CN102050621B - Stepped equilibrium-atmosphere sintering process for soft-magnetic ferrite nitrogen kiln - Google Patents
Stepped equilibrium-atmosphere sintering process for soft-magnetic ferrite nitrogen kiln Download PDFInfo
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- CN102050621B CN102050621B CN201010539318A CN201010539318A CN102050621B CN 102050621 B CN102050621 B CN 102050621B CN 201010539318 A CN201010539318 A CN 201010539318A CN 201010539318 A CN201010539318 A CN 201010539318A CN 102050621 B CN102050621 B CN 102050621B
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Abstract
The invention discloses a stepped equilibrium-atmosphere sintering process for a soft-magnetic ferrite nitrogen kiln, which comprises the following process flows of: closely stacking and loading soft-magnetic ferrite magnetic-ring blanks in strings into a refractory sagger in one step and delivering the refractory sagger into the nitrogen kiln; carrying out first-stage heating treatment on the nitrogen kiln; carrying out second-stage heating treatment on the nitrogen kiln; carrying out third-stage heating treatment on the nitrogen kiln; carrying out staged cooling treatment on the nitrogen kiln according to the key points of an equilibrium-atmosphere curve; delivering the semi-finished product of a soft-magnetic ferrite magnetic ring out of the nitrogen kiln, and carrying out subsequent aging treatment; and carrying out separated detection and final inspection on the semi-finished product of the soft-magnetic ferrite magnetic ring after the aging treatment to obtain qualified products which are finished products. The invention realizes rapid sintering and simultaneously realizes the goals of no cracking or adhesive chip off-falling of soft-magnetic ferrite magnetic rings which are closely stacked in strings, good electrical-performance consistency and great enhancement of equipment production capacity on the premise of shortening the sintering period by more than 20 percent.
Description
Technical field
The present invention relates to sintering soft magnetic ferrite technology, the nitrogen kiln staged balanced atmosphere sintering process of the close knot soft magnet ferrite magnetic ring burnt in a heap of particularly a kind of suitable employing refractory materials saggar bunchiness.
Background technology
Sintering soft magnetic ferrite to be to pursue raising the output, energy-conservation, consumption reduction, promotes product quality simultaneously and is basic goal.Existing sintering soft magnetic ferrite technology is that magnetic ferrite magnetic core or magnet ring pile are sent into nitrogen protection kiln binder removal, intensification, insulation, cooling to load bearing board, through accomplishing sintering process more than 28-30 hour.No matter be soft magnetic ferrite smallclothes magnetic core or magnet ring, pile sintering to the load bearing board, its dress burn pile height and are very limited, and workload is very big, the sintering inefficiency.Pile is too high, because of dislocation takes place in vibration, causes distortion, and because of adhesion causes falling piece, quality product is difficult to guarantee that the sintering cost occupies high.
Summary of the invention
Problem to be solved by this invention just provides a kind of soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process; Realize Fast Sintering; Shorten under the prerequisite of 20% above time of sintering period; Realized that simultaneously soft magnet ferrite magnetic ring bunchiness closed assembly Mi Dui does not ftracture, piece is fallen in adhesion, and electrical property consistency is good, the target that equipment capacity promotes significantly.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme: soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process is characterized in that: comprise following technical process,
1) stows the refractory materials saggar and send in the nitrogen kiln the disposable bunchiness of soft magnet ferrite magnetic ring blank is close;
2) the nitrogen kiln is carried out stage hyperthermic treatment; The nitrogen kiln temperature is raised to 600 ℃ ± 30 ℃ from room temperature; And the speed with 320～480L/ branch continues to send into air when the nitrogen kiln temperature reaches 300 ℃ ± 15 ℃, after the nitrogen kiln temperature reaches 600 ℃ ± 30 ℃, is incubated 5～6 minutes;
3) the nitrogen kiln is carried out the two-stage hyperthermic treatment, the nitrogen kiln temperature is raised to 1250 ± 30 ℃ from 600 ℃ ± 30 ℃, and continue to send into air, after the nitrogen kiln temperature reaches 1250 ± 30 ℃, be incubated 18～22 minutes with the speed that 320～480L/ divides;
4) the nitrogen kiln is carried out the hyperthermic treatment of three stages, the nitrogen kiln temperature is raised to 1350 ± 40 ℃ from 1250 ℃ ± 30 ℃, be incubated processing after reaching 1350 ℃ ± 40 ℃;
5) follow balanced atmosphere curve main points the nitrogen kiln is carried out processing under cooling stage by stage, form the soft magnet ferrite magnetic ring work in-process after processing under cooling is accomplished;
6) see the soft magnet ferrite magnetic ring work in-process off the nitrogen kiln, carry out follow-up burin-in process;
7) the soft magnet ferrite magnetic ring work in-process after the burin-in process are carried out branch and survey and inspection eventually, eligible is a finished product.
Further, said stage hyperthermic treatment comprises following several stages:
1) from room temperature to 200 ℃ ± 10 ℃, heats up with 2.6～3.0 ℃/component velocity;
2), heat up with 1.3～1.5 ℃/component velocity from 200 ℃ ± 10 ℃ to 600 ℃ ± 30 ℃.
Further, said two-stage hyperthermic treatment comprises following several stages:
1), heats up with 2.45～2.75 ℃/component velocity from 600 ℃ ± 30 ℃ to 900 ℃ ± 30 ℃;
2), heat up with 1.60～1.75 ℃/component velocity from 900 ℃ ± 30 ℃ to 1250 ± 30 ℃;
Further, said three stages hyperthermic treatment heats up with 0.9～1.1 ℃/component velocity, reach 1350 ℃ ± 40 ℃ after the insulation treatment time be 5～6 hours, oxygen partial pressure is from 8%～5% gradual change in the nitrogen kiln.
Further, carry out stage by stage to the nitrogen kiln processing under cooling all is incubated 4～6 minutes when the nitrogen kiln temperature reaches 1250 ℃ ± 5 ℃, 1200 ℃ ± 5 ℃, 1180 ℃ ± 5 ℃, 1120 ℃ ± 5 ℃, 1090 ℃ ± 5 ℃, 1060 ℃ ± 5 ℃.
After adopting technique scheme; The present invention has following advantage: in the disposable refractory materials saggar of packing into of the close heap of soft magnet ferrite magnetic ring bunchiness; Reduced secondary row blank process; Practice thrift human and material resources, the blank condemnation factor descends significantly, product deformation, the ratio of falling piece, cracking, defective products descend significantly, satisfy the kiln charge space to greatest extent; Reduce the sintering period significantly, realize 24 hours, not only directly reduced energy consumption, on scheduling of production, help making nitrogen atmosphere protection bell jar kiln to avoid peak of power consumption simultaneously with interior sintering; Take staged balanced atmosphere sintering process curve, it is poor that consistence takes place when in nitrogen tunnel kiln, nitrogen bell jar kiln, having solved the close heap of ordinary sinter process curve sintering, the problem that the goods adhesion is serious; And, produce the suitable required different induction of multiple energy-saving electric light source electronic circuit, the factor, and the soft magnet ferrite magnetic ring of L-T curve through accurate control to process temperature-atmosphere curve; Technology stability, safety, circulation ratio strengthen, and goods consistence, stability promote.
Description of drawings
Below in conjunction with accompanying drawing the present invention is described further:
Fig. 1 among the present invention around the graph of a relation of junction temperature and soft magnet ferrite magnetic ring inductance;
The graph of a relation of the oxygen partial pressure and magnet ring factor when Fig. 2 is the soft magnet ferrite magnetic ring sintering.
Embodiment
Soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process comprises following technical process:
1) stows the refractory materials saggar and send in the nitrogen kiln the disposable bunchiness of soft magnet ferrite magnetic ring blank is close;
2) the nitrogen kiln is carried out stage hyperthermic treatment; The nitrogen kiln temperature is raised to 600 ℃ ± 30 ℃ from room temperature; And the speed with 320～480L/ branch continues to send into air when the nitrogen kiln temperature reaches 300 ℃ ± 15 ℃, after the nitrogen kiln temperature reaches 600 ℃ ± 30 ℃, is incubated 5～6 minutes;
3) the nitrogen kiln is carried out the two-stage hyperthermic treatment, the nitrogen kiln temperature is raised to 1250 ± 30 ℃ from 600 ℃ ± 30 ℃, and continue to send into air, after the nitrogen kiln temperature reaches 1250 ± 30 ℃, be incubated 18～22 minutes with the speed that 320～480L/ divides;
4) the nitrogen kiln is carried out the hyperthermic treatment of three stages, the nitrogen kiln temperature is raised to 1350 ± 40 ℃ from 1250 ℃ ± 30 ℃, be incubated processing after reaching 1350 ℃ ± 40 ℃;
5) follow balanced atmosphere curve main points the nitrogen kiln is carried out processing under cooling stage by stage, form the soft magnet ferrite magnetic ring work in-process after processing under cooling is accomplished;
6) see the soft magnet ferrite magnetic ring work in-process off the nitrogen kiln, carry out follow-up burin-in process;
7) the soft magnet ferrite magnetic ring work in-process after the burin-in process are carried out branch and survey and inspection eventually, eligible is a finished product.
Embodiment one:
Said stage hyperthermic treatment comprises following several stages:
1) from room temperature to 200 ℃, heats up with 2.6 ℃/component velocity;
2), heat up with 1.3 ℃/component velocity, and the speed with the 480L/ branch continues to send into air when the nitrogen kiln temperature reaches 310 ℃, is incubated 5 minutes then from 200 ℃ to 600 ℃.
Said two-stage hyperthermic treatment comprises following several stages:
1), heats up with 2.75 ℃/component velocity, and continue to send into air with the speed that 320L/ divides from 600 ℃ to 900 ℃;
2) from 900 ℃ to 1250 ℃, heat up with 1.75 ℃/component velocity, and continue to send into air with the speed that 320L/ divides, be incubated 22 minutes then.
Said three stages hyperthermic treatment heats up with 1.1 ℃/component velocity, reach 1350 ℃ ± 40 ℃ after the insulation treatment time be 6 hours, oxygen partial pressure is from 8%～5% gradual change in the nitrogen kiln.
Carry out stage by stage to the nitrogen kiln processing under cooling all is incubated 5 minutes when the nitrogen kiln temperature reaches 1250 ℃, 1195 ℃, 1180 ℃, 1115 ℃, 1085 ℃, 1060 ℃.
Embodiment two:
Said stage hyperthermic treatment comprises following several stages:
1) from room temperature to 200 ℃, heats up with 2.8 ℃/component velocity;
2) from 200 ℃ to 600 ℃, heat up with 1.4 ℃/component velocity, be incubated 5 minutes then, and the speed of when the nitrogen kiln temperature reaches 300 ℃, dividing with 400L/ continues to send into air.
Said two-stage hyperthermic treatment comprises following several stages:
1), heats up with 2.6 ℃/component velocity, and continue to send into air with the speed that 400L/ divides from 600 ℃ to 900 ℃;
2) from 900 ℃ to 1250 ℃, heat up with 1.67 ℃/component velocity, and continue to send into air with the speed that 400L/ divides, be incubated 20 minutes then.
Said three stages hyperthermic treatment heats up with 1.0 ℃/component velocity, reach 1350 ℃ ± 40 ℃ after the insulation treatment time be 5 hours, oxygen partial pressure is from 8%～5% gradual change in the nitrogen kiln.
Carry out stage by stage to the nitrogen kiln processing under cooling all is incubated 6 minutes when the nitrogen kiln temperature reaches 1255 ℃, 1205 ℃, 1175 ℃, 1120 ℃, 1090 ℃, 1065 ℃.
Embodiment three:
Said stage hyperthermic treatment comprises following several stages:
1) from room temperature to 200 ℃, heats up with 3.0 ℃/component velocity;
2), heat up with 1.5 ℃/component velocity, and the speed with the 320L/ branch continues to send into air when the nitrogen kiln temperature reaches 285 ℃, is incubated 6 minutes then from 200 ℃ to 600 ℃.
Said two-stage hyperthermic treatment comprises following several stages:
1), heats up with 2.45 ℃/component velocity, and continue to send into air with the speed that 480L/ divides from 600 ℃ to 900 ℃;
2) from 900 ℃ to 1250 ℃, heat up with 1.60 ℃/component velocity, and continue to send into air with the speed that 480L/ divides, be incubated 18 minutes then.
Said three stages hyperthermic treatment heats up with 0.9 ℃/component velocity, reach 1350 ℃ ± 40 ℃ after the insulation treatment time be 5 hours, oxygen partial pressure is from 8%～5% gradual change in the nitrogen kiln.
Carry out stage by stage to the nitrogen kiln processing under cooling all is incubated 5 minutes when the nitrogen kiln temperature reaches 1245 ℃, 1200 ℃, 1185 ℃, 1125 ℃, 1095 ℃, 1055 ℃.
The confirming of the highest temperature during relevant for three stages hyperthermic treatments, promptly 1350 ℃ ± 40 ℃ value confirm, and be as shown in Figure 1, under different sintering top temperatures, obtain different induction intensity product, and inductance intensity is linear direct ratio growth with sintering temperature.Therefore need confirm the nitrogen kiln is carried out the required top temperature that is raised to of three stages hyperthermic treatment according to the product of required production or customer requirement.Oxygen partial pressure PO
2Decision Fe
2+/Fe
3+ the ratio balance, thereby influence the variation of the factor in the soft magnet ferrite magnetic ring, as shown in Figure 2, oxygen partial pressure PO
2With the relation of the factor in the soft magnet ferrite magnetic ring, calculation formula is log PO
2=A-B/T, the coefficient that A, B confirm by test.
Technology of the present invention realizes Fast Sintering; Shorten under the prerequisite of 20% above time of sintering period; Realized that simultaneously soft magnet ferrite magnetic ring 13 only reaches that above bunchiness closed assembly Mi Dui does not ftracture, piece is fallen in adhesion, and electrical property consistency is good, the target that equipment capacity promotes significantly.
Except that above-mentioned preferred embodiment, the present invention also has other embodiment, and those skilled in the art can make various changes and distortion according to the present invention, only otherwise break away from spirit of the present invention, all should belong to the defined scope of accompanying claims of the present invention.
Claims (4)
1. soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process is characterized in that: comprise following technical process,
1) stows the refractory materials saggar and send in the nitrogen kiln the disposable bunchiness of soft magnet ferrite magnetic ring blank is close;
2) the nitrogen kiln is carried out stage hyperthermic treatment; The nitrogen kiln temperature is raised to 600 ℃ ± 30 ℃ from room temperature; And the speed with 320～480L/ branch continues to send into air when the nitrogen kiln temperature reaches 300 ℃ ± 15 ℃, after the nitrogen kiln temperature reaches 600 ℃ ± 30 ℃, is incubated 5～6 minutes;
3) the nitrogen kiln is carried out the two-stage hyperthermic treatment, the nitrogen kiln temperature is raised to 1250 ± 30 ℃ from 600 ℃ ± 30 ℃, and continue to send into air, after the nitrogen kiln temperature reaches 1250 ± 30 ℃, be incubated 18～22 minutes with the speed that 320～480L/ divides;
4) the nitrogen kiln is carried out the hyperthermic treatment of three stages, the nitrogen kiln temperature is raised to 1350 ± 40 ℃ from 1250 ℃ ± 30 ℃, be incubated processing after reaching 1350 ℃ ± 40 ℃;
5) follow balanced atmosphere curve main points the nitrogen kiln is carried out processing under cooling stage by stage; Form the soft magnet ferrite magnetic ring work in-process after processing under cooling is accomplished, wherein carry out stage by stage to the nitrogen kiln processing under cooling all is incubated 4～6 minutes when the nitrogen kiln temperature reaches 1250 ℃ ± 5 ℃, 1200 ℃ ± 5 ℃, 1180 ℃ ± 5 ℃, 1120 ℃ ± 5 ℃, 1090 ℃ ± 5 ℃, 1060 ℃ ± 5 ℃;
6) see the soft magnet ferrite magnetic ring work in-process off the nitrogen kiln, carry out follow-up burin-in process;
7) the soft magnet ferrite magnetic ring work in-process after the burin-in process are carried out branch and survey and inspection eventually, eligible is a finished product.
2. soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process according to claim 1, it is characterized in that: said stage hyperthermic treatment comprises following several stages:
1) from room temperature to 200 ℃ ± 10 ℃, heats up with 2.6～3.0 ℃/component velocity;
2), heat up with 1.3～1.5 ℃/component velocity from 200 ℃ ± 10 ℃ to 600 ℃ ± 30 ℃.
3. soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process according to claim 1, it is characterized in that: said two-stage hyperthermic treatment comprises following several stages:
1), heats up with 2.45～2.75 ℃/component velocity from 600 ℃ ± 30 ℃ to 900 ℃ ± 30 ℃;
2), heat up with 1.60～1.75 ℃/component velocity from 900 ℃ ± 30 ℃ to 1250 ± 30 ℃;
4. soft magnetic ferrite nitrogen kiln staged balanced atmosphere sintering process according to claim 1; It is characterized in that: said three stages hyperthermic treatment heats up with 0.9～1.1 ℃/component velocity; The insulation treatment time is 5～6 hours after reaching 1350 ℃ ± 40 ℃, and oxygen partial pressure is from 8%～5% gradual change in the nitrogen kiln.
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| CN201010539318A CN102050621B (en) | 2010-11-04 | 2010-11-04 | Stepped equilibrium-atmosphere sintering process for soft-magnetic ferrite nitrogen kiln |
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| CN201010539318A CN102050621B (en) | 2010-11-04 | 2010-11-04 | Stepped equilibrium-atmosphere sintering process for soft-magnetic ferrite nitrogen kiln |
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| CN106007736A (en) * | 2016-05-13 | 2016-10-12 | 泰州茂翔电子器材有限公司 | Sintering method for high-performance manganese zinc ferrite material |
| CN106365642B (en) * | 2016-08-31 | 2019-01-22 | 长兴柏成电子有限公司 | A kind of power-type magnetics substrate production technology |
| CN107098693B (en) * | 2017-04-28 | 2021-01-19 | 苏州冠达磁业有限公司 | High-frequency anti-interference manganese-zinc ferrite and preparation method thereof |
| CN115863012B (en) * | 2022-12-26 | 2023-09-05 | 长兴柏成电子有限公司 | Magnetic core and sintering process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1564281A (en) * | 2004-03-19 | 2005-01-12 | 高金海 | Method of preparing communication magnetic core |
| CN1872796A (en) * | 2006-06-23 | 2006-12-06 | 浙江大学 | Method for producing kiln furniture product of andalusite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3003599B2 (en) * | 1996-11-20 | 2000-01-31 | 日本電気株式会社 | Ni-Zn ferrite |
| JP2001302364A (en) * | 2000-04-20 | 2001-10-31 | Nippon Steel Corp | Alumina-magnesia-based castable refractory containing zirconium oxide and molten metal vessel for metal refining |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1564281A (en) * | 2004-03-19 | 2005-01-12 | 高金海 | Method of preparing communication magnetic core |
| CN1872796A (en) * | 2006-06-23 | 2006-12-06 | 浙江大学 | Method for producing kiln furniture product of andalusite |
Non-Patent Citations (2)
| Title |
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| JP特开2001-302364A 2001.10.31 |
| JP特开平10-152371A 1998.06.09 |
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