CN106046862A - Boron nitride-covered spherical aluminum oxide and a preparing method thereof - Google Patents

Boron nitride-covered spherical aluminum oxide and a preparing method thereof Download PDF

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Publication number
CN106046862A
CN106046862A CN201610301797.8A CN201610301797A CN106046862A CN 106046862 A CN106046862 A CN 106046862A CN 201610301797 A CN201610301797 A CN 201610301797A CN 106046862 A CN106046862 A CN 106046862A
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Prior art keywords
boron nitride
ball
aluminium oxide
cladding
aluminum oxide
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CN201610301797.8A
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Chinese (zh)
Inventor
郭庆
王文川
高承兵
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Ya'an Betu New Materials Ltd By Share Ltd
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Ya'an Betu New Materials Ltd By Share Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40Compounds of aluminium
    • C09C1/407Aluminium oxides or hydroxides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • C09C3/063Coating
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/80Particles consisting of a mixture of two or more inorganic phases

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Boron nitride-covered spherical aluminum oxide and a preparing method thereof are provided. A compact boron nitride covering layer is on the surface of the spherical aluminum oxide. The spherical aluminum oxide is covered with boron nitride flaky microparticles, and therefore defects that spherical aluminum oxide is high in abrasion for mixing device molds due to high hardness and causes high damages to power original parts due to high hardness are overcome.

Description

A kind of ball-aluminium oxide of boron nitride cladding and preparation method thereof
Technical field
The present invention relates to the ball-aluminium oxide of a kind of boron nitride cladding, belong to heat filling field.The invention still further relates to State the preparation method of the ball-aluminium oxide of boron nitride cladding.
Background technology
Ball-aluminium oxide is a kind of conventional heat filling, but there is the high shortcoming big to abrasions such as moulds of hardness.Such as exist Chinese patent CN104559136A discloses use aluminium oxide and prepares epoxy resin, compound polyurethane material, although possess good Good heat conductivility, but owing to the high rigidity of aluminium oxide can cause damaging mould in molding process.This external Chinese patent CN102363577A discloses production method of a kind of heat conducting high-temperature alumina filling material and products thereof.Including: (1) is with oxidation Aluminum or aluminium hydroxide are raw material, add mineralizer;(2) shuttle kiln or tunnel cave is utilized to forge at a temperature of 1300-1500 DEG C Burn, insulation;(3) product after sintering soak is ground to form varigrained micropowder, to obtain final product.The inventive method can prepare height Proportion, high fill-ratio, the heat conducting high-temperature alumina filling material of low oil absorbency, obtained product thermal conductivity values is high, oil absorbency≤mg/ 100ml Oleum Ricini, tight dress density is 1.8~2.1g/cm3.Product prepared by the method can filling out as insulating heat-conductive polymer Material, is widely used in the fields such as heat-conducting plastic, heat conductive rubber, heat-conductive bonding agent, heat-conductive coating.But the aluminium oxide of this invention is same There is much higher hard in sample, when mechanographs such as being applied to plastics be can major injury die life, and more mold exchange can be made to enterprise Become the biggest cost burden.
The technology of existing raising heat conduction is to be used in mixed way, ball-aluminium oxide (firmly) and boron nitride owing to aluminium oxide causes firmly Boron nitride sheet crushes, and result heat conduction declines.This patent ball aluminum surface has boron nitride (soft) to be coated with, so not having boron nitride sheet to crush Problem.
From the foregoing, the present inventor have developed the novel cladding on a kind of ball aluminum surface and solves the abrasion of ball aluminum Big problem also improves thermal conductivity simultaneously.
Summary of the invention
Present invention aim at the deficiency for existing aluminium oxide heat filling abrasion mould, it is provided that a kind of novel nitridation Boron coated aluminum oxide, is not only able to effectively prevent and treat mould and is worn and torn by the aluminium oxide of extreme hardness, additionally it is possible to be effectively improved thermal conductivity, Therefore the cost of enterprise is significantly reduced.
The present invention uses following technical scheme:
1, the ball-aluminium oxide of a kind of boron nitride cladding, it is characterised in that alumina surface exists close boron nitride cladding Layer.
2, the ball-aluminium oxide being coated with according to the boron nitride of 1, it is characterised in that: the ball-aluminium oxide of described boron nitride cladding Average spherical degree be more than 0.8.
3, the ball-aluminium oxide being coated with according to the boron nitride of 1 or 2, it is characterised in that: described boron nitride layer is by boron nitride sheet Dress granule composition, the longest particle diameter of its in-plane is less than 5 microns.
4, the ball-aluminium oxide being coated with according to the boron nitride of 3, it is characterised in that: described boron nitride weight content is gross weight 0.1-50%.
5, the ball-aluminium oxide being coated with according to the boron nitride of 4, it is characterised in that the ball-aluminium oxide of described boron nitride cladding Mean diameter is 5 to 150 microns.
6, the preparation method of the ball-aluminium oxide of the boron nitride cladding described in 1-5, it is characterised in that comprise the following steps: will Ball-aluminium oxide and boron nitride carry out mechanical mixture according to the ratio of weight ratio 100: 2-20, incorporation time be 6 minutes little to 1 Time, obtain finished product.
Additionally, organic or inorganic binding agent also can be added in the mixed process of described 6.Organic binder such as asphalt mixtures modified by epoxy resin Fat, acryl resin, polyurethane etc., inorganic binding agent such as silica sol, phosphate cpd, aluminium hydroxide etc. are suitable for this Bright.Cement is usually 0.1 to the 10wt% of boron nitride, preferably 0.4-6wt%, further preferably 0.8-4%, further preferably 1-2%.
Described boron nitride weight content in 0.1-50% (based on aluminium oxide and boron nitride gross weight), preferably 0.5-40%, More preferably 1-30%, further preferably 4-10%, wherein the weight content of boron nitride can also be preferably 2%, 6%, 8%, 12%, 24%, 30%.
Present invention process is simple, by using ball-aluminium oxide and boron nitride to carry out mechanical mixture and be effectively prepared for boron nitride The ball-aluminium oxide that uniform close covers.Laminated structure and effective particle diameter due to boron nitride, it is possible to do not losing heat conduction effect On the premise of Guo, at utmost reduce the ball-aluminium oxide abrasion for mould.And the method for the present invention uses physics completely Mixing, is added without unnecessary small organic agents, the safety of material has been effectively ensured.
Accompanying drawing explanation
Fig. 1 boron nitride cladding ball-aluminium oxide schematic diagram.
Fig. 2 is boron nitride schematic diagram.
Fig. 3 is the boron nitride arrangement in spherical aluminum.
Fig. 4 is the Electronic Speculum figure of raw material spherical aluminum.
Fig. 5 is the spherical aluminum Electronic Speculum figure of cladding boron nitride.
Fig. 6 is the boron nitride details Electronic Speculum figure of cladding 1 micron in spherical aluminum
Drawing reference numeral: 1 ... ball-aluminium oxide 2 ... boron nitride 3 ... direction major diameter 4 in boron nitride face ... Boron nitride
Detailed description of the invention:
Embodiment: 1
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 1 in table 1, within 6 minutes, must be implemented with rotation-revolution mixer Example 1 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.The direction, face of boron nitride is Major diameter is less than 5 microns.
Embodiment: 2
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 2 in table 1, within 15 minutes, must be implemented with rotation-revolution mixer Example 2 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.
Embodiment: 3
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 3 in table 1, within 25 minutes, must be implemented with rotation-revolution mixer Example 3 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.
Embodiment: 4
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 4 in table 1, within 30 minutes, must be implemented with rotation-revolution mixer Example 4 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.
Embodiment: 5
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 5 in table 1, within 60 minutes, must be implemented with rotation-revolution mixer Example 5 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.
Embodiment: 6
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 6 in table 1, within 30 minutes, must be implemented with rotation-revolution mixer Example 6 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.
Embodiment: 7
Boron nitride and ball aluminum are coordinated in the ratio of the embodiment 7 in table 1, within 15 minutes, must be implemented with rotation-revolution mixer Example 7 sample.There is equal borazon clad in ball aluminum surface after mixed processing seen from electron microscopic observation.
Comparative example: 1-7
Using the ball aluminum in embodiment 1-7, carry out wear test in the case of not adding boron nitride, its result is at table In 1, " abrasion (milligram) (container content sample is ball aluminum) of polypropylene containers " part is listed.
Table 1
It can be seen that when using pure ball aluminum to carry out wear test, wear extent is much larger than using boron nitride bag from above-mentioned table Cover the wear extent of ball aluminum.The wherein boron nitride coated ball aluminum of embodiment 4 and 5 wear extent even 0 to mould.
Embodiment 8:
The boron nitride of embodiment 7 is coated with ball-aluminium oxide 250 weight portion and 100 weight portions molecular weight about 90,000 two Disperse with metal three cylinder after methyl-silicone oil mixing, cross and roll 3 times to obtain paste.
Comparative example 8:
By raw material ball-aluminium oxide 250 weight portion without boron nitride cladding and 100 weight portions of mean diameter 45 μm Disperse with metal three cylinder after the dimethicone mixing of molecular weight about 90,000, cross and roll 3 times to obtain paste.
Abrasion roll because of metal with the paste that the paste of embodiment 8 (white substantially) compares comparative example 8 seriously, color Substantially deepen aobvious Dark grey.
Abrasion loss method of testing:
The polypropylene containers weight of first precise rotation-revolution mixer.Add embodiment 1-7 corresponding ball aluminum feedstock Again weigh polypropylene containers and weigh after complete for sample portion being removed after boron nitride coated ball aluminum sample mixed one minute.Before mixing After container weight difference be abrasion loss.
Average spherical degree measuring method:
Taking pictures granule by scanning electron microscope, when particle diameter is more than 30 μm, use amplification is 500 times, particle diameter be 5 μm less than 30 μm time, using amplification is 3000 times, particle diameter be 1 μm with When going up and be less than 5 μm, using amplification is 5000 times, and being less than 1 μm at particle diameter is that the amplification of use is 50000 Times, think that (SEM photograph) measures projected area (A) and the girth (PM) of granule from secondary electron reflection, and obtain by below equation Average spherical degree.That is, if the orbicular area corresponding to girth (PM) is (B), sphericity A/B of its granule represents.False If orbicular girth is identical with the girth of sample granule (PM), because PM=2 π r, B=π r2, so B=π × (PM/2 π)2, The sphericity of this granule=A/B=A × 4 π/(PM)2.The sphericity of any 100 granules is obtained from SEM photograph image, Their meansigma methods is as average spherical degree
Beneficial effect
The present invention can effectively prevent and treat mould and be worn and torn by the aluminium oxide of extreme hardness, additionally it is possible to be effectively improved thermal conductivity.
Above-mentioned only several specific embodiments in the present invention are illustrated, but can not be as the protection model of the present invention Enclose, every zoom in or out according to the equivalence change done by the design spirit in the present invention or modification or equal proportion, all should Think and fall into protection scope of the present invention.

Claims (6)

1. the ball-aluminium oxide of a boron nitride cladding, it is characterised in that alumina surface exists close boron nitride clad.
The ball-aluminium oxide of boron nitride the most according to claim 1 cladding, it is characterised in that: the spherical oxygen of described boron nitride cladding The average spherical degree changing aluminum is more than 0.8.
3. the ball-aluminium oxide being coated with according to the boron nitride of claim 1 or 2, it is characterised in that: described boron nitride layer is by nitrogenizing Boron granule on chip forms, and the longest particle diameter of its in-plane is less than 5 microns.
The ball-aluminium oxide of boron nitride the most according to claim 3 cladding, it is characterised in that: described boron nitride weight content is total The 0.1-50% of weight.
The ball-aluminium oxide of boron nitride the most according to claim 4 cladding, it is characterised in that the spherical oxygen of described boron nitride cladding Change aluminum mean diameter and be 5 to 150 microns.
6. the preparation method of the ball-aluminium oxide of the boron nitride cladding described in claim 1-5, it is characterised in that include following step Rapid: ball-aluminium oxide and boron nitride are carried out mechanical mixture according to the ratio of weight ratio 100: 2-20, incorporation time be 6 minutes extremely 1 hour, obtain finished product.
CN201610301797.8A 2016-05-10 2016-05-10 Boron nitride-covered spherical aluminum oxide and a preparing method thereof Pending CN106046862A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110452418A (en) * 2019-09-25 2019-11-15 桂林电子科技大学 A kind of high thermal conductivity Kapton and preparation method thereof of core-shell structure heat filling preparation
CN114044681A (en) * 2021-11-24 2022-02-15 安徽壹石通材料科技股份有限公司 Boron nitride composite microsphere and preparation method thereof

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CN104448717A (en) * 2014-11-28 2015-03-25 桂林电器科学研究院有限公司 Low-viscosity heat-conducting casting rubber and preparation method thereof
CN105234834A (en) * 2015-08-27 2016-01-13 安徽威铭耐磨材料有限公司 Superfine-grained cubic boron nitride (CBN) grinding wheel with high abrasion resistance and thermal conductivity and preparation method thereof

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CN101544851A (en) * 2008-03-26 2009-09-30 河南富莱格超硬材料有限公司 Metallic bond hollow sphere-shaped super-hard compound material and manufacturing method thereof
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CN105234834A (en) * 2015-08-27 2016-01-13 安徽威铭耐磨材料有限公司 Superfine-grained cubic boron nitride (CBN) grinding wheel with high abrasion resistance and thermal conductivity and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110452418A (en) * 2019-09-25 2019-11-15 桂林电子科技大学 A kind of high thermal conductivity Kapton and preparation method thereof of core-shell structure heat filling preparation
CN110452418B (en) * 2019-09-25 2021-03-02 桂林电子科技大学 High-thermal-conductivity polyimide film prepared from core-shell structure heat-conducting filler and preparation method thereof
CN114044681A (en) * 2021-11-24 2022-02-15 安徽壹石通材料科技股份有限公司 Boron nitride composite microsphere and preparation method thereof
CN114044681B (en) * 2021-11-24 2022-11-04 安徽壹石通材料科技股份有限公司 Boron nitride composite microsphere and preparation method thereof

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Application publication date: 20161026