CN109161648A - A kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band - Google Patents
A kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C21D1/18—Hardening; Quenching with or without subsequent tempering
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- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
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- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
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Abstract
The invention belongs to technical field of magnetic materials, are related to a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band.The iron-based heat treatment mode for quenching state alloy strip steel rolled stock that this method provides is under vacuum or atmosphere of inert gases, state alloy strip steel rolled stock of quenching is heated in a manner of not less than being rapidly heated of 100 DEG C/min to set temperature, is then kept the temperature after 10~20mim furnace cooling or is cooled to room temperature in cooling medium and obtains Fe-based nanocrystalline magnetically soft alloy band.With prepared in current industrial production nano-crystal soft-magnetic band commonly at a slow speed heat up heat treatment process compared with, this method can be effectively improved the brittleness of iron based nano crystal band, reduce its hardness, but do not damage it and integrate soft magnet performance, and because heat treatment time is short, it can also shorten the production cycle, improve efficiency.
Description
Technical field
The invention belongs to field of magnetic material, are related to a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band.
Background technique
Fe-based nanocrystalline magnetically soft alloy has high saturated magnetic induction (Bs), low-coercivity (Hc), high magnetic permeability, low iron
The advantages that damage and low saturated bysteresis coefficient of dilatation, especially comprehensive soft magnet performance is excellent in high frequency, can be applied in high-power
In the electromagnetic devices such as high frequency transformer, high frequency switch power, common mode inductance, sensor, mutual inductor, high-frequency electric machines.From 1988
After Yoshizawa et al. has found FINEMET (Fe-Cu-Nb-Si-B) nano-crystal soft magnetic alloy, this new material is excellent because of its
Soft magnet performance attracts extensive attention.As correlative study is constantly unfolded and gos deep into, people have developed NANOPERM (Fe- in succession
) and HITPERM (Fe-Co-M-B M-B；M=Nb, Zr, Hf) etc. multiple serial nano crystalline substance magnetically soft alloys.Developed recently
The Bs of NANOMET (Fe-Si-B-P-Cu) serial nano peritectic alloy has been further upgraded, and promotes the small of electromagnetic element
Type and lightweight.
Fe-based nanocrystalline magnetically soft alloy has the line and staff control being made of the α-Fe and residual amorphous phase of nanoscale, usually
It is obtained by Amorphous Crystallization method, i.e., makes that uniform, subtle α-Fe is precipitated in amorphous precursor body alloy by suitable heat treatment condition
Low-alloyed average magnetocrystalline, drops in phase, the alternate generation coupling interaction effect of crystallite dimension α-Fe nano-crystalline and amorphous appropriate
The opposite sex makes it show excellent soft magnet performance.But the hardness that the precipitation of α-Fe phase will cause alloy increases, toughness decline.In work
In industry production, generally the amorphous alloy strips obtained by fast quenching mode are placed in heat-treatment furnace, are heated slowly to proper temperature
After keep the temperature 50-60min, finally obtain nanocrystalline strip, the heating rate of heat treatment is generally below 10 DEG C/min.But in this heat
Under treatment process, serious embrittlement phenomena can occur for the nanocrystalline strip that the annealed processing of amorphous precursor body is formed, it is difficult to carry out
Secondary operation and forming bring difficulty for its subsequent applications.For example, needing in advance will be non-when making nanocrystalline transformer core
Crystal zone material coiling forming, then together with fixture integrally annealed, which increase the preparation difficulty of iron core, reduce production efficiency.Iron
The brittleness problems of base nanometer crystal magnetically soft alloy have become keeping in check in its application.
Currently, people are mainly adjusted by alloying component or take new heat treatment mode to improve the crisp of nanometer crystal alloy
Property.In terms of adjusting alloying component, although addition Ni [J Phys Conf Ser 144 (2009): 012065] or Co [Philos
Mag 90(2010):1547；Appl Phys Lett 90 (2007): 212508] element can reduce the crisp of nanometer crystal alloy
Property, but the addition of Ni will lead to the Bs reduction of alloy, and the addition of Co then will increase the cost of alloy.In heat treatment mode side
Face, compared with industrial production commonly heats up at a slow speed heat treatment method, pulse current is heat-treated [Acta Phys Pol A 131
(2017): 672], direct current Joule heating [Sensor Actuat A-Phys 129 (2006): 45] or laser crystallization [middle promulgated by the State Council
Bright patent 200510045640.5] etc. new heat treatment mode can effectively inhibit the embrittlement of nanometer crystal alloy, but at these heat
Reason method needs that pulse or laser heating device, heat treatment operation step is complicated, more stringent requirements are proposed to industrial production.Separately
Outside, laser crystallization mode will lead to crystallization phase volume fraction in alloy and reduce, and drop low-alloyed Bs.Therefore, it invents a kind of simple
Effective nano-crystal soft-magnetic band preparation process, improving its brittleness under the premise of guaranteeing its excellent comprehensive soft magnet performance will be to receiving
The subsequent applications of the brilliant soft magnetism band of rice have great importance.
Summary of the invention
The present invention provides that a kind of to improve its crisp for Fe-based nanocrystalline magnetically soft alloy band embrittlement issue in industrial production
The preparation method of property.This method can not only be effectively improved the brittleness of Fe-based nanocrystalline magnetically soft alloy band, reduce its hardness but also energy
Enough guarantee that its soft magnet performance is without damage.
To achieve the above object, the invention adopts the following technical scheme:
A kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band, which is characterized in that iron-based state alloy strip steel rolled stock of quenching
Heat treatment mode be that iron-based state alloy strip steel rolled stock of quenching is heated to setting using the mode of being rapidly heated under vacuum or atmosphere of inert gases
Determine temperature, then keep the temperature after furnace cooling or be cooled to room temperature in cooling medium obtain Fe-based nanocrystalline magnetically soft alloy band；
The heat treatment mode that is rapidly heated refers to heating rate not less than 100 DEG C/min；
The heat preservation refers to the constant temperature after iron-based state alloy strip steel rolled stock of quenching to be heated to set temperature, holding temperature and heat preservation
Time referring to iron-based state alloy of quenching thermal property and set, the soaking time setting range be 10-20min.
Further, the iron-based structure for quenching state alloy strip steel rolled stock is single amorphous structure, or in noncrystal substrate
It is middle that there are line and staff control's structures of the α-Fe phase of nanoscale.
Further, the heat treatment mode that is rapidly heated refers to that heating rate is 100-600 DEG C/min.
Further, the cooling medium is empty gas and water or oil.
Further, the inert gas refers to nitrogen or argon gas.
Compared with the prior art, the invention has the advantages that:
1, the brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band provided by the invention is without complexity such as pulse, laser
Equipment for Heating Processing, heat treatment operation step is close with industrial processing steps, easily operated；
2, the brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band provided by the invention is not only suitable for single amorphous phase
Band, and it is suitable for the band of the α-Fe line and staff control with amorphous and nanoscale, the requirement to melt spun alloy band reduces；
3, the soaking time provided by the invention for improving the brittle method needs of Fe-based nanocrystalline magnetically soft alloy band compares mesh
Preceding industrial manufacture process is short, can shorten the production cycle of iron based nano crystal band, improve production efficiency.
4, iron-based prepared by the brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band provided through the invention to receive
The brittleness of rice peritectic alloy band is substantially less than industrial band, and hardness (intensity) also decreases, and is conducive to nanocrystalline
The following process of band shapes；
5, iron-based prepared by the brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band provided through the invention to receive
Rice peritectic alloy band can guarantee that its soft magnet performance is suitable or more excellent with industrial band.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The some embodiments recorded in application, for those of ordinary skill in the art, without creative efforts,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 is 1 (Fe of embodiment77Si10.5B9Nb2.5Cu1) state of quenching alloy strip steel rolled stock X-ray diffraction spectrum；
Fig. 2 is 1 (Fe of embodiment77Si10.5B9Nb2.5Cu1) state of quenching alloy strip steel rolled stock is warming up to 400 DEG C/min heating rate
560 DEG C, the X-ray diffraction spectrum of nanocrystalline strip obtained after heat preservation 10min；
Fig. 3 is 1 (Fe of embodiment77Si10.5B9Nb2.5Cu1) state of quenching alloy strip steel rolled stock is respectively with 10 DEG C/min and 400 DEG C/min liter
The hysteresis loop that warm rate is heated to 560 DEG C, keeps the temperature the nanocrystalline strip obtained after 10min；
Fig. 4 is 1 (Fe of embodiment77Si10.5B9Nb2.5Cu1) nanocrystalline strip hardness and breaking strain with heat treatment heat up
The variation rule curve of rate；
Fig. 5 is 1 (Fe of embodiment77Si10.5B9Nb2.5Cu1) nanocrystalline strip fracture after section SEM figure, wherein 5 (a) are
The SEM figure of section after the nanocrystalline strip fracture that heating rate is 10 DEG C/min, 5 (b) be heating rate receiving for 400 DEG C/min
The SEM figure of section after the brilliant strip breaks of rice.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
It is only a part of the embodiment of the present invention, instead of all the embodiments.It is real to the description of at least one exemplary embodiment below
It is merely illustrative on border, never as to the present invention and its application or any restrictions used.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Unless specifically stated otherwise, positioned opposite, the digital table of the component and step that otherwise illustrate in these embodiments
It is not limited the scope of the invention up to formula and numerical value.Simultaneously, it should be clear that for ease of description, each portion shown in attached drawing
The size divided not is to draw according to actual proportionate relationship.Technology known for person of ordinary skill in the relevant, side
Method and equipment may be not discussed in detail, but in the appropriate case, and the technology, method and apparatus should be considered as authorizing explanation
A part of book.In shown here and discussion all examples, appointing should be construed as merely illustratively to occurrence, and
Not by way of limitation.Therefore, the other examples of exemplary embodiment can have different values.It should also be noted that similar label
Similar terms are indicated in following attached drawing with letter, therefore, once it is defined in a certain Xiang Yi attached drawing, then subsequent attached
It does not need that it is further discussed in figure.
In the description of the present invention, it is to be understood that, the noun of locality such as " front, rear, top, and bottom, left and right ", " it is laterally, vertical,
Vertically, orientation or positional relationship indicated by level " and " top, bottom " etc. is normally based on orientation or position shown in the drawings and closes
System, is merely for convenience of description of the present invention and simplification of the description, in the absence of explanation to the contrary, these nouns of locality do not indicate that
It must have a particular orientation or be constructed and operated in a specific orientation with the device or element for implying signified, therefore cannot manage
Solution is limiting the scope of the invention: the noun of locality " inside and outside " refers to inside and outside the profile relative to each component itself.
For ease of description, spatially relative term can be used herein, as " ... on ", " ... top ",
" ... upper surface ", " above " etc., for describing such as a device shown in the figure or feature and other devices or spy
The spatial relation of sign.It should be understood that spatially relative term is intended to comprising the orientation in addition to device described in figure
Except different direction in use or operation.For example, being described as if the device in attached drawing is squeezed " in other devices
It will be positioned as " under other devices or construction after part or construction top " or the device of " on other devices or construction "
Side " or " under its device or construction ".Thus, exemplary term " ... top " may include " ... top " and
" in ... lower section " two kinds of orientation.The device can also be positioned with other different modes and (is rotated by 90 ° or in other orientation), and
And respective explanations are made to the opposite description in space used herein above.
In addition, it should be noted that, limiting components using the words such as " first ", " second ", it is only for be convenient for
Corresponding components are distinguished, do not have Stated otherwise such as, there is no particular meanings for above-mentioned word, therefore should not be understood as to this
The limitation of invention protection scope.
Embodiment 1
Fe77Si10.5B9Nb2.5Cu1
(1) preparation of state of quenching alloy strip steel rolled stock
A, Fe, Si, B, Nb and Cu raw material for being greater than 95% (mass percent) using purity are carried out by alloy nominal composition
Weighing and burden；Using non-consumable arc furnace by raw material melt back four times under an argon atmosphere, the uniform master alloy of ingredient is obtained
Ingot；Band device is got rid of using single roller and prepares state alloy strip steel rolled stock of quenching under an argon atmosphere, state of quenching alloy strip steel rolled stock thickness is about 20 μm, width
About 2mm；
B, state alloy strip steel rolled stock of quenching is detected using X-ray diffractometer (XRD) (Cu K α radiation, wavelength X=0.15406nm)
Structure, Fig. 1 are the XRD spectrum of state alloy strip steel rolled stock of quenching, and can determine that the state alloy strip steel rolled stock of quenching with non crystalline structure by Fig. 1；
(2) heat treatment of state of quenching alloy strip steel rolled stock
A, the state alloy strip steel rolled stock that will quench is packed into infrared ray and is rapidly heated in furnace, the argon for being evacuated to 2Pa, being filled with 0.5 atmospheric pressure
It is sealed after gas, respectively with 10 DEG C/min, 100 DEG C/min, 150 DEG C/min, 200 DEG C/min, 250 DEG C/min, 300 DEG C/min, 350
DEG C/min, 400 DEG C/min, the heating rate of 500 DEG C/min and 600 DEG C/min be heated to 560 DEG C, keep the temperature cold with furnace after 10min
But to room temperature；
B, the state alloy strip steel rolled stock that will quench is packed into quartz ampoule and is evacuated to 3 × 10-3It seals, is subsequently placed into batch-type furnace after Pa,
560 DEG C are heated to the heating rate of 10 DEG C/min, (note: the step is tested as a comparison, mould for furnace cooling after keeping the temperature 60min
Quasi- industrial production heat treatment process)；
C, using the structure of band after XRD detection heat treatment, Fig. 2 is above-mentioned state alloy strip steel rolled stock of quenching with 400 DEG C/min heating
The XRD spectrum that rate is warming up to 560 DEG C, keeps the temperature the nanocrystalline strip obtained after 10min.As shown in Fig. 2, the band tool after heat treatment
There is α-Fe nanocrystalline structure, also obtains nanocrystalline strip under other heat treatment conditions；
(3) performance test of nanocrystalline strip
A, it is tested and is received respectively using vibrating specimen magnetometer (VSM) and DC hysteresis loops instrument (B-H loop tracer)
The B of rice crystal zone materialsAnd Hc.Fig. 3 is after being heated to 560 DEG C with 10 DEG C/min and 400 DEG C/min heating rate respectively, kept the temperature 10min
The hysteresis loop of the nanocrystalline strip of acquisition, illustration are respectively nearly zero externally-applied magnetic field in hysteresis loop zone of saturation and BH curve
The enlarged drawing in region.As shown in figure 3, the soft magnet performance of nanocrystalline strip can be improved by improving heating rate: in BsIt increases
Meanwhile HcIt is significantly reduced.1 alloy of embodiment is listed in table 1 heats and simulate industrial production heat with different heating rates
Treatment process (heating rate: 10 DEG C/min；Soaking time: 60min) heat treatment after magnetic property.As shown in Table 1, when heating speed
When rate increases to 600 DEG C/min from 10 DEG C/min, the B of bands1.46T, H are increased to by 1.45Tc0.4A/ is reduced to from 1.1A/m
m.In addition, the soft magnet performance and simulation industrial manufacture process heat of the sample being heat-treated with the heating rate not less than 100 DEG C/min
The sample of processing is suitable or more excellent；
B, using the hardness of micro Vickers test nanocrystalline strip.Because band is difficult to be stretched or compressed reality
It tests, using plate bending device [Philos Mag 90 (2010): 1547] measurement breaking strain (εf) to evaluate the crisp of band
Property, calculation formula εf=d/ (D-d), the distance between two plates that both ends contact respectively when wherein D is strip breaks, d
It is alloy strip steel rolled stock thickness, εfValue is bigger, shows that the brittleness of band is smaller.Fig. 4 is the hardness and ε of nanocrystalline stripfWith heating rate
Changing rule, heat treatment condition be in 560 DEG C of heat preservation 10min.As shown in figure 4, when heating rate increases to from 10 DEG C/min
When 400 DEG C/min, band hardness is gradually lowered to 1278HV, ε from 1297HVfIt is gradually increased to 1.58% from 1.27%, is shown
The brittleness of band can be improved by improving heating rate.As shown in figure 5, observing nanometer crystal alloy by scanning electron microscope
The fracture apperance of band is it can be found that heating rate is smooth for the sample fracture of 10 DEG C/min, for typical brittle fracture
Feature；And there is chevron style in the sample fracture that heating rate is 400 DEG C/min, shows that it sends out in brittle fracture process
Plastic deformation is given birth to, brittleness is improved.The hardness and ε of band under Different Heat Treatment Conditions are listed in table 1f.Analytical table
Middle data are it is found that the hardness for the sample being heat-treated with the heating rate not less than 100 DEG C/min is below simulation industrial production work
The sample of skill heat treatment, and εfIt increases, i.e. the brittleness of band is improved.
Embodiment 2
Fe73.5Si13.5B9Cu1Nb3
(1) preparation of state of quenching alloy strip steel rolled stock:
Ingredient, master alloy ingot, band preparation and structure detection step are the same as embodiment 1.
(2) heat treatment of state of quenching alloy strip steel rolled stock
Heat treatment step can refer to embodiment 1.This implementation is unlike the first embodiment: set heating rate difference
For 10 DEG C/min, 100 DEG C/min, 200 DEG C/min and 400 DEG C/min；Soaking time is 15min；Cooling condition is band with furnace
It takes out to be placed in air after being cooled to 400 DEG C and be cooled to room temperature.
(3) performance test of nanocrystalline strip
A, with embodiment 1, detailed data is listed in Table 1 magnetism testing step.As shown in Table 1, when heating rate is from 10
DEG C/min is when increasing to 400 DEG C/min, the B of bands1.25T, H are increased to by 1.24Tc0.5A/m is reduced to from 0.8A/m.This
Outside, actual industrial production in the soft magnet performance and comparative example 1 of the sample being heat-treated with the heating rate not less than 100 DEG C/min
Band is suitable or more excellent.
B, with embodiment 1, detailed data is listed in Table 1 the testing procedure of hardness and breaking strain.When heating rate is from 10
DEG C/min is when increasing to 400 DEG C/min, band hardness is gradually lowered to 1321HV, ε from 1342HVfIt is gradually increased to from 1.64%
1.78%, show that the brittleness of band constantly reduces.In addition, with the sample of the heating rate heat treatment not less than 100 DEG C/min
Hardness is lower than the band of actual industrial production in comparative example 1, and εfIt increases, i.e., brittleness is improved.
Embodiment 3
Fe77.7Si4B13Cu1.3Nb4
(1) preparation of state of quenching alloy strip steel rolled stock:
Ingredient, master alloy ingot, band preparation and structure detection step are the same as embodiment 1；
(2) heat treatment of state of quenching alloy strip steel rolled stock
Heat treatment step can refer to embodiment 1.This implementation steps is unlike the first embodiment: set heating rate
Respectively 10 DEG C/min, 300 DEG C/min and 600 DEG C/min；Holding temperature is 510 DEG C；Soaking time is 15min；Simulation industry
The heat treatment condition of production are as follows: holding temperature is 510 DEG C, soaking time 50min；
(3) performance test of nanocrystalline strip
A, with embodiment 1, detailed data is listed in Table 1 magnetism testing step.As shown in Table 1, when heating rate is from 10
DEG C/min is when increasing to 600 DEG C/min, the B of bands1.46T, H are increased to by 1.45Tc1.1A/m is reduced to from 2.4A/m.This
Outside, the soft magnet performance for the sample being heat-treated with the heating rate not less than 300 DEG C/min is superior to simulation industrial manufacture process heat
The sample of processing.
B, with embodiment 1, detailed data is listed in Table 1 the testing procedure of hardness and breaking strain.When heating rate is from 10
DEG C/min is when increasing to 600 DEG C/min, band hardness is gradually lowered to 1180HV, ε from 1198HVfIt is gradually increased to from 1.60%
1.83%, show that the brittleness of band constantly reduces.In addition, with the sample of the heating rate heat treatment not less than 300 DEG C/min
Hardness is lower than the sample of simulation industrial manufacture process heat treatment, and εfIt increases, i.e., brittleness is improved.
Embodiment 4
Fe81.7Si4B13Cu1.3
(1) preparation of state of quenching alloy strip steel rolled stock:
Ingredient, master alloy ingot, band preparation and structure detection step are the same as embodiment 1；
(2) heat treatment of state of quenching alloy strip steel rolled stock
Heat treatment step can refer to embodiment 1.This implementation steps is unlike the first embodiment: set heating rate
Respectively 10 DEG C/min and 200 DEG C/min；Holding temperature is 430 DEG C；Simulate industrial heat treatment condition are as follows: holding temperature
It is 395 DEG C.
(3) performance test of nanocrystalline strip
A, with embodiment 1, detailed data is listed in Table 1 magnetism testing step.As shown in Table 1, when heating rate is from 10
DEG C/min is when increasing to 200 DEG C/min, the B of bands1.74T, H are increased to by 1.72Tc38A/m is reduced to from 229.8A/m.This
Outside, sample of the soft magnet performance for the sample being heat-treated with the heating rate of 200 DEG C/min better than simulation industrial manufacture process heat treatment
Product；
B, with embodiment 1, detailed data is listed in Table 1 the testing procedure of hardness and breaking strain.When heating rate is from 10
DEG C/min is when increasing to 200 DEG C/min, band hardness is reduced to 1250HV, ε from 1265HVfIt is increased to 1.45% from 1.10%,
Show that the brittleness of band constantly reduces.In addition, the hardness for the sample being heat-treated with the heating rate of 200 DEG C/min is lower than simulation work
The sample of industry production technology heat treatment, and εfIt increases, i.e., brittleness is improved.
Embodiment 5
Fe85Si2B8P4Cu1
(1) preparation of state of quenching alloy strip steel rolled stock:
Ingredient, master alloy ingot, band preparation and alloy structure detecting step are referring to embodiment 1.This implementation steps and reality
Apply unlike example 1: used raw material is Fe, Si, B, Cu and Fe that purity is greater than 95wt.%3P；Used melting is set
Standby is induction melting furnace.
(2) heat treatment of state of quenching alloy strip steel rolled stock
Heat treatment step can refer to embodiment 1.This implementation steps is unlike the first embodiment: set heating rate
Respectively 10 DEG C/min, 150 DEG C/min and 300 DEG C/min；Holding temperature is 440 DEG C；Cooling condition is that band is cooled to furnace
It is put into oil and is cooled to room temperature after 400 DEG C.
(3) performance test of nanocrystalline strip
A, with embodiment 1, detailed data is listed in Table 1 magnetism testing step.As shown in Table 1, when heating rate is from 10
DEG C/min is when increasing to 300 DEG C/min, the B of bands1.72T, H are increased to by 1.70TcIt is reduced to 12.5A/m from 130.2A/m,
Show that improving heating rate improves the soft magnet performance of band.
B, with embodiment 1, detailed data is listed in Table 1 the testing procedure of hardness and breaking strain.When heating rate is from 10
DEG C/min is when increasing to 300 DEG C/min, band hardness is gradually lowered to 998HV, ε from 1015HVfIt is gradually increased to from 1.02%
1.27%, show that the increase of heating rate reduces the brittleness of band.
Embodiment 6
Fe81.7Si2B8P6Cu1.3Mo1
(1) preparation of state of quenching alloy strip steel rolled stock:
Ingredient, master alloy ingot, band preparation and structure detection step are referring to embodiment 5.Used raw material is purity
Fe, Si, B, Cu, Fe greater than 95wt.%3P and Mo.
(2) heat treatment of state of quenching alloy strip steel rolled stock
Heat treatment step can refer to embodiment 1.This implementation steps is unlike the first embodiment: set heating rate
Respectively 10 DEG C/min, 200 DEG C/min and 500 DEG C/min；Holding temperature is 440 DEG C；Soaking time is 20min；Cooling condition
It is cooled to room temperature into the water after being cooled to 400 DEG C with furnace for band.
(3) performance test of nanocrystalline strip
A, with embodiment 1, detailed data is listed in Table 1 magnetism testing step.As shown in Table 1, when heating rate is from 10
DEG C/min is when increasing to 500 DEG C/min, the B of bands1.66T, H are increased to by 1.64Tc7.2A/m, table are reduced to from 28.3A/m
The bright soft magnet performance for increasing heating rate and improving band；
B, with embodiment 1, detailed data is listed in Table 1 the testing procedure of hardness and breaking strain.When heating rate is from 10
DEG C/min is when increasing to 500 DEG C/min, band hardness is gradually lowered to 1059HV, ε from 1092HVfIt is gradually increased to from 1.10%
1.36%, show that the raising of heating rate improves the brittleness of band.
Embodiment 7
Fe79.3Si4B13Cu1.7Nb2
(1) preparation of state of quenching alloy strip steel rolled stock:
Ingredient, master alloy ingot, band preparation and structure detection step are referring to embodiment 1.The present embodiment and embodiment 1 are not
With: the state alloy strip steel rolled stock of quenching is with there are line and staff control's structures of α-Fe phase in noncrystal substrate；
(2) heat treatment of state of quenching alloy strip steel rolled stock
Heat treatment step can refer to embodiment 1.This implementation steps is unlike the first embodiment: set heating rate
Respectively 10 and 400 DEG C/min；Holding temperature is 470 DEG C.
(3) performance test of nanocrystalline strip
A, with embodiment 1, detailed data is listed in Table 1 magnetism testing step.As shown in Table 1, when heating rate is from 10
DEG C/min is when increasing to 400 DEG C/min, the B of bands1.56T, H are increased to by 1.55Tc10.2A/m, table are reduced to from 14.1A/m
The bright heating rate that improves improves the soft magnet performance of band.
B, with embodiment 1, detailed data is listed in Table 1 the testing procedure of hardness and breaking strain.When heating rate is from 10
DEG C/min is when increasing to 400 DEG C/min, band hardness is reduced to 1190HV, ε from 1213HVfIt is increased to 1.64% from 1.37%,
Show that the brittleness of band reduces.
Comparative example 1
The nanocrystalline strip (trade mark: 1K107) of actual industrial production, alloying component and embodiment 2 are close.Using embodiment
Test method in 2 measures its magnetic property, hardness and breaking strain numerical value and is listed in Table 1.The breaking strain of the band is
1.55%, lower than with the sample of the heating rate heat treatment preparation not less than 100 DEG C/min, i.e. brittleness is larger, together in embodiment 2
When hardness it is also higher.
Above-described embodiment shows the nanocrystalline conjunction for by high heating rate, shortening the acquisition of soaking time heat treatment mode
While with more excellent comprehensive soft magnet performance, breaking strain increases gold ribbon material, i.e., brittleness is improved, hardness drop
It is low.Heating rate provided by the invention is used to receive not less than 100 DEG C/min, time for prepared by the heat treatment process of 10-20min
The soft magnet performance of rice crystal zone material is suitable with the heating at a slow speed in industrial production, the sample of heat treatment process preparation of long soaking time
Or it is more excellent, and brittleness be improved significantly, hardness it is lower.
The ingredient of alloy, heat treatment condition are (when holding temperature, heating rate, heat preservation in 1 embodiment 1-7 of table and comparative example 1
Between, the type of cooling), magnetic property (saturation induction density Bs, coercivity Hc), hardness and breaking strain contrast table
Note: comparative example 1 is business nanocrystalline strip (trade mark: 1K107).
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (5)
1. a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band, which is characterized in that iron-based state alloy strip steel rolled stock of quenching
Heat treatment mode is to heat iron-based state alloy strip steel rolled stock of quenching under vacuum or atmosphere of inert gases using the mode of being rapidly heated and extremely set
Temperature, then keep the temperature after furnace cooling or be cooled to room temperature in cooling medium obtain Fe-based nanocrystalline magnetically soft alloy band；
The heat treatment mode that is rapidly heated refers to heating rate not less than 100 DEG C/min；
The heat preservation refers to the constant temperature after iron-based state alloy strip steel rolled stock of quenching to be heated to set temperature, holding temperature and soaking time
Referring to iron-based state alloy of quenching thermal property and set, the soaking time setting range be 10-20min.
2. a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band according to claim 1, which is characterized in that
The iron-based structure for quenching state alloy strip steel rolled stock is single amorphous structure, or there are the α-of nanoscale in noncrystal substrate
Line and staff control's structure of Fe phase.
3. a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band according to claim 1, which is characterized in that
The heat treatment mode that is rapidly heated refers to that heating rate is 100-600 DEG C/min.
4. a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band according to claim 1, which is characterized in that
The cooling medium is empty gas and water or oil.
5. a kind of brittle method of improvement Fe-based nanocrystalline magnetically soft alloy band according to claim 1, which is characterized in that
The inert gas refers to nitrogen or argon gas.
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| CN112410531A (en) * | 2020-11-12 | 2021-02-26 | 中国科学院宁波材料技术与工程研究所 | Nanocrystalline alloy and preparation method thereof |
| CN112831641A (en) * | 2021-01-07 | 2021-05-25 | 山东大学 | Heat treatment method for preparing nanocrystalline magnetic core |
| CN113234917A (en) * | 2021-07-13 | 2021-08-10 | 信维通信（江苏）有限公司 | Heat treatment method of low-loss nanocrystalline strip |
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| CN112831641A (en) * | 2021-01-07 | 2021-05-25 | 山东大学 | Heat treatment method for preparing nanocrystalline magnetic core |
| CN113234917A (en) * | 2021-07-13 | 2021-08-10 | 信维通信（江苏）有限公司 | Heat treatment method of low-loss nanocrystalline strip |
| CN113234917B (en) * | 2021-07-13 | 2021-10-26 | 信维通信（江苏）有限公司 | Heat treatment method of low-loss nanocrystalline strip |
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Application publication date: 20190108 |