CN107986629A - A kind of lead-free glass powder with low melting point for nanocrystalline magnetic core insulating wrapped and preparation method thereof - Google Patents
A kind of lead-free glass powder with low melting point for nanocrystalline magnetic core insulating wrapped and preparation method thereof Download PDFInfo
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- CN107986629A CN107986629A CN201711219695.2A CN201711219695A CN107986629A CN 107986629 A CN107986629 A CN 107986629A CN 201711219695 A CN201711219695 A CN 201711219695A CN 107986629 A CN107986629 A CN 107986629A
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- Prior art keywords
- lead
- melting point
- low melting
- glass powder
- free glass
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
- C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
Abstract
The present invention relates to technical field of electronic materials, is specifically a kind of lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped and preparation method thereof.Its weight percent content is：Bi2O350~75%, B2O35~20%, SiO21~10%, ZnO1~20%, Na2O1~15%, Li2O1~10%, CuO1~10%, MnO21~10% and NiO1~10%.Its preparation method is：(1) precise prepares mixture；(2) mixture adds melting in crucible；(3) glass metal after water quenching is melted；(4) ball milling filters after drying；(5) sieving obtains the lead-free glass powder with low melting point that granularity is small, homogeneous after drying.Lead-free glass powder with low melting point produced by the present invention insulation and pressure-resistant functional, can improve Effective permeability, radial direction tensile strength and the ageing resistance of nanocrystalline magnetic core；Reduce it and use caused eddy-current loss in high frequency；And the problems such as solving organic coating agent present in existing insulating wrapped technique not environmentally, dielectric need to be used.
Description
Technical field
The present invention relates to technical field of electronic materials, is specifically a kind of Unlead low-smelting point of nanocrystalline magnetic core insulating wrapped
Glass dust and preparation method thereof.
Background technology
In recent years, all kinds of soft magnetic-powder cores are widely used in the fields such as the energy, electric, communication, auto industry, 21 century power supply
Increasingly to miniaturization, this is more suitable for high-frequency range with regard to inevitable requirement magnetic elements, therefore minimize, is intelligent,
Highly integrated, low-loss becomes the developing direction of magnetic device.Mainly there are ferrocart core, Fe-Si-Al magnetic core, MPP magnetic currently on the market
All kinds of soft magnetic-powder cores such as powder core.But very big, Fe-Si-Al magnetic core DC superposition characteristic and high frequency damage is lost in ferrocart core in high frequency
Excessive cost of consumption, MPP powder cores etc. limits it and further applies；Therefore, it is extremely urgent to develop new soft magnetic-powder core.
Nanocrystalline magnetic core has the excellent characteristics such as high frequency, high DC stacked, Frequency Power Loss compared to other powder cores,
With good development prospect.
The insulating wrapped technique of nanocrystalline magnetic core mainly uses organic coating agent, if any epoxy resin, polyvinyl alcohol, has
Machine silicones etc..Nanocrystalline magnetic core is after organic coating agent cladding, and comprehensive magnetic can preferably, but hybrid technique is complicated and coats
The ageing resistance of nanocrystalline magnetic core afterwards is weak, and magnetic property causes irreversibility to drop with heating problem in use
It is low, so as to reduce its service life；And while using organic coating agent, also need to use dielectric, cause cost to increase.
At present, the inorganic coating agent that in the market uses, if glass powder with low melting point is mostly containing larger to environment, human body harm
PbO, Tl2O, the nitrous oxide such as CdO.The states such as China, America and Europe, Japan also put into effect law in succession, prohibite electronic product
In must not contain lead, mercury, fluorine, Cr VI, smelling of polymerization biphenyl (PBB), polymerize smelling diphenyl ether and other venomous injurants
Matter, it is seen that electronic product is unleaded, Non-toxic is following development trend.
The content of the invention
For above-mentioned shortcoming of the prior art, the present invention is intended to provide a kind of insulation and pressure-resistant functional, energy
Improve Effective permeability, radial direction tensile strength and the ageing resistance of nanocrystalline magnetic core；It is reduced to produce in high frequency use
Eddy-current loss；And solve organic coating agent present in existing insulating wrapped technique not environmentally, dielectric problem need to be used
Lead-free glass powder with low melting point and preparation method thereof.
In order to solve the above technical problems, the Unlead low-smelting point glass for nanocrystalline magnetic core insulating wrapped of the present invention
Powder, its component and weight percent content are：Bi2O350~75%, B2O35~20%, SiO21~10%, ZnO1~20%,
Na2O1~15%, Li2O1~10%, CuO1~10%, MnO21~10% and NiO1~10%.
Preferably, its component and weight percent content are：Bi2O365~75%, B2O35~10%, SiO21~5%,
ZnO5~15%, Na2O1~10%, Li2O1~5%, CuO1~5%, MnO21~5%, NiO1~5%.
A kind of preparation method of the lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped of the present invention, including it is following
Step：
(1) precise is carried out by above-mentioned quality of material percentage, stirring rotation 1h is uniformly mixed in batch mixer；
(2) silica crucible is added mixture into, silica crucible is put into heating melting in Elema resistance furnace, heats melting temperature
Spend for 950~1150 DEG C, smelting time is 40~80min；
(3) glass metal of melting outflow is put into water quenching bucket through Water Quenching；
(4) after the frit after water quenching being dried 8h in 120 DEG C of baking ovens, ball mill wet-milling 40min (230r/min), mistake
Filter；
(5) dry 12~18h, screening in 120 DEG C of baking ovens by the frit after filtering, obtains the small (μ of D90≤10 of granularity
M), homogeneous lead-free glass powder with low melting point.
Wherein, the Bi2O3, B2O3, SiO2, Na2O, Li2O, CuO, MnO2And NiO is the city that purity is more than 99wt%
Sell powder.
Wherein, the step (3) is put into iron stand in water quenching bucket, and brandreth table top is from 1~4cm of the water surface, the glass of high temperature
Liquid is cooled down on table top, is collected after embrittlement, easy to ball mill grinding.
Wherein, when lead-free glass powder with low melting point made from the step (5) being used for nanocrystalline magnetic core insulating wrapped, need
Glass dust is added in nanocrystalline magnetic, the 3-8% of its shared nanocrystalline magnetic.
Beneficial effects of the present invention are：Firstth, lead-free glass powder with low melting point of the invention and nano particle have higher attached
Put forth effort with 85 × 10-7/ DEG C~95 × 10-7/ DEG C of suitable linear expansion coefficient, insulation resistance (40 μm, 800V) >=30G Ω,
Ultra-fine lead-free glass powder with low melting point can be obtained after ball milling sieving, after sintering, may replace traditional organic coating agent and dielectric.The
2nd, lead-free glass powder with low melting point softening temperature of the invention is less than general glass powder with low melting point, minimum up to 440 DEG C, favorably
Nano-crystalline granule is fully coated when lead-free glass powder with low melting point is in sintered molten, insulation performance is more preferable；3rd, nothing of the invention
Lead glass powder with low melting point chemical property is stablized, 500 DEG C -700 DEG C of sintering temperature, the radial direction tension of nanocrystalline magnetic core after sintering
Intensity is up to 250N.
Embodiment
In order to illustrate more clearly of the present invention, with reference to embodiment, the invention will be further described, art technology
Personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and should not limit the present invention's with this
Protection domain.
Embodiment 1
(1) precise Bi by mass percentage2O350%, B2O310%, SiO25%, ZnO15%, Na2O10%,
Li2O3%, CuO3%, MnO23%, NiO1%；
(2) material is put into batch mixer, stirring rotates 1h and is uniformly mixed；
(3) silica crucible is added mixture into, silica crucible is put into heating melting in Elema resistance furnace, heats melting temperature
Spend for 1000 DEG C, smelting time 40min；
(4) glass metal of melting outflow is through Water Quenching；
(5) after the frit after water quenching being dried 8h in 120 DEG C of baking ovens, ball mill wet-milling 40min (230r/min), mistake
Filter；
(6) frit after filtering is dried into 12h in 120 DEG C of baking ovens, sieving, obtains granularity small (D90≤10 μm), matter
The uniform lead-free glass powder with low melting point in ground；
After tested, the softening temperature of gained nanocrystalline magnetic core insulating wrapped lead-free glass powder with low melting point is 480 DEG C, heat
The coefficient of expansion is 85 × 10-7/ DEG C, insulation resistance (40 μm, 800V) 35G Ω；
Gained glass dust is added in nanocrystalline magnetic core according to 5% ratio, 700 DEG C of annealing, the footpath of gained powder core
To tensile strength 230N.
Embodiment 2
(1) precise Bi by mass percentage2O365%, B2O35%, SiO22%, ZnO10%, Na2O5%,
Li2O3%, CuO4%, MnO24%, NiO2%；
(2) material is put into batch mixer, stirring rotates 1h and is uniformly mixed；
(3) silica crucible is added mixture into, silica crucible is put into heating melting in Elema resistance furnace, heats melting temperature
Spend for 1050 DEG C, smelting time 60min；
(4) glass metal of melting outflow is through Water Quenching；
(5) after the frit after water quenching being dried 8h in 120 DEG C of baking ovens, ball mill wet-milling 40min (230r/min), mistake
Filter；
(6) frit after filtering is dried into 18h in 120 DEG C of baking ovens, sieving, obtains granularity small (D90≤10 μm), matter
The uniform lead-free glass powder with low melting point in ground；
After tested, the softening temperature of gained nanocrystalline magnetic core insulating wrapped lead-free glass powder with low melting point is 440 DEG C, heat
The coefficient of expansion is 95 × 10-7/ DEG C, insulation resistance (40 μm, 800V) 35G Ω；
Gained glass dust is added in nanocrystalline magnetic core according to 5% ratio, 700 DEG C of annealing, the footpath of gained powder core
To tensile strength 230N.
Embodiment 3
(1) precise Bi by mass percentage2O375%, B2O310%, SiO21%, ZnO5%, Na2O4%,
Li2O2%, CuO1%, MnO21%, NiO1%；
(2) material is put into batch mixer, stirring rotates 1h and is uniformly mixed；
(3) silica crucible is added mixture into, silica crucible is put into heating melting in Elema resistance furnace, heats melting temperature
Spend for 950 DEG C, smelting time 40min；
(4) glass metal of melting outflow is through Water Quenching；
(5) after the frit after water quenching being dried 8h in 120 DEG C of baking ovens, ball mill wet-milling 40min (230r/min), mistake
Filter；
(6) frit after filtering is dried into 16h in 120 DEG C of baking ovens, sieving, obtains granularity small (D90≤10 μm), matter
The uniform lead-free glass powder with low melting point in ground；
After tested, the softening temperature of gained nanocrystalline magnetic core insulating wrapped lead-free glass powder with low melting point is 450 DEG C, heat
The coefficient of expansion is 90 × 10-7/ DEG C, insulation resistance (40 μm, 800V) 35G Ω；
Gained glass dust is added in nanocrystalline magnetic core according to 5% ratio, 700 DEG C of annealing, the footpath of gained powder core
To tensile strength 230N.
Embodiment 4
(1) precise Bi by mass percentage2O370%, B2O35%, SiO22%, ZnO8%, Na2O7%,
Li2O3%, CuO2%, MnO22%, NiO1%；
(2) material is put into batch mixer, stirring rotates 1h and is uniformly mixed；
(3) silica crucible is added mixture into, silica crucible is put into heating melting in Elema resistance furnace, heats melting temperature
Spend for 1000 DEG C, smelting time 50min；
(4) glass metal of melting outflow is through Water Quenching；
(5) after the frit after water quenching dries 8h in 120 DEG C of baking ovens, ball mill wet-milling 40min (230r/min), mistake
Filter；
(6) frit after filtering is dried into 16h in 120 DEG C of baking ovens, sieving, obtains granularity small (D90≤10 μm), matter
The uniform lead-free glass powder with low melting point in ground；
After tested, the softening temperature of gained nanocrystalline magnetic core insulating wrapped lead-free glass powder with low melting point is 450 DEG C, heat
The coefficient of expansion is 90 × 10-7/ DEG C, insulation resistance (40 μm, 800V) 35G Ω；
Gained glass dust is added in nanocrystalline magnetic core according to 5% ratio, 700 DEG C of annealing, the footpath of gained powder core
To tensile strength 230N.
It is emphasized that above example is only present pre-ferred embodiments, it will be appreciated by those skilled in the art that with
Upper specifically described content is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Claims (6)
1. a kind of lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped, it is characterised in that its component and weight percent
It is than content：Bi2O350~75%, B2O35~20%, SiO21~10%, ZnO1~20%, Na2O1~15%, Li2O1~
10%, CuO1~10%, MnO21~10% and NiO1~10%.
2. the lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped according to claim 1, it is characterised in that its
Component and weight percent content are：Bi2O365~75%, B2O35~10%, SiO21~5%, ZnO5~15%, Na2O1~
10%, Li2O1~5%, CuO1~5%, MnO21~5%, NiO1~5%.
3. the preparation method of the lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped according to claim 1 or 2,
It is characterized in that：Comprise the following steps：
(1) precise is carried out by above-mentioned quality of material percentage, stirring rotation 1h is uniformly mixed in batch mixer；
(2) silica crucible is added mixture into, silica crucible is put into heating melting in Elema resistance furnace, and heating smelting temperature is
950~1150 DEG C, smelting time is 40~80min；
(3) glass metal of melting outflow is put into water quenching bucket through Water Quenching；
(4) after the frit after water quenching being dried 8h in 120 DEG C of baking ovens, ball mill wet-milling 40min (230r/min), filtering；
(5) frit after filtering is dried into 12~18h in 120 DEG C of baking ovens, screening, obtains granularity small (D90≤10 μm), matter
The uniform lead-free glass powder with low melting point in ground.
4. the lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped according to claim 1 or 2, its feature exist
In：The Bi2O3, B2O3, SiO2, Na2O, Li2O, CuO, MnO2And NiO is the commercial powder that purity is more than 99wt%.
5. the preparation method of the lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped according to claim 3, its
It is characterized in that：The step (3) is put into iron stand in water quenching bucket, and brandreth table top exists from 1~4cm of the water surface, the glass metal of high temperature
It is collected on table top after cooling, embrittlement, easy to ball mill grinding.
6. the preparation method of the lead-free glass powder with low melting point of nanocrystalline magnetic core insulating wrapped according to claim 3, its
It is characterized in that：, it is necessary to incite somebody to action when lead-free glass powder with low melting point made from the step (5) is used for nanocrystalline magnetic core insulating wrapped
Glass dust is added in nanocrystalline magnetic, the 3-8% of its shared nanocrystalline magnetic.
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| CN201711219695.2A CN107986629A (en) | 2017-11-28 | 2017-11-28 | A kind of lead-free glass powder with low melting point for nanocrystalline magnetic core insulating wrapped and preparation method thereof |
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| CN201711219695.2A CN107986629A (en) | 2017-11-28 | 2017-11-28 | A kind of lead-free glass powder with low melting point for nanocrystalline magnetic core insulating wrapped and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793756A (en) * | 2018-06-22 | 2018-11-13 | 贵州佰博新材料科技有限公司 | A kind of glass powder and preparation method thereof for Fe-Si-Al magnetic core insulating wrapped |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
| CN110066109A (en) * | 2019-05-28 | 2019-07-30 | 江西陶瓷工艺美术职业技术学院 | A kind of traditional decoration pigment flux and its application method |
| CN112499978A (en) * | 2020-12-24 | 2021-03-16 | 陕西科技大学 | Glass powder for low-melting-point electronic paste and preparation method thereof |
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| CN102010127A (en) * | 2009-09-07 | 2011-04-13 | 上海歌灵新材料科技有限公司 | Lead-free solder glass |
| CN104193180A (en) * | 2014-08-22 | 2014-12-10 | 洛阳兰迪玻璃机器股份有限公司 | Low-melting point glass powder |
| CN106565101A (en) * | 2016-11-08 | 2017-04-19 | 中国建筑材料科学研究总院 | Vacuum glass supporting material, preparation method and vacuum glass |
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| CN102010127A (en) * | 2009-09-07 | 2011-04-13 | 上海歌灵新材料科技有限公司 | Lead-free solder glass |
| CN104193180A (en) * | 2014-08-22 | 2014-12-10 | 洛阳兰迪玻璃机器股份有限公司 | Low-melting point glass powder |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793756A (en) * | 2018-06-22 | 2018-11-13 | 贵州佰博新材料科技有限公司 | A kind of glass powder and preparation method thereof for Fe-Si-Al magnetic core insulating wrapped |
| CN108793756B (en) * | 2018-06-22 | 2021-12-03 | 贵州佰博新材料科技有限公司 | Glass powder for insulating and coating iron-silicon-aluminum magnetic powder core and preparation method thereof |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
| CN110066109A (en) * | 2019-05-28 | 2019-07-30 | 江西陶瓷工艺美术职业技术学院 | A kind of traditional decoration pigment flux and its application method |
| CN112499978A (en) * | 2020-12-24 | 2021-03-16 | 陕西科技大学 | Glass powder for low-melting-point electronic paste and preparation method thereof |
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