CN108172355B - One kind getting rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process - Google Patents
One kind getting rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process Download PDFInfo
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- CN108172355B CN108172355B CN201810062613.6A CN201810062613A CN108172355B CN 108172355 B CN108172355 B CN 108172355B CN 201810062613 A CN201810062613 A CN 201810062613A CN 108172355 B CN108172355 B CN 108172355B
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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
- H01F1/012—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials adapted for magnetic entropy change by magnetocaloric effect, e.g. used as magnetic refrigerating material
- H01F1/015—Metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
Abstract
One kind getting rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process, belongs to La-Fe-Si fibre technology field.The problems such as the invention solves existing La-Fe-Si block alloys there are subsequent high temperature heat treatment time is long, and heat conduction efficiency is low when use, and demagnetizing factor is high.The method of the present invention: one, La-Fe-Si alloy by melt spinning process is prepared into La-Fe-Si fiber；Two, it is subsequently placed in acetone and is cleaned by ultrasonic, it is dry；Three, refractory ceramics pipe is successively subjected to washing and drying treatment, by one end closure, then away from necking processing is carried out at open end overall length 1/4~1/3, fiber is placed in the side of sealing, is reloaded into titanium silk；Four, be passed through high-purity argon gas after then vacuumizing, then vacuumize, repeatedly gas washing at least three times after, open end is sealed；Five, it is air-cooled to room temperature after subsequently heat-treated, cracks refractory ceramics pipe.The method of the present invention obtains the magneto-caloric material that high magnetic heating performance, high heat conductance, low demagnetizing factor, downfield drive.
Description
Technical field
The invention belongs to La-Fe-Si fibre technology fields；Based on melt getting rid of a method more particularly to one kind, to prepare high magnetic hot
It can La-Fe-Si fiber process.
Background technique
With science and technology it is increasingly developed, people propose more requirements for magnetic refrigeration apparatus, compared to tradition
Vapor compression refrigeration technology, the magnetic Refrigeration Technique based on magnetothermal effect have high efficiency, low cost, do not generate greenhouse gases
Advantage is extensively studied in recent years and is paid close attention to.
In recent years, La-Fe-Si ferromagnetic alloy obtains extensive concern because having the advantage that: (1) material preparation is not required to
Want very high purity and the high raw material of price；(2) its thermal conductivity is close with Gd, is better than Gd5(Si, Ge)4With MnAs alloy；(3) magnetic
Refrigeration performance is high；(4) thermo-lag and magnetic lag are small.However, application is limited in actual production for La-Fe-Si block alloy, mainly
There is following reason: (1) uniform La (Fe, Si) can not be obtained using traditional electric arc melting mode13Phase (1:13 phase), that is, generate
The phase of magnetothermal effect, can also generate α-Fe and LaFeSi (1:1:1) phase usually in casting process, and α-Fe and LaFeSi (1:
1:1) opposite magnetic heating performance is almost without contribution；(2) La-Fe-Si alloy, which passes through, occurs peritectic reaction: L+ α-Fe → La (Fe,
Si)13Realize homogenization of composition, peritectic reaction temperature is high, the time is long, therefore block alloy needs prolonged high-temperature heat treatment
To guarantee homogeneity of ingredients；(3) block La-Fe-Si alloy specific surface area is small, low with surrounding medium heat conduction efficiency；(4) it demagnetizes
Coefficient is high；(5) highfield is needed to drive when working.
Summary of the invention
The invention solves existing La-Fe-Si block alloys there are subsequent high temperature heat treatment time is long, heat transfer when use
The problems such as low efficiency, demagnetizing factor is high.
For existing issue, the invention discloses a kind of preparation method of La-Fe-Si fiber and in short-term heat treatment process,
A method is got rid of using melt and prepares the La-Fe-Si fiber that diameter reaches micron-scale, and then to fiber progress, heat treatment can be real in short-term
Structural homogenity is now improved rapidly, enhances the purpose of its magnetic heating performance, to obtain a kind of high magnetic heating performance, high heat conductance, low
The magneto-caloric material that demagnetizing factor, downfield drive.
In order to solve the above technical problems, getting rid of a method the present invention is based on melt prepares high magnetic heating performance La-Fe-Si fiber process
It carries out in the steps below:
Step 1: La-Fe-Si alloy cast ingot, which is cut into certain shapes, (is such as cut into 15~20mm with Wire EDM
Cylinder) to immerse ultrasonic cleaning in acetone soln dry to remove surface and oil contaminant, then passes through melt spinning under high-purity argon gas protection
Silk method prepares La-Fe-Si fiber；
It is cleaned by ultrasonic Step 2: the La-Fe-Si fiber that step 1 obtains is placed in acetone to remove surface and oil contaminant and ash
Dirt, it is dry；
Step 3: refractory ceramics pipe is successively subjected to washing and drying treatment, it is complete by one end closure, then away from open end
Necking processing is carried out at long 1/4~1/3, is initially charged with step 2 treated La-Fe-Si fiber, and the fiber is placed in sealing
Side is reloaded into titanium silk, and minimum range is 50mm between titanium silk and fiber；
Step 4: being passed through high-purity argon gas after then vacuumizing, then vacuumize, repeatedly gas washing at least three times after, by open end
Sealing；
Step 5: being then heat-treated at 1080 DEG C~1120 DEG C with the heating of (5~10) DEG C/min speed, 15min is kept the temperature
It is air-cooled to room temperature after~30min, cracks refractory ceramics pipe to get high magnetic heating performance La-Fe-Si fiber is arrived.
It further limits, step 1 dry 2~4h under the conditions of (373K~423K).
It further limits, melt spinning process described in step 1, which prepares fiber, to be completed by following step:
Ingot casting is put into boron nitride crucible by step 1, and equipment cavity is evacuated to 0.5 × 10-3Pa~5 × 10-3Pa
After be filled with high-purity argon gas；
Step 2, starting metal roller, are arranged molybdenum wheel speed VwFor 1500~1800r/min；
Step 3 opens induction heating apparatus, and adjusting heating power is 20kW~24kW, and alloy solution upper end forms spherical surface
Molten bath；
Step 4, control crucible are mobile to roller direction, and wherein the feed rate of crucible is 30~50 μm/s；
The La-Fe-Si fiber that step 5, molybdenum wheel contact alloy molten bath, i.e. acquisition diameter are 50~100 μm.
It further limits, is put into step 2 in acetone and utilizes 10~15min of ultrasonic cleaning.
It further limits, dries 2~4h in step 2 under the conditions of (353K~393K).
It further limits, the refractory ceramics pipe of both ends open is immersed to dilute nitre of 3%~5% (quality) in step 3
In acid solution, it is cleaned by ultrasonic 30~40min, with distilled water cleaning, drying 20~for 24 hours after taking-up.
It further limits, titanium silk described in step 3 is process by the titanium foil of 200 μ m-thicks.
Since Titanium has the ability of absorption oxygen, titanium silk, which is added, can prevent the oxidation of fiber.
It further limits, step 4 is evacuated to 0.5 × 10-3~5 × 10-3Pa。
High-purity argon gas: meeting national standard GB/T 10624-1995, purity of argon>99.999%, nitrogen content<5ppm, and oxygen contains
Amount < 2ppm, hydrogen content < 1ppm, total carbon content (with methanometer) < 2ppm, moisture content < 4ppm.
Since the specific surface area of fiber is high, by calculating, under the working efficiency of 1HZ, fiber that diameter is 50~200 μm
Heat conduction efficiency is splendid, and fiber is almost nil in upper demagnetizing factor along its length, simultaneously because crystal grain is tiny in fiber,
Its heat treatment time was reduced to 15~30min by 7 days or more.The present invention also can be applied to other and need at high temperature Long Time Thermal
The ferromagnetic alloy that reason can be only achieved homogenization and drive with high magnetic heating performance, high heat conductance, low demagnetizing factor, downfield
In manufacture.
The present invention is long for La-Fe-Si block alloy subsequent high temperature heat treatment time, and heat conduction efficiency is low, demagnetizing factor
The problems such as height, driving magnetic field is big, proposes that a method is got rid of by melt prepares small size fiber, declines crystallite dimension, reduces at heat
Manage the time, increase heat conduction efficiency, the method for making its length direction demagnetizing factor drop to zero, and by by fiber 1080
It keeps the temperature air-cooled after 15~30min at DEG C -1120 DEG C, increases 1:13 phase content in microscopic structure, α-Fe content is reduced, to mention
The magnetic heating performance of high microsteping.
Detailed description of the invention
Fig. 1 is that a La-Fe-Si filamentary electrons scan image for method preparation is got rid of using melt；
Fig. 2 is the backscattered electron scan image after as cast condition La-Fe-Si fiber polishing；
Fig. 3 is the backscattered electron scan image of La-Fe-Si fiber air-cooled after keeping the temperature 20min at 1100 DEG C；
Fig. 4 is that as cast condition fiber line scans constituent analysis as a result, 1-Fe element, 2-Si elements, 3-La are first in Fig. 4 in Fig. 2
Element；
Fig. 5 is that air-cooled fiber line scanning is as a result, in Fig. 5 after keeping the temperature 20min at 1100 DEG C in Fig. 3,1-Fe element,
2-Si elements, 3-La elements；
Fig. 6 is as cast condition fiber, and the block quenched after keeping the temperature 14 days at air-cooled fiber after 20min and 1050 DEG C is kept the temperature at 1100 DEG C
X-ray diffraction (XRD) image of body alloy (with fiber identical component)；
Fig. 7 is the intensity of magnetization-temperature (M-T) of the as cast condition fiber in the case where magnetic field (H) is 200Oe and 50kOe in temperature-rise period
Relation curve；
Fig. 8 is the intensity of magnetization-temperature of the fiber in the case where magnetic field (H) is 200Oe and 50kOe in temperature-rise period after heat treatment
(M-T) relation curve；
Fig. 9 be after high temperature long heat treatment block alloy in the case where magnetic field (H) is 200Oe and 50kOe in temperature-rise period
The intensity of magnetization-temperature (M-T) relation curve.
Specific embodiment
Specific embodiment 1: the preparation method of the La-Fe-Si alloy cast ingot of present embodiment is to carry out in the steps below
:
Step (1) prepares raw material according to the mass ratio of required element, and being designed to of sample is divided into LaFe13.2Si0.7
(atomic percent), bulk sample quality are 50g, and the purity of La, Fe, Si are respectively 99.99%, 99.99%, 99.999%, are matched
First prepare Fe and Si when processed, when melting prepares La again.Consider to be easy to aoxidize and compromised quality in La element fusion process, when preparation
The content of La adds 2% on the basis of learning metering ratio.
Step (2), sample carry out melting using the method for electric arc melting, for the uniformity for guaranteeing ingredient in alloy, will close
Gold is overturn 5 times in arc-melting furnace, and then inhaling and casting diameter is 10.1mm, and length is the ingot casting of 80mm.
A method is got rid of based on melt using above-mentioned La-Fe-Si alloy cast ingot and prepares high magnetic heating performance La-Fe-Si fiber process
It carries out in the steps below:
Step 1: La-Fe-Si alloy cast ingot to be cut into the cylinder of 15mm with Wire EDM, immerse in acetone soln
Ultrasonic cleaning removal surface and oil contaminant, takes out after dry 3h under the conditions of 373K, then passes through melt spinning under high-purity argon gas protection
Method prepares La-Fe-Si fiber；
Fibre composition is La6.71Fe88.59Si4.70(atomic percent), as shown in Figure 1, fibre diameter is 70 μm, and diameter
It is of uniform size.
Wherein, the melt spinning process, which prepares fiber, is completed by following step:
The ingot casting is put into boron nitride crucible by step 1, and equipment cavity is evacuated to 2 × 10-3It is filled with after Pa high-purity
Argon gas；
Step 2, starting metal roller, are arranged molybdenum wheel speed VwFor 1500r/min；
Step 3 opens induction heating apparatus, and adjusting heating power is 20kW, and alloy solution upper end forms spherical surface molten bath；
Step 4, control crucible are mobile to roller direction, and wherein the feed rate of crucible is 50 μm/s；
The La-Fe-Si fiber that step 5, molybdenum wheel contact alloy molten bath, i.e. acquisition average diameter are 50~60 μm.
It is cleaned by ultrasonic 10 minutes removal surfaces Step 2: the La-Fe-Si fiber that 10mg step 1 obtains is placed in acetone
Greasy dirt and dust are put into drying box and take out after dry 3h under the conditions of 373K；
Step 3: the quartz ampoule of the both ends open of 9 × 300mm of Ф is immersed in the dilute nitric acid solution of 4% (quality), place
It is cleaned by ultrasonic for 30~minute in supersonic wave cleaning machine, is cleaned after taking-up with distilled water, is put into drying in drying box and for 24 hours, utilizes
Flame by one end closure, then away from open end overall length 1/3 carry out necking handle to Ф 4mm (can necking handle to 3~Ф of Ф
5mm), it is initially charged with step 2 treated the side that La-Fe-Si fiber is placed in sealing, then away from being packed into 2 at open end overall length 1/2
The a length of 20mm of root (or 3), the titanium silk that width is 1mm and thickness is 0.2mm；
Titanium silk is that the titanium foil of 200 μ m-thicks is cut into filiform.
Step 4: being passed through high-purity argon gas after then vacuumizing, then it is evacuated to 2 × 10-3Pa, repeatedly gas washing three times after, will
Open end sealing keeps being in vacuum state in ceramic tube；
Step 5: being then placed in chamber type electric resistance furnace, with the heating of 10 DEG C/min speed, it is heat-treated, keeps the temperature at 1100 DEG C
It is air-cooled to room temperature (2~3min of time-consuming) after 20min, cracks quartz ampoule to get high magnetic heating performance La-Fe-Si fiber is arrived.
The high-purity argon gas: meeting national standard GB/T 10624-1995, purity of argon>99.999%, nitrogen content<5ppm,
Oxygen content < 2ppm, hydrogen content < 1ppm, total carbon content (with methanometer) < 2ppm, moisture content < 4ppm.
Fig. 2 and Fig. 3 is respectively La-Fe-Si as cast condition fiber and is kept the temperature after 20min at 1100 DEG C after air-cooled fiber polishing
Back scattering scan image, as shown in the figure, it can be seen that backscattered electron contrast is uniform, illustrates the ingredient in fiber macroscopically
It is evenly distributed, does not find out bulk precipitated phase.
Fig. 4 and Fig. 5 is respectively the line scanning result carried out in Fig. 2 and Fig. 3 along fibre diameter direction, it can be seen that
Fiber before heat treatment after distributed components on longitudinal section, and after being heat-treated fiber average assay
(La7.33Fe78.17Si14.50) in α-Fe content be less than heat treatment before fiber (La7.27Fe78.92Si13.81), illustrate in Re Chu
Peritectic reaction occurs during reason in fiber microscopic structure, part α-Fe generates 1:13 phase with liquid phase reactor.
Fig. 6 is as cast condition fiber, and the phase quenched after keeping the temperature 14 days at air-cooled fiber after 20min and 1050 DEG C is kept the temperature at 1100 DEG C
X-ray diffraction (XRD) image of congruent block alloy.It is available from figure 4, fiber organize after the heat treatment in α-Fe phase with
As cast condition fiber compared to significantly reducing, the block alloy (with fiber identical component) of content and high temperature long heat treatment quite,
Illustrate that small size fibrous material can effectively reduce the content of α-Fe phase under conditions of heat treatment time is greatly shortened.X is penetrated
Line diffraction analysis shows, all contains α-Fe phase, but because α-Fe crystal grain in air-cooled fiber after as cast condition and 1100 DEG C of heat preservation 20min
It is too tiny, it is nanoscale, does not observe in the scan image of Fig. 2 and Fig. 3.
Block after Fig. 7 and Fig. 8 respectively the La-Fe-Si alloy fiber of heat treatment front and back and heat treatment identical with its ingredient
The body alloy intensity of magnetization-temperature (M-T) curve at 200Oe and 50kOe.As shown, the fiber after high temperature, short time heat treatment
M-T slope of a curve significantly increases, and illustrates that the increase of 1:13 phase amount after being heat-treated leads to being greatly enhanced for magnetic phase transition degree.
Fig. 8 and Fig. 9 are compared as can be seen that the fiber after being heat-treated at 50kOe and the block alloy intensity of magnetization after heat treatment
It is close with the M-T slope of curve, illustrate heat treatment after fiber in the case where heat treatment time is greatly reduced, can obtain with
Magnetothermal effect similar in block alloy after long heat treatment.Fig. 9 is compared with Fig. 7,8 simultaneously can be seen that, fibrous material
It is easier to magnetize than block alloy under downfield, magnetic phase transition occurs and generates magnetothermal effect, therefore compared with block materials, small ruler
Very little fibrous material can be applied in bigger magnetic field section.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: by 20mg step in step 2
The one La-Fe-Si fiber obtained, which is placed in acetone, to be cleaned by ultrasonic.Other steps and parameter concrete mode one are identical.
Specific embodiment 3: the present embodiment is different from the first embodiment in that: equipment cavity is true in step 1
Empty pump is to 3 × 10-3Pa.Other steps and parameter concrete mode one are identical.
Specific embodiment 4: the present embodiment is different from the first embodiment in that: molybdenum wheel speed V in step 1w
For 1600r/min.Other steps and parameter concrete mode one are identical.
Specific embodiment 5: the present embodiment is different from the first embodiment in that: induction heating fills in step 1
It sets heating power and is adjusted to 22kW.Other steps and parameter concrete mode one are identical.
Specific embodiment 6: the present embodiment is different from the first embodiment in that: the feeding of crucible in step 1
Rate is adjusted to 40 μm/s.Other steps and parameter concrete mode one are identical.
Specific embodiment 7: the present embodiment is different from the first embodiment in that: fiber is put into step 2
Ultrasonic cleaning 12min is utilized in acetone.Other steps and parameter concrete mode one are identical.
Specific embodiment 8: the present embodiment is different from the first embodiment in that: fiber is in 380K in step 2
Lower dry 3h.Other steps and parameter concrete mode one are identical.
Specific embodiment 9: the present embodiment is different from the first embodiment in that: by both ends open in step 3
Refractory ceramics pipe immerse 4% (quality) dilute nitric acid solution in, be cleaned by ultrasonic 35min, after taking-up with distilled water clean, do
Dry 22h.Other steps and parameter concrete mode one are identical.
Specific embodiment 10: the present embodiment is different from the first embodiment in that: by both ends open in step 3
Refractory ceramics pipe immerse 4% (quality) dilute nitric acid solution in, be cleaned by ultrasonic 35min, after taking-up with distilled water clean, do
Dry 22h.Other steps and parameter concrete mode one are identical.
Specific embodiment 11: the present embodiment is different from the first embodiment in that: ceramic tube is taken out in step 4
It is passed through high-purity argon gas after vacuum, then vacuumizes, repeatedly after gas washing four times, open end is sealed.Other steps and parameter are specifically square
Formula one is identical.
Specific embodiment 12: the present embodiment is different from the first embodiment in that: 8 DEG C/min speed in step 5
Degree heating, is heat-treated at 1080 DEG C, is air-cooled to room temperature after keeping the temperature 30min, cracks refractory ceramics pipe to get hot to high magnetic
It can La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 13: the present embodiment is different from the first embodiment in that: 8 DEG C/min speed in step 5
Degree heating, is heat-treated at 1090 DEG C, is air-cooled to room temperature after keeping the temperature 20min, cracks refractory ceramics pipe to get hot to high magnetic
It can La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 14: the present embodiment is different from the first embodiment in that: 9 DEG C/min speed in step 5
Degree heating, is heat-treated at 1090 DEG C, is air-cooled to room temperature after keeping the temperature 30min, cracks refractory ceramics pipe to get hot to high magnetic
It can La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 15: the present embodiment is different from the first embodiment in that: 9 DEG C/min speed in step 5
Degree heating, is heat-treated at 1100 DEG C, is air-cooled to room temperature after keeping the temperature 25min, cracks refractory ceramics pipe to get hot to high magnetic
It can La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 16: the present embodiment is different from the first embodiment in that: 10 DEG C/min in step 5
Speed heating, is heat-treated at 1110 DEG C, is air-cooled to room temperature after keeping the temperature 15min, cracks refractory ceramics pipe to get hot to high magnetic
Performance La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 17: the present embodiment is different from the first embodiment in that: 10 DEG C/min in step 5
Speed heating, is heat-treated at 1110 DEG C, is air-cooled to room temperature after keeping the temperature 20min, cracks refractory ceramics pipe to get hot to high magnetic
Performance La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 18: the present embodiment is different from the first embodiment in that: 8 DEG C/min speed in step 5
Degree heating, is heat-treated at 1120 DEG C, is air-cooled to room temperature after keeping the temperature 15min, cracks refractory ceramics pipe to get hot to high magnetic
It can La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 19: the present embodiment is different from the first embodiment in that: 9 DEG C/min speed in step 5
Degree heating, is heat-treated at 1120 DEG C, is air-cooled to room temperature after keeping the temperature 20min, cracks refractory ceramics pipe to get hot to high magnetic
It can La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Specific embodiment 20: the present embodiment is different from the first embodiment in that: 10 DEG C/min in step 5
Speed heating, is heat-treated at 1120 DEG C, is air-cooled to room temperature after keeping the temperature 25min, cracks refractory ceramics pipe to get hot to high magnetic
Performance La-Fe-Si fiber.Other steps and parameter concrete mode one are identical.
Claims (10)
1. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process, it is characterised in that the La-Fe-Si
The preparation method of fiber carries out in the steps below:
It is cleaned by ultrasonic Step 1: La-Fe-Si alloy cast ingot to be cut into certain shapes and immerse in acetone soln, it is dry, then in height
La-Fe-Si fiber is prepared by melt spinning process under straight argon gas shielded；
It is cleaned by ultrasonic Step 2: the La-Fe-Si fiber that step 1 obtains is placed in acetone, it is dry；
Step 3: refractory ceramics pipe is successively carried out washing and drying treatment, by one end closure, then away from open end overall length 1/
Necking processing is carried out at 4 ~ 1/3, is initially charged with step 2 treated La-Fe-Si fiber, the fiber is placed in the side of sealing,
It is reloaded into titanium silk, minimum range is 50mm between titanium silk and fiber；
Step 4: being passed through high-purity argon gas after then vacuumizing, then vacuumize, repeatedly gas washing at least three times after, open end is sealed；
Step 5: be then heat-treated at 1080 DEG C ~ 1120 DEG C with 5 DEG C/min ~ 10 DEG C/min speed heating, heat preservation 15min ~
It is air-cooled to room temperature after 30min, cracks refractory ceramics pipe to get high magnetic heating performance La-Fe-Si fiber is arrived.
2. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is step 1 dry 2 ~ 4h under the conditions of 373K ~ 423K.
3. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign, which is that melt spinning process described in step 1 prepares fiber, to be completed by following step:
Ingot casting is put into boron nitride crucible by step 1, is filled after equipment cavity is evacuated to 0.5 × 10-3Pa ~ 5 × 10-3Pa
Enter high-purity argon gas；
Step 2, starting metal roller, setting molybdenum wheel speed Vw are 1500 ~ 1800r/min；
Step 3 opens induction heating apparatus, and adjusting heating power is 20kW ~ 24kW, and alloy solution upper end forms spherical surface molten bath；
Step 4, control crucible are mobile to roller direction, and wherein the feed rate of crucible is 30 ~ 50 μm/s；
The La-Fe-Si fiber that step 5, molybdenum wheel contact alloy molten bath, i.e. acquisition diameter are 50 ~ 100 μm.
4. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign, which is to be put into step 2 in acetone, utilizes 10 ~ 15min of ultrasonic cleaning.
5. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is in step 2 dry 2 ~ 4h under the conditions of 353K ~ 393K.
6. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is to immerse the refractory ceramics pipe of both ends open in the dilute nitric acid solution that mass concentration is 3% ~ 5% in step 3, ultrasound
30 ~ 40min is cleaned, with distilled water cleaning, drying 20 ~ for 24 hours after taking-up.
7. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is that the fiber of every 10mg in step 3 need to be packed into that length is 20mm, width is 1mm and with a thickness of titanium silk 2 ~ 3 of 0.2mm.
8. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is that titanium silk described in step 3 is process by the titanium foil of 200 μ m-thicks.
9. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is that step 4 is evacuated to 0.5 × 10-3 ~ 5 × 10-3Pa.
10. one kind gets rid of a method based on melt and prepares high magnetic heating performance La-Fe-Si fiber process according to claim 1, special
Sign is to be heat-treated at 1100 DEG C with the heating of 5 ~ 10 DEG C/min speed, kept the temperature 20min.
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| CN106929737A (en) * | 2017-03-29 | 2017-07-07 | 哈尔滨工业大学 | A kind of method for making melt pull Ni Mn Ga Fe metallic fiber crystal grain grow up |
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| Microstructure and magnetocaloric properties of melt-extracted La-Fe-Si microwires;J.D.Dong等;《Journal of Magnetism and Magnetic Materials》;20140121;第74页 * |
| Ni-Mn-Ga记忆合金纤维组织结构及热驱动/磁热特性;钱明芳;《中国博士学位论文全文数据库工程科技Ⅰ辑》;20170215;第2章、正文第52页 * |
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