CN109440023B - A kind of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy and preparation method thereof - Google Patents
A kind of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy and preparation method thereof Download PDFInfo
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- CN109440023B CN109440023B CN201811597955.4A CN201811597955A CN109440023B CN 109440023 B CN109440023 B CN 109440023B CN 201811597955 A CN201811597955 A CN 201811597955A CN 109440023 B CN109440023 B CN 109440023B
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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
- C22C45/02—Amorphous alloys with iron as the major constituent
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—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 hard-magnetic materials
- H01F1/04—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 hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/03—Amorphous or microcrystalline structure
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C2200/00—Crystalline structure
- C22C2200/02—Amorphous
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/04—Nanocrystalline
Abstract
The invention discloses a kind of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloys and preparation method thereof, this method comprises: nitrogen-containing material progress melting is obtained nitrogen coupling ferrous alloy ingot casting by (1)；(2) by obtained nitrogen coupling ferrous alloy ingot casting after broken, remelting, Fe-based amorphous alloy is coupled using the nitrogen that completely amorphous state is prepared in quick chilling technology of preparing；(3) the nitrogen coupling Fe-based amorphous alloy of obtained completely amorphous state is successively subjected to two sections of annealing and tempering obtains high magnetic strength nitrogen and couples Fe-based amorphous nanocrystalline alloy, the temperature of the first segment annealing of two sections of annealing is 20~50 DEG C lower than the first crystallization start temperature, and the temperature of second stage annealing is between the first crystallization start temperature and the second crystallization start temperature.The above method improves the saturation induction density of Fe-based amorphous nanocrystalline alloy, while also improving iron-based amorphous and nanocrystalline soft magnetic alloy in military service performance complicated, in rugged environment.
Description
Technical field
The present invention relates to magneto-electric functional material fields, and in particular to a kind of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy
And preparation method thereof.
Background technique
With the development of electron electric power industry, there is an urgent need to develop a kind of alloy materials of high saturated magnetic induction.Iron
Based amorphous nano alloy has the advantages that coercivity is low, Effective permeability is high, iron loss is low etc., and it is low in cost, production technology is simple
It is single, it is widely paid close attention in recent years.
Notification number is that the patent specification of 101796207 B of CN discloses a kind of amorphous alloy of excellent workability
Strip, the Fe that embodiment 1 providesSurplusCu0.98Nb3.1Si13.4B9.3The saturation induction density of amorphous alloy band is 1.24T.
The patent specification of 106917042 A of Publication No. CN discloses a kind of iron-based nanometer of high frequency high magnetic flux density
Brilliant magnetically soft alloy and preparation method thereof carries out melting under inert atmosphere protection, and smelting temperature is 1300~1800 DEG C, protects after fusing
10~20min of temperature, it is cooling to obtain master alloy ingot, continuous amorphous alloy is prepared by single roller chilling method after master alloy ingot is broken,
Cooling obtains high frequency high magnetic flux density Fe-based nanocrystalline magnetically soft alloy after being finally heat-treated 1~90min at 500~600 DEG C,
Saturation induction density is 1.30~1.55T.
However, Fe-based amorphous nanocrystalline alloy is in research and development, there are still lot of challenges with application aspect, such as:
(1) brittleness problems of amorphous alloy.Fe-based amorphous alloy, especially nanometer crystal alloy, that there are ductility is low, brittleness is big
The problem of, it needs to further investigate the factor for influencing its ductility, explores the method for promoting ductility, guarantee using safe.
(2) Saturation magnetic sense intensity is still relatively low, and comprehensive magnetic performance still needs to be further improved.It needs further to study new work
Skill or the better alloy of craftsmanship make alloy have high saturation magnetic induction intensity, low coercivity and high magnetic conductivity, that is, are had
There are the Fe-based amorphous alloy or amorphous nano peritectic alloy of Good All-around Property.
(3) lack efficient amorphous alloy processing technology.Amorphous alloy/nanometer crystal alloy because hardness is high, more crisp, processing compared with
Difficulty, processing efficiency be not high.It needs to further investigate the factor for influencing amorphous/nanocrystalline alloy processing performance, explores and improve processing
Efficiency and the technical method for guaranteeing processing quality.
(4) exploitation meets soft magnetic amorphous/nanometer crystal alloy system of different demands.Different industrial products are to amorphous alloy magnetic
There are great differences for the requirement of performance, needs for different application field, different product, exploitation meets different product needs
A variety of soft magnetic amorphous nanometer crystal alloy systems.
In addition, raising of the Fe-based amorphous nanocrystalline alloy with saturation induction density, the Forming ability of amorphous can be gradually
Decline, is unfavorable for obtaining generous amorphous nanocrystalline strip alloy.Moreover, Fe-based amorphous nanocrystalline alloy, especially has height
The Fe-based amorphous nanocrystalline alloy of saturation induction density, the poor corrosion resistance under the adverse circumstances such as hot humid, causes
Its military service stability is poor.
So how to guarantee that Fe-based amorphous nanocrystalline alloy corrosion resistance and amorphous formation ability while improve system
Saturation induction density have great importance.
The introducing of nitrogen is conducive to improve amorphous formation ability, thus it is possible to vary the spin phase interaction between alloy atom
With being effectively improved the saturation induction density of system, the phase pick-up behavior of alloy can also be regulated and controled and corroded
Ionic species and ion behavior in medium.Such as added in right amount in steel nitrogen can greatly improve steel corrosion resistance and
Mechanical property.
The method that nitrogen is introduced in master alloy is referred to as nitriding.Common nitriding method is under nitrogen containing atmosphere to mother
Alloy carries out melting.The method usually requires prolonged high-temperature process, and on the one hand by nitrogen, solubility is influenced in master alloy,
On the other hand it generally requires to carry out under high pressure, thus often nitrogen content is relatively low for the product after nitriding, and the method operation difficulty
It is larger.If above-mentioned nitriding method is applied to Fe-based amorphous material, easily leads to Fe-based amorphous material and be changed into nitriding process
Crystal structure is unable to get amorphous state product.In addition, above-mentioned nitriding method can only make nitrogen be distributed in Fe-based amorphous material surface,
And nitrogen is unevenly distributed.
Therefore, this field research is also deposited other than there are problems that low efficiency and be unable to get completely amorphous structure
The nitrogen caused by traditional nitriding method is unevenly distributed, be enriched in material surface and nitriding after material become fragile, processing difficulties
The problem of.This field needs the side for the nitrogen coupling Fe-based amorphous nanocrystalline alloy that one kind can obtain high tenacity and nitrogen is evenly distributed
Method.
Summary of the invention
For shortcoming existing for this field, the present invention provides a kind of high magnetic strength nitrogen coupling iron-based amorphous nanometer crystallines to close
The preparation method of gold, is prepared using nitrogen-containing material, not only greatly increases the saturation magnetic of Fe-based amorphous nanocrystalline alloy
Induction, and subsequent nitridation steps are omitted, overcome previous Fe-based amorphous alloy nitrating difficulty, nitrogen distribution not
Uniform problem, has many advantages, such as to be simple and efficient, is at low cost, product quality is controllable and is suitble to large-scale production, to improving material
The saturation induction density of material has directive significance.
A kind of preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy, comprising:
(1) by Fe, amorphous formation element, thick atom dimension elements and nanocrystalline forming core element simple substance and/or compound,
And nitride as raw material carry out melting obtain nitrogen coupling ferrous alloy ingot casting, the amorphous formation element be selected from Al, B,
P, at least one of C or Si, thick atom dimension elements are selected from least one of IV B, V B or VI B race element, nanocrystalline
Forming core element is selected from least one of Cu, Ag or Zn；
(2) obtained nitrogen coupling ferrous alloy ingot casting is prepared after broken, remelting using quick chilling technology of preparing
The nitrogen of completely amorphous state couples Fe-based amorphous alloy；
(3) the nitrogen coupling Fe-based amorphous alloy of obtained completely amorphous state is successively subjected to two sections of annealing and tempering obtains height
Magnetic strength nitrogen couples Fe-based amorphous nanocrystalline alloy, and the temperature of the first segment annealing of two sections of annealing starts temperature than the first crystallization
Low 20~50 DEG C are spent, the temperature of second stage annealing is between the first crystallization start temperature and the second crystallization start temperature.
In step (1), it is preferable that the thick atom dimension elements in Zr, Cr, Nb, Mo, W or Hf at least one
Kind.
Preferably, nanocrystalline forming core element is Cu.
Preferably, the nitride fusing point is lower, and nitrogen is not easily decomposed spilling, is specifically as follows FexN、ZrN、
One of CrN, NbN, AlN and MoN or a variety of, wherein x=2~4, to realize the regulation of nitrogen content.It is highly preferred that described
Nitride be FexN, wherein x=2~4.
Nitride can guarantee that the nitrogen that nitrogen is present in the form of nitride couples iron-based conjunction as the raw material of melting
In golden alloy of ingot.Compared to traditional steel material nitriding, in the nitrogen coupling ferrous alloy alloy of ingot that this method obtains
The existence form of nitrogen is more stable, is not easily decomposed as nitrogen spilling.
The melting can be induction melting or electric arc melting, for guarantee mother alloy ingot it is not contaminated and do not occur compared with
Big ingredient loses ratio, and it is clean that when melting keeps cavity, and melting carries out under protective atmosphere.
Preferably, the melting carries out in rare gas atmosphere or nitrogen atmosphere.
Preferably, the temperature of the melting is 1300~1800 DEG C, soaking time after melting sources is 15~
45min。
Fusion process needs to reach certain holding temperature and certain soaking time to guarantee that ingredient is uniform.Temperature is too low
Or soaking time it is shorter when will lead to nitride fusing not exclusively, nitride and nitrogen are unevenly distributed, and then are caused subsequent
It generates serious heterogeneous forming core during single-roller rapid quenching with quenching or gas atomization preparation amorphous alloy and completely amorphous state can not be obtained
Alloy；Temperature is excessively high or soaking time is longer, will lead to nitrogen and is overflowed in the form of nitrogen, not can guarantee in product
Nitrogen content keeps the effect of nitrating unobvious.
Incomplete amorphous state or the non-uniform nitrogen coupling Fe-based amorphous alloy of component distributing can not be by further annealing
Controllable and uniform nanocrystalline of size is obtained, the high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy significantly reduced
Performance.On the other hand, this incomplete amorphous state or the non-uniform nitrogen coupling Fe-based amorphous alloy of component distributing are due to having occurred
It is partially-crystallized, cause toughness to be greatly reduced, so that also significantly limiting nitrogen coupling Fe-based amorphous alloy further processes life
It produces.
The melting can make the distributed components of alloy by the heat preservation of long period, therefore avoid fast later
Quench and annealing process in generate heterogeneous forming core, and then cause partially-crystallized.Simultaneously as nitrogen-atoms and other composition members
There are biggish atomic size differences and negative heat of mixing between element avoids crystallization so that the long-range of atom be inhibited to spread.At annealing
It will form the lower elementide centered on nitrogen of energy during reason, these clusters, which need to cross higher energy barrier, can just send out
It is raw to develop, therefore the thermal stability of nitrogen coupling alloy has obtained effective raising.
In step (2), the quick chilling technology of preparing can be single-roller rapid quenching with quenching or gas atomization.
Single-roller rapid quenching with quenching is that molten alloy is sprayed to high-speed rotating cooling roller surface, forms one when injection on roll surface
Dynamic balancing weld pool, the method that molten alloy rapid curing forms continuous amorphous or crystallite band.Single-roller rapid quenching with quenching can be prepared into
Nitrogen to completely amorphous state couples iron-based amorphous alloy ribbon material.
Gas atomization is fluid impact quickly to move or by metal or alloy liquid crushing is otherwise tiny
Drop is followed by condensed into the method for solid powder.The nitrogen that completely amorphous state can be prepared in gas atomization couples Fe-based amorphous conjunction
Bronze end.
The single-roller rapid quenching with quenching and gas atomization is required to first be vacuumized, and disguises single roller rapid quenching device or aerosol
Then air pressure in setting is re-filled with rare gas or nitrogen, makes single roller rapid quenching device or gas atomization device no more than 0.02Pa
Interior gas pressure is lower than 0.09~0.04MPa of standard atmospheric pressure.
Preferably, to avoid band crystallization or oxidation, the copper roller linear velocity of the single-roller rapid quenching with quenching is 20~40m/s.
The remelting carries out in rare gas atmosphere or nitrogen atmosphere.
Remelting, single roller rapid quenching preparation are carried out after can be placed in quartz ampoule after the nitrogen coupling ferrous alloy ingot casting is broken
Band or gas-atomized powder.By the control remelting time, quartzy nozzle lower end jet size, quartz ampoule to copper roller away from
The band or powder of good completely amorphous state are obtained from, quartz ampoule internal and external pressure difference and copper roller revolving speed.
The remelting, which can be, heats remelting by induction coil in quartz ampoule, and the draught head inside and outside quartz ampoule is
200~300Pa, while the nozzle width control of quartz ampoule lower end is 0.4~0.8mm, to control the band that single roller rapid quenching obtains
For material with a thickness of 22~28 μm, the partial size for the powder that control aerosolization obtains is 75~100 μm.
In step (3), two sections of annealing couple the crystallization of Fe-based amorphous alloy for regulating and controlling the nitrogen of completely amorphous state
Behavior, the high magnetic strength nitrogen controlled couple crystallite dimension nanocrystalline in Fe-based amorphous nanocrystalline alloy, and precipitation helps to mention
The crystal phase of high corrosion-resistant and saturation induction density, and then effectively improve the full of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy
And magnetic induction intensity, high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy is improved in military service complicated, in rugged environment
Can, greatly widen the application range of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy.
Two sections of annealing and tempering carry out under rare gas atmosphere and nitrogen atmosphere protection, avoid completely amorphous state
Nitrogen coupling Fe-based amorphous alloy annealing and drawing process in occur oxidation or surface crystallization.
If without the condition that rare gas atmosphere and nitrogen atmosphere are protected, two sections of annealing and tempering can under a high vacuum into
Row need to guarantee vacuum degree no more than 1.0 × 10-2Pa。
The first crystallization start temperature refer to start in heat treatment process be precipitated α-Fe temperature, generally 480~
530℃。
First crystallization terminates temperature and refers to the temperature that α-Fe is precipitated completely, generally 590~610 DEG C.
The second crystallization start temperature refers to other phases that may be adversely affected to magnetic property in addition to α-Fe
Start the temperature being precipitated, it is often different in the alloy system containing different impurities.
The temperature of the second stage annealing should be in the area of the first crystallization start temperature Yu the second crystallization start temperature
In, to make α-Fe precipitation as much as possible and avoid the magnetic precipitation for deteriorating phase.
The purpose of the first segment annealing is that Fe is precipitated3N and Fe4N nano particle, it is preferable that the temperature of first segment annealing
It can be considered nitride Precipitation Temperature, be 460~510 DEG C, the time is 10~20min.
The purpose of the second stage annealing is that α-Fe nanocrystal is precipitated, and can be considered quenching treatment, it is preferable that second segment
The temperature of annealing is 530~750 DEG C, and the time is 10~60min.
It is tempered again after water quenching chilling can be used after second stage annealing reducing rapidly alloy temperature.
The tempering is the pick-up behavior in order to regulate and control nitride, promotes part Fe3N、Fe4N and unordered α '-geneva
Body phase Fe-base compound is changed into orderly α "-Fe16N2, so that the saturation induction density of Fe-based amorphous nanocrystalline alloy be made to obtain
To raising.Preferably, the temperature of the tempering is 150~250 DEG C, and the time is 60~120min.
The preparation method for the high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy that invention further provides a kind of according to
The nitrogen for the completely amorphous state being prepared couples Fe-based amorphous alloy.
The nitrogen coupling Fe-based amorphous alloy of the completely amorphous state is the preparation side of nitrogenous Fe-based nanocrystalline magnetically soft alloy
Intermediate product during method preparation, nitrogen content is high, is 500~1100ppm, can bear maximum bending angle and be not less than 180 °,
With excellent bending toughness, be conducive to the progress of further nano-crystallization processing and mechanical coiling process process.
In a preferred example, the composition of the nitrogen coupling Fe-based amorphous alloy of the completely amorphous state includes Fe80-91M3- 10B3-10N0-0.5, one or both of M Nb, Mo, Zr, Hf, Al and V, the nitrogen coupling Fe-based amorphous alloy of the composition form
There are biggish negative heat of mixing and atomic size difference big between atom, thus couples Fe-based amorphous nanometer as high magnetic strength nitrogen is prepared
The presoma of peritectic alloy has higher amorphous stability.
The preparation method for the high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy that the present invention also provides a kind of according to
The high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy being prepared.
The nanocrystalline crystallite dimension of the high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy is 10~15nm, saturation
Magnetic induction intensity is high, is 1.37~1.84T, and corrosion resistance is good, and corrosion rate is low, in the item that corrosive medium is 0.5M NaCl solution
Under part, corrosion rate is not more than 0.12mm/a.
The high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy can be one of following composition:
Fe73-84Si3-16B8-12M2.4-3Cu0.6-3N0-0.5、
Fe80-91M3-10B3-10Cu0-3N0-0.5、
Fe33-66Co20-52M2-7B3-10Cu0.6-3N0-0.5、
Fe75-81Si9-14B3-9Cu0.6-1.3(NbxMy)N0-0.5、
Fe80-91M3-10B3-10N0-0.5,
Wherein, one or both of M Nb, Mo, Zr, Hf, Al, Cr, Ta and V, 1.2≤x+y≤2.5.
Preferably, the composition of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy includes Fe80-91M3-10B3- 10N0-0.5, one or both of M Nb, Mo, Zr, Hf, Al and V.Fe80-91M3-10B3-10As Nanoperm type nano soft magnetic
One of classical ingredient of material has high saturation induction density, about 1.63T, and can get later by nitride doping
The saturation induction density of 1.71~1.84T.
Compared with prior art, the present invention major advantage includes:
(1) purpose of nitrogen coupling has been effectively achieved, can get the Fe-based amorphous nanocrystalline alloy of high nitrogen-containing, and nitrogen contains
Amount is controllable.
(2) the problem of overcoming Fe-based amorphous crystallization during nitrating, toughness becomes after solving Fe-based amorphous alloy nitrating
Problem poor, not easy to be processed, is simple and efficient, at low cost, and product quality is controllable, is suitble to large-scale production.
(3) intermediate product is that the nitrogen of completely amorphous state couples Fe-based amorphous alloy, can bear maximum bending angle and be not less than
180 °, there is excellent bending toughness, nitrogen content is high, is 500~1100ppm.
(4) be prepared high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy nanocrystalline crystallite dimension be 10~
15nm, saturation induction density is high, is 1.37~1.84T, and corrosion resistance is good, and corrosion rate is low, is 0.5M NaCl in corrosive medium
Under conditions of solution, corrosion rate is not more than 0.12mm/a.
In conclusion the present invention improves the saturation induction density of Fe-based amorphous nanocrystalline alloy, also improve simultaneously
Iron-based amorphous and nanocrystalline soft magnetic alloy can farthest cater to current electronics in military service performance complicated, in rugged environment
" miniaturization, efficient, lightweight and the greenization " that electrical device requires, has greatly widened the conjunction of iron-based amorphous nanometer crystalline soft magnetism
The application range of gold, there is great application prospect and research significance.
Detailed description of the invention
Fig. 1 is the high magnetic strength that the nitrogen that is prepared of embodiment 1 couples iron-based amorphous alloy ribbon material, embodiment 2 is prepared
The nitrogen-free iron-based amorphous alloy ribbon material and comparative example 2 that nitrogen coupling Fe-based amorphous nanocrystalline alloy band, comparative example 1 are prepared are made
X-ray diffraction (XRD) figure of standby obtained nitrogen-free Fe-based amorphous nanocrystalline alloy band；
Fig. 2 is the transmission electron microscope photograph that the high magnetic strength nitrogen that embodiment 2 is prepared couples Fe-based amorphous nanocrystalline alloy band
Piece；
Fig. 3 is that the high magnetic strength nitrogen that embodiment 2 is prepared couples Fe-based amorphous nanocrystalline alloy band and prepared by comparative example 2
The room temperature hysteresis loop comparison diagram of obtained nitrogen-free Fe-based amorphous nanocrystalline alloy band；
Fig. 4 is that the high magnetic strength nitrogen that embodiment 2 is prepared couples Fe-based amorphous nanocrystalline alloy band and prepared by comparative example 2
The polarization curve comparison diagram of obtained nitrogen-free Fe-based amorphous nanocrystalline alloy band.
Specific embodiment
With reference to the accompanying drawing and specific embodiment, the present invention is further explained.It should be understood that these embodiments are merely to illustrate
The present invention rather than limit the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to
Normal condition, or according to the normal condition proposed by manufacturer.
Embodiment 1
Nitrogen coupling iron-based amorphous alloy ribbon material is prepared, chemical molecular formula is (Fe90Zr7B3)99.75N0.25。
(1) simple substance Fe, Zr and B and ZrN are uniformly mixed by above-mentioned stoichiometric ratio, are prepared using arc-melting furnace
The uniform nitrogen of ingredient couples ferrous alloy ingot casting.It is evacuated to air pressure first lower than 2.0 × 10-2Pa is then charged with argon gas to gas
Pressure is that 0.05MPa carries out multiple melting, and by the cooling 30min of molten alloy ingot after melting, it is iron-based to obtain the uniform nitrogen coupling of ingredient
Alloy cast ingot.
(2) obtained nitrogen coupling ferrous alloy ingot casting is ground off into surface impurity with grinding wheel, bottom is packed into after broken, remelting and is set
Have in the quartz ampoule of nozzle, the width of nozzle is 0.8mm, and adjusting furnace chamber gas pressure is to adjust lower than standard atmospheric pressure 0.09MPa
Quartz pipe internal and external pressure difference is 300Pa, is got rid of in the single roller rapid quenching device for having nitrogen atmosphere to protect with the linear velocity of 40m/s
Band obtains nitrogen and couples iron-based amorphous alloy ribbon material, and nitrogen content 900ppm, surface is smooth, with a thickness of 23 μm.
As shown in Figure 1, obtained (Fe90Zr7B3)99.75N0.25It is completely amorphous state that nitrogen, which couples iron-based amorphous alloy ribbon material,.
The nitrogen coupling iron-based amorphous alloy ribbon material of obtained completely amorphous state has excellent bending toughness, can doubling
180°。
It is further wound using obtained completely amorphous nitrogenous iron-based amorphous alloy ribbon material and iron core product is made, it is made
Iron core product have the characteristics that nitrogen is evenly distributed.
Embodiment 2
Hypertonic solutions are carried out to the nitrogen coupling iron-based amorphous alloy ribbon material that embodiment 1 is prepared and obtain high magnetic strength nitrogen
Fe-based amorphous nanocrystalline alloy band is coupled, chemical molecular formula is (Fe90Zr7B3)99.75N0.25。
The nitrogen of obtained completely amorphous state coupling iron-based amorphous alloy ribbon material is placed in quartz ampoule, it is evacuated to 5.0 ×
10-3Quartz ampoule is placed in heat-treatment furnace by Pa, is risen to 510 DEG C with the heating rate of about 2 DEG C/s, is warming up to after keeping the temperature 15min
630 DEG C, 1h is kept the temperature, quartz ampoule taking-up is then placed in quenching-in water to room temperature rapidly, 90min is then carried out at 200 DEG C
High vacuum tempering, obtain high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band.
The nitrogen content of obtained high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band is 890ppm, and saturation induction is strong
Degree is 1.73T, and under conditions of corrosive medium is 0.5M NaCl solution, corrosion rate 0.12mm/a has excellent saturation
Magnetic induction intensity and resistance to corrosion.
The XRD diagram of obtained high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band is as shown in Figure 1, transmission electron microscope photo
As shown in Fig. 2, nanocrystalline crystallite dimension is about 13nm, a small amount of Fe has been precipitated3N and ZrN.
Embodiment 3
Prepare high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band, chemical molecular formula Fe76.5Si12.7B8Cu1
(Nb0.75Mo0.75)N0.3。
(1) simple substance Fe, Si, B, Cu, Nb and Mo and NbN are put into induction by above-mentioned stoichiometric ratio after mixing
In alumina crucible in smelting furnace, air pressure is evacuated to lower than 2.0 × 10-2Pa, being then charged with argon gas to air pressure is 0.05MPa
Melting is carried out, 25min is kept the temperature after fusing, molten alloy ingot is then poured into cooling 30min in copper mold, obtains the uniform nitrogen of ingredient
Couple ferrous alloy ingot casting.
(2) obtained nitrogen coupling ferrous alloy ingot casting is ground off into surface impurity with grinding wheel, bottom is packed into after broken, remelting and is set
Have in the quartz ampoule of nozzle, the width of nozzle is 0.8mm, and regulating stove cavity pressure is to adjust stone lower than standard atmospheric pressure 0.09MPa
English pipe internal and external pressure difference is 300Pa, gets rid of band in the single roller rapid quenching device for having nitrogen atmosphere to protect with the linear velocity of 40m/s, obtains
The nitrogen of completely amorphous state couples iron-based amorphous alloy ribbon material, nitrogen content 760ppm, surface is smooth.
(3) the nitrogen coupling iron-based amorphous alloy ribbon material of obtained completely amorphous state is placed in quartz ampoule, is evacuated to 5.0
×10-3Quartz ampoule is placed in heat-treatment furnace by Pa, is risen to 490 DEG C with the heating rate of about 2 DEG C/s, is risen again after keeping the temperature 15min
Temperature keeps the temperature 10min to 560 DEG C, and quartz ampoule taking-up is then placed in quenching-in water to room temperature rapidly, finally high at 200 DEG C
Vacuum tempering 1h obtains high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band.
The saturation induction density of obtained high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band is up to 1.63T.
The patent specification of 106917042 A of Publication No. CN discloses a kind of chemical molecular formula
Fe76.5Si12.7B8Cu1(Nb0.75Mo0.75) nitrogen-free Fe-based amorphous nanocrystalline alloy band, saturation induction density 1.50T.
Notification number is that disclose a kind of chemical molecular formula be Fe to the patent specification of 101796207 B of CNSurplus
Cu0.98Nb3.1Si13.4B9.3Amorphous alloy band, saturation induction density 1.24T.
Compared with technical solution disclosed in above-mentioned two patent specification, the high magnetic strength nitrogen coupling of the present embodiment is iron-based
Amorphous nano-crystalline alloy strip steel rolled stock possesses higher saturation induction density.
Embodiment 4
Prepare high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band, chemical molecular formula Fe76Si11.75B8.5P0.5
Nb1.4V0.1Mo0.5Cu1N0.25。
(1) purity is greater than to 99.8% raw material Fe, Si, B, Fe3P, Nb, FeV, Mo, Cu and NbN are based on above-mentioned chemistry
In the alumina crucible that amount ratio is put into the induction melting furnace cleaned out, air pressure is evacuated to lower than 0.02Pa, is then charged with
Argon gas to air pressure is that 0.05MPa carries out melting, and smelting temperature is 1300 DEG C, 20min is kept the temperature after fusing, then by molten alloy ingot
Cooling 20min in copper mold is poured into, the uniform nitrogen coupling ferrous alloy ingot casting of ingredient is obtained；
(2) obtained nitrogen coupling ferrous alloy ingot casting is packed into the stone that bottom is equipped with the nozzle that width is 0.8mm after broken
Ying Guanzhong, adjusting furnace chamber gas pressure is lower than standard atmospheric pressure 0.09MPa, and adjusting quartz ampoule internal and external pressure difference is 300Pa, is adopted
With single-roller rapid quenching with quenching, band is got rid of with the speed of 40m/s in nitrogen atmosphere, the nitrogen coupling that continuous completely amorphous state is made is iron-based non-
Peritectic alloy band；
(3) obtained nitrogen coupling iron-based amorphous alloy ribbon material is placed in quartz ampoule, be evacuated to air pressure no more than 5.0 ×
10-3Quartz ampoule is placed in heat-treatment furnace by Pa, rises to 480 DEG C with the heating rate of about 3 DEG C/min, is kept the temperature after 10min again
560 DEG C are warming up to, 10min is kept the temperature, quartz ampoule taking-up is then placed in quenching-in water to room temperature, finally at 150 DEG C rapidly
The high vacuum for carrying out 90min is tempered to obtain high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band.
The saturation induction density of obtained high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band is up to 1.57T.
Embodiment 5
High magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy powder is prepared, chemical molecular formula is (Fe78Nb8B13Cu1)99.63N0.37。
(1) simple substance Fe, Nb, B and Cu and NbN are uniformly mixed by above-mentioned stoichiometric ratio, utilize arc-melting furnace system
The standby uniform nitrogen of ingredient couples ferrous alloy ingot casting.It is evacuated to air pressure first lower than 2.0 × 10-2Pa is then charged with argon gas extremely
Air pressure is that 0.05MPa carries out multiple melting to uniform, by the cooling 30min of molten alloy ingot after melting, obtains the uniform nitrogen of ingredient
Couple ferrous alloy ingot casting.
(2) obtained nitrogen coupling ferrous alloy ingot casting is ground off into surface impurity with grinding wheel, aerosolization obtains completely amorphous state
Nitrogen couple Fe-based amorphous alloy powder, partial size be 75~100 μm, nitrogen content 960ppm.
(3) obtained nitrogen coupling Fe-based amorphous alloy powder is put into quartz ampoule, with the heating rate of about 3 DEG C/min
It rises to 480 DEG C, is warming up to 550 DEG C again after keeping the temperature 10min, keep the temperature 30min, vacuum degree is not in guarantee quartz ampoule when two sections of annealing
Higher than 5.0 × 10-3Pa then takes out quartz ampoule and is rapidly cooled to room temperature in water, then carries out under the conditions of 150 DEG C
The high vacuum of 90min is tempered, and obtains high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy powder.
It is coupled using the high magnetic strength nitrogen of obtained high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy powder preparation iron-based non-
Brilliant nanocrystalline magnetic core has the characteristics that nitrogen is evenly distributed, nitrogen content 960ppm.
Comparative example 1
Compared with Example 1, difference, which is only that in raw material, is added without ZrN, and other conditions are identical, obtain chemical molecular formula and are
Fe90Zr7B3Nitrogen-free iron-based amorphous alloy ribbon material.
Comparative example 2
Using the iron-based amorphous alloy ribbon material of comparative example 1, two sections of annealing and tempering same as Example 2 are carried out,
Obtain nitrogen-free Fe-based amorphous nanocrystalline alloy band.
Fe-based amorphous nanocrystalline alloy is coupled using the high magnetic strength nitrogen that vibrating specimen magnetometer testing example 2 is prepared
The soft magnet performance for the nitrogen-free Fe-based amorphous nanocrystalline alloy band that band and comparative example 2 are prepared.As shown in figure 3, comparative example 2
The saturation induction density for the nitrogen-free Fe-based amorphous nanocrystalline alloy band being prepared is 1.63T, what embodiment 2 was prepared
The saturation induction density of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band is 1.73T.
Fe-based amorphous nanocrystalline alloy band is coupled with the high magnetic strength nitrogen that electrochemical workstation testing example 2 is prepared
Polarization curve of the nitrogen-free Fe-based amorphous nanocrystalline alloy band being prepared with comparative example 2 in 0.5MNaCl solution, characterization
Corrosion resistance.
As shown in figure 4, embodiment 2 is made compared with the nitrogen-free Fe-based amorphous nanocrystalline alloy band that comparative example 2 is prepared
Standby obtained high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band has the corrosion potential of smaller corrosion current, corrigendum.
Under conditions of corrosive medium is 0.5M NaCl solution, nitrogen-free iron-based amorphous nanometer crystalline that comparative example 2 is prepared
The corrosion rate of alloy strip steel rolled stock is 0.3mm/a, and the high magnetic strength nitrogen that embodiment 2 is prepared couples Fe-based amorphous nanocrystalline alloy band
The corrosion rate of material is substantially reduced, and is 0.12mm/a, illustrates that the high magnetic strength nitrogen that embodiment 2 is prepared couples Fe-based amorphous receive
The corrosion resistance of rice peritectic alloy band is much better than the nitrogen-free Fe-based amorphous nanocrystalline alloy band that comparative example 2 is prepared.
This is because nanocrystalline Educt of crystals behavior obtains after iron-based amorphous nanometer crystalline system adulterates nitrogen by nitride
Control.As shown in Fig. 2 B, 2C, the high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy band that embodiment 2 is prepared is obtained
Fe3The precipitation of N phase and ZrN phase, therefore, the high magnetic strength nitrogen that embodiment 2 is prepared couple Fe-based amorphous nanocrystalline alloy band
There is the corrosion potential of smaller corrosion current, corrigendum.
Comparative example 3
Iron-based amorphous alloy ribbon material is coupled using the nitrogen of embodiment 1, is handled using conventional annealing.It is complete by what is obtained first
Amorphous nitrogen coupling iron-based amorphous alloy ribbon material is placed in quartz ampoule, is evacuated to 5.0 × 10-3Then Pa sets quartz ampoule
In heat-treatment furnace, 630 DEG C are risen to the heating rate of about 2 DEG C/s, keeps the temperature 1h, is finally rapidly placed in quartz ampoule taking-up
Quenching-in water then carries out the lonneal of 90min at 200 DEG C, obtains nitrogen coupling Fe-based amorphous nanocrystalline alloy to room temperature
Band, nitrogen content 890ppm, saturation induction density 1.68T.
Comparative example 4
Iron-based amorphous alloy ribbon material is coupled using the nitrogen of embodiment 1, is made annealing treatment using same as Example 2 two sections,
But without tempering, nitrogen coupling Fe-based amorphous nanocrystalline alloy band is obtained, nitrogen content 890ppm, saturation induction is strong
Degree is 1.67T.
In addition, it should also be understood that, those skilled in the art can be to this hair after having read foregoing description content of the invention
Bright to make various changes or modifications, these equivalent forms also fall within the scope of the appended claims of the present application.
Claims (6)
1. a kind of preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy, comprising:
(1) by Fe, amorphous formation element, thick atom dimension elements and nanocrystalline forming core element simple substance and/or compound, and
Nitride as raw material carry out melting obtain nitrogen coupling ferrous alloy ingot casting, the amorphous formation element be selected from Al, B, P, C or
At least one of Si, thick atom dimension elements are selected from least one of IV B, V B or VI B race element, nanocrystalline forming core
Element is selected from least one of Cu, Ag or Zn；
(2) obtained nitrogen coupling ferrous alloy ingot casting is prepared completely after broken, remelting using quick chilling technology of preparing
Amorphous nitrogen couples Fe-based amorphous alloy；
(3) the nitrogen coupling Fe-based amorphous alloy of obtained completely amorphous state is successively subjected to two sections of annealing and tempering obtains high magnetic strength
Nitrogen couples Fe-based amorphous nanocrystalline alloy, and the temperature of the first segment annealing of two sections of annealing is lower than the first crystallization start temperature
20 ~ 50 DEG C, the temperature of second stage annealing is between the first crystallization start temperature and the second crystallization start temperature；
The first crystallization start temperature refers to the temperature for starting that α-Fe is precipitated in heat treatment process, is 480 ~ 530 DEG C；
The second crystallization start temperature refer to may adversely affecting magnetic property in addition to α-Fe other mutually start
The temperature of precipitation.
2. the preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy according to claim 1, which is characterized in that
The nitride is Fe x N, one of ZrN, CrN, NbN, AlN and MoN or a variety of, whereinx = 2~4。
3. the preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy according to claim 1, which is characterized in that
The thick atom dimension elements are selected from least one of Zr, Cr, Nb, Mo, W or Hf.
4. the preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy according to claim 1, which is characterized in that
The quick chilling technology of preparing is single-roller rapid quenching with quenching or gas atomization.
5. the preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy according to claim 1, feature exist
In, the temperature of the described first segment annealing is 460 ~ 510 DEG C, and the time is 10 ~ 20 min, the temperature of second stage annealing is 530 ~
750 DEG C, the time is 10 ~ 60 min.
6. the preparation method of high magnetic strength nitrogen coupling Fe-based amorphous nanocrystalline alloy according to claim 1, feature exist
In the temperature of the tempering is 150 ~ 250 DEG C, and the time is 60 ~ 120 min.
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