphous alloy.
Preferably, in the method of the present invention, when the amorphous alloy is an iron-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 100-.
Preferably, in the method of the present invention, the Fe-based amorphous alloy is Fe78Si9B13、Fe40Ni40P14B6Or Fe56Co7Ni7Zr10B20And (3) amorphous alloy.
Preferably, in the method of the present invention, when the amorphous alloy is a zirconium-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 100-.
Preferably, in the method of the present invention, the zirconium-based amorphous alloy is Zr65Cu15Ni10Al10、Zr46Cu46Al8、Zr55Ni5Al10Cu30Or Zr52.5Ti5Cu17.9Ni14.6Al10And (3) amorphous alloy.
Preferably, in the method of the present invention, when the amorphous alloy is a lanthanum-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 400mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 400 kHz.
Preferably, in the method of the present invention, the lanthanum-based amorphous alloy is La55Ni25Al20、La60Ni20Al20Or La55Al25Ni10Cu10And (3) amorphous alloy.
Preferably, in the method of the present invention, when the amorphous alloy is a cerium-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 800mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 400 kHz.
Preferably, in the method of the present invention, the cerium-based amorphous alloy is Ce65Al10Cu20Co5、Ce60Al20Cu20Or Ce70Al10Ni10Cu10And (3) amorphous alloy.
Preferably, in the method of the present invention, the washing in the step (1) is performed by ultrasonic washing with alcohol or acetone.
Preferably, in the method of the present invention, before the step (1) of cleaning the amorphous alloy, a step of cutting the amorphous alloy into a sample strip is further included.
Preferably, in the method of the present invention, the fixing in step (2) is performed by fixing the washed amorphous alloy on a glass slide by carbon paste.
In the method of the present invention, the laser-treated region may also be observed by an optical microscope to preliminarily screen the amorphous and crystallized regions. Then, an X-ray diffractometer is used for judging whether the area after laser processing is crystallized or not.
The invention has the following beneficial effects:
(1) the method adopts laser to detect the critical crystallization time of the amorphous alloy. The laser processing sample has high speed, and can be processed on a small sample at high flux by changing experimental parameters.
(2) The laser pulse width is short, the method is suitable for searching the critical crystallization time of the amorphous alloy with millisecond magnitude, and the time resolution is high.
(3) By the detection method, the structure from the amorphous state to the crystalline state is accurately judged. The detection method is simple and effective, and the amorphous alloy critical crystallization time detected by the method is high in precision and small in error.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic temperature-time-transformation diagram of an amorphous alloy;
FIG. 2a shows Fe in example 1 of the present invention78Si9B13An optical microscope photograph of the laser-treated area of the amorphous alloy ribbon, wherein the repetition frequency is 300 kHz;
FIG. 2b is Fe in example 1 of the present invention78Si9B13An optical microscope photograph of the laser treated area of the amorphous alloy ribbon, wherein the repetition frequency is 350 kHz;
FIG. 3a is Fe in example 1 of the present invention78Si9B13An X-ray diffraction pattern of the laser treated area of the amorphous alloy ribbon with a repetition frequency of 300 kHz;
FIG. 3b is Fe according to example 1 of the present invention78Si9B13An X-ray diffraction pattern of the laser treated area of the amorphous alloy ribbon with a repetition frequency of 350 kHz;
FIG. 4a shows Zr in example 4 of the present invention65Cu15Ni10Al10An optical microscope photograph of the laser treated area of the amorphous alloy ribbon, wherein the repetition frequency is 250 kHz;
FIG. 4b shows Zr in example 4 of the present invention65Cu15Ni10Al10Laser treatment of amorphous alloy ribbonOptical microscopy of a region with a repetition frequency of 300 kHz;
FIG. 5a shows Zr in example 4 of the present invention65Cu15Ni10Al10An X-ray diffraction pattern of the laser treated area of the amorphous alloy ribbon with a repetition frequency of 250 kHz;
FIG. 5b shows Zr in example 4 of the present invention65Cu15Ni10Al10An X-ray diffraction pattern of the laser treated area of the amorphous alloy ribbon with a repetition frequency of 300 kHz;
FIG. 6a is La of example 8 of the present invention55Ni25Al20An optical microscope photograph of the laser-treated area of the amorphous alloy ribbon, wherein the pulse width is 2 ns;
FIG. 6b shows La of example 8 of the present invention55Ni25Al20An optical microscope photograph of the laser-treated area of the amorphous alloy ribbon, wherein the pulse width is 4 ns;
FIG. 7a is La of example 8 of the present invention55Ni25Al20An X-ray diffraction pattern of the laser treated area of the amorphous alloy strip, wherein the pulse width is 2 ns;
FIG. 7b shows La of example 8 of the present invention55Ni25Al20An X-ray diffraction pattern of the laser treated area of the amorphous alloy ribbon with a pulse width of 4 ns;
FIG. 8a is Ce of example 11 of the present invention65Al10Cu20Co5An optical microscope photograph of the laser-treated area of the amorphous alloy ribbon, wherein the pulse width is 4 ns;
FIG. 8b is Ce of example 11 of the present invention65Al10Cu20Co5An optical microscope photograph of the laser treated area of the amorphous alloy ribbon, wherein the pulse width is 6 ns;
FIG. 9a is Ce of example 11 of the present invention65Al10Cu20Co5An X-ray diffraction pattern of the laser treated area of the amorphous alloy ribbon with a pulse width of 4 ns;
FIG. 9b is Ce of example 11 of the present invention65Al10Cu20Co5Laser treated areas of amorphous alloy ribbonWherein the pulse width is 6 ns.
Detailed Description
The present invention is described in further detail below with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
Fe with the thickness of 25 microns is selected78Si9B13The amorphous alloy strip is firstly cleaned in advance by ultrasound, then fixed on a glass slide by carbon glue, and scribed on the amorphous alloy strip by different laser process parameters. Selecting the laser power P as 10W and the spot diameter D as 0.05mm, observing the effect after laser treatment by naked eyes, and further selecting the following laser process parameter range, wherein the scanning speed v is 100-200mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 200-400 kHz. Then observing the surface appearance of the scribed position of the sample by using an optical microscope, and further reducing the range of technological parameters, wherein delta f is 50 kHz; Δ v is 20 mm/s. Finally, accurately judging the amorphous alloy Fe by utilizing an X-ray diffractometer78Si9B13Whether the sample is crystallized or not. And then finding out the critical laser process parameters, wherein the power is 10W, the diameter of a light spot is 0.05mm, the scanning speed is 160mm/s, the pulse width is 4ns, and the repetition frequency is 350 kHz. Fig. 2 is an optical microscope photograph of fe-based amorphous ribbon. The appearance of the amorphous sample is obviously different from that of the crystallized sample through the appearance of the surface of the sample, and the crystallization (with the characteristic of a microstructure with a certain appearance) is preliminarily judged by the spherical small-grain sample which is formed in the laser scribing at 350 kHz. FIG. 3 is an X-ray diffraction pattern of Fe-based amorphous bands, confirming the preliminary judgment in the optical micrograph, i.e., 300kHz underline remains amorphous while crystallization occurs at 350 kHz. The diameter of the light spot is D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f0350kHz, with the formula t D0f0τ0/v0The critical crystallization time can be calculated to be 0.44 microseconds.
Example 2
Is selected to be thickFe with a degree of 30 microns40Ni40P14B6The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 100-40Ni40P14B6The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 350 kHz. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 4ns, the repetition frequency is 400kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.5 microseconds.
Example 3
Fe with the thickness of 30 microns is selected56Co7Ni7Zr10B20The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 100-56Co7Ni7Zr10B20The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 350 kHz. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 4ns, the repetition frequency is 400kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.50 microseconds.
Example 4
Selecting a thickness of 25 muZr of rice65Cu15Ni10Al10The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 100-65Cu15Ni10Al10The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, the laser process parameters are found to be scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 200kHz, and fig. 5a shows that the sample is not crystallized after the treatment. Whereas the laser process parameters were scan speed 160mm/s, pulse width 4ns, repetition frequency 250kHz, fig. 5b shows that the sample crystallized after treatment. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f 0250 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.31 microseconds.
Example 5
Zr with the thickness of 40 microns is selected46Cu46Al8The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 100-46Cu46Al8The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 150 kHz. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 4ns, the repetition frequency is 200kHz, and the sample is crystallized. So as to obtain the critical crystallization laser process parameter as the scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f 0200 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.26 microseconds.
Example 6
Zr with the thickness of 40 microns is selected55Ni5Al10Cu30The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 100-55Ni5Al10Cu30The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the laser process parameters are found to be scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 200kHz, so that the sample is not crystallized. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 4ns, the repetition frequency is 250kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f 0250 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.31 microseconds.
Example 7
Zr with the thickness of 30 microns is selected52.5Ti5Cu17.9Ni14.6Al10. The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 100-52.5Ti5Cu17.9Ni14.6Al10The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 250 kHz. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 4ns, the repetition frequency is 300kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f 0300 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.38 microseconds.
Example 8
La with the thickness of 40 microns is selected55Ni25Al20The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 160-400mm/s, a laser pulse width tau of 2-250ns, a repetition frequency f of 200-400kHz, and a pulse width of La55Ni25Al20The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, the laser process parameters are found to be scanning speed of 160mm/s, pulse width of 2ns and repetition frequency of 400kHz, and fig. 7a shows that the sample is not crystallized after the treatment. Whereas the laser process parameters were scan speed 160mm/s, pulse width 4ns, repetition frequency 400kHz, fig. 7b shows that the sample crystallized after treatment. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.50 microseconds.
Example 9
Selecting La with the thickness of 50 microns60Ni20Al20The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 160-400mm/s, a laser pulse width tau of 2-250ns, a repetition frequency f of 200-400kHz, and a pulse width of La60Ni20Al20The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 160mm/s, pulse width of 2ns and repetition frequency of 400 kHz. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 4ns, the repetition frequency is 400kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ04ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.50 microseconds.
Example 10
Selecting La with the thickness of 50 microns55Al25Ni10Cu10The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 160-400mm/s, a laser pulse width tau of 2-250ns, a repetition frequency f of 200-400kHz, and a pulse width of La55Al25Ni10Cu10The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 160mm/s, pulse width of 4ns and repetition frequency of 400 kHz. However, the laser process parameters are that the scanning speed is 160mm/s, the pulse width is 6ns, the repetition frequency is 400kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0160mm/s, pulse width τ06ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.75 microseconds.
Example 11
Ce with the thickness of 30 micrometers is selected65Al10Cu20Co5The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 400-800mm/s, a laser pulse width tau of 2-250ns, a repetition frequency f of 200-400kHz, and a specific ratio of Ce to the specific ratio of65Al10Cu20Co5The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, the laser process parameters are found to be the scanning speed of 400mm/s, the pulse width of 4ns and the repetition frequency of 400kHz, and fig. 9a shows that the sample is not crystallized after the treatment. Whereas the laser process parameters were scan speed 400mm/s, pulse width 6ns, repetition frequency 400kHz, fig. 9b shows that the sample crystallized after treatment. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0400mm/s, pulse width τ06ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.30 microseconds.
Example 12
Ce with the thickness of 20 microns is selected60Al20Cu20The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 400-800mm/s, a laser pulse width tau of 2-250ns, a repetition frequency f of 200-400kHz, and a specific ratio of Ce to the specific ratio of60Al20Cu20The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 400mm/s, pulse width of 2ns and repetition frequency of 400 kHz. However, the laser process parameters are that the scanning speed is 400mm/s, the pulse width is 4ns, the repetition frequency is 400kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0400mm/s, pulse width τ04ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.20 microseconds.
Example 13
Ce with the thickness of 60 micrometers is selected70Al10Ni10Cu10The procedure for the amorphous alloy ribbon was the same as in example 1. Selecting a fixed laser power P of 10W, a spot diameter D of 0.05mm, a scanning speed v of 400-800mm/s, a laser pulse width tau of 2-250ns, a repetition frequency f of 200-400kHz, and a specific ratio of Ce to the specific ratio of70Al10Ni10Cu10The amorphous strip is processed. Whether the sample is crystallized or not is accurately judged by an X-ray diffractometer, and the sample is found to be not crystallized when the laser process parameters are scanning speed of 400mm/s, pulse width of 4ns and repetition frequency of 400 kHz. However, the laser process parameters are that the scanning speed is 400mm/s, the pulse width is 6ns, the repetition frequency is 400kHz, and the sample is crystallized. Thus obtaining the critical crystallization laser process parameters: spot diameter of D00.05mm, scanning speed v0400mm/s, pulse width τ06ns, repetition frequency f0400 kHz. Then by the formula t ═ D0f0τ0/v0The critical crystallization time was calculated to be 0.20 microseconds.
Claims (13)
1. A method for detecting the critical crystallization time of an amorphous alloy comprises the following steps:
(1) cleaning the amorphous alloy;
(2) after the cleaned amorphous alloy is fixed, processing the amorphous alloy by adopting laser under the air condition, and judging whether a laser processing area is crystallized by adopting an X-ray diffractometer; the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 800mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 400 kHz;
when the laser is adopted to process the amorphous alloy, the power and the spot diameter in the selected process parameters are unchanged, and the scanning speed v, the laser pulse width tau and the repetition frequency f are randomly changed; wherein, the step length delta f when the repetition frequency f is changed is less than or equal to 50 kHz; the step length of the scanning speed is that delta v is less than or equal to 20 mm/s;
(3) judging whether the laser processing area is crystallized or not by an X-ray diffractometer, finding out laser process conditions for enabling the amorphous alloy to be in an amorphous state or in a crystalline state, defining the corresponding laser process parameters when the amorphous alloy is crystallized as the critical crystallization laser process parameters of the amorphous alloy, and recording the corresponding repetition frequency as f0The scanning speed is denoted by v0Laser pulse width is recorded as τ0The spot diameter is recorded as D0；
Calculating the critical crystallization time t of the amorphous alloy by the following formula:
t＝D0f0τ0/v0wherein D is0＝0.05。
2. The method of claim 1, wherein the amorphous alloy is an iron-based, zirconium-based, lanthanum-based, or cerium-based amorphous alloy.
3. The method of claim 1, wherein when the amorphous alloy is an iron-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 100-.
4. The method of claim 3, wherein the Fe-based amorphous alloy is Fe78Si9B13、Fe40Ni40P14B6Or Fe56Co7Ni7Zr10B20And (3) amorphous alloy.
5. The method of claim 1, wherein when the amorphous alloy is a zirconium-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 100-.
6. The method according to claim 5, wherein the zirconium based amorphous alloy is Zr65Cu15Ni10Al10、Zr46Cu46Al8、Zr55Ni5Al10Cu30Or Zr52.5Ti5Cu17.9Ni14.6Al10And (3) amorphous alloy.
7. The method of claim 1, wherein when the amorphous alloy is a lanthanum-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 400mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 400 kHz.
8. The method of claim 7, wherein the lanthanum-based amorphous alloy is La55Ni25Al20、La60Ni20Al20Or La55Al25Ni10Cu10And (3) amorphous alloy.
9. The method of claim 1, wherein when the amorphous alloy is a cerium-based amorphous alloy, the laser adopts the following process parameters:
the power P is 10W, the spot diameter D is 0.05mm, the scanning speed v is 800mm/s, the laser pulse width tau is 2-250ns, and the repetition frequency f is 400 kHz.
10. The method of claim 9, wherein the cerium-based amorphous alloy is Ce65Al10Cu20Co5、Ce60Al20Cu20Or Ce70Al10Ni10Cu10And (3) amorphous alloy.
11. The method according to claim 1, wherein the washing in the step (1) is performed by ultrasonic washing with alcohol or acetone.
12. The method according to claim 1, wherein before the step (1) of cleaning the amorphous alloy, the method further comprises the step of cutting the amorphous alloy into a sample strip.
13. The method according to claim 1, wherein the fixing in the step (2) is performed by fixing the washed amorphous alloy on the slide glass by carbon paste.
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