CN104030673B - The ferritic preparation method of a kind of high-performance superfine NiZn - Google Patents
The ferritic preparation method of a kind of high-performance superfine NiZn Download PDFInfo
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- CN104030673B CN104030673B CN201410291401.7A CN201410291401A CN104030673B CN 104030673 B CN104030673 B CN 104030673B CN 201410291401 A CN201410291401 A CN 201410291401A CN 104030673 B CN104030673 B CN 104030673B
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- 229910003962 NiZn Inorganic materials 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000002485 combustion reaction Methods 0.000 claims abstract description 19
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 18
- 239000011780 sodium chloride Substances 0.000 claims abstract description 17
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000000376 reactant Substances 0.000 claims abstract description 8
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 7
- 238000009413 insulation Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 206010013786 Dry skin Diseases 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims abstract 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- -1 soaks 12 ~ 24 hours Chemical compound 0.000 abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000005415 magnetization Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000005049 combustion synthesis Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002902 ferrimagnetic material Substances 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Abstract
The ferritic preparation method of a kind of high-performance superfine NiZn, the mol ratio first calculating reactant feed is Ni:Zn=0.4: 0.6, gets Fe, ZnO, NiO, Fe
2o
3and NaClO
4as raw material, wherein Fe, Fe
2o
3and NaClO
4mol ratio be 2k: (1-k): 0.75k, 0.5 < k < 1; Then reaction mass is loaded ball milling in ball mill; Make round pie blank at the pressure of 15MPa, put detonator at blank end face; Cause the material generation combustion reactions that it closes on, discharge a large amount of heat, close heater switch immediately, combustion reactions proceeds until material total overall reaction simultaneously; Afterfire obtains NiZnFe after terminating again
2o
4with the mixture of NaCl, products of combustion is pulverized after stove is cooled to room temperature, then adds distilled water, soaks 12 ~ 24 hours, NaCl impurity is dissolved in distilled water completely, filtering and washing, and circulate 6 times, then product is 110 DEG C of dryings; Finally by the NiZnFe of synthesis
2o
4powder at 1050 DEG C of insulation 2h with the temperature rise rate of 300 DEG C/h, is cooled to room temperature and can obtains NiZn ferrite powder.
Description
Technical field
The present invention relates to synthesis NiZnFe
2o
4the method of superfine powder, is applicable to ultra-fine NiZnFe
2o
4the suitability for industrialized production of powder.
Background technology
NiZn ferrite belongs to ferrimagnetic material, because it has higher resistivity, and high frequency stability and higher saturation magnetization and lower coercive force and eddy-current loss and in magnetic electronic technology, have application widely.At present, along with the development of global electronic information industry, the ferritic main Main Trends of The Development of NiZn is high frequency, miniaturization and slimming, for national defence, the field such as electronics and medical science is to transformer, inducer, the miniaturization of reactance coil and other electromagnetic element, the requirement of lightness and slimming, to ferrite researchdevelopment to ultra-fine or nm regime.
At present, the preparation method of ultra-fine NiZn ferrite powder mainly contains traditional conventional ceramic technique, but due to the sintering activity of raw material not high, the lack of homogeneity of mixing, product performance are not high, can not meet the demand of socio-economic development; Though it is higher that sol-gel method and chemical coprecipitation can obtain purity, the product of better performances, because its preparation cost is higher, a series of reasons such as equipment is complicated can not realize scale operation.The NiZn ferrite prepared with combustion synthesis method is compared with traditional technique, there is energy consumption low, generated time is short, product purity is high, powder diameter is evenly distributed, and production efficiency is high, easily obtains metastable phase in products of combustion simultaneously, there is good sintering activity, and the maximum feature of conbustion synthesis utilizes the chemical energy of reactant inside to carry out synthetic materials.Once lighting, react self―sustaining at once, generally not in supplementing energy.At present, although to adopt combustion synthesis method to synthesize purity higher for researchers, evengranular ferrite powder, its synthesis technique is not but suitable for suitability for industrialized production, and the performance of ferrite powder also awaits improving.
Summary of the invention
The object of this invention is to provide the ferritic preparation method of a kind of high-performance superfine NiZn.
The present invention is the ferritic preparation method of a kind of high-performance superfine NiZn, the steps include:
(1) mol ratio calculating reactant feed is Ni:Zn=0.4: 0.6, gets Fe, ZnO, NiO, Fe
2o
3and NaClO
4as raw material, wherein Fe, Fe
2o
3and NaClO
4mol ratio be 2k: (1-k): 0.75k, 0.5 < k < 1;
(2) load weighted reaction mass is loaded in ball grinder, then ball grinder is placed in ball mill ball milling;
(3) material mixed is positioned in mould, makes round pie blank at the pressure of 15MPa, blank is put into autoclave, put detonator at blank end face; During room temperature, in reactor, be filled with argon gas to pressure is 0.5MPa, 10min final vacuum is heated, being filled with argon gas to pressure after being again vented when temperature of reaction kettle rises to 180 DEG C is 2MPa, and insulation 30min continues heating, detonator burning when question response temperature in the kettle rises to 250 DEG C, cause the material generation combustion reactions that it closes on, discharge a large amount of heat, close heater switch immediately, combustion reactions proceeds until material total overall reaction simultaneously;
(4) burning obtains NiZnFe after terminating
2o
4with the mixture of NaCl, products of combustion is pulverized cool to room temperature with the furnace under argon shield after, then adds distilled water, soak 12 ~ 24 hours, NaCl impurity is dissolved in distilled water completely, filtering and washing, suction filtration again, circulates 6 times, and then product was at 110 DEG C of dry 3-5 hours;
(5) by the NiZnFe of synthesis
2o
4powder at 1050 DEG C of insulation 2h with the temperature rise rate of 300 DEG C/h, is cooled to room temperature and can obtains the NiZnFe after annealing
2o
4powder.
NaCl is used for the ferritic preparation of NiZn as thinner by the present invention first, and its usefulness is: 1. because NaCl has larger solubleness, just can effectively be removed by washing; 2. add thinner NaCl and can mention NiZn ferrite degree of crystallinity, make pattern approximate rule spherical; 3. amount of diluent increase can reduce the ferritic particle size of NiZn; 4. the ferritic saturation magnetization of NiZn is with the increase first increases and then decreases of thinner consumption, and maximum value is 63.07emu/g.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of NiZn ferrite powder, and Fig. 2 is the ferritic scanning electron microscope diagram sheet of NiZn, and Fig. 3 is the magnetic hysteresis loop figure of NiZn iron oxygen.
Embodiment
The present invention is the ferritic preparation method of high-performance superfine NiZn, the steps include:
(1) mol ratio calculating reactant feed is Ni:Zn=0.4: 0.6, gets Fe, ZnO, NiO, Fe
2o
3and NaClO
4as raw material, wherein Fe, Fe
2o
3and NaClO
4mol ratio be 2k: (1-k): 0.75k, 0.5 < k < 1;
(2) load weighted reaction mass is loaded in ball grinder, then ball grinder is placed in ball mill ball milling;
(3) material mixed is positioned in mould, makes round pie blank at the pressure of 15MPa, blank is put into autoclave, put detonator at blank end face; During room temperature, in reactor, be filled with argon gas to pressure is 0.5MPa, 10min final vacuum is heated, being filled with argon gas to pressure after being again vented when temperature of reaction kettle rises to 180 DEG C is 2MPa, and insulation 30min continues heating, detonator burning when question response temperature in the kettle rises to 250 DEG C, cause the material generation combustion reactions that it closes on, discharge a large amount of heat, close heater switch immediately, combustion reactions proceeds until material total overall reaction simultaneously;
(4) burning obtains NiZnFe after terminating
2o
4with the mixture of NaCl, products of combustion is pulverized cool to room temperature with the furnace under argon shield after, then adds distilled water, soak 12 ~ 24 hours, NaCl impurity is dissolved in distilled water completely, filtering and washing, suction filtration again, circulates 6 times, and then product was at 110 DEG C of dry 3-5 hours;
(5) by the NiZnFe of synthesis
2o
4powder at 1050 DEG C of insulation 2h with the temperature rise rate of 300 DEG C/h, is cooled to room temperature and can obtains the NiZnFe after annealing
2o
4powder.
According to above-described preparation method, ball mill is planetary ball mill.
According to above-described preparation method, the ball milling parameter of setting is: ratio of grinding media to material 2: 1, drum's speed of rotation 150r/min, and Ball-milling Time is 8h, and ball mill mode of operation is for rotating forward 600s, and shut down 60s, then reverse 600s, shuts down 60s, and so ball milling is carried out in circulation.
According to above-described preparation method, the diameter of the round pie blank made at the pressure of 15MPa is 5.0cm, and highly, or thickness is 1.0cm.
According to above-described preparation method, it is characterized in that the thinner used is sodium-chlor.
The present invention is launched further below by more specifically embodiment.
Embodiment 1
Be 1500g(k=0.5 by quality) reactant compound in add the thinner NaCl of 9wt% after mixing put into planetary ball mill ball milling; arranging ball milling parameter is: ratio of grinding media to material 2:1; drum's speed of rotation 150r/min; Ball-milling Time is 10h; ball mill mode of operation is for rotating forward 600s, and shut down 60s, then reverse 600s; shut down 60s, so circulate.The pressure of the sample powder 15MPa after ball milling is made diameter to be 5.0cm, to be highly the blank of 1.0cm, blank is put into autoclave and carry out combustion reactions, after burning terminates, obtain NiZnFe
2o
4with the mixture of NaCl, material after combustion reactions is pulverized, add distilled water, soak 12-24 hour, NaCl impurity is dissolved in distilled water completely, and filtering and washing, at suction filtration, circulate 6 times, then obtained NiZn ferrite powder with 110 DEG C by the dry materials 3-5 after washing hour in an oven.Record the saturation magnetization Ms=58.23 emu/g of NiZn ferrite powder synthesized when amount of diluent is 9wt%, coercivity H=16.58 Oe, residual magnetization Mr=2.27 emu/g.
Embodiment 2:
Be 1500g(k=0.7 by quality) reaction mixture material put into planetary ball mill ball milling; arranging ball milling parameter is: ratio of grinding media to material 2:1; drum's speed of rotation 150r/min; Ball-milling Time is 10h; ball mill mode of operation is for rotating forward 600s, and shut down 60s, then reverse 600s; shut down 60s, so circulate.The pressure of the sample powder 15MPa after ball milling is made diameter to be 5.0cm, to be highly the blank of 1.0cm, blank is put into autoclave and carry out combustion reactions, after burning terminates, obtain NiZnFe
2o
4with the mixture of NaCl, the material after combustion reactions is pulverized, adds distilled water, soak 12-24 hour, NaCl impurity is dissolved in distilled water completely, filtering and washing, suction filtration again, circulates 6 times, and then washed product obtained NiZn ferrite powder at 110 DEG C of dry 3-5 hours.Record the saturation magnetization Ms=65.90 emu/g of NiZn ferrite powder synthesized when reactant quality is 1500g, coercivity H=20.5 Oe, residual magnetization Mr=3.01 emu/g.
Embodiment 3:
Be 1500g(k=1 by quality) reaction mixture material put into planetary ball mill ball milling; arranging ball milling parameter is: ratio of grinding media to material 2:1; drum's speed of rotation 150r/min; Ball-milling Time is 10h; ball mill mode of operation is for rotating forward 600s, and shut down 60s, then reverse 600s; shut down 60s, so circulate.The pressure of the sample powder 15MPa after ball milling is made diameter to be 5.0cm, to be highly the blank of 1.0cm, blank is put into autoclave and carry out combustion reactions, after burning terminates, obtain NiZnFe
2o
4with the mixture of NaCl, the material after combustion reactions is pulverized, adds distilled water, soak 12-24 hour, NaCl impurity is dissolved in distilled water completely, filtering and washing, suction filtration again, circulates 6 times, and then washed product obtained NiZn ferrite powder at 110 DEG C of dry 3-5 hours.Record the saturation magnetization Ms=64.95 emu/g of NiZn ferrite powder synthesized when reactant quality is 1500g, coercivity H=21.26 Oe, residual magnetization Mr=4.32 emu/g.
Claims (1)
1. the ferritic preparation method of high-performance superfine NiZn, the steps include:
(1) mol ratio calculating reactant feed is Ni:Zn=0.4: 0.6, gets Fe, ZnO, NiO, Fe
2o
3and NaClO
4as raw material, wherein Fe, Fe
2o
3and NaClO
4mol ratio be 2k: (1-k): 0.75k, 0.5 < k < 1;
(2) load weighted reaction mass is loaded in ball grinder, then ball grinder is placed in planetary ball mill and carries out ball milling; Ball milling parameter is set to: ratio of grinding media to material 2: 1, drum's speed of rotation 150r/min, and Ball-milling Time is 8h, and ball mill mode of operation is for rotating forward 600s, and shut down 60s, then reverse 600s, shuts down 60s, and so ball milling is carried out in circulation;
(3) material mixed is positioned in mould, at the pressure of the 15MPa round pie blank that to make diameter be 5.0cm, highly (thickness) is 1.0cm, blank is put into autoclave, puts detonator at blank end face; During room temperature, in reactor, be filled with argon gas to pressure is 0.5MPa, 10min final vacuum is heated, being filled with argon gas to pressure after being again vented when temperature of reaction kettle rises to 180 DEG C is 2MPa, and insulation 30min continues heating, detonator burning when question response temperature in the kettle rises to 250 DEG C, cause the material generation combustion reactions that it closes on, discharge a large amount of heat, close heater switch immediately, combustion reactions proceeds until material total overall reaction simultaneously;
(4) burning obtains the mixture of NiZn ferrite and NaCl after terminating, and products of combustion is pulverized cool to room temperature with the furnace under argon shield after, distilled water washing, suction filtration, washing, suction filtration, and circulate 6 times, then product is 110 DEG C of dryings;
(5) by synthesis NiZn ferrite powder 1050 DEG C of anneal, insulation 2h, be cooled to room temperature can obtain anneal after NiZn ferrite powder.
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