CN108817412A - A kind of preparation method of FePt/Co Nano composite granules - Google Patents
A kind of preparation method of FePt/Co Nano composite granules Download PDFInfo
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- CN108817412A CN108817412A CN201810771986.0A CN201810771986A CN108817412A CN 108817412 A CN108817412 A CN 108817412A CN 201810771986 A CN201810771986 A CN 201810771986A CN 108817412 A CN108817412 A CN 108817412A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01F1/0302—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
- H01F1/0306—Metals or alloys, e.g. LAVES phase alloys of the MgCu2-type
Abstract
The invention discloses a kind of preparation methods of FePt/Co Nano composite granules, and steps are as follows：NaCl is dried, ball milling in ball grinder is poured into together with normal heptane；Platinum tetrachloride is dissolved in acetone, ferric chloride hexahydrate is dissolved in ethyl alcohol, and above two solution is mixed, and ultrasound mixes, ball milling with NaCl, dries, is put into silica crucible, is placed in tube furnace and calcines to obtain black calcined product；Deionized water is added into black calcined product, stands and sinks to beaker bottom completely to suspended matter, removes supernatant, remaining liq is then put into a centrifuge into separation, repeats 5-7 times, obtains FePt nano particle；CoCl is added to FePt obtained above2·6H2Sheet output is ground and is poured into alumina crucible at powder, then crucible is put into tube furnace and is calcined by O, ultrasound, dry out solvent, and cooling to obtain the final product.The FePt/Co Nano composite granules of this method preparation have excellent magnetic property.
Description
Technical field
The present invention relates to a kind of preparation methods of FePt/Co Nano composite granules.
Background technique
The development of magnetic recording material is maked rapid progress, due to electronic equipment lightweight, miniaturization, multifunction demand, obtain
The magnetic recording material of high magnetic storage density is always target that people are pursued.High packing density bring is individually to record
The area of position reduces, however the demand of high s/n ratio, then makes individually to record the position carrying a lot of magnetic crystal grain of quantity, so single
The size of a crystal grain just receives stringent restriction.However too small particle size can be such that the recording status time reduces, here it is
The bottleneck of magnetic recording material, i.e. superparamagnetic limit.
Magnetic nanoparticle is suffered from many aspects and is widely applied, and the overwhelming majority is required still to be had under small scale
High magnetic property, as required nanoparticle size to be maintained at 2-10nm in terms of magnetic recording.However up to the present magnetic Nano
The research of grain is concentrated mainly on oxide nano particles, such as Fe2O3、Fe3O4Deng.These oxide saturation magnetizations are low, lower
Magnetocrystalline anisotropy be even more to make oxide particle there have been superparamagnetic limits under tens nanometers of size.Therefore, it prepares
Hard magnetic phase with high magnetocrystalline anisotropy Ku, further increasing magnetic storage density becomes urgent problem to be solved instantly.
FePt nanomagnets, by feat of excellent chemical stability, thermal stability and inoxidizability, good single shaft magnetocrystalline
Anisotropy (Ku=7 × 107erg/cm3) and minimum superparamagnetic critical dimension, huge answer is possessed in terms of magnetic storage
Use prospect.Using the FePt of high-coercive force as hard magnetic phase, the soft magnetic phase of high saturation and magnetic intensity is coated, is prepared while having
The nanometer double-phase composite of high-coercive force, high saturation and magnetic intensity is always the research in magnetic Nano material field in recent years
Hot spot.FePt magnetic nanoparticle preparation method has：High temeperature chemistry thermally decomposes salt method, co-reducing process, electrochemical process etc..
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of FePt/Co Nano composite granules.
The present invention is realized by following technical solution：
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：10-20 parts of NaCl are put into vacuum
In drying box, then 30-40 DEG C of vacuum drying 9-11h is poured into ball grinder together with 45-55 portions of normal heptanes, and sealing is fixed simultaneously
It is put into ball milling 37-39h in planetary ball mill；4-6 parts of platinum tetrachlorides are dissolved in 20-30 parts of acetone, 7-13 parts of ferric chloride hexahydrates
30-40 parts of ethyl alcohol are dissolved in, above two solution is mixed, ultrasonic vibration 25-35min, by the above-mentioned solution and NaCl mixed
Powder mixes again, ball milling 14-16h, and the mixed-powder taking-up after ball milling is put into 50-60 DEG C of drying in baking oven, is put into quartz
In crucible, it is placed in tube furnace and is calcined；Tube furnace need to first lead to Ar air purge gas 3 times to exclude the air in furnace, then in Ar
And H2Mixed flow gas under conditions of start to warm up, H2Percent by volume be 2%-4%, mixed gas flow 340-
360mL/min rises to 470-490 DEG C of heat preservation 2.5-3.5h with the heating rate of 8 DEG C/min, continues to ventilate after heat preservation terminates
Until being cooled to room temperature, black calcined product is obtained；80-90 parts of deionized waters are added into black calcined product, stand 47-
49h waits for that suspended matter sinks to beaker bottom completely, removes supernatant, remaining liq is then put into a centrifuge separation, continues to wash
NaCl is removed, repeats 5-7 times, obtains FePt nano particle；5-15 parts of CoCl are added to FePt obtained above2·6H2O, the two are mixed
Sheet output is ground and is poured into alumina crucible at powder, then by crucible by ultrasonic vibration 40-50min after conjunction, dry out solvent
It is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, 85-95 DEG C of heat preservation 25- is warming up to 6 DEG C/min heating rate
35min continues to be warming up to 520-540 DEG C of heat preservation 2.5-3.5h with 8 DEG C/min heating rate, then keeps atmosphere state until cold
But to room temperature to obtain the final product；Each raw material is parts by weight.
Preferably, in the preparation method, 35 DEG C of vacuum drying 10h.
Preferably, in the preparation method, sealing is fixed and is put into ball milling 38h in planetary ball mill.
Preferably, in the preparation method, ultrasonic vibration 30min.
Preferably, in the preparation method, ball milling 15h.
Preferably, in the preparation method, H2Percent by volume be 3%.
Preferably, in the preparation method, mixed gas flow 350mL/min.
Preferably, in the preparation method, 480 DEG C of heat preservation 3h are risen to the heating rate of 8 DEG C/min.
Preferably, in the preparation method, 90 DEG C of heat preservation 30min are warming up to 6 DEG C/min heating rate.
Preferably, in the preparation method, 530 DEG C of heat preservation 3h are warming up to 8 DEG C/min heating rate.
The technology of the present invention effect：
This method is easy, quick, easy to operate, and the FePt/Co Nano composite granules of preparation are of uniform size, has excellent magnetic
Performance.
Specific embodiment
Essentiality content of the invention is specifically introduced below with reference to embodiment.
Embodiment 1
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：15 parts of NaCl are put into vacuum drying
In case, then 35 DEG C of vacuum drying 10h are poured into ball grinder together with 50 portions of normal heptanes, and sealing is fixed and is put into planetary ball mill
Ball milling 38h in machine；5 parts of platinum tetrachlorides are dissolved in 25 parts of acetone, 10 parts of ferric chloride hexahydrates are dissolved in 35 parts of ethyl alcohol, will be above two
Solution mixing, ultrasonic vibration 30min mix the above-mentioned solution mixed with NaCl powder, ball milling 15h, after ball milling again
Mixed-powder taking-up be put into baking oven 55 DEG C of drying, be put into silica crucible, be placed in tube furnace and calcined；Tube furnace needs
First lead to Ar air purge gas 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up, H2
Percent by volume be 3%, mixed gas flow 350mL/min, 480 DEG C of heat preservation 3h are risen to the heating rate of 8 DEG C/min,
Continue ventilation after heat preservation terminates until being cooled to room temperature, obtains black calcined product；85 are added into black calcined product
Part deionized water stands 48h and waits for that suspended matter sinks to beaker bottom completely, removes supernatant, remaining liq is then put into centrifugation
It is separated in machine, continues to wash away NaCl, be repeated 6 times, obtain FePt nano particle；10 parts are added to FePt obtained above
CoCl2·6H2Sheet output is ground and pours into aluminium oxide earthenware at powder by O, ultrasonic vibration 45min after the two mixing, dry out solvent
In crucible, then crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, is warming up to 6 DEG C/min heating rate
90 DEG C of heat preservation 30min continue to be warming up to 530 DEG C of heat preservation 3h with 8 DEG C/min heating rate, then keep atmosphere state until cooling
To room temperature to obtain the final product；Each raw material is parts by weight.
Embodiment 2
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：10 parts of NaCl are put into vacuum drying
In case, then 30 DEG C of vacuum drying 9h are poured into ball grinder together with 45 portions of normal heptanes, and sealing is fixed and is put into planetary ball mill
Middle ball milling 37h；4 parts of platinum tetrachlorides are dissolved in 20 parts of acetone, 7 parts of ferric chloride hexahydrates are dissolved in 30 parts of ethyl alcohol, will be above two molten
Liquid mixing, ultrasonic vibration 25min mix the above-mentioned solution mixed with NaCl powder, ball milling 14h, after ball milling again
Mixed-powder taking-up is put into 50 DEG C of drying in baking oven, is put into silica crucible, is placed in tube furnace and is calcined；Tube furnace needs elder generation
Lead to Ar air purge gas 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up, H2's
Percent by volume is 2%, mixed gas flow 340mL/min, rises to 470 DEG C of heat preservation 2.5h with the heating rate of 8 DEG C/min,
Continue ventilation after heat preservation terminates until being cooled to room temperature, obtains black calcined product；80 are added into black calcined product
Part deionized water stands 47h and waits for that suspended matter sinks to beaker bottom completely, removes supernatant, remaining liq is then put into centrifugation
It is separated in machine, continues to wash away NaCl, be repeated 5 times, obtain FePt nano particle；5 parts of CoCl are added to FePt obtained above2·
6H2Sheet output is ground and is poured into alumina crucible at powder, so by O, ultrasonic vibration 40min after the two mixing, dry out solvent
Crucible is put into tube furnace afterwards, high-purity Ar gas is led into furnace, gas washing 3 times, 85 DEG C of heat preservations are warming up to 6 DEG C/min heating rate
25min continues to be warming up to 520 DEG C of heat preservation 2.5h with 8 DEG C/min heating rate, then keeps atmosphere state until being cooled to room temperature
To obtain the final product；Each raw material is parts by weight.
Embodiment 3
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：20 parts of NaCl are put into vacuum drying
In case, then 40 DEG C of vacuum drying 11h are poured into ball grinder together with 55 portions of normal heptanes, and sealing is fixed and is put into planetary ball mill
Ball milling 39h in machine；6 parts of platinum tetrachlorides are dissolved in 30 parts of acetone, 13 parts of ferric chloride hexahydrates are dissolved in 40 parts of ethyl alcohol, will be above two
Solution mixing, ultrasonic vibration 35min mix the above-mentioned solution mixed with NaCl powder, ball milling 16h, after ball milling again
Mixed-powder taking-up be put into baking oven 60 DEG C of drying, be put into silica crucible, be placed in tube furnace and calcined；Tube furnace needs
First lead to Ar air purge gas 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up, H2
Percent by volume be 4%, mixed gas flow 360mL/min, 490 DEG C of heat preservations are risen to the heating rate of 8 DEG C/min
3.5h continues ventilation until being cooled to room temperature after heat preservation terminates, obtains black calcined product；Add into black calcined product
Enter 90 parts of deionized waters, stands 49h and wait for that suspended matter sinks to beaker bottom completely, remove supernatant, be then put into remaining liq
It is separated in centrifuge, continues to wash away NaCl, be repeated 7 times, obtain FePt nano particle；15 parts are added to FePt obtained above
CoCl2·6H2Sheet output is ground and pours into aluminium oxide earthenware at powder by O, ultrasonic vibration 50min after the two mixing, dry out solvent
In crucible, then crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, is warming up to 6 DEG C/min heating rate
95 DEG C of heat preservation 35min continue to be warming up to 540 DEG C of heat preservation 3.5h with 8 DEG C/min heating rate, then keep atmosphere state until cold
But to room temperature to obtain the final product；Each raw material is parts by weight.
Embodiment 4
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：12 parts of NaCl are put into vacuum drying
In case, then 31 DEG C of vacuum drying 10.5h are poured into ball grinder together with 46 portions of normal heptanes, and sealing is fixed and is put into planet ball
Ball milling 37.5h in grinding machine；4.5 parts of platinum tetrachlorides are dissolved in 21 parts of acetone, 8 parts of ferric chloride hexahydrates are dissolved in 31 parts of ethyl alcohol, will be upper
Two kinds of solution mixing are stated, ultrasonic vibration 26min mixes the above-mentioned solution mixed with NaCl powder, ball milling 14.5h again,
Mixed-powder taking-up after ball milling is put into 51 DEG C of drying in baking oven, is put into silica crucible, is placed in tube furnace and is calcined；
Tube furnace need to first lead to Ar air purge gas 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of open
Begin to heat up, H2Percent by volume be 2%, mixed gas flow 342mL/min, rise to 472 with the heating rate of 8 DEG C/min
DEG C heat preservation 2.6h, continues ventilation until being cooled to room temperature after heat preservation terminates, obtains black calcined product；It calcines and produces to black
82 parts of deionized waters are added in object, stands 47.5h and waits for that suspended matter sinks to beaker bottom completely, remove supernatant, it then will be remaining
Liquid puts into a centrifuge separation, continues to wash away NaCl, be repeated 5 times, and obtains FePt nano particle；Add to FePt obtained above
Enter 6 parts of CoCl2·6H2Sheet output is ground and pours into oxidation at powder by O, ultrasonic vibration 42min after the two mixing, dry out solvent
In aluminium crucible, then crucible is put into tube furnace, the logical high-purity Ar gas into furnace, gas washing 3 times, with 6 DEG C/min heating rate liter
Temperature continues to be warming up to 522 DEG C of heat preservation 2.7h with 8 DEG C/min heating rate, then keeps atmosphere state straight to 86 DEG C of heat preservation 26min
To being cooled to room temperature to obtain the final product；Each raw material is parts by weight.
Embodiment 5
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：14 parts of NaCl are put into vacuum drying
In case, then 32 DEG C of vacuum drying 9.5h are poured into ball grinder together with 48 portions of normal heptanes, and sealing is fixed and is put into planetary ball mill
Ball milling 38h in machine；5 parts of platinum tetrachlorides are dissolved in 24 parts of acetone, 9 parts of ferric chloride hexahydrates are dissolved in 34 parts of ethyl alcohol, will be above two
Solution mixing, ultrasonic vibration 28min mix the above-mentioned solution mixed with NaCl powder, ball milling 14h, after ball milling again
Mixed-powder taking-up be put into baking oven 52 DEG C of drying, be put into silica crucible, be placed in tube furnace and calcined；Tube furnace needs
First lead to Ar air purge gas 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up, H2
Percent by volume be 2.5%, mixed gas flow 344mL/min, 475 DEG C of heat preservations are risen to the heating rate of 8 DEG C/min
2.8h continues ventilation until being cooled to room temperature after heat preservation terminates, obtains black calcined product；Add into black calcined product
Enter 84 parts of deionized waters, stands 48.5h and wait for that suspended matter sinks to beaker bottom completely, remove supernatant, then put remaining liq
Enter in centrifuge and separate, continue to wash away NaCl, be repeated 7 times, obtains FePt nano particle；8 parts are added to FePt obtained above
CoCl2·6H2Sheet output is ground and pours into aluminium oxide earthenware at powder by O, ultrasonic vibration 44min after the two mixing, dry out solvent
In crucible, then crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, is warming up to 6 DEG C/min heating rate
88 DEG C of heat preservation 28min continue to be warming up to 524 DEG C of heat preservation 2.8h with 8 DEG C/min heating rate, then keep atmosphere state until cold
But to room temperature to obtain the final product；Each raw material is parts by weight.
Embodiment 6
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：16 parts of NaCl are put into vacuum drying
In case, then 33 DEG C of vacuum drying 9h are poured into ball grinder together with 51 portions of normal heptanes, and sealing is fixed and is put into planetary ball mill
Middle ball milling 37h；5.5 parts of platinum tetrachlorides are dissolved in 26 parts of acetone, 10 parts of ferric chloride hexahydrates are dissolved in 36 parts of ethyl alcohol, will be above two
Solution mixing, ultrasonic vibration 32min mix the above-mentioned solution mixed with NaCl powder, ball milling 15.5h, by ball milling again
Mixed-powder taking-up afterwards is put into 54 DEG C of drying in baking oven, is put into silica crucible, is placed in tube furnace and is calcined；Tube furnace
Ar air purge gas need to first be led to 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up,
H2Percent by volume be 3%, mixed gas flow 346mL/min, 482 DEG C of heat preservations are risen to the heating rate of 8 DEG C/min
3.1h continues ventilation until being cooled to room temperature after heat preservation terminates, obtains black calcined product；Add into black calcined product
Enter 86 parts of deionized waters, stands 47h and wait for that suspended matter sinks to beaker bottom completely, remove supernatant, be then put into remaining liq
It is separated in centrifuge, continues to wash away NaCl, be repeated 5 times, obtain FePt nano particle；11 parts are added to FePt obtained above
CoCl2·6H2Sheet output is ground and pours into aluminium oxide earthenware at powder by O, ultrasonic vibration 46min after the two mixing, dry out solvent
In crucible, then crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, is warming up to 6 DEG C/min heating rate
92 DEG C of heat preservation 31min continue to be warming up to 526 DEG C of heat preservation 3.1h with 8 DEG C/min heating rate, then keep atmosphere state until cold
But to room temperature to obtain the final product；Each raw material is parts by weight.
Embodiment 7
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：18 parts of NaCl are put into vacuum drying
In case, then 36 DEG C of vacuum drying 10h are poured into ball grinder together with 52 portions of normal heptanes, and sealing is fixed and is put into planetary ball mill
Ball milling 38.5h in machine；4 parts of platinum tetrachlorides are dissolved in 27 parts of acetone, 11 parts of ferric chloride hexahydrates are dissolved in 37 parts of ethyl alcohol, by above-mentioned two
Kind solution mixing, ultrasonic vibration 33min mix the above-mentioned solution mixed with NaCl powder, ball milling 16h, by ball milling again
Mixed-powder taking-up afterwards is put into 56 DEG C of drying in baking oven, is put into silica crucible, is placed in tube furnace and is calcined；Tube furnace
Ar air purge gas need to first be led to 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up,
H2Percent by volume be 3.5%, mixed gas flow 352mL/min, 485 DEG C of guarantors are risen to the heating rate of 8 DEG C/min
Warm 3.2h continues ventilation until being cooled to room temperature after heat preservation terminates, obtains black calcined product；Into black calcined product
88 parts of deionized waters are added, stands 48h and waits for that suspended matter sinks to beaker bottom completely, remove supernatant, then put remaining liq
Enter in centrifuge and separate, continue to wash away NaCl, be repeated 6 times, obtains FePt nano particle；12 parts are added to FePt obtained above
CoCl2·6H2Sheet output is ground and pours into aluminium oxide earthenware at powder by O, ultrasonic vibration 48min after the two mixing, dry out solvent
In crucible, then crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, is warming up to 6 DEG C/min heating rate
93 DEG C of heat preservation 32min continue to be warming up to 532 DEG C of heat preservation 3.2h with 8 DEG C/min heating rate, then keep atmosphere state until cold
But to room temperature to obtain the final product；Each raw material is parts by weight.
Embodiment 8
A kind of preparation method of FePt/Co Nano composite granules, includes the following steps：19 parts of NaCl are put into vacuum drying
In case, then 38 DEG C of vacuum drying 10.5h are poured into ball grinder together with 54 portions of normal heptanes, and sealing is fixed and is put into planet ball
Ball milling 39h in grinding machine；6 parts of platinum tetrachlorides are dissolved in 28 parts of acetone, 12 parts of ferric chloride hexahydrates are dissolved in 38 parts of ethyl alcohol, by above-mentioned two
Kind solution mixing, ultrasonic vibration 34min mix the above-mentioned solution mixed with NaCl powder, ball milling 15h, by ball milling again
Mixed-powder taking-up afterwards is put into 58 DEG C of drying in baking oven, is put into silica crucible, is placed in tube furnace and is calcined；Tube furnace
Ar air purge gas need to first be led to 3 times to exclude the air in furnace, then in Ar and H2Mixed flow gas under conditions of start to warm up,
H2Percent by volume be 4%, mixed gas flow 355mL/min, 488 DEG C of heat preservations are risen to the heating rate of 8 DEG C/min
3.4h continues ventilation until being cooled to room temperature after heat preservation terminates, obtains black calcined product；Add into black calcined product
Enter 89 parts of deionized waters, stands 49h and wait for that suspended matter sinks to beaker bottom completely, remove supernatant, be then put into remaining liq
It is separated in centrifuge, continues to wash away NaCl, be repeated 7 times, obtain FePt nano particle；14 parts are added to FePt obtained above
CoCl2·6H2Sheet output is ground and pours into aluminium oxide earthenware at powder by O, ultrasonic vibration 49min after the two mixing, dry out solvent
In crucible, then crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, is warming up to 6 DEG C/min heating rate
94 DEG C of heat preservation 34min continue to be warming up to 535 DEG C of heat preservation 3.4h with 8 DEG C/min heating rate, then keep atmosphere state until cold
But to room temperature to obtain the final product；Each raw material is parts by weight.
This method is easy, quick, easy to operate, and the FePt/Co Nano composite granules of preparation are of uniform size, has excellent magnetic
Performance.
Claims (10)
1. a kind of preparation method of FePt/Co Nano composite granules, it is characterised in that include the following steps：By 10-20 parts of NaCl
It is put into vacuum oven, then 30-40 DEG C of vacuum drying 9-11h is poured into ball grinder together with 45-55 portions of normal heptanes, close
Sealing is determined and is put into ball milling 37-39h in planetary ball mill；4-6 parts of platinum tetrachlorides are dissolved in 20-30 parts of acetone, six water of 7-13 part
Close iron chloride be dissolved in 30-40 parts of ethyl alcohol, above two solution is mixed, ultrasonic vibration 25-35min, by it is above-mentioned mix it is molten
Liquid mixes again with NaCl powder, ball milling 14-16h, and the mixed-powder taking-up after ball milling is put into 50-60 DEG C of drying in baking oven,
It is put into silica crucible, is placed in tube furnace and is calcined；Tube furnace need to first lead to Ar air purge gas 3 times to exclude the air in furnace,
Then in Ar and H2Mixed flow gas under conditions of start to warm up, H2Percent by volume be 2%-4%, mixed gas stream
Amount is 340-360mL/min, 470-490 DEG C of heat preservation 2.5-3.5h is risen to the heating rate of 8 DEG C/min, after heat preservation terminates
Continue ventilation until being cooled to room temperature, obtains black calcined product；80-90 parts of deionized waters are added into black calcined product,
It stands 47-49h and waits for that suspended matter sinks to beaker bottom completely, remove supernatant, remaining liq is then put into a centrifuge into separation,
Continue to wash away NaCl, repeats 5-7 times, obtain FePt nano particle；5-15 parts of CoCl are added to FePt obtained above2·6H2O,
Sheet output is ground and is poured into alumina crucible at powder, then by ultrasonic vibration 40-50min after the two mixing, dry out solvent
Crucible is put into tube furnace, high-purity Ar gas is led into furnace, gas washing 3 times, 85-95 DEG C of guarantor is warming up to 6 DEG C/min heating rate
Warm 25-35min continues to be warming up to 520-540 DEG C of heat preservation 2.5-3.5h with 8 DEG C/min heating rate, then keeps atmosphere state
Until being cooled to room temperature to obtain the final product；Each raw material is parts by weight.
2. preparation method according to claim 1, it is characterised in that：35 DEG C of vacuum drying 10h.
3. preparation method according to claim 1, it is characterised in that：Sealing is fixed and is put into ball milling in planetary ball mill
38h。
4. preparation method according to claim 1, it is characterised in that：Ultrasonic vibration 30min.
5. preparation method according to claim 1, it is characterised in that：Ball milling 15h.
6. preparation method according to claim 1, it is characterised in that：H2Percent by volume be 3%.
7. preparation method according to claim 1, it is characterised in that：Mixed gas flow is 350mL/min.
8. preparation method according to claim 1, it is characterised in that：480 DEG C of heat preservations are risen to the heating rate of 8 DEG C/min
3h。
9. preparation method according to claim 1, it is characterised in that：90 DEG C of heat preservations are warming up to 6 DEG C/min heating rate
30min。
10. preparation method according to claim 1, it is characterised in that：530 DEG C of guarantors are warming up to 8 DEG C/min heating rate
Warm 3h.
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| CN201810771986.0A CN108817412A (en) | 2018-07-13 | 2018-07-13 | A kind of preparation method of FePt/Co Nano composite granules |
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| CN201810771986.0A Withdrawn CN108817412A (en) | 2018-07-13 | 2018-07-13 | A kind of preparation method of FePt/Co Nano composite granules |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109604628A (en) * | 2019-02-01 | 2019-04-12 | 东南大学 | A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle |
| CN110202166A (en) * | 2019-06-24 | 2019-09-06 | 东北大学 | The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle |
-
2018
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109604628A (en) * | 2019-02-01 | 2019-04-12 | 东南大学 | A kind of preparation method of ordered phase nanometer Fe-Pt particle and cobalt platinum nano particle |
| CN109604628B (en) * | 2019-02-01 | 2021-12-24 | 东南大学 | Preparation method of ordered phase iron platinum nano-particles and cobalt platinum nano-particles |
| CN110202166A (en) * | 2019-06-24 | 2019-09-06 | 东北大学 | The chemical method of liquid phase assisted Solid-state sintering synthesis fct-FePt nanoparticle |
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