CN114561644B - Amorphous nanocrystalline alloy with reticular structure and preparation method and application thereof - Google Patents
Amorphous nanocrystalline alloy with reticular structure and preparation method and application thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 41
- 239000000956 alloy Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims abstract description 27
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 23
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000006698 induction Effects 0.000 abstract description 8
- 238000000137 annealing Methods 0.000 abstract description 5
- 230000035699 permeability Effects 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 28
- 229910001004 magnetic alloy Inorganic materials 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 11
- 238000010791 quenching Methods 0.000 description 6
- 230000000171 quenching effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000155 melt Substances 0.000 description 5
- 239000005300 metallic glass Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000003292 glue Substances 0.000 description 3
- 239000002159 nanocrystal Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910002555 FeNi Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000007578 melt-quenching technique Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
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Abstract
The invention relates to a netlike amorphous nanocrystalline alloy, a preparation method and application thereof, and the preparation method comprises the following steps: (1) Fixing an amorphous alloy sample with the thickness smaller than 50 mu m on a bracket of an ion thinning instrument; (2) Adjusting angles of a left ion gun and a right ion gun of the ion thinning instrument, and preprocessing a sample for a first target duration under a first target voltage; (3) And (3) reducing the angles of the left ion gun and the right ion gun, reducing the applied voltage to a second target voltage, and processing the sample obtained in the step (2) for a second target time under the second target voltage to obtain the amorphous nanocrystalline alloy with the network structure. The ion thinning instrument equipment is adopted, so that the influence of high temperature on an amorphous alloy sample is eliminated, and the limit of the annealing brittleness of the amorphous alloy on industrial application can be effectively solved; secondly, the nanocrystalline of the amorphous nanocrystalline alloy prepared by the invention is uniformly dispersed in an amorphous framework, so that higher saturation induction intensity and permeability can be obtained.
Description
Technical Field
The invention belongs to the technical field of alloys, and particularly relates to an amorphous nanocrystalline alloy with a reticular structure, and a preparation method and application thereof.
Background
Amorphous metal refers to a solid metal in which atoms are spatially arranged without long-term processes, i.e. without a crystalline structure. For thousands of years, metallic materials in contact and use have translational symmetry of atomic arrangement, both crystalline metals. The appearance of amorphous metal is due to breakthrough of amorphous metal process technology, and as early as 20 th century 30 people have obtained amorphous metal films by utilizing a vapor deposition method, and in 1969 Pond, madden and the like, rapidly cooling metal melt by utilizing a rapidly rotating metal roller is reported for the first time, so that a new way for preparing amorphous alloy continuous long strips is opened up for industrial production of amorphous metal. The development of amorphous alloy and the corresponding rapid quenching technology greatly promotes the development of amorphous magnetic materials, and the three earliest amorphous soft magnetic alloy series batch application is Fe-based, co-based and FeNi-based amorphous soft magnetic alloy strips.
The nanocrystalline magnetically soft alloy has a single homogeneous crystalline phase structure, and the grain size is less than 100nm. It is well known that the physical precondition of high magnetic permeability of soft magnetic alloys is that both the magnetocrystalline anisotropy constant K and the saturation magnetostriction coefficient lambda s of the alloy tend to be zero. To obtain good soft magnetic properties, the magnetocrystalline anisotropy of the alloy is suppressed in addition to the lambda s being small. The domain wall width in the nanocrystalline thin strip is about 0.5-10 microns, and nanoscale grain clusters cannot pin domain walls, so that the coercivity is very low, and the magnetic permeability is very high. The coercivity H c and initial permeability μ i versus K of a material at small grain sizes can be expressed as: Wherein, P c and P u are constants, D is the grain size, K 1 is the magnetocrystalline anisotropy constant of the nanocrystalline grain, A is the exchange constant, M s is the saturation magnetization, and μ 0 is the vacuum permeability.
In industry, a nanocrystalline thin strip is usually prepared by a melt quenching method, and then annealed at a certain temperature for a proper time to obtain nanocrystalline. The transition of the method depends on long-distance diffusion among atoms, the size of the formed nano crystal is not easy to control, the crystal/amorphous ratio is low, and the increase of the saturation induction intensity and the decrease of the coercive force are limited.
Disclosure of Invention
Based on the defects and shortcomings in the prior art, the invention aims to provide amorphous nanocrystalline alloy with a net structure, and a preparation method and application thereof.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
The preparation method of the amorphous nanocrystalline alloy with the reticular structure comprises the following steps:
(1) Fixing an amorphous alloy sample with the thickness smaller than 50 mu m on a bracket of an ion thinning instrument;
(2) Adjusting angles of a left ion gun and a right ion gun of the ion thinning instrument, and preprocessing a sample for a first target duration under a first target voltage;
(3) And (3) reducing the angles of the left ion gun and the right ion gun, reducing the applied voltage to a second target voltage, and processing the sample obtained in the step (2) for a second target time under the second target voltage to obtain the amorphous nanocrystalline alloy with the network structure.
Preferably, in the step (1), the amorphous alloy sample is an Fe-based, co-based, feCo-based, feNi-based, ni-based, ndFeB-based or rare earth-based amorphous alloy.
Preferably, in the step (2), the angles of the left and right ion guns are not lower than ±5°, the first target voltage is not lower than 5keV, and the first target duration is not lower than 30min.
In the step (2), the angles of the left and right ion guns are respectively 8 degrees, -8 degrees, the first target voltage is 8keV, and the first target duration is 120min.
In the step (3), the angles of the left and right ion guns are not higher than ±5°, the second target voltage is not higher than 5keV, the second target duration is not higher than 60 minutes, and the second target duration is smaller than the first target duration.
In the step (3), the angles of the left and right ion guns are respectively 4 degrees and-4 degrees, the second target voltage is 3keV, and the second target duration is 15min.
Preferably, the support of the ion attenuation instrument is a Cu support or a Mo support.
Preferably, in the step (1), if the thickness of the amorphous strip sample is greater than 50 μm, 2000 mesh SiC sandpaper is used to make the thickness smaller than 50 μm.
The invention also provides the amorphous nanocrystalline alloy with the network structure, which is prepared by the preparation method according to any scheme, and the amorphous nanocrystalline alloy is of a network structure consisting of an amorphous framework and nanocrystalline.
The invention also provides application of the amorphous nanocrystalline alloy according to any scheme, which is used for a transformer, a switching power supply, a transformer or an iron core strip.
Compared with the prior art, the invention has the beneficial effects that:
The ion thinning instrument device adopted by the invention gets rid of the influence of high temperature on the amorphous alloy sample, and can effectively solve the limitation of the annealing brittleness of the amorphous alloy on industrialized application; secondly, the nanocrystalline of the amorphous nanocrystalline alloy prepared by the invention is uniformly dispersed in an amorphous framework, the proportion of the nanocrystalline to the total volume is high and can reach 80% at most, and higher saturation magnetic induction intensity and magnetic conductivity can be obtained. In addition, the amorphous nanocrystalline alloy with excellent soft magnetic property and mechanical property can be obtained by optimizing the technological parameters and precisely regulating the amorphous and nanocrystalline duty ratio.
Drawings
FIG. 1 is an XRD spectrum of an amorphous alloy of Fe 0.8Co0.2)84B14Si1Cu1 according to example 1 of the present invention;
FIG. 2 is a TEM photograph of an amorphous alloy of Fe 0.8Co0.2)84B14Si1Cu1 and a corresponding Fourier transform diagram of example 1 of the present invention;
FIG. 3 is a TEM photograph of an amorphous nanocrystalline alloy of Fe 0.8Co0.2)84B14Si1Cu1 and its corresponding Fourier transform plot according to example 1 of the present invention;
FIG. 4 is a HADDF view of the (Fe 0.8Co0.2)84B14Si1Cu1 amorphous nanocrystalline alloy and its corresponding surface scan) of example 1 of the present invention;
FIG. 5 is a TEM photograph of an amorphous nanocrystalline alloy of Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 and its corresponding Fourier transform plot according to example 2 of the present invention;
FIG. 6 is a TEM photograph of comparative example 1 (Fe 0.8Co0.2)84B14Si1Cu1 amorphous nanocrystalline alloy at various magnifications;
FIG. 7 is a TEM photograph of an amorphous alloy Fe 0.8Co0.2)84B14Si1Cu1 and its corresponding Fourier transform plot of comparative example 2 of the present invention;
FIG. 8 is a graph showing the hysteresis loop comparison of the alloys of the examples and comparative examples of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the following specific examples.
Example 1:
the amorphous nanocrystalline of the network structure of this embodiment (the preparation method of the Fe 0.8Co0.2)84B14Si1Cu1 soft magnetic alloy, including the steps of:
Step 1: the structure of the (Fe 0.8Co0.2)84B14Si1Cu1 amorphous alloy prepared by a melt rapid quenching method is characterized by an X-ray diffractometer and a transmission electron microscope, the XRD spectrum structure is shown in figure 1, the TEM photo is shown in figure 2, and the (Fe 0.8Co0.2)84B14Si1Cu1 amorphous alloy strip selected in the embodiment is of an amorphous structure;
step 2: fixing the amorphous alloy strip on a Cu bracket by using AB glue, placing the amorphous alloy strip into a chamber of an ion thinning instrument, and vacuumizing;
step 3: the angles of the left and right ion guns are adjusted to be 8 degrees and 8 degrees respectively, the applied voltage value is set to be 8keV, and the thinning time of the ion gun is set to be 30min.
Repeating the process of the step 3 for 4 times at intervals of 5min until the light-transmitting holes appear in the middle.
Step 4: the angles of the left ion gun and the right ion gun are adjusted to be 4 degrees and 4 degrees respectively, the applied voltage value is set to be 3keV, the thinning time of the ion gun is set to be 15min, and the amorphous nanocrystalline (Fe 0.8Co0.2)84B14Si1Cu1 soft magnetic alloy) is obtained.
The amorphous nanocrystalline (Fe 0.8Co0.2)84B14Si1Cu1 soft magnetic alloy of this example was characterized as follows:
(1) The sample obtained in the step 4 is characterized by using a transmission electron microscope, and the result is shown in fig. 3, which shows that the prepared amorphous nanocrystalline alloy with the sample structure of a network structure has a central nanocrystalline core of 5-10nm, an amorphous framework of 3-8nm and the nanocrystalline core accounts for 63% of the total area.
(2) The sample obtained in step4 was subjected to element distribution characterization by a transmission electron microscope, and the results are shown in fig. 4.
(3) The alloy obtained in step 1 (original sample) and the alloy obtained in step 4 were tested for saturation induction B s by using a vibrating sample magnetometer, and the results are shown in fig. 8.
Example 2:
The amorphous nanocrystalline of the network structure of this embodiment (the preparation method of the Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy, including the steps of:
step 1: the (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 amorphous alloy) prepared by the melt rapid quenching method is selected, and the selected strip material is determined to be an amorphous structure by an X-ray diffractometer and a transmission electron microscope.
Step 2: fixing the amorphous strip on a Cu bracket by using AB glue, placing the amorphous strip into a chamber of an ion thinning instrument, and vacuumizing;
Step 3: the angles of the left and right ion guns are adjusted to be 10 degrees and minus 10 degrees respectively, the applied voltage value is set to be 8keV, and the thinning time of the ion gun is set to be 30min.
Repeating the process of the step 3 for 3 times at intervals of 5min until the light-transmitting holes appear in the middle.
Step 4: the angles of the left and right ion guns are adjusted to be 5 degrees and minus 5 degrees respectively, the applied voltage value is set to be 5keV, and the thinning time of the ion gun is set to be 30min.
The above procedure of step 4 was repeated 2 times at 5min intervals.
Step 5: the angles of the left ion gun and the right ion gun are respectively adjusted to be 3 degrees and 3 degrees, the applied voltage value is set to be 1.5keV, the thinning time of the ion gun is set to be 10min, and the amorphous nanocrystalline (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy) is obtained.
The amorphous nanocrystalline (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy sample obtained in step 5 is characterized by using a transmission electron microscope, the result is shown in fig. 5, the prepared amorphous nanocrystalline alloy with a sample structure of a net structure can be illustrated, the size of a central nanocrystalline core is 10-30nm, the thickness of an amorphous skeleton is 1-3nm, and the nanocrystalline core accounts for 73% of the total area.
Amorphous nanocrystals (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy, saturated magnetic induction (B s) were also tested using a vibrating sample magnetometer and the results are shown in fig. 8.
Comparative example 1:
The common amorphous nanocrystalline magnetically soft alloy is obtained by a heat treatment method in the comparative example, and specifically comprises the following steps:
Step 1: the (Fe 0.8Co0.2)84B14Si1Cu1 amorphous alloy) prepared by the melt rapid quenching method is selected, and the selected strip material is determined to be an amorphous structure by an X-ray diffractometer and a transmission electron microscope.
Step 2: and (3) carrying out heat treatment on the amorphous strip in the step (1) for 10 minutes at the optimal temperature by utilizing a high vacuum annealing furnace to obtain the common amorphous nanocrystalline magnetically soft alloy.
And (3) characterizing the common amorphous nanocrystalline magnetically soft alloy sample obtained in the step (2) by using an X-ray diffractometer, and determining that the sample is an amorphous nanocrystalline structure.
Step 3: the annealed sample is subjected to ion thinning by an ion thinning instrument, the sample obtained in the step 3 is characterized by using a transmission electron microscope again, and the result is shown in fig. 6, so that the prepared amorphous nanocrystalline alloy with the sample structure of a common structure can be illustrated.
The saturation induction intensity B s of the alloy obtained in step 2 was tested by using a vibrating sample magnetometer, and the result is shown in fig. 8.
Comparative example 2:
The comparative example is a heat treatment method for performing stress relief annealing on (Fe 0.8Co0.2)84B14Si1Cu1 amorphous alloy), and specifically comprises the following steps:
Step 1: the (Fe 0.8Co0.2)84B14Si1Cu1 amorphous alloy) prepared by the melt rapid quenching method is selected, and the selected strip material is determined to be an amorphous structure by an X-ray diffractometer and a transmission electron microscope.
Step 2: and (3) carrying out heat treatment on the amorphous strip in the step (1) for 3 minutes at the optimal temperature by using a high vacuum annealing furnace.
And (3) characterizing the sample in the step (2) by using an X-ray diffractometer, and determining that the sample is of an amorphous structure.
Step 3: the annealed sample is subjected to ion thinning by an ion thinning instrument, the sample obtained in the step 3 is characterized by using a transmission electron microscope again, and the result is shown in fig. 7, so that the prepared amorphous alloy with the sample structure of a common structure can be illustrated, and the amorphous alloy is mainly characterized in that atoms are arranged randomly and have no specific periodicity.
The saturation induction intensity B s of the alloy was also obtained in step 2 using a vibrating sample magnetometer, and the results are shown in fig. 8.
Comparative example 3:
the amorphous nanocrystalline of the network structure of this comparative example (preparation method of Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy, comprising the steps of:
step 1: the (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 amorphous alloy) prepared by the melt rapid quenching method is selected, and the selected strip material is determined to be an amorphous structure by an X-ray diffractometer and a transmission electron microscope.
Step 2: fixing the amorphous strip on a Cu bracket by using AB glue, placing the amorphous strip into a chamber of an ion thinning instrument, and vacuumizing;
Step 3: the angles of the left and right ion guns are adjusted to be 10 degrees and minus 10 degrees respectively, the applied voltage value is set to be 8keV, and the thinning time of the ion gun is set to be 30min.
Repeating the process of the step 3 for 4 times at intervals of 5min until the light-transmitting holes appear in the middle.
Step 4: the angles of the left and right ion guns are adjusted to be 5 degrees and minus 5 degrees respectively, the applied voltage value is set to be 5keV, and the thinning time of the ion gun is set to be 30min.
The above procedure of step 4 was repeated 3 times at 5min intervals.
Step 5: the angles of the left ion gun and the right ion gun are respectively adjusted to be 3 degrees and 3 degrees, the applied voltage value is set to be 1.5keV, the thinning time of the ion gun is set to be 10min, and the amorphous nanocrystalline (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy) is obtained.
And (3) characterizing the amorphous nanocrystalline (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy sample) obtained in the step (5) by using a transmission electron microscope, wherein the prepared sample structure is amorphous nanocrystalline alloy with a net structure, the size of a central nanocrystalline core is 30-50nm, the thickness of an amorphous skeleton is 1-3nm, and the nanocrystalline core accounts for 84% of the total area.
Amorphous nanocrystals (Fe 0.8Co0.2)84B14Si1Cu1Nb0.5 soft magnetic alloy, saturated magnetic induction (B s) were also tested using a vibrating sample magnetometer and the results are shown in table 1.
The following summary of the process structure and performance parameters of the soft magnetic alloys prepared in examples 1-2 and comparative examples 1-3 is shown in Table 1.
TABLE 1 Process Structure and performance parameters for Soft magnetic alloys prepared in examples 1-2 and comparative examples 1-3
In comparative example 3, by increasing the ion thinning time, part of small-sized nanocrystalline grains are combined, and part of amorphous matrix is continuously converted into nanocrystalline, so that the overall nanocrystalline size in the alloy is increased, and the coercivity is remarkably increased.
The foregoing is only illustrative of the preferred embodiments and principles of the present invention, and changes in specific embodiments will occur to those skilled in the art upon consideration of the teachings provided herein, and such changes are intended to be included within the scope of the invention as defined by the claims.
Claims (8)
1. The preparation method of the amorphous nanocrystalline alloy with the net structure is characterized by comprising the following steps:
(1) Fixing an amorphous alloy sample with the thickness smaller than 50 mu m on a bracket of an ion thinning instrument;
(2) Adjusting angles of a left ion gun and a right ion gun of the ion thinning instrument, and preprocessing a sample for a first target duration under a first target voltage;
In the step (2), the angles of the left and right ion guns are not lower than +/-5 degrees, the first target voltage is not lower than 5 keV, and the first target duration is not lower than 30 min; repeating the step (2) until a light-transmitting hole appears in the middle;
(3) Reducing the angles of the left ion gun and the right ion gun, reducing the applied voltage to a second target voltage, and processing the sample obtained through the step (2) for a second target time under the second target voltage to obtain the amorphous nanocrystalline alloy with the reticular structure;
In the step (3), the angles of the left and right ion guns are not higher than + -5 degrees, the second target voltage is not higher than 5 keV degrees, the second target duration is not higher than 60 min, and the second target duration is smaller than the first target duration.
2. The method according to claim 1, wherein in the step (1), the amorphous alloy sample is an Fe-based, co-based, feCo-based, feNi-based, ni-based, ndFeB-based or rare earth-based amorphous alloy.
3. The method according to claim 1, wherein in the step (2), the angles of the left and right ion guns are respectively 8 °, -8 °, the first target voltage is 8 keV, and the first target duration is 120 min.
4. The method according to claim 1, wherein in the step (3), the angles of the left and right ion guns are respectively 4 °, -4 °, the second target voltage is 3 keV, and the second target duration is 15 min.
5. The method for preparing a net-structured amorphous nanocrystalline alloy according to any one of claims 1 to 4, wherein the support of the ion attenuation apparatus is a Cu support or a Mo support.
6. The method according to any one of claims 1 to 4, wherein in the step (1), if the thickness of the amorphous strip sample is greater than 50 μm, 2000 mesh SiC sandpaper is used to make the thickness smaller than 50 μm.
7. The amorphous nanocrystalline alloy of a network structure produced by the production method according to any one of claims 1 to 6, wherein the amorphous nanocrystalline alloy is a network structure composed of an amorphous skeleton and nanocrystalline.
8. Use of the amorphous nanocrystalline alloy according to claim 7, for transformers, switching power supplies, transformers or core tapes.
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