CN102623124B - Be coated with phosphatic ferrite powder and preparation method thereof - Google Patents
Be coated with phosphatic ferrite powder and preparation method thereof Download PDFInfo
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- CN102623124B CN102623124B CN201110033855.0A CN201110033855A CN102623124B CN 102623124 B CN102623124 B CN 102623124B CN 201110033855 A CN201110033855 A CN 201110033855A CN 102623124 B CN102623124 B CN 102623124B
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Abstract
Be coated with phosphatic ferrite powder and preparation method thereof, be wherein coated with phosphatic ferrite powder and be applicable to as electromagnetic wave inhibiting material or manufacture magnetic conduction thin slice.This is coated with the phosphate on surface that phosphatic ferrite powder comprises ferrite powder and is coated on ferrite powder completely.And method comprises pulverizing ferrite to obtain ferrite powder; In phosphoric acid is water-soluble, ethanol or acetone, to prepare, there is the phosphoric acid solution that molarity is 0.2 to 1.0M; Ferrite powder to be placed in phosphoric acid solution and to stir 0.5 to 2 hour; Ferrite powder is filtered out, to obtain filtration ferrite powder by phosphoric acid solution; And in 250 DEG C to 500 DEG C to this filtration ferrite powder heating at least 5 minutes, make to filter ferrite powder dehydration, be coated with phosphatic ferrite powder to obtain.
Description
Technical field
The present invention relates to and be coated with phosphatic ferrite (Ferrite) powder and preparation method thereof, and in particular to being applicable to as electromagnetic wave inhibiting material or being coated with phosphatic ferrite powder and preparation method thereof for the manufacture of magnetic conduction thin slice.
Background technology
Along with the mankind are for the increase of demand carrying out exchanges data between every electronic product, simultaneously in order to avoid the inconvenience that the connection line used during swap data causes, therefore derive the demand for wireless telecommunications science and technology.But in wireless telecommunications, electronic product is easily subject to the electromagnetic interference needed for communication, and produces unnecessary noise in the circuit of electronic product, and then affects the performance of electronic product itself.
In the prior art, for suppressing electronic product to be subject to electromagnetic interference, the normal ferrite that uses makes ferrite bead, or utilizes ferrite powder and macromolecular material to make composite material, with as the electromagnetic wave inhibiting material stopping Electromagnetic Interference.In addition, also available iron ferrite powder and the composite material made by macromolecular material make magnetic conduction thin slice, use the metal interference overcome in radio-frequency communication.
The above is the application of Ferrite Material at high-frequency range.But, when ferrite application is in high-frequency range, often there is the problem that insulating properties is not enough and magnetic loss is too high.For electromagnetic wave inhibiting material (being usually made into flake), insulation is not enough by the penetration depth of minimizing electromagnetic wave in thin slice.In addition, for magnetic conduction thin slice, insulation is not enough will form vortex flow with magnetic loss is too high, affect the energy transferring of radio-frequency communication.
Summary of the invention
Therefore, the object of this invention is to provide and be coated with phosphatic ferrite powder and preparation method thereof, utilize the phosphate coated by ferrite powder surface to increase insulating properties, can magnetic loss be reduced simultaneously.
According to one embodiment of the invention, provide be applicable to as electromagnetic wave inhibiting material or manufacture magnetic conduction thin slice be coated with phosphatic ferrite powder.This is coated with phosphatic ferrite powder and comprises ferrite powder and be coated on the phosphate on above-mentioned ferrite powder surface completely.
According to another embodiment of the present invention, provide preparation to be coated with the method for phosphatic ferrite powder, be wherein coated with phosphatic ferrite powder and be applicable to as electromagnetic wave inhibiting material or manufacture magnetic conduction thin slice.The method comprises ferrite powder is broken to predetermined particle diameter, and to obtain ferrite powder, wherein ferrite powder comprises multiple predetermined composition; In phosphoric acid is water-soluble, ethanol or acetone, to prepare the phosphoric acid solution with predetermined molar concentration (M), wherein predetermined molar concentration is 0.2M to 1.0M; Be placed in phosphoric acid solution by above-mentioned ferrite powder, and stir the first scheduled time slot, wherein the first scheduled time slot is 0.5 little of 2 hours; Ferrite powder is filtered out, to obtain filtration ferrite powder by above-mentioned phosphoric acid solution; And in predetermined temperature to above-mentioned filtration ferrite powder heating at least the second scheduled time slot, make to filter ferrite powder dehydration, be coated with phosphatic ferrite powder to obtain, wherein above-mentioned predetermined temperature is 250 DEG C to 500 DEG C, and above-mentioned second scheduled time slot is 5 minutes.
According to another embodiment of the present invention, be coated with in phosphatic ferrite powder and preparation method thereof above-mentioned, ferrite powder is MnZn (Mn-Zn) ferrite powder.And manganese-zinc ferrite powder comprises following in the Multiple components of molar percentage (mol%), this little composition is: the di-iron trioxide (Fe of 51 ~ 55 mol%
2o
3), the zinc oxide (ZnO) of 8 ~ 25 mol%, inevitably impurity and the surplus that is made up of manganese monoxide (MnO).
According to another embodiment of the present invention, be coated with in phosphatic ferrite powder and preparation method thereof above-mentioned, ferrite powder is nickel zinc (Ni-Zn) ferrite powder.And nickel-zinc ferrite powder comprises following in the Multiple components of mol%, this little composition is: the Fe of 45 ~ 50 mol%
2o
3, the ZnO of 17 ~ 32 mol%, the copper monoxide (CuO), the inevitably impurity that are less than 15 mol% and the surplus be made up of nickel oxide (NiO).
Advantage of the present invention is: by ferrite powder surface applying phosphate completely, can increase the insulating properties of ferrite powder and reduce magnetic loss, and then promoting the performance of ferrite powder product and competitiveness.
Accompanying drawing explanation
Preferably understand to have viewpoint of the present invention, please refer to above-mentioned detailed description and coordinate corresponding figure.It is emphasized that according to the standard normal of industry, the various features in accompanying drawing do not illustrate to scale.In fact, for clearly demonstrating following embodiment, the size of various feature at random can be zoomed in or out.The description of contents of correlation diagram is as follows.
Fig. 1 is the flow chart preparing the method being coated with phosphatic ferrite powder according to one embodiment of present invention.
Fig. 2 is the relation curve schematic diagram between dielectric loss constant according to an embodiment of the invention and frequency.
Fig. 3 is the magnetic loss constant of the embodiment of Fig. 2 and the relation curve schematic diagram of frequency.
Fig. 4 is the relation curve schematic diagram of dielectric loss constant according to another embodiment of the present invention and frequency.
Fig. 5 is the magnetic loss constant of the embodiment of Fig. 4 and the relation curve schematic diagram of frequency.
Fig. 6 be surface-coated have phosphatic manganese-zinc ferrite powder mix with PU glue manufactured by thin slice observe the metallographic structure of gained with SEM.
Fig. 7 be surface uncoated have phosphatic manganese-zinc ferrite powder mix with PU glue manufactured by thin slice observe the metallographic structure of gained with SEM.
Embodiment
Please refer to the 1st figure, it illustrates the flow chart being coated with the method for phosphatic ferrite powder according to one embodiment of the invention preparation.And the above-mentioned ferrite powder being coated with phosphide is applicable to as electromagnetic wave inhibiting material, or be applicable to manufacture magnetic conduction thin slice.Preparation is coated with the method 100 of phosphatic ferrite powder (for simplicity, hereinafter referred to as " method 100 ") start from step 102, ferrite powder is broken to predetermined particle diameter, and to obtain ferrite powder, wherein above-mentioned ferrite powder includes multiple predetermined composition.
In certain embodiments, if above-mentioned ferrite powder is manganese-zinc ferrite powder, then ferrite powder comprises following in the Multiple components of mol%, and wherein this little composition is: the Fe of 51 ~ 55 mol%
2o
3, the ZnO of 8 ~ 25 mol%, inevitably impurity and the surplus that is made up of MnO.
In certain embodiments, if above-mentioned ferrite powder is nickel-zinc ferrite powder, then ferrite powder comprises following in the Multiple components of mol%, and wherein this little composition is: the Fe of 45 ~ 50 mol%
2o
3, the ZnO of 17 ~ 32 mol%, the CuO, the inevitably impurity that are less than 15 mol% and the surplus be made up of NiO.
Method 100 continues to step 104, and in phosphoric acid is water-soluble, ethanol or acetone, to prepare the phosphoric acid solution with predetermined molar concentration, wherein above-mentioned predetermined molar concentration is 0.2M to 1.0M.After completing step 104, then carry out step 106, to be placed in phosphoric acid solution by above-mentioned ferrite powder, and stir the first scheduled time slot, wherein above-mentioned first scheduled time slot can be such as 0.5 little of 2 hours.
Then, method 100 proceeds to step 108, to filter out ferrite powder in the phosphoric acid solution obtained by above-mentioned steps 104, and then obtains filtration ferrite powder.
Finally, method 100 carry out step 110, in predetermined temperature to above-mentioned filtration ferrite powder heating at least the second scheduled time slot, makes to filter ferrite powder dehydration, uses acquisition and be coated with phosphatic ferrite powder.In step 110, predetermined temperature can be such as 250 DEG C to 500 DEG C, and the second scheduled time slot can be then such as 5 minutes.
In certain embodiments, the above-mentioned step (step 108) by filtering out ferrite powder in phosphoric acid solution more can comprise preheating steps.In this preheating steps, heating, drying is by the ferrite powder filtered out in phosphoric acid solution in advance, obtains above-mentioned filtration ferrite powder by this.This preheating steps main purpose is the portion of water removed in advance in ferrite powder, makes dehydration in following step 110 can be more complete, and then guarantees finally obtained be coated with phosphatic ferrite powder and can not comprise any moisture.
Referring again to the 1st figure, in the present embodiment, method 100 more can comprise step 109, with upper be set forth in predetermined temperature to the step (step 110) of filtering ferrite powder heating at least the second scheduled time slot before, and after filtering out the step (step 108) of ferrite powder in by phosphoric acid solution, filtration ferrite powder is placed in a nitrogen atmosphere.The main object of step 109 is to avoid the heating process in subsequent step 110 to make to filter the gas comprised in ferrite powder and reaction chamber to produce and react, and then guarantees the quality of surface phosphoric acid salt of the ferrite powder finally obtained.
In the present embodiment scheme, needed for meeting in order to ensure the particle diameter being coated with phosphatic ferrite powder, method 100 more can comprise step 112, so that the phosphatic ferrite powder that is coated with after dehydration is crushed to required particle diameter.
Below then further illustrate the present invention with practical embodiments, only scope of the present invention does not limit by this little embodiment.
Embodiment 1
First, get the magnetic of business-like manganese-zinc ferrite, after being compressed, sintering is to remove adhesive (Binder).Then, institute after sintering is produced the magnetic stamen pulverizing of putting into manganese-zinc ferrite, and filter out the powder being less than Unite States Standard (US Standard) 325 order number (Mesh).Above-mentioned manganese-zinc ferrite powder comprises the Fe of 52 ~ 54 mol%
2o
3, the ZnO of 20 ~ 25 mol%, inevitably impurity and the surplus that is made up of MnO.
Subsequently phosphoric acid is dissolved in ethanol, to prepare the phosphoric acid solution of 0.8M.Above-mentioned gained manganese-zinc ferrite powder is placed in described phosphoric acid solution, and stirs 30 minutes.
From phosphoric acid solution, filter out manganese-zinc ferrite powder, and carry out in advance heating, drying manganese-zinc ferrite powder to obtain above-mentioned filtration manganese-zinc ferrite powder.Then, in 250 DEG C, 5 minutes are heated to filtration ferrite powder, make manganese-zinc ferrite powder dewater by this, be coated with phosphatic ferrite powder to obtain.
Subsequently the phosphatic manganese-zinc ferrite powder that is coated with after dehydration is crushed to required particle diameter, and filters out the powder being less than Unite States Standard 325 order number further.The final manganese-zinc ferrite powder of above-mentioned acquisition and PU glue (as adhesive) are laminated with the ratio that weight ratio is 95/5.
After completing the making of above-mentioned thin slice, observe its metallographic structure with scanning electron microscope (SEM), above-mentionedly observe the metallographic structure of gained as the 6th figure with SEM.From the 6th figure, the surface-coated of manganese-zinc ferrite powder has one deck phosphate.
In addition, more detect above-mentioned thin slice with electric impedance analyzer [such as the E4991A of Agilent Technologies (Agilent Technology) company], and the result of its dielectric loss constant (ε ") and magnetic loss constant (μ ") is recorded in the 2nd and 3 figure respectively.
The following comparative example 1 corresponding with embodiment 1, embodiment 2, embodiment 3 and respectively with embodiment 2 and 3 corresponding comparative examples 2 and 3 among, implementation step is similar to the implementation step of embodiment 1, thus following only just difference be therebetween illustrated.
Comparative example 1
In comparative example 1, get equally as the commercialization manganese-zinc ferrite magnetic in embodiment 1, compressed, sinter, the magnetic stamen after sintering is pulverized and filter out the powder being less than Unite States Standard 325 order number.Then, directly manganese-zinc ferrite and PU glue are laminated with the ratio that weight ratio is 95/5.
Observe the metallographic structure of above-mentioned thin slice with SEM, observed result is as the 7th figure.From the 7th figure, because the surface of manganese-zinc ferrite powder is not coated with phosphate, therefore the surface presentation smooth state of manganese-zinc ferrite powder.
In addition, detect above-mentioned thin slice with the E4991A electric impedance analyzer of such as Agilent Technologies equally, and the result of its dielectric loss constant (ε ") and magnetic loss constant (μ ") is recorded respectively as in the 2nd and 3 figure.
Embodiment 2
In example 2, commercialization manganese-zinc ferrite magnetic in embodiment 1 is replaced to commercialization nickel-zinc ferrite magnetic.And obtained the after crushed nickel-zinc ferrite powder of above-mentioned nickel-zinc ferrite magnetic comprises the Fe of 51 ~ 53mol%
2o
3, the ZnO of 20 ~ 25 mol%, the CuO of 3 ~ 6 mol%, inevitably impurity and the surplus that is made up of NiO.In addition, the order number of screening changes to 200 by 325 of embodiment 1, and phosphoric acid solution concentration changes to 0.6M by the 0.8M of embodiment 1.
Moreover, the final nickel-zinc ferrite powder that said process obtains by the ratio being 95/5 with weight ratio equally and PU glue are laminated, then utilize electric impedance analyzer to detect, and the result of its dielectric loss constant and magnetic loss constant is recorded respectively as in the 4th and 5 figure.
Comparative example 2
In comparative example 2, all process steps and condition are similar to embodiment 2, and wherein difference is, the nickel-zinc ferrite powder of comparative example 2 is not placed in phosphoric acid solution.The nickel-zinc ferrite powder system of comparative example 2 directly with weight ratio be 95/5 ratio and PU glue laminate, then carry out electric impedance analyzer detection, and the result of its dielectric loss constant and magnetic loss constant recorded respectively as in the 4th and 5 figure.
Above-described embodiment 1 to 2 and comparative example 1 to 2 are shown in the dielectric loss constant of frequency 100 MHz (MHz) and 1000MHz and magnetic loss constant especially with following table one.
Table one
Data according to above table one and Fig. 2 to Fig. 7:
1. in embodiment 1 made by manganese-zinc ferrite powder and PU glue thin slice, in high-frequency range, its dielectric loss constant all compared with in comparative example 1 made by manganese-zinc ferrite powder and PU glue thin slice little more than 5 times.The above results shows, and the insulativity through the manganese-zinc ferrite powder of surface-coated process significantly increases.
2. in embodiment 1 made by manganese-zinc ferrite powder and PU glue thin slice, in high-frequency range, its magnetic loss constant all compared with in comparative example 1 made by manganese-zinc ferrite powder and PU glue thin slice little more than 1.5 times.The above results shows, and the magnetic loss through the manganese-zinc ferrite powder of surface-coated process significantly reduces.
3. in embodiment 2 made by nickel-zinc ferrite powder and PU glue thin slice, in high-frequency range, its dielectric loss constant all compared with in comparative example 2 made by nickel-zinc ferrite powder and PU glue thin slice little more than 4 times.
4. in embodiment 2 made by nickel-zinc ferrite powder and PU glue thin slice, in high-frequency range, its magnetic loss constant all compared with in comparative example 2 made by nickel-zinc ferrite powder and PU glue thin slice little more than 4 times.
Comprehensive the above, adopt the ferrite powder that method of the present invention obtains, the insulativity of the electromagnetic wave inhibiting material manufactured by it or magnetic conduction thin slice and magnetic loss can obtain significant improvement.
Although the present invention discloses as above with execution mode; so itself and be not used to limit the present invention; any those skilled in the art; without departing from the spirit and scope of the present invention; certainly can do various change and retouching, therefore protection scope of the present invention is when being as the criterion depending on the accompanying claim person of defining.
[reference numeral explanation]
Claims (9)
1. be coated with phosphatic ferrite powder, be applicable to as electromagnetic wave inhibiting material or manufacture magnetic conduction thin slice, wherein this is coated with phosphatic ferrite powder and comprises:
Ferrite powder; And
Phosphate, wherein this phosphate is coated on the surface of this ferrite powder completely;
Wherein this is coated with phosphatic ferrite powder and is obtained by the preparation method comprising following steps:
Ferrite powder is broken to predetermined particle diameter, and to obtain ferrite powder, wherein this ferrite powder comprises the predetermined composition of plural number kind;
In phosphoric acid is water-soluble, ethanol or acetone, to prepare the phosphoric acid solution with predetermined molar concentration (M), wherein this predetermined molar concentration is 0.2M to 1.0M;
Be placed in this phosphoric acid solution by this ferrite powder, and stir the first scheduled time slot, wherein this first scheduled time slot is 0.5 little of 2 hours;
This ferrite powder is filtered out, to obtain filtration ferrite powder by this phosphoric acid solution; And
In predetermined temperature to this filtration ferrite powder heating at least the second scheduled time slot, this filtration ferrite powder is dewatered, be coated with phosphatic ferrite powder to obtain this, wherein this predetermined temperature is 250 DEG C to 500 DEG C, and this second scheduled time slot is 5 minutes.
2. be coated with phosphatic ferrite powder as claimed in claim 1, wherein this ferrite powder is manganese-zinc ferrite powder, this manganese-zinc ferrite powder comprises following in the plurality of components of molar percentage (mol%), and those compositions are the di-iron trioxide of 51 ~ 55 mol%, the zinc oxide of 8 ~ 25 mol%, inevitably impurity and the surplus be made up of manganese monoxide.
3. be coated with phosphatic ferrite powder as claimed in claim 1, wherein this ferrite powder is nickel-zinc ferrite powder, this nickel-zinc ferrite powder comprises following in the plurality of components of molar percentage (mol%), and those compositions are the di-iron trioxide of 45 ~ 53 mol%, the zinc oxide of 17 ~ 32 mol%, the copper monoxide, the inevitably impurity that are less than 15 mol% and the surplus be made up of nickel oxide.
4. be coated with the preparation method of phosphatic ferrite powder, wherein this is coated with phosphatic ferrite powder and is applicable to as electromagnetic wave inhibiting material or manufactures magnetic conduction thin slice, and this preparation method comprises:
Ferrite powder is broken to predetermined particle diameter, and to obtain ferrite powder, wherein this ferrite powder comprises the predetermined composition of plural number kind;
In phosphoric acid is water-soluble, ethanol or acetone, to prepare the phosphoric acid solution with predetermined molar concentration (M), wherein this predetermined molar concentration is 0.2M to 1.0M;
Be placed in this phosphoric acid solution by this ferrite powder, and stir the first scheduled time slot, wherein this first scheduled time slot is 0.5 little of 2 hours;
This ferrite powder is filtered out, to obtain filtration ferrite powder by this phosphoric acid solution; And
In predetermined temperature to this filtration ferrite powder heating at least the second scheduled time slot, this filtration ferrite powder is dewatered, be coated with phosphatic ferrite powder to obtain this, wherein this predetermined temperature is 250 DEG C to 500 DEG C, and this second scheduled time slot is 5 minutes.
5. preparation method as claimed in claim 4, wherein comprises preheating steps further by the step filtering out this ferrite powder in this phosphoric acid solution, with this ferrite powder of heating, drying in advance, obtains this filtration ferrite powder by this.
6. preparation method as claimed in claim 4, comprises further:
Be that this predetermined temperature is to before the step of this filtration ferrite powder heating at least this second scheduled time slot, and after filtering out the step of this ferrite powder in by this phosphoric acid solution, this filtration ferrite powder be placed in nitrogen atmosphere.
7. preparation method as claimed in claim 4, wherein comprises in this predetermined temperature further to the step that this filtration ferrite powder heats at least this second scheduled time slot:
This after dehydration is coated with phosphatic ferrite powder and is crushed to required particle diameter.
8. preparation method as claimed in claim 4, those predetermined compositions that wherein this ferrite powder comprises are that those are predetermined to be and are divided in molar percentage (mol%): the di-iron trioxide of 51 ~ 55 mol%, the zinc oxide of 8 ~ 25 mol%, inevitably impurity and the surplus be made up of manganese monoxide.
9. preparation method as claimed in claim 4, those predetermined compositions that wherein this ferrite powder comprises are that those are predetermined to be and are divided in molar percentage (mol%): the di-iron trioxide of 45 ~ 50 mol%, the zinc oxide of 17 ~ 32 mol%, the copper monoxide, the inevitably impurity that are less than 15 mol% and the surplus be made up of nickel oxide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110033855.0A CN102623124B (en) | 2011-01-31 | 2011-01-31 | Be coated with phosphatic ferrite powder and preparation method thereof |
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|---|---|---|---|
| CN201110033855.0A CN102623124B (en) | 2011-01-31 | 2011-01-31 | Be coated with phosphatic ferrite powder and preparation method thereof |
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| CN102623124A CN102623124A (en) | 2012-08-01 |
| CN102623124B true CN102623124B (en) | 2015-10-14 |
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2011
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Non-Patent Citations (2)
| Title |
|---|
| Soft magnetic composite materials(SMCs);H.Shokrollahi et al;《Materials Processing Technology》;20071231;第1-12页 * |
| 铁粉基软磁复合材料绝缘包覆层的研究;刘菲菲等;《材料开发与应用》;20071031;第22卷(第5期);第11页左栏-第14页右栏 * |
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