CN107240495A - A kind of high density high stability network bead preparation method - Google Patents
A kind of high density high stability network bead preparation method Download PDFInfo
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- CN107240495A CN107240495A CN201710494907.1A CN201710494907A CN107240495A CN 107240495 A CN107240495 A CN 107240495A CN 201710494907 A CN201710494907 A CN 201710494907A CN 107240495 A CN107240495 A CN 107240495A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
- B22F3/101—Changing atmosphere
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- Mechanical Engineering (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The present invention relates to a kind of soft magnetic material, and in particular to a kind of high density high stability network bead preparation method；Including pre-sintered, grinding, sintering and application coiling, wherein pre-sintered included dry-pressing formed magnetic core blank, a point three phases sintering is placed in vertical heater, i.e., sintering temperature is brought up to 780~920 DEG C from room temperature through 4~6 hours；Kept for 1~2 hour at 780~920 DEG C；Eventually pass 3~5 hours and cool the temperature to less than 100 DEG C；There is high density, high stability, low stress using a kind of high density high stability network bead preparation method of this programme.
Description
Technical field
The present invention relates to soft magnetic material technical field, and in particular to a kind of high density high stability network bead
Preparation method.
Background technology
For meet device smaller volume, more low-power consumption and it is more inexpensive the need for, manufacture magnetic elements during
Employ multiple technologies.Connection is integrated into by changing component profile size, by magnetic element modularization and by magnetic element
Turn into three kinds of basic technologies on device.ADSL network communication transformers belong to low-power linear transformer.It is used primarily in low
In power consumption, the circuit of small-signal, require it is that high conversion efficiency, the distortion factor be low, small volume.In order to reach these requirements, become
Depressor magnetic core generally uses MnZn ferrite material with high magnetic conductivity, it is desirable to which material is in wide temperature range (- 40 DEG C~85 DEG C) magnetic permeability μ
I is high by 7000~15000, and with higher Q values.The need for adapting to telecommunication apparatus miniaturization, network bead performance is carried
More stringent requirement is gone out, while magnetic core external diameter reduces, internal diameter increases, height reduces, has also needed to meet 0 DEG C~70 DEG C bars
Inductance value under part.There is problem in reality is：In network transformer process, magnetic core is often insulated by Parylene
The external carbuncle of the aspect of pressure, coils press power, varnish and pressure during silica gel fixed coil of layer etc. three, due to magnet ring very little
Inductance is influenceed to change greatly by external force.Conventional iron core model R10kH2.54*1.40*0.76, deposit after packaging 0 DEG C of inductance value by
Stress influence drop is obvious, it is impossible to meet under 24 circle test conditions, inductance value LSMore than 350 μ H requirement.
The content of the invention
The invention is intended to provide a kind of high density, high stability, low stress and high performance high density high stability net
Network bead preparation method.
A kind of high density high stability network bead preparation method in this programme, comprises the following steps, (1) pre-burning
Knot, by dry-pressing formed magnetic core blank, is placed in vertical heater a point three phases sintering, i.e., through 4~6 hours by sintering temperature from room
Temperature brings up to 780~920 DEG C；Kept for 1~2 hour at 780~920 DEG C；Eventually pass cool the temperature within 3~5 hours 100 DEG C with
Under；(2) grind, take the magnetic core after pre-sintering to be put into grinder, while adding the grinding with magnetic core same material in grinder
Medium ball, is ground；The weight ratio of magnetic core and abrasive media ball is=1:6, grinder rotating speed is 20 revs/min, during grinding
Between be 1 hour；The dust and fragment on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into
Toasted in baking oven, remove moisture content；(3) sinter, the half-mature base after pre-sintered grinding be placed in clock hood type furnace point six stages sintering,
First stage, sintering temperature is brought up to 900 DEG C from room temperature through 5~6 hours；Second stage, will sintering temperature by 3~5 hours
Degree brings up to 1360 DEG C~1390 DEG C, and the stage needs to pour nitrogen to furnace chamber, and Control for Oxygen Content is 0.01%~12.0%；The
In three stages, sintered 3~6 hours at 1360 DEG C~1390 DEG C；Fourth stage, then 900 DEG C were cooled the temperature to through 2~4 hours, should
Stage needs to pour nitrogen to furnace chamber；5th stage, then by cooling the temperature to 500 DEG C or so within 6~8 hours, during oxygen
Content is controlled below 0.001%；In 6th stage, eventually pass 3~5 hours and cool the temperature to 100 DEG C or so, during oxygen contain
Amount control is below 0.001%；(4) finished product is made after application, coiling.
It is an advantage of the invention that：Pre-sintered purpose has three, and one can arrange the moisture content in magnetic core blank and PVA adhesives
Remove；Secondly by core portion spinel, being easy to the problems such as follow-up grinding technics removes flash removed, step during with some strength；
Thirdly pre-sintering can shorten follow-up sintering time and sintering temperature, Stress in Magnetic Core is reduced.
Present invention sintering key point is in pre-sintered, sintering second stage and sintering three aspects of the 5th stage.Pre-sintering row
Except moisture content and PVA adhesives, incomplete solid phase reaction generating portion spinel structure ferrite occurs for magnetic core；Sinter second stage
Using densification profiles, stomata is excluded, density is improved, prevent lattice defect and crystallizes uneven factor, reduces magnetic core internal stress；
Sintering for the 5th stage takes slow cooling technique, eliminates the stress caused by lattice strain and ion, room skewness.
Technological design science, it is advanced reasonable, it is simple and easy to do.So that iron core, 24 circles, 0 DEG C, inductance value LSReach 400 μ H.Especially
It is the inductance value L at 0 DEG CSCompared with conventional sintering magnetic core, inductance value LSImprove 15%~30%.
Sintering temperature is low, and traditional handicraft sintering MnZn R10 materials sintering temperature is more than 1400 DEG C, new sintering process its
Sintering temperature is less than 1390 DEG C, and while meeting user and requiring, energy consumption is low, big to life-span for improving clock hood type furnace and refractory material
It is helpful.
Further, in step (1), sintering temperature is respectively increased to 780 DEG C from room temperature through 5 hours, in 780 DEG C of holdings
1.5 hours, eventually pass 4.5 hours and cool the temperature to less than 100 DEG C.
Further, in step (1), sintering temperature is brought up to 820 DEG C from room temperature through 5 hours, it is small in 820 DEG C of holdings 1.5
When, eventually pass 4.5 hours and cool the temperature to less than 100 DEG C
Further, in step (1), sintering temperature is brought up to 860 DEG C from room temperature through 5 hours, it is small in 860 DEG C of holdings 1.5
When, eventually pass 4.5 hours and cool the temperature to less than 100 DEG C.
Further, in step (1), sintering temperature is brought up to 900 DEG C from room temperature through 5 hours, it is small in 900 DEG C of holdings 1.5
When, eventually pass 4.5 hours and cool the temperature to less than 100 DEG C.
Further, in step (3), the first stage, sintering temperature is brought up to 900 DEG C from room temperature through 5 hours.
Further, in step (3), second stage is crossed and sintering temperature was brought up into 1380 DEG C in 3.5 hours, and the stage needs
Nitrogen is poured to furnace chamber, Control for Oxygen Content is 0.25%.
Further, in step (3), the phase III, sintered 4 hours at 1380 DEG C.
Further, in step (3), fourth stage, then 900 DEG C were cooled the temperature to through 3 hours, the stage needs to rush to furnace chamber
Enter nitrogen, oxygen content from 20.6% be gradually dropped to 900 DEG C when 0.001%.
Further, in step (3), in the 5th stage, 500 DEG C or so were cooled the temperature to by 6 hours.
Brief description of the drawings
Fig. 1 is preparation technology flow chart of the present invention；
Fig. 2 is the sintering temperature curve of pre-sintering step of the present invention；
Fig. 3 is the sintering temperature curve of real sintering step of the invention.
Embodiment
Embodiment 1
The iron core model R10KH2.54*1.40*0.76 that dry-pressing formed magnetic core blank, the present embodiment are selected, is placed in
Point three phases sintering in vertical heater, through 5 hours by sintering temperature from room temperature be respectively increased to 780 DEG C, 820 DEG C, 860 DEG C, 900
DEG C, sample 1~4 is designated as respectively, is kept for 1.5 hours in the corresponding temperature, four kinds of sample all sames of processing mode below,
Eventually pass 4.5 hours and cool the temperature to less than 100 DEG C.
The magnetic core after pre-sintering is taken to be put into grinder, while adding the abrasive media with magnetic core same material in grinder
Ball, is ground.The percentage by weight of magnetic core and abrasive media ball is 1：6, grinder rotating speed is 20 revs/min, milling time
For 1 hour.The dust and debris on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into baking
Toasted in case, remove moisture content.
The magnetic core rinsed well is placed in clock hood type furnace point six stage sintering：
First stage：Sintering temperature is brought up to 900 DEG C from room temperature through 5 hours, the stage is protected without nitrogen；
Second stage：Again by sintering temperature being brought up into 1380 DEG C in 3.5 hours, the stage needs to pour nitrogen to furnace chamber
Gas, Control for Oxygen Content is 0.25%；
Phase III：Sintered 4 hours at 1380 DEG C, the stage is protected without nitrogen；
Fourth stage：900 DEG C were cooled the temperature to through 3 hours again, the stage needs nitrogen to protect, that is, need to pour to furnace chamber
Nitrogen, oxygen content from 20.6% be gradually dropped to 900 DEG C when 0.001%；
5th stage：Then by cooling the temperature to 500 DEG C or so within 6 hours, during Control for Oxygen Content 0.001% with
Under；
6th stage：Eventually pass 4 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under.
Magnetic core will be finally sintered, puts into and application is carried out in vacuum vapor deposition machine, coating material is Parylene N powder.
Measurement result
The inductance value of magnetic core is tested with the analyzer of Agilent 4284 and calculates magnetic conductivity, milky way GL601DF type high/low temperatures
Chamber provides -40 DEG C~85 DEG C test environments.The testing result of sample 1-4 after application, coiling is listed in table 1.
Table 1
Embodiment 2
The iron core model R10KH2.54*1.40*0.76 that dry-pressing formed magnetic core blank, the present embodiment are selected, simultaneously
The experiment of 4 same samples is carried out, sample 5~8 is designated as, a point three phases sintering is placed in vertical heater, will sintering temperature through 5 hours
Degree brings up to 820 DEG C from room temperature, is kept for 1.5 hours at 820 DEG C, eventually passes 4.5 hours and cool the temperature to less than 100 DEG C.
The magnetic core after pre-sintering is taken to be put into grinder, while adding the abrasive media with magnetic core same material in grinder
Ball, is ground.The percentage by weight of magnetic core and abrasive media ball is 1：6, grinder rotating speed is 20 revs/min, milling time
For 1 hour.
The dust and fragment on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into baking
Toasted in case, remove moisture content.
The magnetic core rinsed well is placed in clock hood type furnace point six stage sintering：
First stage：Sintering temperature is brought up to 900 DEG C from room temperature through 5 hours, the stage is protected without nitrogen；
Second stage：Again by sintering temperature being brought up into 1380 DEG C in 4 hours, the stage needs to pour nitrogen to furnace chamber,
The amount of pouring of control nitrogen makes the oxygen content of 4 kinds of samples control respectively 0.01%, 0.1%, 1.0%, 20.6%；
Phase III：Sintered 4 hours at 1380 DEG C, the stage is protected without nitrogen；
Fourth stage：900 DEG C were cooled the temperature to through 4 hours again, the stage needs nitrogen to protect, that is, need to pour to furnace chamber
Nitrogen, oxygen content from 20.6% be gradually dropped to 900 DEG C when 0.001%；
5th stage：Then by cooling the temperature to 500 DEG C or so within 6 hours, during Control for Oxygen Content 0.001% with
Under；
6th stage：Eventually pass 4 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under.
Magnetic core will be finally sintered, puts into and application is carried out in vacuum vapor deposition machine, coating material is Parylene N powder.
The testing result of sample 5-8 after application, coiling is listed in table 2.
Table 2
Embodiment 3
The iron core model R10KH2.54*1.40*0.76 that dry-pressing formed magnetic core blank, the present embodiment are selected, simultaneously
The experiment of 4 same samples is carried out, sample 9~12 is designated as, a point three phases sintering is placed in vertical heater, will sintering through 5 hours
Temperature brings up to 820 DEG C from room temperature, is kept for 1.5 hours at 820 DEG C, eventually passes 4.5 hours and cool the temperature to less than 100 DEG C.
The magnetic core after pre-sintering is taken to be put into grinder, while adding the abrasive media with magnetic core same material in grinder
Ball, is ground.The percentage by weight of magnetic core and abrasive media ball is 1：6, grinder rotating speed is 20 revs/min, milling time
For 1 hour.The dust and fragment on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into baking
Toasted in case, remove moisture content.
The magnetic core rinsed well is placed in clock hood type furnace point six stage sintering：
First stage：Sintering temperature is brought up to 900 DEG C from room temperature through 5 hours, the stage is protected without nitrogen；
Second stage：Again by sintering temperature being brought up into 1380 DEG C in 4 hours, the stage needs to pour nitrogen to furnace chamber,
Control for Oxygen Content is 0.1%；
Phase III：Sintered 4 hours at 1380 DEG C, the stage is protected without nitrogen；
Fourth stage：Cooled the temperature to 900 DEG C through 4 hours again, the stage needs nitrogen to protect, oxygen content from 20.6% by
0.001% when gradually dropping to 900 DEG C；
5th stage：Then 4 samples 9~12 cooled the temperature to 500 respectively through 5 hours, 6 hours, 7 hours, 8 hours
DEG C or so, during Control for Oxygen Content below 0.001%；
6th stage：Eventually pass 4 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under.
Magnetic core will be finally sintered, puts into and application is carried out in vacuum vapor deposition machine, coating material is Parylene N powder.
The testing result of sample 9-12 after application, coiling is listed in table 3.
Table 3
Present invention process prepares magnetic core, sample 2, sample 5,6, sample 10,11,12, and in 100kHz, magnetic conductivity can reach
More than 10000 high level, magnetic core volume density reaches 5.08g/cm3More than；- 40 DEG C simultaneously, 24 circle inductance value LSMore than 320 μ H；
0 DEG C, 24 circle inductance value LSMore than 400 μ H；25 DEG C, 24 circle inductance value LSMore than 500 μ H；70 DEG C, 85 DEG C, 24 circle inductance value LSGreatly
In 550 μ H.The iron core is when as network transformer iron core, and with proof stress is strong, that stability high and low temperature inductance drop range is small is excellent
Good characteristic, can be in ADSL network communications with playing huger effect in transformer use.
Embodiment 4
The iron core model R10KH2.54*1.40*0.76 that dry-pressing formed magnetic core blank, the present embodiment are selected, is placed in
Point three phases sintering, sintering temperature is respectively increased to 780 DEG C from room temperature through 4 hours, holding 1 hour, finally in vertical heater
Less than 100 DEG C were cooled the temperature to by 3 hours.
The magnetic core after pre-sintering is taken to be put into grinder, while adding the abrasive media with magnetic core same material in grinder
Ball, is ground.The percentage by weight of magnetic core and abrasive media ball is 1：6, grinder rotating speed is 20 revs/min, milling time
For 1 hour.The dust and debris on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into baking
Toasted in case, remove moisture content.
The magnetic core rinsed well is placed in clock hood type furnace point six stage sintering：
First stage：Sintering temperature is brought up to 900 DEG C from room temperature through 5 hours, the stage is protected without nitrogen；
Second stage：Again by sintering temperature being brought up into 1360 DEG C in 3 hours, the stage needs to pour nitrogen to furnace chamber,
Control for Oxygen Content is 0.01%；
Phase III：Sintered 3 hours at 1360 DEG C, the stage is protected without nitrogen；
Fourth stage：900 DEG C were cooled the temperature to through 2 hours again, the stage needs nitrogen to protect, that is, need to pour to furnace chamber
Nitrogen, oxygen content from 20.6% be gradually dropped to 900 DEG C when 0.001%；
5th stage：Then by cooling the temperature to 500 DEG C or so within 6 hours, during Control for Oxygen Content 0.001% with
Under；
6th stage：Eventually pass 3 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under.Magnetic core will be finally sintered, puts into and application is carried out in vacuum vapor deposition machine, coating material is Parylene N powder.Sample 13 is detected
As a result table 4 is seen.
Table 4
Embodiment 5
The iron core model R10KH2.54*1.40*0.76 that dry-pressing formed magnetic core blank, the present embodiment are selected, is placed in
Point three phases sintering, sintering temperature is respectively increased to 850 DEG C from room temperature through 5 hours, holding 1.5 hours, most in vertical heater
Afterwards less than 100 DEG C were cooled the temperature to by 4 hours.
The magnetic core after pre-sintering is taken to be put into grinder, while adding the abrasive media with magnetic core same material in grinder
Ball, is ground.The percentage by weight of magnetic core and abrasive media ball is 1：6, grinder rotating speed is 20 revs/min, milling time
For 1 hour.The dust and debris on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into baking
Toasted in case, remove moisture content.
The magnetic core rinsed well is placed in clock hood type furnace point six stage sintering：
First stage：Sintering temperature is brought up to 900 DEG C from room temperature through 5.5 hours, the stage is protected without nitrogen；
Second stage：Again by sintering temperature being brought up into 1370 DEG C in 4 hours, the stage needs to pour nitrogen to furnace chamber,
Control for Oxygen Content is 6.00%；
Phase III：Sintered 4 hours at 1380 DEG C, the stage is protected without nitrogen；
Fourth stage：900 DEG C were cooled the temperature to through 3 hours again, the stage needs nitrogen to protect, that is, need to pour to furnace chamber
Nitrogen, oxygen content from 20.6% be gradually dropped to 900 DEG C when 0.001%；
5th stage：Then by cooling the temperature to 500 DEG C or so within 7 hours, during Control for Oxygen Content 0.001% with
Under；
6th stage：Eventually pass 4 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under.Magnetic core will be finally sintered, puts into and application is carried out in vacuum vapor deposition machine, coating material is Parylene N powder.Sample 14 is detected
As a result table 5 is seen.
Table 5
Embodiment 6
The iron core model R10KH2.54*1.40*0.76 that dry-pressing formed magnetic core blank, the present embodiment are selected, is placed in
Point three phases sintering, sintering temperature is respectively increased to 920 DEG C from room temperature through 6 hours, holding 2 hours, finally in vertical heater
Less than 100 DEG C were cooled the temperature to by 5 hours.
The magnetic core after pre-sintering is taken to be put into grinder, while adding the abrasive media with magnetic core same material in grinder
Ball, is ground.The percentage by weight of magnetic core and abrasive media ball is 1：6, grinder rotating speed is 20 revs/min, milling time
For 1 hour.The dust and debris on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into baking
Toasted in case, remove moisture content.
The magnetic core rinsed well is placed in clock hood type furnace point six stage sintering：
First stage：Sintering temperature is brought up to 900 DEG C from room temperature through 6 hours, the stage is protected without nitrogen；
Second stage：Again by sintering temperature being brought up into 1390 DEG C in 5 hours, the stage needs to pour nitrogen to furnace chamber,
Control for Oxygen Content is 12.00%；
Phase III：Sintered 6 hours at 1390 DEG C, the stage is protected without nitrogen；
Fourth stage：900 DEG C were cooled the temperature to through 4 hours again, the stage needs nitrogen to protect, that is, need to pour to furnace chamber
Nitrogen, oxygen content from 20.6% be gradually dropped to 900 DEG C when 0.001%；
5th stage：Then by cooling the temperature to 500 DEG C or so within 8 hours, during Control for Oxygen Content 0.001% with
Under；
6th stage：Eventually pass 5 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under.Magnetic core will be finally sintered, puts into and application is carried out in vacuum vapor deposition machine, coating material is Parylene N powder.
Above-described is only that the known general knowledge such as concrete structure and characteristic is not made herein in embodiments of the invention, scheme
Excessive description., without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these should also be considered as protection scope of the present invention, these are implemented all without the influence present invention
Effect and practical applicability.The testing result of sample 15 sees table 6.
Table 6
Claims (10)
1. a kind of high density high stability network bead preparation method, it is characterised in that：Comprise the following steps,
(1) it is pre-sintered, by dry-pressing formed magnetic core blank, be placed in vertical heater a point three phases sintering, i.e., will through 4~6 hours
Sintering temperature brings up to 780~920 DEG C from room temperature；Kept for 1~2 hour at 780~920 DEG C；3~5 hours are eventually passed by temperature
Degree is down to less than 100 DEG C；
(2) grind, take the magnetic core after pre-sintering to be put into grinder, while adding the grinding with magnetic core same material in grinder
Medium ball, is ground；The weight ratio of magnetic core and abrasive media ball is=1：6, grinder rotating speed is 20 revs/min, during grinding
Between be 1 hour；The dust and fragment on magnetic core surface after grinding are cleaned with 80~99 DEG C of hot water, the magnetic core after rinsing well is put into
Toasted in baking oven, remove moisture content；
(3) sinter, the half-mature base after pre-sintered grinding be placed in clock hood type furnace point six stages sintering,
First stage, sintering temperature is brought up to 900 DEG C from room temperature through 5~6 hours,
Second stage, brought up to 1360 DEG C~1390 DEG C, the stage needs to pour to furnace chamber by 3~5 hours by sintering temperature
Nitrogen, Control for Oxygen Content 0.01%~12.0%,
Phase III, sintered 3~6 hours at 1360 DEG C~1390 DEG C,
Fourth stage, then 900 DEG C were cooled the temperature to through 2~4 hours, the stage needs to pour nitrogen to furnace chamber,
5th stage, then by cooling the temperature to 500 DEG C or so within 6~8 hours, during Control for Oxygen Content 0.001% with
Under,
In 6th stage, eventually pass 3~5 hours and cool the temperature to 100 DEG C or so, during Control for Oxygen Content 0.001% with
Under；
(4) finished product is made after application, coiling.
2. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
(1) in, sintering temperature is respectively increased to 780 DEG C from room temperature through 5 hours, is kept for 1.5 hours at 780 DEG C, eventually passes 4.5 small
When cool the temperature to less than 100 DEG C.
3. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
(1) in, sintering temperature is brought up to 820 DEG C from room temperature through 5 hours, kept for 1.5 hours at 820 DEG C, eventually passing 4.5 hours will
Temperature is down to less than 100 DEG C.
4. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
(1) in, sintering temperature is brought up to 860 DEG C from room temperature through 5 hours, kept for 1.5 hours at 860 DEG C, eventually passing 4.5 hours will
Temperature is down to less than 100 DEG C.
5. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
(1) in, sintering temperature is brought up to 900 DEG C from room temperature through 5 hours, kept for 1.5 hours at 900 DEG C, eventually passing 4.5 hours will
Temperature is down to less than 100 DEG C.
6. a kind of high density high stability network bead preparation method according to claim 2, it is characterised in that：Step
(3) in, the first stage, sintering temperature is brought up to 900 DEG C from room temperature through 5 hours.
7. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
(3) in, second stage is crossed and sintering temperature was brought up into 1380 DEG C in 3.5 hours, the stage needs to pour nitrogen to furnace chamber, and oxygen contains
Amount control is 0.25%.
8. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
(3) in, the phase III, sintered 4 hours at 1380 DEG C.
9. a kind of high density high stability network bead preparation method according to claim 2, it is characterised in that：Step
(3) in, fourth stage, then cooled the temperature to 900 DEG C through 3 hours, the stage needs to pour nitrogen to furnace chamber, oxygen content from
20.6% is gradually dropped to 0.001% at 900 DEG C.
10. a kind of high density high stability network bead preparation method according to claim 1, it is characterised in that：Step
Suddenly in (3), in the 5th stage, 500 DEG C or so were cooled the temperature to by 6 hours.
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