CN1065836C - Technology for preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method - Google Patents
Technology for preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method Download PDFInfo
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- CN1065836C CN1065836C CN98117768A CN98117768A CN1065836C CN 1065836 C CN1065836 C CN 1065836C CN 98117768 A CN98117768 A CN 98117768A CN 98117768 A CN98117768 A CN 98117768A CN 1065836 C CN1065836 C CN 1065836C
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- high activity
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- 239000000843 powder Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000000694 effects Effects 0.000 title claims abstract description 11
- 230000005293 ferrimagnetic effect Effects 0.000 title claims description 7
- 238000005516 engineering process Methods 0.000 title description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 239000012266 salt solution Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 35
- 238000002360 preparation method Methods 0.000 claims description 17
- 230000002269 spontaneous effect Effects 0.000 claims description 10
- 238000002485 combustion reaction Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- YSXLJTGZMRNQSG-UHFFFAOYSA-L disodium;6-amino-5-[[2-[4-[2-[4-[2-[(2-amino-5-sulfonatonaphthalen-1-yl)diazenyl]phenyl]sulfonyloxyphenyl]propan-2-yl]phenoxy]sulfonylphenyl]diazenyl]naphthalene-1-sulfonate Chemical compound [Na+].[Na+].C1=CC=C2C(N=NC3=CC=CC=C3S(=O)(=O)OC3=CC=C(C=C3)C(C)(C=3C=CC(OS(=O)(=O)C=4C(=CC=CC=4)N=NC=4C5=CC=CC(=C5C=CC=4N)S([O-])(=O)=O)=CC=3)C)=C(N)C=CC2=C1S([O-])(=O)=O YSXLJTGZMRNQSG-UHFFFAOYSA-L 0.000 claims description 6
- 239000012456 homogeneous solution Substances 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 17
- 238000005245 sintering Methods 0.000 description 12
- 239000011701 zinc Substances 0.000 description 10
- 230000035699 permeability Effects 0.000 description 6
- 238000005469 granulation Methods 0.000 description 5
- 230000003179 granulation Effects 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 238000009766 low-temperature sintering Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 3
- 229910001864 baryta Inorganic materials 0.000 description 3
- 238000009841 combustion method Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- -1 Xiao Suangu Chemical compound 0.000 description 1
- 229910007565 Zn—Cu Inorganic materials 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- QXOLLBTXUCQAEQ-UHFFFAOYSA-N cobalt;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Co].OC(=O)CC(O)(C(O)=O)CC(O)=O QXOLLBTXUCQAEQ-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000035922 thirst Effects 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
Images
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- Compounds Of Iron (AREA)
- Soft Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
The present invention relates to a process for preparing the high activity superfine powder of plane hexagonal structural soft magnetic ferrite by a gel method, which comprises the steps that the salt solutions of raw materials are first mixed according to a stoichiometric ratio to be stirred; then, citric acid is added into the salt solutions to be heated to a certain temperature; ammonia water is added into the salt solutions, and the salt solutions are in neutrality to be dried; absolute alcohol is poured to be ignited, and the superfine powder of soft magnetic ferrite is formed. The particles of the powder which is prepared are thin, and have little agglomeration and high chemical activity. New production equipment does not need to be invested.
Description
The present invention relates to a kind of method of preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method, belong to electronic devices and components novel material, novel method field.
Growing along with the SMT technology, more and more higher to the performance requriements of SMD element, cost is but more and more lower.As one of important composition element of SMD element, the development trend of chip inductor also is like this.Soft magnetic ferrite is a main raw of making chip inductor, for reducing the cost of components and parts, can only select to reduce sintering temperature and less expensive inner electrode at present.Ag or Ag-Pd alloy electrode are the most frequently used cheap inner electrodes, but its fusing point is no more than 961 ℃, for the co-sintering of realizing soft magnetic ferrite and low melting point inner electrode with prevent that Ag from spreading to element internal, final sintering temperature that must the reduction chip inductor.
Middle and high frequency Ni-Zn-Cu soft magnetic ferrite commonly used is successfully realized the low-temperature sintering of chip inductor and is applied to producing by preparation ultrafine high activity powder.But the hexaplanar that is applicable to VHF band is Co
2Z (Ba
3Co
2Fe
24O
41) the type soft magnetic ferrite, because the complicacy of this body structure and composition, fail to realize low-temperature sintering always.Along with the high speed development of ICT (information and communication technology), more and more higher to the performance requriements of chip inductor, people thirst for realizing Co more and more urgently
2Z-iron oxysome low-temperature sintering and with corresponding inductance product release in market.
The objective of the invention is to propose a kind of method of preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method, set about from the chemical kinetics angle, utilize new softening method synthetic method, it is gel spontaneous combustion method, prepare plane hexagonal Z type structure ultrafine high activity ferrite powder, utilize this powder to synthesize Co in lower sintering temperature
2Z type and Zn, Cu doping vario-property ferrite, compare with traditional oxide high-temperature sintering method, the ferrite sintered The grain size of gel spontaneous combustion method is little and even, the density height of material after the low-temperature sintering, procedure is simple relatively, and the inductance component over-all properties of making is also very good.
The method of the preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method of the present invention's design is applicable to pure Co
2Z (Ba
3Co
2Fe
24O
41) and with Cu, Zn doping vario-property ferrite Co
2-x-yZn
xCu
yThe preparation of Z powder also is applicable to and uses Bi
2O
3Prepare corresponding powder as fusing assistant.
The method of preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method of the present invention, form by following each step:
(1) with the Fe of stoichiometric ratio
3+, Co
2+, Ba
2+, Zn
2+, Cu
2+Salt solution mix, stirring, form even brown clear solution;
(2) citric acid solution is slowly poured in the solution of (1) step preparation by mole ratio 1: 1-2, heated 40-90 ℃ and stirring, form homogeneous solution;
(3) ammoniacal liquor is slowly added in the solution of (2) step preparation, make it to mix fully, be neutral, make pH=6-8 until solution;
(4) solution with the preparation of (3) step places 80-150 ℃ baking oven to dry, until forming filemot xerogel;
(5) pour a small amount of dehydrated alcohol in the xerogel and ignite, afterwards, xerogel generation spontaneous combustion forms a kind of fluffy chocolate powder, is the soft magnetic ferrite high-active superfine powder.
The present invention adopts from the chemical kinetics angle, adopt softening method, prepared powder granule is thin, reunite less, the chemically reactive height, and need not invest new production unit, replace pre-burning with the gel spontaneous combustion, can obviously shorten the sintering time of ferrite sample, thereby improve labour productivity, significantly reduce the production cost of powder and inductor product.With pure Co
2Z is an example, can make sintering temperature reduce about 300 ℃, and crystal grain is evenly distributed the also not tangible decline of magnetic property; For Co
2-x-yZn
xCu
yThe Z ferrite adopts the present invention, can remove the pre-burning process from, and directly at sintering below 900 ℃, comprehensive magnetic property is also better than doping fusing assistant conventional ceramic technique.
Description of drawings:
Fig. 1 is the XRD spectrum after gel spontaneous combustion powder and differing temps (500 ℃, 700 ℃, 900 ℃) are handled.
Fig. 2 is the performance of gel spontaneous combustion method, soild oxide method sintered sample, and wherein μ i represents initial permeability, and Q represents quality factor.Dotted line A and solid line B represent that respectively gel method, soild oxide legal system are equipped with the performance curve of sample.
Introduce embodiments of the invention below.
Embodiment 1 (Ba
3Co
1.5Zn
0.3Cu
0.2Fe
24O
41):
Select for use analytically pure iron nitrate, nitrate of baryta, Cobaltous diacetate, zinc acetate, neutralized verdigris, citric acid, ammoniacal liquor and deionized water some.
(1) with the Fe of stoichiometric ratio
3+, Co
2+, Ba
2+, Zn
2+, Cu
2+Salt solution mix, stirring, form even brown clear solution;
(2) citric acid solution is slowly poured by mole ratio in the homogeneous solution of (1) step preparation at 1: 1.5, suitably heating (about 90 ℃) is also stirred, and forms homogeneous solution;
(3) ammoniacal liquor is slowly added in the solution of (2) step preparation, make it to mix fully, be neutral until solution, PH=7;
(4) solution with the preparation of (3) step places 90 ℃ baking oven to dry, until forming filemot xerogel;
(5) pour a small amount of dehydrated alcohol in the xerogel and ignite, afterwards, xerogel generation spontaneous combustion forms a kind of fluffy dark gray powder, can make Z-iron oxysome powder.
Go on foot the PVA solution (concentration 5%) that adds in the powder that makes about 6-10wt% toward aforementioned (5), granulation is pressed into the ring-type sample then, places 870-900 ℃ box-type furnace to calcine in sample, the initial permeability that records sample is 3.5, and sintered density is 4.91g/cm
3
Embodiment 2 (Ba
3Co
2Fe
24O
41):
Select analytically pure iron nitrate, nitrate of baryta, citric acid cobalt, citric acid, ammoniacal liquor and deionized water for use.
(1) with the Fe of stoichiometric ratio
3+, Co
2+, Ba
2+Salt solution mix, stirring, form even brown clear solution:
(2) citric acid solution is slowly poured by mole ratio in the solution of (1) step preparation at 1: 1.3, suitably heating (about 70 ℃) is also stirred, and forms homogeneous solution;
(3) ammoniacal liquor is slowly added in the solution of (2) step preparation, make it to mix fully, be neutral until solution, PH=7;
(4) solution with the preparation of (3) step places 120 ℃ baking oven to dry, until forming filemot xerogel;
(5) pour a small amount of dehydrated alcohol in the xerogel and ignite, afterwards, xerogel generation spontaneous combustion forms a kind of fluffy chocolate powder;
(6) for guaranteeing that Z-iron oxysome powder fully generates, can be with above-mentioned chocolate powder in 900 ℃ of directly calcinings.
Go on foot the PVA solution (concentration 5%) that adds in the powder that makes about 6-10wt% toward aforementioned (6), granulation is pressed into the ring-type sample then, places 1000 ℃ box-type furnace to calcine in sample, the initial permeability that records sample is 8.6, and sintered density is 4.80g/cm
3
Embodiment 3 (Ba
3Co
1.7Zn
0.3Fe
24O
41):
Select analytically pure iron nitrate, nitrate of baryta, Xiao Suangu, zinc nitrate, citric acid, ammoniacal liquor and deionized water for use.
(1) with the Fe of stoichiometric ratio
3+, Co
2+, Ba
2+, Zn
2+Nitrate solution mix, stir, form even brown clear solution;
(2) citric acid solution is slowly poured by mole ratio in the solution of (1) step preparation at 1: 1.2, suitably heating (about 70 ℃) is also stirred, and forms homogeneous solution;
(3) ammoniacal liquor is slowly added in the solution of (2) step preparation, make it to mix fully, be neutral until solution;
(4) solution with the preparation of (3) step places 120 ℃ baking oven to dry, until forming filemot xerogel;
(5) pour a small amount of dehydrated alcohol in the xerogel and ignite, afterwards, xerogel generation spontaneous combustion forms a kind of fluffy chocolate powder;
(6) for guaranteeing that Z-iron oxysome powder fully generates, can be with above-mentioned chocolate powder in 900 ℃ of directly calcinings.
Add the PVA solution (concentration 5%) about 8wt% in aforementioned (6) powder that makes of step, granulation is pressed into the ring-type sample then, places 1000 ℃ box-type furnace to calcine in sample, and the initial permeability that records sample is 10, and sintered density is 4.82g/cm
3
Comparative example 1 (Ba
3Co
2Fe
24O
41):
In order to compare with method of the present invention, adopt common solid oxide compound ferrite sintering process to prepare the ferrite ultrafine powder, take by weighing an amount of analytical pure material powder BaCO in molar ratio
3, Co
2O
3, Fe
2O
3, in ethanol, be that with the steel ball medium ball milling mixed 24 hours, 1200 ℃ of pre-burnings 3 hours in air, the PVA solution (concentration 8%) of adding 8%wt in the pre-burning powder, granulation, moulding, sintering in 1270 ℃ of air.The initial permeability that records sample is 10, and sintered density is 4.4g/cm
3
Comparative example 2 (Ba
3Co
1.5Zn
0.3Cu
0. 2Fe
24O
41):
Adopt common solid oxide compound ferrite sintering process, take by weighing an amount of analytical pure material powder BaCO in molar ratio
3, Co
2O
3, Fe
2O
3, ZnO, CuO, Bi
2O
3, in ethanol, being medium ball milling mixing 24 hours with the steel ball, (60 order) sieves after the oven dry; 1140 ℃ of pre-burnings 3 hours in air, add Bi afterwards
2O
3, ball milling is 48 hours again, and the oven dry back adds the PVA solution (concentration 5%) of 8%wt, granulation, moulding, sintering in 880 ℃ of air.The initial permeability that records sample is 2.5, and sintered density is 4.64g/cm
3
Claims (1)
1, a kind of method of preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method is characterized in that, is made up of following each step:
(1) with the Fe of stoichiometric ratio
3+, Co
2+, Ba
2+, Zn
2+, Cu
2+Salt solution mix, stirring, form even brown clear solution;
(2) citric acid solution is slowly poured in the solution of (1) step preparation by mole ratio 1: 1-2, heated 40-90 ℃ and stirring, form homogeneous solution;
(3) ammoniacal liquor is slowly added in the solution of (2) step preparation, make it to mix fully, be neutral, make PH=6-8 until solution;
(4) solution with the preparation of (3) step places 80-150 ℃ baking oven to dry, until forming filemot xerogel;
(5) pour a small amount of dehydrated alcohol in the xerogel and ignite, afterwards, xerogel generation spontaneous combustion forms a kind of fluffy chocolate powder, is the soft magnetic ferrite high-active superfine powder.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98117768A CN1065836C (en) | 1998-09-18 | 1998-09-18 | Technology for preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98117768A CN1065836C (en) | 1998-09-18 | 1998-09-18 | Technology for preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1212959A CN1212959A (en) | 1999-04-07 |
| CN1065836C true CN1065836C (en) | 2001-05-16 |
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ID=5225692
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|---|---|---|---|
| CN98117768A Expired - Fee Related CN1065836C (en) | 1998-09-18 | 1998-09-18 | Technology for preparing plane haxagon structural soft ferrimagnetics high activity superfine powder by gel method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408233C (en) * | 2006-08-23 | 2008-08-06 | 北京科技大学 | Magnetic field jel injection molding forming method for large scale rare earth aeolotropic binding magnet |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182044B (en) * | 2007-11-12 | 2010-06-02 | 浙江大学 | Method for preparing nano ferrite |
| KR101105595B1 (en) * | 2008-08-13 | 2012-01-18 | 주식회사 이엠따블유 | Manufacture method of ferrite |
| CN112679205B (en) * | 2020-12-29 | 2022-02-22 | 横店集团东磁股份有限公司 | Z-type ferrite and preparation method thereof |
| CN113968730B (en) * | 2021-11-11 | 2023-01-10 | 横店集团东磁股份有限公司 | Z-type ferrite composite material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5487878A (en) * | 1994-09-01 | 1996-01-30 | Oh; Young Jei | Method for preparing perpendicularly magnetizable material usable on magnetic recording media |
| CN1139648A (en) * | 1995-07-06 | 1997-01-08 | 南京理工大学 | Preparation method for ultra thin hexagonal crystal system ferrite |
-
1998
- 1998-09-18 CN CN98117768A patent/CN1065836C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5487878A (en) * | 1994-09-01 | 1996-01-30 | Oh; Young Jei | Method for preparing perpendicularly magnetizable material usable on magnetic recording media |
| CN1139648A (en) * | 1995-07-06 | 1997-01-08 | 南京理工大学 | Preparation method for ultra thin hexagonal crystal system ferrite |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100408233C (en) * | 2006-08-23 | 2008-08-06 | 北京科技大学 | Magnetic field jel injection molding forming method for large scale rare earth aeolotropic binding magnet |
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