JP5838289B2 - 超高硬度ナノ双晶窒化ホウ素バルク材料及びその合成方法 - Google Patents
超高硬度ナノ双晶窒化ホウ素バルク材料及びその合成方法 Download PDFInfo
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- 229910052582 BN Inorganic materials 0.000 title claims description 125
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 125
- 239000013590 bulk material Substances 0.000 title claims description 22
- 238000001308 synthesis method Methods 0.000 title description 4
- 239000002245 particle Substances 0.000 claims description 27
- 239000013078 crystal Substances 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 18
- 230000015572 biosynthetic process Effects 0.000 claims description 16
- 238000003786 synthesis reaction Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 229910052950 sphalerite Inorganic materials 0.000 claims description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000002159 nanocrystal Substances 0.000 claims 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical group [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 description 29
- 238000002441 X-ray diffraction Methods 0.000 description 14
- 239000010432 diamond Substances 0.000 description 13
- 229910003460 diamond Inorganic materials 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 230000036316 preload Effects 0.000 description 4
- 239000003870 refractory metal Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000005121 nitriding Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 241001596784 Pegasus Species 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- -1 borate ester Chemical class 0.000 description 1
- 238000012769 bulk production Methods 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000005555 metalworking Methods 0.000 description 1
- MLSKXPOBNQFGHW-UHFFFAOYSA-N methoxy(dioxido)borane Chemical compound COB([O-])[O-] MLSKXPOBNQFGHW-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- WXRGABKACDFXMG-UHFFFAOYSA-N trimethylborane Chemical compound CB(C)C WXRGABKACDFXMG-UHFFFAOYSA-N 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- 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
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Description
(1)ナノ球状窒化ホウ素(オニオンライク構造)粒子を原料として、金型に投入し、プレフォームに押し付ける。
(2)プレフォームを高圧合成金型に投入して、4〜25GPa、1200〜2300℃の条件下で合成する。
(3)減圧して冷却させる。
1)ナノ双晶窒化ホウ素バルクの体積は1〜2000mm3であり、例えば1〜1500mm3、5〜1500mm3、5〜1000mm3、10〜1500mm3、10〜800mm3、10〜500mm3、或10〜200mm3である。
2)ナノ双晶窒化ホウ素バルクのビッカース硬度は60〜120GPaであり、例えば65、70、75、80、85又は90GPaから100、105、110又は115GPaまでである。
3)ナノ双晶窒化ホウ素バルクの破壊靭性(K1C)は5〜15MPa・m1/2であり、例えば、6〜14MPa・m1/2、又は8〜13MPa・m1/2である。
4)ナノ双晶窒化ホウ素バルクの結晶粒径は5〜100nmであり、例えば、6、8、10、12、15、18又は20nmから70、75、80、85、90又は95nmまでである。
5)双晶構造は結晶粒の5〜30%を備え、双晶の平均的な厚さが1〜15nmである。
6)ナノ双晶窒化ホウ素バルクは、無色(或いはライトブルー)で透明な結晶体である。
1)本発明は、工芸が簡単で、反応原料に対して特別な処理が要らなく、高圧合成パラーメータが制御し易い。
2)バルク材料が高温超高圧合成方法で製造され、材料の密度が高い。
3)超硬ナノ双晶多結晶立方(又は複相)窒化ホウ素バルクは1〜2000mm3の範囲の相対的に大きな体積を有する。
4)ナノ双晶窒化ホウ素バルク材料の破壊靭性(K1C)は5〜15MPa・m1/2である。
5)ナノ双晶窒化ホウ素バルクの結晶粒径は5〜100nmである。
6)ナノ双晶窒化ホウ素バルクは無色(或いはライトブルー)の透明な晶体である。
Claims (10)
- 超高硬度ナノ双晶窒化ホウ素バルク材料の高圧合成製造方法であって、(1)オニオンライク構造を有するナノ球状窒化ホウ素粒子を原料として、金型に投入してプレフォームに押し込むステップと、
(2)前記プレフォームを高圧合成金型に投入して、4〜25GPaと1200〜2300℃で合成させるステップと、
(3)減圧して冷却させるステップと
を備える製造方法。 - 前記ナノ双晶窒化ホウ素バルク材料のビッカース硬度が60〜120GPaであることを特徴とする請求項1に記載の製造方法。
- 前記超高硬度ナノ双晶窒化ホウ素バルク材料の体積が1〜2000mm3であることを特徴とする請求項1又は2に記載の製造方法。
- 前記超高硬度ナノ双晶窒化ホウ素バルク材料は、内部に、結晶粒径が5〜100nmの閃亜鉛鉱構造のナノ結晶である高密度双晶を備えることを特徴とする請求項1又は2に記載の製造方法。
- 前記オニオンライク構造を有するナノ球状窒化ホウ素の粒径が5〜70nmであることを特徴とする請求項1に記載の製造方法。
- 前記ステップ(2)を1〜120分間行うことを特徴とする請求項1に記載の製造方法。
- 立方構造であり、結晶粒径5〜100nm、ビッカース硬度60〜120GPaのナノ双晶を、内部に備える超高硬度ナノ双晶窒化ホウ素バルク材料。
- 前記窒化ホウ素バルク材料的体積が1〜2000mm3であることを特徴とする請求項7に記載の超高硬度ナノ双晶窒化ホウ素バルク材料。
- 前記超高硬度ナノ双晶窒化ホウ素バルク材料は、
晶体構造が、立方晶閃亜鉛鉱の単相、又は、立方晶閃亜鉛鉱と少量の六方晶系ウルツ鉱とからなる相であり、
結晶内に、双晶厚さが2〜15nmであり、双晶密度が5〜30%である双晶構造が形成されている、
ことを特徴とする請求項7に記載の超高硬度ナノ双晶窒化ホウ素バルク材料。 - 前記超高硬度ナノ双晶窒化ホウ素バルク材料の破壊靭性(K1C)が5〜15 MP・m1/2であることを特徴とする請求項7〜9のいずれかに記載の超高硬度ナノ双晶窒化ホウ素バルク材料。
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