JPH03202140A - Method for growing large cubic boron nitride single crystal - Google Patents
Method for growing large cubic boron nitride single crystalInfo
- Publication number
- JPH03202140A JPH03202140A JP34436989A JP34436989A JPH03202140A JP H03202140 A JPH03202140 A JP H03202140A JP 34436989 A JP34436989 A JP 34436989A JP 34436989 A JP34436989 A JP 34436989A JP H03202140 A JPH03202140 A JP H03202140A
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- boron nitride
- cubic boron
- single crystal
- diamond
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 133
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 47
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 16
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 32
- 239000010432 diamond Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000002093 peripheral effect Effects 0.000 claims abstract description 5
- 238000012545 processing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052796 boron Inorganic materials 0.000 abstract description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 abstract 1
- 239000006061 abrasive grain Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- -1 boron Chemical compound 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- IDBFBDSKYCUNPW-UHFFFAOYSA-N lithium nitride Chemical compound [Li]N([Li])[Li] IDBFBDSKYCUNPW-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/062—Diamond
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/0645—Boronitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/066—Boronitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0675—Structural or physico-chemical features of the materials processed
- B01J2203/068—Crystal growth
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、立方晶窒化ホウ素単結晶の育成方法に係り、
特に工具鋼やステンレス鋼等の鉄系材料の超精密切削工
具材料として使用可能な、高品質で大型の立方晶窒化ホ
ウ素単結晶の育成方法に関する。[Detailed Description of the Invention] (Industrial Application Field) The present invention relates to a method for growing a cubic boron nitride single crystal,
In particular, the present invention relates to a method for growing high-quality, large-sized cubic boron nitride single crystals that can be used as ultra-precision cutting tool materials for ferrous materials such as tool steel and stainless steel.
（従来の技術及び解決しようとする課題）立方晶窒化ホ
ウ素の大型結晶育成法の一つとして、例えば、「ジャー
ナル・アプライド・フィジックス（Ｊｏｕｒｎａｌ Ａ
ｐｐｌｉｅｄ Ｐｈｙｓｉｃｓ）」、 Ｖｏｌ。(Prior art and problems to be solved) As one of the methods for growing large crystals of cubic boron nitride, for example, "Journal Applied Physics (Journal A
pplied Physics)”, Vol.
６１、Ｎｏ、８（１９８７）ｐ、２８２２〜２８２５に
示されるような方法が知られている。61, No. 8 (1987) p. 2822-2825 is known.
この方法は、高温・高圧下で密閉された育成容器中に高
温部と低温部を作り、窒化ホウ素を溶解し得る溶媒を挾
んで、高温部に原料窒化ホウ素供給源を置き、低温部に
立方晶窒化ホウ素の単結晶からなる種結晶を置き、温度
による溶解度差を利用して、低温部に置いた前記種結晶
上に立方晶窒化ホウ素単結晶を育成する温度差法である
。In this method, a high-temperature section and a low-temperature section are created in a growth container that is sealed at high temperature and high pressure, a solvent capable of dissolving boron nitride is placed between them, a source of boron nitride is placed in the high-temperature section, and a cubic chamber is placed in the low-temperature section. This is a temperature difference method in which a seed crystal consisting of a single crystal of crystalline boron nitride is placed, and a cubic boron nitride single crystal is grown on the seed crystal placed in a low-temperature part by utilizing the solubility difference due to temperature.
しかし、この方法では、種結晶に立方晶窒化ホウ素結晶
が用いられるが、溶媒中に設置されるため、結晶育成が
種結晶面上に進行する前に種結晶自身の溶解が進行する
。そこで、種結晶の溶解を少しでも抑えるため、種結晶
は、第１図に示すように容器１の上端に設けられた小さ
な穴に配置される。この場合、育成方向は種結晶の溶媒
側に限られる。また、このようにしても、種結晶は、溶
媒に接しているため、表面が溶解を受けて荒れ、良質結
晶の育成が妨げられる。更に、種結晶として使用する砥
粒用窒化ホウ素は、大きさが通常０゜２１１１ｍと小さ
く、上記溶解を受けやすいと共に結晶性も良くない。However, in this method, a cubic boron nitride crystal is used as a seed crystal, but because it is placed in a solvent, the seed crystal itself dissolves before crystal growth progresses on the seed crystal surface. Therefore, in order to suppress dissolution of the seed crystal as much as possible, the seed crystal is placed in a small hole provided at the upper end of the container 1, as shown in FIG. In this case, the growth direction is limited to the solvent side of the seed crystal. Moreover, even if this is done, since the seed crystal is in contact with the solvent, the surface will be roughened by dissolution, and growth of high-quality crystals will be hindered. Furthermore, boron nitride for abrasive grains used as a seed crystal has a small size, usually 0°2111 m, and is susceptible to the above-mentioned dissolution and has poor crystallinity.
上述の理由から、大型良質単結晶の育成をより困難とし
、その結果、その潜在能力を期待されながら産業界で利
用できない原因となっている５本発明は、上記従来技術
の欠点を解消し、従来得ることのできなかった超精密切
削工具材料として利用可能な、高品質で大型の立方晶窒
化ホウ素単結晶を育成し得る方法を提供することを目的
とするものである。For the above-mentioned reasons, it has become more difficult to grow large, high-quality single crystals, and as a result, although their potential is expected, they cannot be used in industry. The purpose of the present invention is to provide a method for growing high-quality, large-sized cubic boron nitride single crystals that can be used as materials for ultra-precision cutting tools that could not be obtained conventionally.
（課題を解決するための手段）
本発明者等は、前記目的を達成すべく鋭意研究を重ねた
結果、種結晶として、従来用いられてきた砥粒用立方晶
窒化ホウ素単結晶の代わりに、ダイヤモンド単結晶が使
用できることを見い出し、ここに本発明をなしたもので
ある。(Means for Solving the Problems) As a result of intensive research to achieve the above object, the present inventors have developed a seed crystal, instead of the conventionally used cubic boron nitride single crystal for abrasive grains. It was discovered that a diamond single crystal could be used, and the present invention was created based on this discovery.
ホウ素原料を置き、低温部に種結晶としてダイヤモンド
結晶を置き、立方晶窒化ホウ素の熱力学的安定域の高温
・高圧下で処理することにより、ダイヤモンド結晶を核
として、その外周面上にそれと結晶面、結晶方位が一致
した立方晶窒化ホウ素単結晶を育成することを特徴とす
る立方晶窒化ホウ素大型単結晶の育成方法を要旨とする
ものである。A boron raw material is placed, a diamond crystal is placed as a seed crystal in a low-temperature part, and the process is carried out under high temperature and high pressure within the thermodynamic stability range of cubic boron nitride. The gist of this invention is a method for growing a large cubic boron nitride single crystal, which is characterized by growing a cubic boron nitride single crystal with matching planes and crystal orientations.
以下に本発明を更に詳細に説明する。The present invention will be explained in more detail below.
（作用）
ダイヤモンドの単結晶は、天然品、合成品に拘らず、良
質で大型のものが比較的簡単に入手でき、また、一般に
立方晶窒化ホウ素単結晶の育成に使用する溶媒に侵され
ない。更に、ダイヤモンドは立方晶窒化ホウ素と同一の
結晶構造をとり、格子定数も１％程度異なるに過ぎない
。(Function) Diamond single crystals, whether natural or synthetic, are relatively easy to obtain in good quality and large sizes, and are generally not affected by the solvent used to grow cubic boron nitride single crystals. Furthermore, diamond has the same crystal structure as cubic boron nitride, and the lattice constant is only about 1% different.
このため、ダイヤモンド結晶を種結晶に用いると、育成
溶媒に侵されることなく、また大きな歪３−
−
みを伴うことなく、ダイヤモンド結晶上に立方晶窒化ホ
ウ素の良質単結晶を育成させることが可能となる。Therefore, when a diamond crystal is used as a seed crystal, it is possible to grow a high-quality single crystal of cubic boron nitride on the diamond crystal without being attacked by the growth solvent or accompanied by large strains. becomes.
ダイヤモンド結晶を種結晶にした立方晶窒化ホウ素結晶
の育成は、具体的には、次の方法によって行われる。Specifically, the growth of a cubic boron nitride crystal using a diamond crystal as a seed crystal is performed by the following method.
第１図及び第２図は単結晶育成容器構成を示しており、
高圧・高温下で密閉された、例えば、モリブデン製の育
成容器１中に、高温部と低温部を作り、高温部に窒化ホ
ウ素原料２を置き、窒化ホウ素を溶解し得る溶媒３、例
えば、ホウ窒化リチウム（Ｌｉ２ Ｂ Ｎ２）を挾んで
、低温部に種結晶４としてダイヤモンド結晶を置く。Figures 1 and 2 show the configuration of the single crystal growth container.
A high temperature section and a low temperature section are created in a growth container 1 made of, for example, molybdenum, which is sealed under high pressure and high temperature, a boron nitride raw material 2 is placed in the high temperature section, and a solvent 3 that can dissolve boron nitride, such as boron, is placed in the high temperature section. A diamond crystal is placed as a seed crystal 4 in the low temperature part, sandwiching lithium nitride (Li2 B N2).
種結晶であるダイヤモンド結晶の大きさは、任意に選ぶ
ことができる。種結晶としてはダイヤモンドの単結晶の
ほか、ホウ素をドープした半導体ダイヤモンド結晶も使
用可能である。The size of the diamond crystal serving as the seed crystal can be arbitrarily selected. As a seed crystal, in addition to a diamond single crystal, a semiconductor diamond crystal doped with boron can also be used.
また、ダイヤモンド結晶の配置の仕方は、第１図に示す
従来法のように育成容器の上部の小さな穴に置いても、
或いは第２図に示すように育成容器内上端に置いても、
いずれでもよいが、より大型の単結晶育成という面から
すると、後者の方が任意の大きさの種結晶を利用できる
ので好ましい。In addition, the diamond crystals can be placed in a small hole at the top of the growth container as in the conventional method shown in Figure 1.
Alternatively, as shown in Figure 2, you can place it at the top of the growth container.
Either method may be used, but from the standpoint of growing a larger single crystal, the latter method is preferable because a seed crystal of any size can be used.
育成圧力、温度は、立方晶窒化ホウ素が熱力学的に安定
な圧力（４〜７ＧＰａ）及び温度（１３００〜２０００
℃）の範囲で行う。好ましくは５〜６ＧＰａの圧力、１
６００−１８００℃の温度である。The growth pressure and temperature are the pressure (4 to 7 GPa) and temperature (1300 to 2000 GPa) at which cubic boron nitride is thermodynamically stable.
(℃) range. Preferably a pressure of 5 to 6 GPa, 1
The temperature is 600-1800°C.
所定の高温・高圧で処理することにより、温度による溶
解度差を利用して、低温部に置いたダイヤモンド単結晶
上に立方晶窒化ホウ素単結晶を析出成長させることがで
きる。By processing at a predetermined high temperature and high pressure, a cubic boron nitride single crystal can be precipitated and grown on a diamond single crystal placed in a low-temperature part by utilizing the solubility difference due to temperature.
育成された単結晶は、種結晶（ダイヤモンド結晶）を核
とし、その外周面上にそれと結晶面、結晶方位が完全に
一致して包接されている。The grown single crystal has a seed crystal (diamond crystal) as its core, and is enclosed on its outer peripheral surface with the crystal plane and crystal orientation completely matching.
種結晶（ダイヤモンド結晶）と育成結晶（立方晶窒化ホ
ウ素単結晶）との両者間の接合強度は強く、このため、
種結晶を包接したまま、育成結晶を超精密切削工具材料
として利用することができる。The bonding strength between the seed crystal (diamond crystal) and the growing crystal (cubic boron nitride single crystal) is strong, and therefore,
The grown crystal can be used as an ultra-precision cutting tool material while containing the seed crystal.
（実施例） 次に本発明の実施例を示す。(Example) Next, examples of the present invention will be shown.
失凰鮭よ
従来法で種結晶として立方晶窒化ホウ素単結晶を用いた
育成実験に通常使用している育成容器構成を用いて、単
結晶育成実験を行った。A single-crystal growth experiment was conducted using a growth container configuration that is commonly used in conventional growth experiments using cubic boron nitride single crystals as seed crystals.
この育成容器は、第１図に示すように、種結晶（立方晶
窒化ホウ素単結晶）の溶解をできるだけ防ぐために、容
器１の上部に種結晶４を配置するための小さな穴が設け
られている。As shown in Fig. 1, this growth container is provided with a small hole in the upper part of the container 1 for placing the seed crystal 4 in order to prevent the seed crystal (cubic boron nitride single crystal) from dissolving as much as possible. .
本例では、上記育成容器構成において、原料２として立
方晶窒化ホウ素砥粒粉末（昭和電工製。In this example, in the above-mentioned growth container configuration, the raw material 2 is cubic boron nitride abrasive grain powder (manufactured by Showa Denko).
５ＢＮ−Ｔ、＃３２５−４００）を用い、溶媒３として
Ｌｉ、ＢＮ２を用い、種結晶４として平均粒径Ｑ 、
５ ｍｍの砥粒用ダイヤモンド単結晶を用いて、圧力が
５．５０Ｐａ、原料部の温度が約１７００℃となるよう
に加圧・加熱し、そのままの状態で３時間保持した。5BN-T, #325-400), Li and BN2 were used as the solvent 3, and the average particle size Q was used as the seed crystal 4.
Using a 5 mm diamond single crystal for abrasive grains, the material was pressurized and heated to a pressure of 5.50 Pa and a temperature of about 1700° C., and the material was kept in that state for 3 hours.
その結果、種結晶であるダイヤモンド単結晶上に、これ
を包接する形で、厚さ０．１〜０．３ｍｍの立方晶窒化
ホウ素の単結晶が育成された。育成された結晶は、自形
面を持つもので、結晶面の方位は種結晶であるダイヤモ
ンドの自形面と完全に一致していた。育成結晶の破面を
走査型電子顕微鏡間
で観察したところ、第３図に示すように、臂弊面の違い
から接合面が見られた。上側が種結晶領域で、下側が育
成結晶領域であり、それらの接合面は一様であって破壊
は生じておらず、両者が原子オーダーで強固に結合し、
完全に一体化していることが確かめられた。As a result, a cubic boron nitride single crystal having a thickness of 0.1 to 0.3 mm was grown on and surrounding the diamond single crystal as the seed crystal. The grown crystal had an euhedral plane, and the orientation of the crystal plane completely matched the euhedral plane of the seed crystal, diamond. When the fractured surface of the grown crystal was observed using a scanning electron microscope, a bonding surface was observed due to the difference in the arm and back surfaces, as shown in FIG. The upper side is the seed crystal region, the lower side is the growing crystal region, and their bonding surfaces are uniform and no breakage occurs, and the two are strongly bonded on the atomic order.
It was confirmed that they were completely integrated.
失亀虹至
第２図に示すように、容器上部に穴のおいていない育成
容器を用い、種結晶４として粒径約２１１Ｉ１１で温度
差法により育成した自形面の良く発達した合成ダイヤモ
ンド単結晶を容器上端に置き、他の構成は実施例１と同
一にして、育成時間１５時間で育成実験を行った。As shown in Figure 2, a synthetic diamond monomer with a well-developed euhedral surface was grown as a seed crystal 4 by the temperature difference method with a grain size of approximately 211I11 using a growth container without a hole in the upper part of the container. The crystal was placed at the top of the container, the other configuration was the same as in Example 1, and a growth experiment was conducted for a growth time of 15 hours.
その結果、実施例１と同様に、種結晶であるダイヤモン
ドを包接するように、厚さ約２ｍｍの立方晶窒化ホウ素
の単結晶膜を持った粒径約５ｍ＋ｎの結晶が育成された
。結晶は自形面を持つもので、結７
８−
晶面の方位は種結晶であるダイヤモンドの自形面と一致
していた。また、実施例」と同様、立方晶窒化ホウ素の
成長層とダイヤモンド種結晶の境界は強く結合していた
。As a result, as in Example 1, crystals with a grain size of about 5 m+n and having a single crystal film of cubic boron nitride with a thickness of about 2 mm were grown so as to include the diamond seed crystal. The crystal had an euhedral plane, and the orientation of the crystal 7 8 - crystal plane coincided with the euhedral plane of the diamond, which was the seed crystal. Further, as in Example 1, the boundary between the cubic boron nitride growth layer and the diamond seed crystal was strongly bonded.
（発明の効果）
以上詳述したように、本発明によれば、ダイヤモンド単
結晶を種結晶として用い、その外周面に立方晶窒化ホウ
素単結晶を育成するので、一種の複合結晶ではあるが、
従来得ることの難しかった大型立方晶窒化ホウ素単結晶
を得ることが可能である。この育成単結晶は、種結晶と
育成結晶間の接合面が完全に一体化しており、接合面を
起点にして破壊が生じていないものである。(Effects of the Invention) As detailed above, according to the present invention, a diamond single crystal is used as a seed crystal and a cubic boron nitride single crystal is grown on its outer peripheral surface, so although it is a kind of composite crystal,
It is possible to obtain large cubic boron nitride single crystals, which have been difficult to obtain in the past. In this grown single crystal, the joint surfaces between the seed crystal and the grown crystal are completely integrated, and no breakage occurs starting from the joint surface.
切削加工具として利用した場合、結晶全体の強度が高く
、切削加工点における被削材との耐摩耗性が充分得られ
るので、超精密切削工具として好適である。When used as a cutting tool, the crystal as a whole has high strength and provides sufficient wear resistance with the work material at the cutting point, making it suitable as an ultra-precision cutting tool.
また、本発明によって得られる単結晶は、本質的にヘテ
ロエピタキシャル成長による接合結晶であるので、結晶
を半導体化させることにより電子・光学素子として利用
することも可能となる。例えば、種結晶として、ホウ素
をドープしたｐ型半導体ダイヤモンド結晶を用い、溶媒
中にシリコンを混入させてｎ型の半導体立方晶窒化ホウ
素単結晶を育成させると、ｐ−ｎ接合ダイオードができ
る。Further, since the single crystal obtained by the present invention is essentially a bonded crystal formed by heteroepitaxial growth, it can also be used as an electronic/optical element by converting the crystal into a semiconductor. For example, if a p-type semiconductor diamond crystal doped with boron is used as a seed crystal and silicon is mixed in a solvent to grow an n-type semiconductor cubic boron nitride single crystal, a p-n junction diode is produced.
これは、極端条件下で使用可能な電子素子として。It can be used as an electronic device under extreme conditions.
また紫外線領域の発光素子として期待される。It is also expected to be used as a light-emitting element in the ultraviolet region.
第１図及び第２図は立方晶窒化ホウ素単結晶を育成する
ための育成容器の構成を示す図で、第１図は育成容器の
上部に設けた小さい穴に種結晶を置く場合を示し、第２
図は種結晶を直接育成容器上部に置く場合を示し、
第３図は実施例で育成した立方晶窒化ホウ素単結晶破面
の走査型電子顕微鏡写真である。
１・・・モリブデン製育成容器、２・・・窒化ホウ素原
料、３・・・育成溶媒、４・・・種結晶。
第
２
図
第
図Figures 1 and 2 are diagrams showing the structure of a growth container for growing cubic boron nitride single crystals, and Figure 1 shows the case where a seed crystal is placed in a small hole provided at the top of the growth container. Second
The figure shows the case where a seed crystal is directly placed on the top of the growth container, and FIG. 3 is a scanning electron micrograph of a fractured surface of a cubic boron nitride single crystal grown in an example. DESCRIPTION OF SYMBOLS 1... Molybdenum growth container, 2... Boron nitride raw material, 3... Growth solvent, 4... Seed crystal. Figure 2
Claims (1)
を挾んで高温部に窒化ホウ素原料を置き、低温部に種結
晶としてダイヤモンド結晶を置き、立方晶窒化ホウ素の
熱力学的安定域の高温・高圧下で処理することにより、
ダイヤモンド結晶を核として、その外周面上にそれと結
晶面、結晶方位が一致した立方晶窒化ホウ素単結晶を育
成することを特徴とする立方晶窒化ホウ素大型単結晶の
育成方法。In a single crystal growth vessel, a boron nitride raw material is placed in the high temperature section with a solvent capable of dissolving boron nitride in between, and a diamond crystal is placed as a seed crystal in the low temperature section, and the temperature and pressure within the thermodynamic stability range of cubic boron nitride are increased. By processing below,
A method for growing a large cubic boron nitride single crystal, which is characterized by using a diamond crystal as a core and growing a cubic boron nitride single crystal on the outer peripheral surface of the diamond crystal whose crystal plane and crystal orientation coincide with that of the diamond crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34436989A JPH03202140A (en) | 1989-12-28 | 1989-12-28 | Method for growing large cubic boron nitride single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP34436989A JPH03202140A (en) | 1989-12-28 | 1989-12-28 | Method for growing large cubic boron nitride single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03202140A true JPH03202140A (en) | 1991-09-03 |
| JPH0478336B2 JPH0478336B2 (en) | 1992-12-10 |
Family
ID=18368707
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP34436989A Granted JPH03202140A (en) | 1989-12-28 | 1989-12-28 | Method for growing large cubic boron nitride single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03202140A (en) |
-
1989
- 1989-12-28 JP JP34436989A patent/JPH03202140A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0478336B2 (en) | 1992-12-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100577894C (en) | Large area, uniformly low dislocation density GaN substrate and process for making the same | |
| Dwiliński et al. | On GaN crystallization by ammonothermal method | |
| US7078731B2 (en) | Gallium nitride crystals and wafers and method of making | |
| US7097707B2 (en) | GaN boule grown from liquid melt using GaN seed wafers | |
| JP4942270B2 (en) | Crystalline gallium nitride and method of forming crystalline gallium nitride | |
| Korostelin et al. | Vapour growth and characterization of bulk ZnSe single crystals | |
| JP2007015918A (en) | Method for reducing defect concentration in crystal | |
| US6844084B2 (en) | Spinel substrate and heteroepitaxial growth of III-V materials thereon | |
| JP4184441B2 (en) | Mechanical and chemical polishing of crystals and epitaxial layers of GaN and Ga ▲ lower 1-xy ▼ Al ▲ lower x ▼ In ▲ lower y ▼ N | |
| US6153165A (en) | Single crystal and method of producing the same | |
| US6187279B1 (en) | Single crystal SIC and method of producing the same | |
| Syväjärvi et al. | Anisotropic etching of SiC | |
| CN102969241A (en) | Annealing method for reducing epitaxial film defects and epitaxial film obtained by using same | |
| Bockowski | Growth and doping of GaN and AlN single crystals under high nitrogen pressure | |
| KR100288473B1 (en) | SINGLE CRYSTAL SiC AND PROCESS FOR PREPARING THE SAME | |
| JPH03202140A (en) | Method for growing large cubic boron nitride single crystal | |
| Hanser et al. | Growth and fabrication of 2 inch free-standing GaN substrates via the boule growth method | |
| Bean et al. | Epitaxial CdTe films on GaAs/Si and GaAs substrates | |
| JPH1112100A (en) | Single crystal sic and its production | |
| JP2006265149A (en) | Method for producing dast crystal and method for planting seed crystal | |
| WO2021210398A1 (en) | Method for producing aluminum nitride substrate, aluminum nitride substrate, and method for suppressing introduction of dislocation into aluminum nitride growth layer | |
| WO2021210397A1 (en) | Method for manufacturing semiconductor substrate, semiconductor substrate, and method for suppressing introduction of displacement to growth layer | |
| WO2023188575A1 (en) | Group iii element nitride substrate and production method for group iii element nitride substrate | |
| JP2932559B2 (en) | Synthesis method of large diamond single crystal | |
| WO2023188574A1 (en) | Group iii element nitride substrate and production method for group iii element nitride substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |