WO2015122379A1 - 球状窒化ホウ素微粒子およびその製造方法 - Google Patents
球状窒化ホウ素微粒子およびその製造方法 Download PDFInfo
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- WO2015122379A1 WO2015122379A1 PCT/JP2015/053489 JP2015053489W WO2015122379A1 WO 2015122379 A1 WO2015122379 A1 WO 2015122379A1 JP 2015053489 W JP2015053489 W JP 2015053489W WO 2015122379 A1 WO2015122379 A1 WO 2015122379A1
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0646—Preparation by pyrolysis of boron and nitrogen containing compounds
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the present invention relates to spherical boron nitride fine particles suitable for high thermal conductive fillers and the like and a method for producing the same.
- Hexagonal boron nitride (hereinafter referred to as “boron nitride”) has lubricity, high thermal conductivity, insulation, etc., for solid lubricants, mold release agents such as molten gas and aluminum, and heat dissipation materials Widely used for fillers. Particularly in recent years, the importance of heat dissipation measures has increased due to the high performance of computers and electronic devices, and the high thermal conductivity of boron nitride has attracted attention.
- boron nitride has been studied for the purpose of imparting high thermal conductivity and insulating properties to resin layers such as resin substrates for printed wiring boards and flexible copper-clad laminates.
- the average particle diameter of general boron nitride is several ⁇ m to 20 ⁇ m, but the thickness of resin layers such as resin substrates for printed wiring boards and flexible copper clad laminates is about several tens of ⁇ m. If the average particle size of the resin is large, the dispersibility in the resin is poor and the surface smoothness cannot be obtained.
- Submicron class (0.1 ⁇ m) boron nitride fine particles are required.
- boron nitride In order for boron nitride to exhibit high thermal conductivity, it needs to be highly pure and highly crystalline. This does not change even with submicron class (0.1 ⁇ m) boron nitride fine particles.
- boron nitride has a characteristic scaly shape, and its thermal characteristics are overwhelmingly superior in the major axis or minor axis direction compared to the thickness direction. Therefore, for example, the thermal characteristics of a composite material in which boron nitride is filled in a resin such as silicone are greatly influenced by the directionality of the boron nitride fine particles in the composite material. However, for example, when a sheet-shaped composite material is produced, in many cases, the boron nitride fine particles lie down in the horizontal direction and do not exhibit sufficient thermal characteristics required in the vertical direction.
- boron nitride in order for boron nitride to be suitable as a highly thermally conductive filler, it is necessary to reduce the influence of directionality by making it spherical or agglomerated.
- Boron nitride is generally obtained by reacting a boron source (boric acid, borax, etc.) and a nitrogen source (urea, melamine, ammonia, etc.) at a high temperature, and scaly primary particles are formed from boric acid and melamine.
- a boron source boric acid, borax, etc.
- a nitrogen source urea, melamine, ammonia, etc.
- Aggregated “pine cone” boron nitride has been proposed (Patent Document 1).
- the aggregated particle diameter of boron nitride produced by this method is 50 ⁇ m or more, and it is difficult to produce submicron-class boron nitride fine particles that are the object of the present invention.
- Patent Documents 2 to 4 methods for obtaining boron nitride fine particles by vapor phase synthesis have been reported.
- Patent Documents 2 to 4 methods for obtaining boron nitride fine particles by vapor phase synthesis have been reported.
- the boron nitride fine particles obtained by these methods have low crystallinity, the lubricity and high thermal conductivity that are characteristic of boron nitride are insufficient.
- An object of the present invention is to provide submicron spherical boron nitride fine particles with high sphericity.
- the present invention employs the following means in order to solve the above problems.
- Spherical boron nitride fine particles having an average particle diameter of 0.01 to 1.0 ⁇ m, an orientation index of 1 to 15, a boron nitride purity of 98.0% by mass or more, and an average circularity of 0.80 or more.
- Ammonia / boric acid alkoxide boric acid alkoxide having a molar ratio of 1 to 10 and ammonia are reacted in an inert gas stream at 750 ° C or more within 30 seconds, and then inert with ammonia gas or ammonia gas.
- submicron spherical boron nitride fine particles having high sphericity can be provided.
- FIG. 1 It is the schematic of the manufacturing apparatus of the boron nitride fine particle of the baking conditions 1.
- FIG. 1 It is the schematic of the manufacturing apparatus of the boron nitride fine particle of the baking conditions 2.
- a white powder is continuously synthesized by a so-called gas phase reaction between volatilized boric acid alkoxide and ammonia in an inert gas stream using a tubular furnace 3 (firing condition 1).
- this white powder is fired in a tubular furnace 3 (resistance heating furnace) (firing condition 2).
- the fired product is placed in a boron nitride crucible and fired in an induction heating furnace to produce boron nitride fine particles (firing condition 3).
- “%” is based on a mass standard unless otherwise specified.
- firing condition 1 750 ° C. or higher
- firing condition 2 1,000 to 1,600 ° C.
- firing condition 3 1,800 to 2,200.
- a resistance heating method can be used as the tubular furnace 3
- an induction heating type electric furnace can be used as the tubular furnace 3 as the firing condition 3.
- the apparatus for producing boron nitride fine particles used in firing condition 1 includes a tubular furnace 3 (resistance heating furnace), a reaction tube (quartz tube) 2, a borate alkoxide container 1, a borate alkoxide introduction tube 4, and introduction of ammonia gas. It consists of a tube 5 and a sample collection container 6.
- the spherical boron nitride fine particles of the present invention are continuously synthesized by a so-called gas phase reaction between volatilized boric acid alkoxide and ammonia. For this reason, an apparatus capable of continuous synthesis is required, and in firing condition 1, for example, an apparatus using a tubular furnace 3 illustrated in FIG. 1 is preferably used.
- the tubular furnace 3 is not particularly limited, but it is preferable to use an electric furnace that is easy to handle.
- the basic principle of an electric furnace is to heat a heating element or the like constituting the furnace by energization to heat the inside of the furnace, and the electric furnace is subdivided according to the heating method and the material of the heating element.
- heating up to around 1,700 ° C. is possible by a resistance heating method using a heating element, but heating around 2,000 ° C. requires an induction heating method using a coil.
- silicon carbide, carbon, etc. are used for the material of a heat generating body, it is not specifically limited.
- the material of the reaction tube 2 used in the present invention is not particularly limited, but it is preferable to use alumina or quartz that is chemically stable and has good heat resistance.
- the quartz tube 2 is installed in the resistance heating furnace 3 and heated to a predetermined temperature. Trimethyl borate is put in the container 1 and introduced into the quartz tube 2 through the introduction tube 4 by nitrogen. On the other hand, ammonia is also introduced into the quartz tube 2 via the introduction tube 5. The introduced trimethyl borate and ammonia react in the heated quartz tube 2 to produce white powder (firing condition 1). Part of the generated white powder adheres to the quartz tube 2, but most of it is transported to the recovery container 6 by nitrogen or unreacted ammonia. A white powder (product 7) as a product is recovered from the recovery container 6.
- the temperature of the tubular furnace 3 is preferably 750 ° C. or higher.
- the average particle diameter of the boron nitride fine particles to be generated may be larger than 1.0 ⁇ m.
- the reaction between trimethyl borate and ammonia is completed within 30 seconds. If it exceeds 30 seconds, the average particle diameter of the boron nitride fine particles may be larger than 1.0 ⁇ m.
- trimethyl borate triethyl borate, triisopropyl borate and the like can be used. From the viewpoint of easy reaction with ammonia and availability, trimethyl borate is used. It is preferable to use it.
- trimethyl borate there is a trade name “TMB” manufactured by Tama Chemical Industry Co., Ltd. in addition to the reagents of each company.
- ammonia used in the present invention is not particularly limited, but a so-called “high purity” type containing no impurities is preferable.
- the inert gas is not particularly limited, but is a gas that does not easily cause a chemical reaction.
- Examples thereof include noble gases such as helium, neon, and argon, and nitrogen.
- the mixing ratio of boric acid alkoxide and ammonia is 1 to 10 in terms of molar ratio of ammonia / boric acid alkoxide.
- ammonia / boric acid alkoxide molar ratio is less than 1, the purity of the boron nitride fine particles may be lower than 98.0%, and when the molar ratio is higher than 10, the average particle diameter of the boron nitride fine particles is smaller than 0.01 ⁇ m. There is.
- boric acid alkoxide and ammonia The introduction of boric acid alkoxide and ammonia is stopped, the power of the tubular furnace 3 is turned off, and the white powder synthesized under the firing condition 1 is collected and fired under the firing condition 2 using, for example, the apparatus shown in FIG.
- the apparatus used under the firing condition 2 uses an alumina tube as the reaction tube 2 ′ in the resistance heating furnace 3 ′, and fills the center of the reaction tube with the white powder (product 7) synthesized under the firing condition 1, After setting in the heating furnace 3 ′, nitrogen was introduced from the introduction pipe 4 ′ and ammonia was introduced from the introduction pipe 5 ′. After raising the temperature to a predetermined temperature, baking is performed for a predetermined time. After firing, the resistance heating furnace 3 'is cooled and the fired product is recovered. In firing condition 2, it is also possible to use an induction heating furnace.
- the temperature of the resistance heating furnace 3 is 1,000 to 1,600 ° C. Outside this range, the orientation index of boron nitride fine particles may be greater than 15.
- the reaction time under calcination condition 2 is 1 hour or more. If it is less than 1 hour, the orientation index of the boron nitride fine particles may be larger than 15, and the boron nitride fine particles may have a scale shape and low circularity.
- the atmosphere of firing condition 2 is preferably an atmosphere of ammonia gas or a mixed gas of ammonia gas and inert gas.
- the boron nitride fine particles may have an orientation index greater than 15, a purity less than 98.0%, or a scale-like and low average circularity.
- the fired product fired under firing condition 2 is placed in a boron nitride crucible and further fired under firing condition 3 in which it is fired at a predetermined temperature in a nitrogen atmosphere in an induction heating furnace. Since the firing temperature is as high as about 2,000 ° C., it is preferable to use an induction heating furnace as the firing furnace.
- the temperature under firing condition 3 is 1,800-2,200 ° C. If it is lower than 1,800 ° C., the purity of the boron nitride fine particles may be lower than 98.0%, and if it is higher than 2,200 ° C., the boron nitride fine particles may be collapsed.
- the reaction time in calcination condition 3 is 0.5 hours or more. If it is less than 0.5 hour, the purity of the boron nitride fine particles may be lower than 98.0%.
- the average particle size of the boron nitride fine particles produced in the present invention is 0.05 to 1.0 ⁇ m. Outside this range, the dispersibility in the resin is poor and the surface smoothness cannot be obtained, and when dispersed, there is a problem that the resin layer cannot be kept high in strength.
- the alignment index of boron nitride particles produced in the present invention the ratio of the intensity I 100 of the by powder X-ray diffraction (002) plane and intensity I 002 of diffraction line (100) plane of the diffraction line (I 002 / I 100 ) and 1 to 15 from the viewpoint of obtaining high thermal conductivity.
- the boron nitride purity of the boron nitride fine particles produced in the present invention is 98.0% or more from the viewpoint of obtaining high thermal conductivity.
- the average circularity of the boron nitride fine particles produced in the present invention is 0.80 or more from the viewpoint of obtaining high thermal conductivity.
- the white powder recovered under firing condition 1 was fired with the apparatus shown in FIG.
- the white powder (product) collected under the firing condition 1 was filled in the center of the alumina tube 2 ′ and set in the resistance heating furnace 3 ′, and then nitrogen and ammonia were introduced from the introduction tubes 4 ′ and 5 ′, respectively.
- Firing condition 3 The fired product obtained under firing condition 2 was placed in a boron nitride crucible and fired at a predetermined temperature shown in Table 1 in an induction heating furnace in a nitrogen atmosphere. The average particle diameter, orientation index, boron nitride purity, and average circularity of the obtained boron nitride fine particles were measured. The results are shown in Table 1. The temperature, time, and firing atmosphere of firing conditions 1, 2, and 3 are also shown in firing conditions 1, 2, and 3, respectively. Moreover, the electron micrograph of the Example of this invention is shown in FIG. 3, and the electron micrograph of a comparative example is shown in FIG.
- Trimethyl borate Reagents manufactured by Wako Pure Chemical Industries, Ltd. Trimethoxyborane ammonia: High purity type commercial product
- Average particle diameter The average particle diameter was measured using a Coulter laser diffraction scattering particle size distribution analyzer, trade name “LS-230”.
- SEM scanning electron microscope
- TEM transmission electron microscope
Abstract
Description
特に近年、コンピューターや電子機器の高性能化により、放熱対策の重要性が増しており、窒化ホウ素の高熱伝導性が注目されている。
一般的な窒化ホウ素の平均粒子径は、数μm~20μmであるが、プリント配線板用樹脂基板やフレキシブル銅張積層板等の樹脂層の厚みには数十μm程度のものもあり、窒化ホウ素の平均粒子径が大きいと、樹脂への分散性が悪く、表面の平滑性が得られない、また、分散させた場合、ブツが発生し、樹脂層の強度を高く保つことができないことがあり、サブミクロンクラス(0.1μm)の窒化ホウ素微粒子が要求されている。
しかしながら、例えば、シート形状の複合材料を作製した場合、多くの場合、窒化ホウ素微粒子は横方向に寝てしまい、縦方向に必要な充分な熱特性を示さない。
しかしながら、この方法で作製された窒化ホウ素の凝集粒子径は50μm以上であり、本発明の目的のサブミクロンクラスの窒化ホウ素微粒子を作製するのは困難である。
しかしながら、これらの方法で得られた窒化ホウ素微粒子は、結晶性が低いため、窒化ホウ素の特徴である潤滑性や高熱伝導性が不充分である。
(1)平均粒子径0.01~1.0μm、配向性指数1~15、窒化ホウ素純度98.0質量%以上、及び平均円形度0.80以上であることを特徴とする球状窒化ホウ素微粒子である。
(2)アンモニア/ホウ酸アルコキシドのモル比1~10のホウ酸アルコキシドとアンモニアを不活性ガス気流中、750℃以上、30秒以内で反応させた後、アンモニアガス、又は、アンモニアガスと不活性ガスの混合ガスの雰囲気下、1,000~1,600℃、1時間以上で熱処理後、さらに、不活性ガス雰囲気下、1,800~2,200℃、0.5時間以上で焼成することを特徴とする球状窒化ホウ素微粒子の製造方法である。
なお、本発明における%は、特に断らない限り質量規準で示す。
一般的に、1,700℃付近までの加熱は、発熱体を用いた抵抗加熱方式で可能であるが、2,000℃付近の加熱は、コイルを用いた誘導加熱方式が必要となる。
なお発熱体の材質には、炭化ケイ素やカーボンなどが用いられるが特に限定されるものではない。
焼成条件2では、誘導加熱炉を用いることも可能である。
なお焼成温度が2,000℃前後と高温のため、焼成炉として誘導加熱炉を用いることが好ましい。
焼成条件1
石英管2を抵抗加熱炉3に設置し、所定温度に加熱する。ホウ酸トリメチルを容器1に入れ、窒素により導入管4を経由して石英管2に導入した。一方、アンモニアも導入管5を経由して石英管2に導入した。導入されたホウ酸トリメチルとアンモニアは加熱された石英管2内で反応し、白色粉末を生成した。生成した白色粉末(生成物)を回収容器6より回収した。
焼成条件1で回収した白色粉末を図2に示す装置で焼成した。
アルミナ管2’の中心に焼成条件1で回収した白色粉末(生成物)を充填し、抵抗加熱炉3’にセットした後、導入管4’、5’より窒素、アンモニアをそれぞれ導入した。表1に示す所定温度まで昇温した後に所定時間焼成し、焼成終了後、冷却し、焼成物を回収した。
焼成条件2で得られた焼成物を窒化ホウ素製ルツボに入れ、誘導加熱炉で窒素雰囲気下、表1に示す所定温度で焼成した。得られた窒化ホウ素微粒子の平均粒子径、配向性指数、窒化ホウ素純度、及び平均円形度を測定した。結果を表1に示す。
なお、焼成条件1、2、及び3の温度、時間、及び焼成雰囲気を各々焼成条件1、2、及び3に併記した。
また、本発明の実施例の電子顕微鏡写真を図3に、比較例の電子顕微鏡写真を図4に示す。
ホウ酸トリメチル:和光純薬工業社製試薬、トリメトキシボラン
アンモニア:高純度タイプ市販品
平均粒子径:平均粒子径の測定にはコールター製レーザー回折散乱法粒度分布測定装置、商品名「LS-230」を用いた。
配向性指数:X線回折装置(理学電機社製「Geiger Flex 2013型」)にて2θ=30°~25°の範囲で測定し、2θ=27~28°付近((002)面)の回折線の強度I002、2θ=41°付近((100)面)の回折線の強度I100を求めた。配向性指数は窒化ホウ素のX線回折のピーク強度比より、配向性指数=I002/I100で算出した。
窒化ホウ素純度:窒化ホウ素純度は次の方法により求めた。試料を水酸化ナトリウムでアルカリ分解後、水蒸気蒸留法によってアンモニアを蒸留し、これをホウ酸液に捕集した。この捕集液を硫酸規定液で滴定し、窒素量(N)を求めた後、以下の式より窒化ホウ素純度(BN)を算出した。
BN(%)=N(%)×1.772
平均円形度:走査型電子顕微鏡(SEM)もしくは透過型電子顕微鏡(TEM)で粒子像を撮影した後、画像解析(例えば、マウンテック社製、商品名「MacView」)を用いて粒子の投影面積(S)と周囲長(L)を測定した。円形度は以下の式で求めた。
円形度=4πS/L2
任意に選んだ100個の粒子について円形度を測定し、それらの平均値を該試料の平均円形度とした。
2 反応管(石英管)
2' 反応官(アルミナ管)
3、3’ 管状炉(抵抗加熱炉)
4 ホウ酸アルコキシドの導入管
4' 窒素の導入管
5、5’ アンモニアガスの導入管
6 サンプルの回収容器
7 生成物
Claims (2)
- 平均粒子径0.01~1.0μm、配向性指数1~15、窒化ホウ素純度98.0質量%以上、及び平均円形度0.80以上であることを特徴とする球状窒化ホウ素微粒子。
- アンモニア/ホウ酸アルコキシドのモル比が1~10のホウ酸アルコキシドとアンモニアを不活性ガス気流中、750℃以上、30秒以内で反応させた後、アンモニアガス、又は、アンモニアガスと不活性ガスの混合ガスの雰囲気下、1,000~1,600℃、1時間以上で熱処理後、さらに、不活性ガス雰囲気下、1,800~2,200℃、0.5時間以上で焼成することを特徴とする球状窒化ホウ素微粒子の製造方法。
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CN201580008547.9A CN105980298B (zh) | 2014-02-12 | 2015-02-09 | 球状氮化硼微粒及其制造方法 |
KR1020167021931A KR102258544B1 (ko) | 2014-02-12 | 2015-02-09 | 구상 질화붕소 미립자 및 그 제조 방법 |
JP2015562810A JP6467650B2 (ja) | 2014-02-12 | 2015-02-09 | 球状窒化ホウ素微粒子およびその製造方法 |
EP15749281.0A EP3106430B1 (en) | 2014-02-12 | 2015-02-09 | Spherical boron nitride particles and production method thereof |
US15/117,853 US10017386B2 (en) | 2014-02-12 | 2015-02-09 | Spherical boron nitride fine particles and production method thereof |
US15/955,211 US20180230012A1 (en) | 2014-02-12 | 2018-04-17 | Method of producing spherical boron nitride fine particles |
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2015193504A (ja) * | 2014-03-31 | 2015-11-05 | ナガセケムテックス株式会社 | 窒化ホウ素粒子、樹脂組成物および熱伝導性シート |
WO2017034003A1 (ja) * | 2015-08-26 | 2017-03-02 | デンカ株式会社 | 熱伝導性樹脂組成物 |
WO2019073690A1 (ja) * | 2017-10-13 | 2019-04-18 | デンカ株式会社 | 窒化ホウ素粉末、その製造方法及びそれを用いた放熱部材 |
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WO2021111909A1 (ja) * | 2019-12-06 | 2021-06-10 | デンカ株式会社 | 窒化ホウ素粒子及びその製造方法 |
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TWI639553B (zh) | 2018-11-01 |
US20160368769A1 (en) | 2016-12-22 |
EP3106430B1 (en) | 2018-07-18 |
JPWO2015122379A1 (ja) | 2017-03-30 |
CN105980298A (zh) | 2016-09-28 |
TW201536671A (zh) | 2015-10-01 |
EP3106430A4 (en) | 2017-11-08 |
KR102258544B1 (ko) | 2021-05-28 |
JP6467650B2 (ja) | 2019-02-13 |
KR20160122725A (ko) | 2016-10-24 |
US10017386B2 (en) | 2018-07-10 |
US20180230012A1 (en) | 2018-08-16 |
CN105980298B (zh) | 2018-12-18 |
EP3106430A1 (en) | 2016-12-21 |
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