CN110369055A - A method of soft magnetic ferrite ball-milling medium is used as using zirconia ball - Google Patents
A method of soft magnetic ferrite ball-milling medium is used as using zirconia ball Download PDFInfo
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- CN110369055A CN110369055A CN201910788101.2A CN201910788101A CN110369055A CN 110369055 A CN110369055 A CN 110369055A CN 201910788101 A CN201910788101 A CN 201910788101A CN 110369055 A CN110369055 A CN 110369055A
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- ball
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- zirconia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
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- Food Science & Technology (AREA)
- Soft Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
Abstract
The invention discloses a kind of methods for being used as soft magnetic ferrite ball-milling medium using zirconia ball, it includes: to weigh di-iron trioxide 50.2~64%, mangano-manganic oxide 25~32% by mass percentage, and surplus is to be used as raw material after zinc oxide mixes；Pure water and dispersing agent are added in raw material；It is dried for standby after the mixed slurry that the interior addition ball-milling medium zirconia ball of raw material starts ball milling；Slurry after drying is subjected to pre-burning；Additive is added in Preburning material and carries out ball milling；It adds pure water and 1.5~2wt% dispersing agent is added；It is packed into ball-milling medium zirconia ball, starts ball milling and obtains mixed slurry；Mixed slurry is spray-dried to obtain dry powder；Powder is subjected to high temperature sintering；Knot obtains soft magnetic ferrite；The prior art is solved using steel ball as ball-milling medium, deposits that impurities of materials content is exceeded, and Ball-milling Time, which is grown, leads to energy consumption height；The material particle size ground is not through reaching requirement the problems such as high.
Description
Technical field
The invention belongs to technical field of electronic ceramic；More particularly to a kind of use zirconia ball is used as soft magnetic ferrite
The method of ball-milling medium.
Background technique
Ball milling is to be uniformly mixed powder in ball-grinding machine, and the technical process further milled, and is manufacture soft magnet
The important procedure of ferrite.The production of soft magnetic ferrite uses the technique of secondary ball milling, the mixing after main material ingredient
For first time ball milling, main purpose is to be uniformly mixed raw material, and further levigate, to increase raw material activity, is conducive to pre-
Solid phase reaction when burning.Ball milling after additive is added after pre-burning is secondary ball milling, and main purpose is that Preburning material is rolled into one
The powder of particle size is determined, in favor of forming and being sintered.Mechanical milling process is a complicated physical and chemical process, it not only makes powder
End attenuates, but also changes the physicochemical properties of powder.For example, can greatly improve powder surface energy by ball milling, increase
Add the imperfection of lattice, form the unformed layer in surface, so that entire particle energy be made to increase.This change of properties of powder,
Subsequent handling is directly influenced, that is, forms the improvement with sintering character.
Traditional soft magnetic ferrite ball-milling technology generally uses steel ball as ball-milling medium, but in mechanical milling process
In, steel ball and barrel can wear and bring certain impurity into, and soft magnetic ferrite is very stringent to the control of ingredient, slightly partially
Difference influences greatly performance bring, and composition tolerances can then be related to subsequent feed supplement, and feed supplement is not only cumbersome, can also draw
Enter unnecessary impurity；Since ball hardness is inadequate when simultaneously using steel ball as ball-milling medium；There are Ball-milling Time length to cause
Energy consumption is high；The material particle size ground, which does not often reach requirement, leads to problems such as consumptive material high at high cost.
Summary of the invention
The problem to be solved in the present invention is: provide it is a kind of using zirconia ball be used as soft magnetic ferrite ball-milling medium
There is the material ground to solve prior art soft magnetic ferrite ball-milling technology using steel ball as ball-milling medium in method
Impurity content exceeding index, since ball hardness is inadequate when using steel ball as ball-milling medium；There are Ball-milling Time length to lead to energy consumption height；
The material particle size ground, which does not often reach requirement, leads to problems such as consumptive material high at high cost.
The technical scheme is that
A method of soft magnetic ferrite ball-milling medium being used as using zirconia ball, it includes:
Step 1, prepare raw material, weigh by mass percentage di-iron trioxide 50.2~64%, mangano-manganic oxide 25~
32%, surplus is to be used as raw material after zinc oxide mixes；
The weight ratio of step 2, the dispersing agent that pure water and 1.5~2wt% are added in raw material, water and raw material is 1:1.5；
Ball-milling medium zirconia ball is added in step 3 in raw material；
Step 4 starts ball milling, and Ball-milling Time is after 2-4h obtains mixed slurry, and taking-up is dried for standby；
Slurry after drying is carried out pre-burning by step 5, and sintering temperature is 900~1000 DEG C；Time 2-5 hour；
Additive progress ball milling is added in Preburning material by step 6；
Step 7 adds pure water, and water and raw material weight ratio are 1:1.5；And 1.5~2wt% dispersing agent is added；
Step 8 is packed into ball-milling medium zirconia ball, and zirconia ball and raw material gross weight ratio are 5:1；Start ball milling, ball
Time consuming is that 1-2h obtains mixed slurry；
Mixed slurry is spray-dried to obtain dry powder by step 9；
Powder is carried out high temperature sintering by step 10, and knot obtains soft magnetic ferrite.
Additive described in step 6 accounts for the mass percent of Preburning material are as follows: silica 0.05~0.1%；Calcium carbonate 0.4~
1.2% and cobaltosic oxide 1~2%.
Ball-milling medium zirconia ball is added described in step 3 in raw material, zirconia ball and raw material gross weight ratio are 5:1.
Ball-milling medium zirconia ball is packed into described in step 8, zirconia ball and raw material gross weight ratio are 5:1.
Beneficial effects of the present invention:
In soft magnetic ferrite preparation process, ball milling process replaces with zirconia ball by original steel ball and makees the present invention
For ball-milling medium, first is that can reduce in mechanical milling process, the impurity that the abrasion of ball-milling medium is brought into；Second is that ingredient can be reduced
Deviation saves the time from the correction without carrying out composition tolerances in the follow-up process again, saves manufacturing cost；Third is that ingredient
Stable phase should bring the stability of properties of product, fourth is that reduce Ball-milling Time；Solves prior art soft magnetic ferrite material
For pellet grinding process using steel ball as ball-milling medium, it is exceeded to there is the impurities of materials content ground, using steel ball as ball milling Jie
Since ball hardness is inadequate when matter；There are Ball-milling Time length to lead to energy consumption height；The material particle size ground, which does not often reach requirement, leads
The problems such as causing consumptive material high at high cost.
Specific embodiment:
A method of soft magnetic ferrite ball-milling medium being used as using zirconia ball, steps are as follows:
Each component, di-iron trioxide 50.2~64%, mangano-manganic oxide 25~32% are weighed by mass percentage, and surplus is
Zinc oxide；
The above main material is weighed into mixing according to quantity, suitable pure water is added, water and raw material weight ratio are 1:1.5；And add
Enter 1.5~2wt% dispersing agent；It is packed into ball-milling medium zirconia ball, zirconia ball and main material total weight ratio are 5:1；Using
When steel ball is as ball-milling medium, ball milling facility load is aggravated, because steel ball density is larger, the steel ball of same volume accumulated amount, quality is oxygen
Change about the 1/4 of zirconium ball.
Start ball milling, Ball-milling Time is 2-4h (when using steel ball ball milling, Ball-milling Time can also extend about 1h), to raw material point
After dissipating into about 1.5 μm of partial size of mixed slurry, taking-up is dried for standby；
Slurry after drying is subjected to pre-burning, sintering temperature is 900~1000 DEG C；Time 2-5 hour；
Additive is added in Preburning material and carries out ball milling；Additive accounts for the mass fraction of Preburning material are as follows: and silica 0.05~
0.1%；Calcium carbonate 0.4~1.2%；Cobaltosic oxide 1~2%；Suitable pure water is added, water and raw material weight ratio are 1:
1.5；And 1.5~2wt% dispersing agent is added, it is packed into ball-milling medium zirconia ball, zirconia ball and main material total weight ratio are
5:1；Start ball milling, Ball-milling Time 1-2h is spare at the mixed slurry of appropriate particle size to stock dispersion；According to steel ball ball
Mill, since steel ball itself can bring impurity F e etc. into, so that Fe content deviation is larger in ingredient, and the especially high magnetic conductance of soft magnetic materials
The soft magnetic materials of rate is very stringent to component content control, and the impurity brought into using steel ball ball milling influences performance very big.
Mixed slurry is spray-dried, dry powder is obtained.
Powder is subjected to high temperature sintering, sintering temperature is 900~1000 DEG C；Time 2-5 hour；
Obtain soft magnetic ferrite.
Embodiment 1:
Each component is weighed by mass percentage, and di-iron trioxide 58%, mangano-manganic oxide 29%, surplus is zinc oxide；It will
The above main material weighs mixing according to quantity, and suitable pure water is added, and water and raw material weight ratio are 1:1.5；And it is added 1.5wt% points
Powder, is packed into ball-milling medium zirconia ball, and zirconia ball and main material total weight ratio are 5:1；Start ball milling, Ball-milling Time is
3h, after stock dispersion is at the mixed slurry of appropriate particle size, taking-up is dried for standby；Drying material is taken out into a small amount of progress composition detection
(testing result is labeled as red material ingredient 1)；Slurry after drying is subjected to pre-burning, sintering temperature is 950 DEG C；Preburning material is added
Additive carries out ball milling；Additive accounts for the mass fraction of Preburning material are as follows: silica 0.1%；Calcium carbonate 0.8%；Four oxidations three
Cobalt 1.5%；Suitable pure water is added, water and raw material weight ratio are 1:1.5；And 1.5wt% dispersing agent is added, it is packed into ball milling
Medium oxidizing zirconium ball, zirconia ball and main material total weight ratio are 5:1；Start ball milling, Ball-milling Time 2h, to stock dispersion
It is spare at the mixed slurry of appropriate particle size；Mixed slurry in step 5 is spray-dried, dry powder is obtained；It will do
Dry powder takes out a small amount of progress composition detection (testing result is labeled as black material ingredient 1)；Powder is subjected to high temperature sintering, is obtained soft
Magnetic ferrite material.
Comparative example: the ball-milling medium in embodiment 1 is replaced with into steel ball, remaining condition is constant.
Each component is weighed by mass percentage, and di-iron trioxide 58%, mangano-manganic oxide 29%, surplus is zinc oxide；It will
The above main material weighs mixing according to quantity, and suitable pure water is added, and water and raw material weight ratio are 1:1.5；And it is added 1.5wt% points
Powder, is packed into ball-milling medium steel ball, and steel ball and main material total weight ratio are 5:1；Start ball milling, Ball-milling Time 3h, to original
After material is dispersed into the mixed slurry of appropriate particle size, taking-up is dried for standby；Drying material is taken out into a small amount of composition detection that carries out and (detects knot
Fruit is labeled as red material ingredient 2)；Slurry after drying is subjected to pre-burning, sintering temperature is 950 DEG C；Additive is added in Preburning material
Carry out ball milling；Additive accounts for the mass fraction of Preburning material are as follows: silica 0.1%；Calcium carbonate 0.8%；Cobaltosic oxide
1.5%；Suitable pure water is added, water and raw material weight ratio are 1:1.5；And 1.5wt% dispersing agent is added, it is packed into ball milling and is situated between
Matter steel ball, steel ball and main material total weight ratio are 5:1；Start ball milling, Ball-milling Time 2h, to stock dispersion at appropriate particle size
Mixed slurry it is spare；Mixed slurry in step 5 is spray-dried, dry powder is obtained；Dry powder is taken out
It is a small amount of to carry out composition detection (testing result is labeled as black material ingredient 2)；Powder is subjected to high temperature sintering, obtains soft magnetic ferrite material
Material.
Embodiment 1 and its comparative example are subjected to ingredient, partial size comparison, as (wherein, ingredient is converted into for table 1, table 2
Oxide content, and ingredient of the content lower than 100PPm is ignored):
The red material ingredient comparison of table 1-1
| The name of an article | Fe2O3 | Mn3O4 | ZnO | SiO2 | Ca0 | Al2O3 |
| Food ingredient | 58% | 29% | 13% | |||
| Red material ingredient 1 | 58.05% | 28.93% | 13.02% | |||
| Red material ingredient 2 | 58.83% | 28.44% | 12.66% | 0.04% | 0.02% | 0.01% |
The black material ingredient comparison of table 1-2
The comparison of the black material partial size of table 2
| The name of an article | Black material ingredient 1 | Black material ingredient 2 |
| Partial size (μm) | 1.47 | 1.72 |
To sum up, it is formulated using the powder content that zirconia ball comes out as ball-milling medium ball milling closer to calculating, Er Qiexiang
In the case of Ball-milling Time and the ball-milling medium of identical weight, zirconia ball is more careful as the ball milling partial size of ball-milling medium.It can
See, zirconia ball is smaller as composition influence of the ball-milling medium to soft magnetic ferrite, thus the material of subsequent technique production
Performance is more stable；Also it can be shortened Ball-milling Time, reduce energy consumption.
Claims (4)
1. a kind of method for being used as soft magnetic ferrite ball-milling medium using zirconia ball, it includes:
Step 1 prepares raw material, weighs di-iron trioxide 50.2~64%, mangano-manganic oxide 25~32% by mass percentage, remaining
Amount is to be used as raw material after zinc oxide mixes；
The weight ratio of step 2, the dispersing agent that pure water and 1.5~2wt% are added in raw material, water and raw material is 1:1.5；
Ball-milling medium zirconia ball is added in step 3 in raw material；
Step 4 starts ball milling, and Ball-milling Time is after 2-4h obtains mixed slurry, and taking-up is dried for standby；
Slurry after drying is carried out pre-burning by step 5, and sintering temperature is 900~1000 DEG C, time 2-5 hour；
Additive progress ball milling is added in Preburning material by step 6；
Step 7 adds pure water, and water and raw material weight ratio are 1:1.5；And 1.5~2wt% dispersing agent is added；
Step 8 is packed into ball-milling medium zirconia ball, and zirconia ball and raw material gross weight ratio are 5:1；Start ball milling, when ball milling
Between obtain mixed slurry for 1-2h；
Mixed slurry is spray-dried to obtain dry powder by step 9；
Powder is carried out high temperature sintering by step 10, and knot obtains soft magnetic ferrite.
2. a kind of method for being used as soft magnetic ferrite ball-milling medium using zirconia ball according to claim 1,
Be characterized in that: additive described in step 6 accounts for the mass percent of Preburning material are as follows: silica 0.05~0.1%；Calcium carbonate 0.4
~1.2% and cobaltosic oxide 1~2%.
3. a kind of method for being used as soft magnetic ferrite ball-milling medium using zirconia ball according to claim 1,
It is characterized in that: ball-milling medium zirconia ball is added described in step 3 in raw material, zirconia ball and raw material gross weight ratio are 5:1.
4. a kind of method for being used as soft magnetic ferrite ball-milling medium using zirconia ball according to claim 1,
It is characterized in that: being packed into ball-milling medium zirconia ball described in step 8, zirconia ball and raw material gross weight ratio are 5:1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910788101.2A CN110369055A (en) | 2019-08-26 | 2019-08-26 | A method of soft magnetic ferrite ball-milling medium is used as using zirconia ball |
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| CN201910788101.2A CN110369055A (en) | 2019-08-26 | 2019-08-26 | A method of soft magnetic ferrite ball-milling medium is used as using zirconia ball |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367645A (en) * | 2008-08-06 | 2009-02-18 | 中国地质大学（北京） | Novel method for preparing ferrite ceramic soft magnetic material |
| CN104446409A (en) * | 2014-10-31 | 2015-03-25 | 广东风华高新科技股份有限公司 | Manganese zinc ferrite material and preparation method thereof |
| CN105367048A (en) * | 2015-11-12 | 2016-03-02 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material and preparation technology thereof |
| CN108766705A (en) * | 2018-06-28 | 2018-11-06 | 上海安费诺永亿通讯电子有限公司 | A kind of wireless charging manganese-zinc ferrite magnetic sheet and preparation method thereof |
-
2019
- 2019-08-26 CN CN201910788101.2A patent/CN110369055A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367645A (en) * | 2008-08-06 | 2009-02-18 | 中国地质大学（北京） | Novel method for preparing ferrite ceramic soft magnetic material |
| CN104446409A (en) * | 2014-10-31 | 2015-03-25 | 广东风华高新科技股份有限公司 | Manganese zinc ferrite material and preparation method thereof |
| CN105367048A (en) * | 2015-11-12 | 2016-03-02 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material and preparation technology thereof |
| CN108766705A (en) * | 2018-06-28 | 2018-11-06 | 上海安费诺永亿通讯电子有限公司 | A kind of wireless charging manganese-zinc ferrite magnetic sheet and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 傅膑: "宽温低功耗MnZn铁氧体材料及变压器仿真", 《中国优秀硕士学位论文全文数据库工程科技II辑》 * |
| 霍骅鑫: "高频低功耗功率铁氧体的制备和研究", 《中国优秀硕士学位论文全文数据库工程科技II辑》 * |
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Application publication date: 20191025 |