CN100443616C - Fast microwave crystallizing process for preparing nanometer crystalline iron-base soft magnetic alloy - Google Patents

Abstract

The present invention discloses fast microwave crystallizing process for preparing nanometer crystalline iron-base soft magnetic alloy. The technological process includes the following steps: 1. smelting alloy with Fe, Cu, Nb, Si and B in the ratio of Fe73.5Cu1Nb3Si13.5B9 in an induction furnace at vacuum 3-10 Pa in high purity Ar; 2. setting coarsely crushed alloy inside quartz pipe with nozzle in the bottom, setting the quartz pipe inside induction coil in a belt spinning machine, and melting the mother alloy in protecting Ar atmosphere; 3. spraying the alloy liquid under the pressure of Ar to the surface of rotating copper roller to form non-crystalline alloy belt; and 4. sealing the thin belt in quartz tube and crystallizing treatment in a microwave sintering furnace at 400-900 deg.c for 10-180 min to obtain ideal nanometer crystal structure.

Description

Fast microwave crystallizing prepares the method for Fe-based nanocrystalline magnetically soft alloy

Technical field

The present invention relates to the method that a kind of fast microwave crystallizing prepares nano-crystal soft magnetic alloy, particularly relate to the method that a kind of fast microwave crystallizing prepares homogeneous microstructure, Fe-based nanocrystalline magnetically soft alloy that saturation magnetization is high.

Background technology

Yoshizawa added Cu and M (M=Nb, Mo, W, Ta etc.) in the matrix of Fe-Si-B non-crystaline amorphous metal in 1988, and through having obtained the nano-crystal soft magnetic alloy of excellent performance behind the subsequent annealing, its typical composition is Fe _73.3Cu ₁Nb ₃Si _13.5B ₉Because nano-crystal soft magnetic alloy has high saturation magnetic induction degree, high initial permeability, low coercive force, low high frequency magnetic loss, good strong hardness, wear resistance and erosion resistance, good characteristics such as temperature stability, started the upsurge of research amorphous nanocrystalline soft magnetic material in the world wide.The comprehensive magnetic property of nano crystal soft magnetic material is much better than silicon steel, soft magnetic ferrite, permalloy and non-crystaline amorphous metal, can be widely used in transformer, reactance coil, flat ripple reactance and leakage switch iron core etc. in large power supply transformer, the switch power supply.

Lu Ke is in the micromechanism of nineteen ninety proposition amorphous alloy crystallization process, and promptly orderly atom group shear sedimentation mechanism has developed a kind of novel method for preparing nanocrystal---amorphous crystallization.Iron-base nanometer crystal alloy generally adopts the preparation of amorphous crystallization method, and promptly the crystallization generation crystal grain by amorphous alloy is the super-fine material of nano-scale.This method has become one of three kinds of main preparation methods of the nano material of generally acknowledging in the world at present.This method is the amorphous ribbon crystallization nanocrystalline material that becomes to have certain grain-size under certain conditions that makes metal or alloy by thermal treatment process.This method provides new way for direct production bulk nano-crystalline magnetic material.Non-crystalline state is a kind of thermodynamics metastable state, easily changes more stable crystalline state under certain condition into.When the non-crystalline state sample is heat-treated, when irradiation and trickle mechanical disintegration, non-crystalline state just changes polycrystalline into.Its size and chemical ingredients and annealing conditions have confidential relation.The iron based nano crystal matrix material mainly adopts amorphous annealing preparation, comprising: the conventional annealing method of amorphous, stress annealing method, ultrashort pulse current processing nano-crystallization method, low frequency pulsed magnetic fields processing etc.But these methods more easily cause the grain-size of precipitated phase excessive, and generate the deleterious Fe-B phase of magnetic property, and technology is complicated.Microwave field is a kind of special higher frequency electromagnetic field, and frequency generally can reach 2.45GHz, but the microwave current heating is all synthetic at pottery or inorganic materials, uses less in the preparation of metal alloy.

Summary of the invention

Technical problem to be solved by this invention provides the short heat treatment time of a kind of needs and lower thermal treatment temp can obtain α-Fe (Si) that homogeneous microstructure, grain-size that saturation magnetization is high be about 15nm prepares Fe-based nanocrystalline magnetically soft alloy mutually with the fast microwave crystallizing of the iron based nano crystal soft magnetic materials of amorphous phase composition method.

In order to solve the problems of the technologies described above, the processing step that the fast microwave crystallizing that the present invention adopts prepares the method for Fe-based nanocrystalline magnetically soft alloy is: (A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Proportioning be put in the induction furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting; (B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting; (C), under the effect of argon pressure, the alloy liquation generates amorphous alloy band through the nozzle ejection of silica tube bottom to the copper roller surface of high speed rotating, the speed on copper roller surface is adjustable continuously in 5～45m/s scope; (D), with the vacuum-sealing of gained amorphous alloy band in silica tube, put into microwave agglomerating furnace then and carry out the crystallization processing, the temperature and time scope that crystallization is handled in the microwave agglomerating furnace is carried out 10min-180min at 400-900 ℃, promptly obtains the ideal nanometer crystal microstructure.

For guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process.

The temperature and time scope that crystallization is handled in the microwave agglomerating furnace serves as better to carry out 15min-120min at 400-800 ℃, is the best to carry out 20min-60min at 450-600 ℃.

Iron based nano crystal soft magnetic materials of the present invention comprises iron (Fe), silicon (Si), copper (Cu), niobium (Nb) and boron (B).Preferably contain α-Fe (Si) principal phase in this nano-crystalline magnetic material.This nano-crystalline magnetic material preferably adopts the melt-quenching method preparation, and carries out crystallization and handle in microwave field, to obtain the ideal nanocrystalline structure.

Magneticsubstance of the present invention preferably adopts the medium frequency induction melting furnace melting.

The fast microwave crystallizing of employing technique scheme prepares the method for Fe-based nanocrystalline magnetically soft alloy, and when non-crystaline amorphous metal carried out the crystallization processing under microwave action, the alloy microwave energy absorbed can be represented by the formula:

P＝ω(ε ₀ε″E ²+μ ₀μ″H ²) (3)

ω is a microwave frequency in the formula, ε ₀" dielectric loss, E are microwave electric field intensity, μ to be spatial dielectric constant, ε ₀" magnetic loss, H is a microwave magnetic field intensity to be space permeability, μ.

Each magnetized state that domain motion changed when non-crystaline amorphous metal magnetized in magnetic field all is the balance of corresponding energy, and what play a major role in the free energy of non-crystaline amorphous metal is that foreign field can E _HWith magnetoelastic energy E _λ(magnetostriction energy).Foreign field energy wherein

$G_H={\mathrm{\μ}}_0{\stackrel{\→}{M}}_s\·{\stackrel{\→}{H}}_p=-{\mathrm{\μ}}_0{M}_s{H}_p---\left(4\right)$

In the formula, μ ₀Be very aerial magnetic permeability, M _sBe the spontaneous magnetization of magnetic domain, H _pBe pulsed magnetic field intensity.And magnetoelastic energy

$G_{\mathrm{\&lambda;}}=-\frac{2}{3}{\mathrm{\&lambda;}}_s\mathrm{\&sigma;}{\mathrm{<figure-callout\; id="2"\; label="cos"\; filenames="C20071003460200111.png,C20071003460200112.png"\; state="\{\{state\}\}">cos</figure-callout>}}^2\mathrm{\&phi;}---\left(5\right)$

In the formula, φ is stress σ direction and M _sThe angle of direction, λ _sBe the saturation magnetostriction coefficient.If the energy variation that electric field causes is G _E(φ), then under the microwave field total free energy be:

G＝G _H+G _λ+G _E (6)

$G=-{\mathrm{\&mu;}}_0{M}_s{H}_p\sin \mathrm{\&phi;}-\frac{2}{3}{\mathrm{\&lambda;}}_s\mathrm{\&sigma;}{\mathrm{<figure-callout\; id="2"\; label="cos"\; filenames="C20071003460200111.png,C20071003460200112.png"\; state="\{\{state\}\}">cos</figure-callout>}}^2\mathrm{\&phi;}+G_E\left(\mathrm{\&phi;}\right)---\left(7\right)$

Three kinds act under the condition that satisfies the THERMODYNAMICAL STUDY free energy principle of the minimum (promptly $\&PartialD;G/\&PartialD;\mathrm{\&phi;}=0$ ) reach balance.During outer field action, must in non-crystaline amorphous metal, produce the line magnetostriction.Non-crystaline amorphous metal with the formation of melt supercooled method, because internal stress fluctuation, the fluctuation that atomic density distributes will be produced, the compression zone that causes existing atomic density to be higher than mean density in the non-crystaline amorphous metal is that the expansion area that p type district and atomic density are lower than mean density is n type district, and wherein more room is contained in n type district.In a pulse width, magneticstrength Hp changes within the specific limits, and the high-frequency current of magnetostriction and microwave will promote atomic vibration and the migration that produces interstitial diffusion and vacancy-like defects at non-intracrystalline.Simultaneously for reducing non-crystaline amorphous metal system energy, the supersaturation boron atom in the amorphous gap will be to the room transition, separates out for the preferential forming core of matrix metal phase α-Fe (Si) to create conditions.The energy that vibration atom boron atom obtains is high more, and is fast more to the speed of room transition, helps the nucleation rate of matrix metal phase α-Fe (Si) phase to increase, and promotes nano-crystallization.

According to Fe of the present invention _73.3Cu ₁Nb ₃Si _13.5B ₉The temperature range that alloy crystallization in microwave field is handled has been done many groups of experiments, and comparative study adopt the performance and the microstructure of such alloy of traditional crystallization treatment technology preparation, specifically technology and performance are as shown in table 1.The alloy of sequence number 1-5 for adopting the microwave field crystallization to handle, sequence number 6-7 is for adopting the alloy of traditional crystallization Processing of Preparation.After the following 480 ℃ of crystallization of microwave field were handled 5min, the volume fraction of alloy crystallization phase was greater than 70%; But when traditional crystallization was handled, alloy was handled 5min in 550 ℃ of crystallization, and the volume fraction of crystallization phase only has an appointment 10%.So the microwave field crystallization is handled the nucleation rate that can quicken the crystallization phase, shorten crystallization time, save energy.480 ℃ of crystallization are handled behind the 30min magnet and are had maximum saturation magnetization and reach 1.79T in microwave field.

The crystallization treatment process and the magnetic property of table 1 embodiment of the invention

Sequence number	Crystallization temperature/℃	Crystallization time t/min	Ms /T	Phase structure	The crystallization phase volume fraction
						1	480	5	1.18	α-Fe(Si)	＞70％
2	480	20	1.51	α-Fe(Si)	＞70％
						3	480	30	1.79	α-Fe(Si)	＞70％
4	700	20	1.02	α-Fe(Si)	＞70％
						5	850	20	0.86	α-Fe(Si)	＞70％
6	550	5	1.50	α-Fe(Si)	＜10％
						7	600	40	1.20	α-Fe(Si)	＞70％

The advantage of invention and extremely long-pending effect:

1. technology of the present invention is simple, and cost is lower, and key link includes only melting, system band and microwave crystallization and handles.In microwave crystallization treating processes, only need short heat treatment time and lower thermal treatment temp, can obtain the excellent magnetism energy.

2. by the enforcement of this programme, the microstructure of alloy system improves, and magnetic property is improved, and especially saturation magnetization obtains bigger raising.

Description of drawings

Fig. 1 is a microwave agglomerating furnace cavity configuration synoptic diagram;

Fig. 2 is Fe _73.3Cu ₁Nb ₃Si _13.5B ₉Handling M-H curve after 30min, 700 ℃ of crystallization handle 20min and 850 ℃ of crystallization to handle 20min in 480 ℃ of crystallization under the microwave field effect;

Fig. 3 is Fe _73.3Cu ₁Nb ₃Si _13.5B ₉In the TEM microstructure after 480 ℃ of crystallization are handled 30min under the microwave field effect;

Fig. 4 is Fe _73.3Cu ₁Nb ₃Si _13.5B ₉In the XRD analysis after 480 ℃ of crystallization processing 30min, 700 ℃ of crystallization are handled 20min under the microwave field effect.

Embodiment

Embodiment 1:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, the nozzle ejection of alloy liquation process silica tube bottom is to the copper roller surface of high speed rotating, the speed on copper roller surface is adjustable continuously in 5～45m/s scope, the present embodiment medium velocity is 20m/s, being prepared into thickness is 10 μ m, and width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 850 ℃, and the time is 20min.The Ms of alloy is 0.86T.

Embodiment 2:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃S _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting;

(C), under the effect of argon pressure, the nozzle ejection of alloy liquation process silica tube bottom is to the copper roller surface of high speed rotating, the speed on copper roller surface is adjustable continuously in 5～45m/s scope, the present embodiment medium velocity is 20m/s, being prepared into thickness is 10 μ m, and width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 700 ℃, and the time is 20min.On vibrating sample magnetometer, measure the M-H curve and see Fig. 2 (a), see Fig. 4 (a) with X-ray diffraction analysis phase structure, grain-size and crystal parameters.The Ms=1.02T of alloy, phase structure is by α-Fe (Si) phase, non-remaining amorphous phase and small amount of Fe ₃B constitutes mutually, and the grain-size of α-Fe (Si) phase is 27.9nm.

Embodiment 3:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, the nozzle ejection of alloy liquation process silica tube bottom is to the copper roller surface of high speed rotating, the speed on copper roller surface is adjustable continuously in 5～45m/s scope, the present embodiment medium velocity is 20m/s, being prepared into thickness is 10 μ m, and width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 480 ℃, and the time is 30min.On vibrating sample magnetometer, measure the M-H curve and see Fig. 2 (b), see Fig. 3, see Fig. 4 (a) with X-ray diffraction analysis phase structure, grain-size and crystal parameters with the transmission electron microscope observation microstructure.On vibrating sample magnetometer, measure the M-H curve, microstructure tem observation and XRD analysis.The Ms=1.79T of alloy, phase structure is made of α-Fe (Si) phase and a small amount of non-remaining amorphous phase, and α-Fe (Si) is embedded in the remaining amorphous phase mutually, and grain-size is about 15nm.

Embodiment 4:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, to the copper roller surface of high speed rotating, the speed on copper roller surface is 20m/s to the alloy liquation through the nozzle ejection of silica tube bottom, being prepared into thickness is 10 μ m, width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 400 ℃, and the time is 120min.The Ms=1.45T of alloy.

Embodiment 5:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, to the copper roller surface of high speed rotating, the speed on copper roller surface is 20m/s to the alloy liquation through the nozzle ejection of silica tube bottom, being prepared into thickness is 10 μ m, width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 900 ℃, and the time is 15min.The Ms=0.62T of alloy.

Embodiment 6:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, to the copper roller surface of high speed rotating, the speed on copper roller surface is 30m/s to the alloy liquation through the nozzle ejection of silica tube bottom, being prepared into thickness is 10 μ m, width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 800, and the time is 10min.The Ms=0.90T of alloy.

Embodiment 7:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃S _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, to the copper roller surface of high speed rotating, the speed on copper roller surface is 30m/s to the alloy liquation through the nozzle ejection of silica tube bottom, being prepared into thickness is 10 μ m, width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 600, and the time is 20min.The Ms=1.31T of alloy.

Embodiment 8:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, to the copper roller surface of high speed rotating, the speed on copper roller surface is 30m/s to the alloy liquation through the nozzle ejection of silica tube bottom, being prepared into thickness is 10 μ m, width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 480, and the time is 5min.The Ms=1.18T of alloy.

Embodiment 9:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Ratio put into medium frequency induction melting furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting, for guaranteeing the homogeneity of alloying constituent, remelting is twice in the alloy melting process;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting,

(C), under the effect of argon pressure, to the copper roller surface of high speed rotating, the speed on copper roller surface is 30m/s to the alloy liquation through the nozzle ejection of silica tube bottom, being prepared into thickness is 10 μ m, width is the amorphous alloy band of 4mm;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, vacuum tightness is 1 * 10 ^-5Pa puts into microwave agglomerating furnace then and carries out the crystallization processing, and referring to Fig. 1,1 is temperature-measuring port, and 2 is microwave source, and 3 is microwave susceptor, and 4 is sample, and 5 is porous alumina, and crystallization is handled in the microwave agglomerating furnace, and crystallization temperature is 480 ℃, and the time is 20min.The Ms=1.51T of alloy.

Claims (5)

1, a kind of fast microwave crystallizing prepares the method for Fe-based nanocrystalline magnetically soft alloy, it is characterized in that: the processing step of employing is:

(A), with purity greater than 99.9% Fe, Cu, Nb, Si, B presses Fe _73.5Cu ₁Nb ₃Si _13.5B ₉Proportioning be put in the induction furnace after preparing, be evacuated down to 10 ^-3More than the Pa, feed high-purity argon gas then and carry out melting;

(B), with the alloy cast ingot of coarse breaking after the melting pack into the bottom have in the silica tube of nozzle, silica tube is placed get rid of band machine chamber intravital ruhmkorff coil central authorities then, vacuumize, under argon shield, make the mother alloy induction melting;

(C), under the effect of argon pressure, the alloy liquation generates amorphous alloy band through the nozzle ejection of silica tube bottom to the copper roller surface of high speed rotating, the speed on copper roller surface is adjustable continuously in 5～45m/s scope;

(D), with the vacuum-sealing of gained amorphous alloy band in silica tube, put into microwave agglomerating furnace then and carry out the crystallization processing, the temperature and time scope that crystallization is handled in the microwave agglomerating furnace is carried out 10min-180min at 400-900 ℃, promptly obtains the ideal nanometer crystal microstructure.

2, fast microwave crystallizing according to claim 1 prepares the method for Fe-based nanocrystalline magnetically soft alloy, it is characterized in that: twice of above-mentioned processing step (A) interalloy fusion process interalloy remelting.

3, fast microwave crystallizing according to claim 1 and 2 prepares the method for Fe-based nanocrystalline magnetically soft alloy, it is characterized in that: the temperature and time scope that crystallization is handled in the microwave agglomerating furnace in the above-mentioned processing step (D) is carried out 15min-120min at 400-800 ℃.

4, fast microwave crystallizing according to claim 1 and 2 prepares the method for Fe-based nanocrystalline magnetically soft alloy, it is characterized in that: the temperature and time scope that crystallization is handled in the microwave agglomerating furnace in the above-mentioned processing step (D) is carried out 20min-60min at 450-600 ℃.

5, fast microwave crystallizing according to claim 1 and 2 prepares the method for Fe-based nanocrystalline magnetically soft alloy, it is characterized in that: the induction furnace in the above-mentioned processing step (A) is a medium frequency induction melting furnace.

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