JPH04157159A - Method and device for synthesis of cubic boron nitride - Google Patents
Method and device for synthesis of cubic boron nitrideInfo
- Publication number
- JPH04157159A JPH04157159A JP28307190A JP28307190A JPH04157159A JP H04157159 A JPH04157159 A JP H04157159A JP 28307190 A JP28307190 A JP 28307190A JP 28307190 A JP28307190 A JP 28307190A JP H04157159 A JPH04157159 A JP H04157159A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- plasma
- substrate
- high frequency
- light source
- 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.)
- Pending
Links
- 230000015572 biosynthetic process Effects 0.000 title claims description 17
- 238000003786 synthesis reaction Methods 0.000 title claims description 10
- 229910052582 BN Inorganic materials 0.000 title claims description 7
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 7
- 238000000034 method Methods 0.000 title description 7
- 239000000758 substrate Substances 0.000 claims abstract description 43
- 125000004433 nitrogen atom Chemical group N* 0.000 claims abstract description 9
- 229910052796 boron Inorganic materials 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 86
- 239000002994 raw material Substances 0.000 claims description 12
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical group [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 238000001308 synthesis method Methods 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract 2
- 125000004429 atom Chemical group 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000010571 fourier transform-infrared absorption spectrum Methods 0.000 description 10
- 230000005284 excitation Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005281 excited state Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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- Chemical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、切削工具等の工具材料やヒートシンク等の電
子材料となる立方晶窒化硼素の合成方法および装置に関
する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method and apparatus for synthesizing cubic boron nitride, which can be used as tool materials such as cutting tools and electronic materials such as heat sinks.
［従来の技術］
立方晶窒化硼素（ｃ−Ｂ Ｎ ）は、ダイヤモンドに次
ぐ硬さと熱伝導率を有し、鉄族合金に対して極めて化学
的に安定であり、切削工具、金型等の耐久性向上への応
用あるいは半導体素子１発光素子等への応用など、幅広
い用途が考えられる。一般に、ｃ−ＢＮの製造には、プ
ラズマを用いた各種製造方法が知られている。[Prior art] Cubic boron nitride (c-BN) has hardness and thermal conductivity second only to diamond, is extremely chemically stable to iron group alloys, and is used for cutting tools, molds, etc. A wide range of applications can be considered, such as applications to improve durability or applications to semiconductor devices, light emitting devices, etc. Generally, various manufacturing methods using plasma are known for manufacturing c-BN.
従来、ＣＶＤ法を用いた立方晶窒化硼素（ｃ−ＢＮＩの
合成方法としては、特開昭６２−２０５２７７号公報に
開示されるように、マイクロ波ＣＶＤ法により、硼素原
子含有ガス、窒素原子含有ガスおよび水素ガスの混合ガ
スをマイクロ波無極放電中を通過させ、熱分解反応によ
り、３００〜１３００℃に加熱されている基板の表面に
ｃ−ＢＮを析出させる方法が知られている。Conventionally, as a method for synthesizing cubic boron nitride (c-BNI) using the CVD method, as disclosed in JP-A-62-205277, boron atom-containing gas and nitrogen atom-containing gas are synthesized by microwave CVD method. A method is known in which c-BN is deposited on the surface of a substrate heated to 300 to 1300° C. by a thermal decomposition reaction by passing a mixed gas of gas and hydrogen gas through a microwave non-polar discharge.
また、特開昭６３−１３４６６２号公報には、硼素原子
含有ガスおよび窒素原子含有ガスをエキシマレーザＣＶ
Ｄ法にて分解、励起状態とした後、高周波プラズマ中を
通過させ、３００〜２０００℃に加熱した基板の表面に
導入し、ｃ−ＢＮを析出させる方法が開示されている。Furthermore, Japanese Patent Application Laid-Open No. 63-134662 discloses that a boron atom-containing gas and a nitrogen atom-containing gas are heated using an excimer laser CV.
A method is disclosed in which c-BN is precipitated by being decomposed and brought into an excited state by method D, then passed through high-frequency plasma, and introduced onto the surface of a substrate heated to 300 to 2000°C.
［発明が解決しようとする課題］
しかし、特開昭６２−２０５２７７号公報の従来の合成
方法においては、基板表面を３００〜１３００℃と高温
状態にする必要があり、工具等の被膜に用いる場合、材
料に制限が生じてしまい、一般に加工性の良い金属では
使用できない場合もあり、また反応に用いるガスの条件
にも制約が多く、成膜状態の再現性が良くなかった。[Problems to be Solved by the Invention] However, in the conventional synthesis method disclosed in JP-A No. 62-205277, it is necessary to heat the substrate surface to a high temperature of 300 to 1300°C. However, there are restrictions on the materials, and metals that generally have good workability may not be used, and there are also many restrictions on the gas conditions used for the reaction, resulting in poor reproducibility of the film formation state.
一方、特開昭６３−１３４６６２号公報の従来法では、
上記従来法と同様に、基板が非常に高温にさらされると
いう問題に加え、反応ガスの分解、励起源として高価な
エキシマレーザを用いなければならないという問題があ
った。また特に、エキシマレーザは、励起ガスとして危
険性の高いガスを使用しているので、排ガス設備等にも
多大な投資を必要とするという問題もあった。On the other hand, in the conventional method disclosed in JP-A-63-134662,
Similar to the conventional method described above, in addition to the problem that the substrate is exposed to extremely high temperatures, there is also the problem that an expensive excimer laser must be used as an excitation source for decomposing the reaction gas. In particular, since excimer lasers use highly dangerous gases as excitation gases, there is a problem in that they require a large amount of investment in exhaust gas equipment and the like.
本発明は、かかる従来の問題点に鑑みてなされたもので
、ＣＶＤ法において、ｃ−ＢＮ形成に有利で、しかも安
価な紫外光源を使用し、低温で成膜可能なｃ−ＢＮの合
成方法および装置を提供することを目的とする。The present invention has been made in view of such conventional problems, and is a method for synthesizing c-BN that is advantageous for forming c-BN in the CVD method and can be formed into a film at a low temperature using an inexpensive ultraviolet light source. and equipment.
［課題を解決するための手段］
上記目的を達成するために、本発明は、ｃ−ＢＮを合成
するにあたり、硼素原子含有ガスおよび窒素原子含有ガ
スを原料ガスとして用い、真空チャンバ内に希ガス、Ｎ
２ガスまたはＮ２ガスの少なくとも１種をプラズマ光源
用ガスとして導入し、このガスをマイクロ波で励起させ
たプラズマを光源として原料ガスを分解励起させるとと
もに、原料ガスを３００Ｗ以上の高周波プラズマ中を通
過させ、３００Ｗ以上の高周波を加えた基板上にｃ−Ｂ
Ｎ膜を形成することとした。[Means for Solving the Problems] In order to achieve the above object, the present invention uses a boron atom-containing gas and a nitrogen atom-containing gas as source gases when synthesizing c-BN, and injects a rare gas into a vacuum chamber. , N
2 gas or N2 gas is introduced as a plasma light source gas, this gas is excited with microwaves, and the plasma is used as a light source to decompose and excite the raw material gas, and the raw material gas is passed through a high frequency plasma of 300 W or more. c-B on a board to which a high frequency of 300W or more was applied.
It was decided to form an N film.
また、本発明は、ｃ−ＢＮの合成装置において、マイク
ロ波プラズマ発生機構を備え、プラズマ光源と成膜室と
を同一チャンバ内に配置し、マイクロ波プラズマ発生機
構よりも基板側でかつ原料ガスの導入部と基板との間に
高周波プラズマ発生機構を備え、さらに基板外周にも高
周波発生機構を備えることとした。In addition, the present invention provides a c-BN synthesis apparatus that is equipped with a microwave plasma generation mechanism, that a plasma light source and a film forming chamber are arranged in the same chamber, and that the source gas is located closer to the substrate than the microwave plasma generation mechanism. A high-frequency plasma generation mechanism is provided between the introduction part and the substrate, and a high-frequency plasma generation mechanism is also provided on the outer periphery of the substrate.
すなわち、本発明は、硼素原子含有ガスおよび窒素原子
ガスをマイクロ波プラズマを光源とした光および高周波
プラズマにより分解、励起させ、基板上にｃ−ＢＮ膜を
形成するもので、硼素原子含有ガス以外の希ガス、Ｈｚ
ガスまたはＮ２ガスをマイクロ波無極放電内を通過させ
、プラズマを発生させてそのプラズマ発光を光源とし、
別系統から導入した硼素原子含有ガスおよび窒素原子含
有ガスを分解、励起させ、さらに高周波プラズマ中を通
過させて分解、励起を促進し、高周波によるバイアスを
加えた基板上にｃ−ＢＮ膜を成膜する。That is, the present invention forms a c-BN film on a substrate by decomposing and exciting a boron atom-containing gas and a nitrogen atom-containing gas using light from microwave plasma as a light source and high-frequency plasma. noble gas, Hz
Gas or N2 gas is passed through a microwave non-polar discharge to generate plasma and the plasma emission is used as a light source,
A boron atom-containing gas and a nitrogen atom-containing gas introduced from another system are decomposed and excited, and then passed through a high-frequency plasma to promote decomposition and excitation, forming a c-BN film on a substrate biased by the high frequency. To form a film.
［作 用］
光エネルギーのみでは、励起状態の硼素原子と窒素原子
とが互いに結合するエネルギーが不足してしまう。そこ
で、本発明では、高周波プラズマを用いて、さらに基板
に高周波バイアスを加えることでエネルギー準位を高め
、硼素原子と窒化原子とを結合させるに充分なエネルギ
ーを得ることとした。[Effect] Light energy alone lacks the energy for the excited state boron atoms and nitrogen atoms to bond with each other. Therefore, in the present invention, it was decided to use high frequency plasma and further apply a high frequency bias to the substrate to increase the energy level and obtain enough energy to bond boron atoms and nitride atoms.
なお、本発明において、マイクロ波の出力は、０．５〜
１．２ ｋＷが最も好ましい。出力が０．５ｋＷより小
さいと励起エネルギーが不足し、１．２ｋＷより大きい
とマイクロ波によるプラズマの分布が広がってしまい、
基板の温度上昇をもたらしてしまうからである。また、
高周波出力を３００Ｗ以上としたのは、３００Ｗより小
さいと励起エネルギーが不足してしまうからである。In addition, in the present invention, the output of the microwave is 0.5 to
1.2 kW is most preferred. If the output is less than 0.5kW, the excitation energy will be insufficient, and if it is greater than 1.2kW, the distribution of plasma due to the microwave will spread,
This is because the temperature of the substrate increases. Also,
The reason why the high frequency output is set to 300 W or more is because if it is smaller than 300 W, the excitation energy will be insufficient.
本発明において、プラズマ光源用ガスとしては、希ガス
、Ｈ，ガスまたはＮ２ガスのうちの少なくとも１種が用
いられる。また、硼素原子含有ガスとしては、ＢｚＨａ
、 Ｂｕｓ 、 ＢＢｒａ等が用いられ、窒素原子含有
ガスとしては、Ｎ、、 ＮＨ，等が用いられる。In the present invention, at least one of rare gas, H gas, and N2 gas is used as the plasma light source gas. In addition, as the boron atom-containing gas, BzHa
, Bus, BBra, etc. are used, and as the nitrogen atom-containing gas, N, , NH, etc. are used.
一方、合成装置において、プラズマ中心と基板との距離
は、マイクロ波の出力を０．５〜１．２ ｋＷとした場
合、５００〜７００ｍｍが最も好ましい。 ５００１未
満であると基板温度が上昇してしまい、また７００ｍｍ
を越えると基板上に到達する光が弱くなってしまうから
である。On the other hand, in the synthesis apparatus, the distance between the plasma center and the substrate is most preferably 500 to 700 mm when the microwave output is 0.5 to 1.2 kW. If it is less than 5001, the substrate temperature will rise, and if it is less than 700 mm
This is because if the value exceeds 1, the light reaching the substrate becomes weak.
［実施例］
（第１実施例）
図は、本実施例で用いた合成装置を示すもので、１で示
すのはチャンバ２の一端側に接続されたプラズマ光源用
ガス供給装置で、チャンバ２に設置されたマイクロ波導
波管３を通過する部分で光源用ガスはプラズマ化され、
励起光として利用される。４はマイクロ波発振装置であ
る。また、チャンバ２内の他端側内部には、サセプタ５
が設置されており、このサセプタ５上には基板６が載置
されている。サセプタ５は図示を省略したヒータにより
加熱可能である。[Example] (First Example) The figure shows a synthesis apparatus used in this example. Reference numeral 1 indicates a plasma light source gas supply device connected to one end of the chamber 2. The light source gas is turned into plasma in the part where it passes through the microwave waveguide 3 installed in the
Used as excitation light. 4 is a microwave oscillation device. Further, inside the other end side of the chamber 2, a susceptor 5 is provided.
is installed, and a substrate 6 is placed on this susceptor 5. The susceptor 5 can be heated by a heater (not shown).
マイクロ波導波管３と基板６との間には、原料ガス供給
装置７からチャンバ２内に原料ガスを供給する原料ガス
導入口８が設けられている。また、この原料ガス導入口
８と基板６との間のチャンバ２外周には、高周波プラズ
マ発生用コイル９が巻装されている。１０は高周波電源
である。この高周波電源１０は、サセプタ５にも接続さ
れている。さらに、チャンバ２には、排気−置１１が接
続されている。A source gas inlet 8 is provided between the microwave waveguide 3 and the substrate 6 to supply source gas into the chamber 2 from the source gas supply device 7 . Further, a high-frequency plasma generation coil 9 is wound around the outer periphery of the chamber 2 between the raw material gas inlet 8 and the substrate 6. 10 is a high frequency power source. This high frequency power source 10 is also connected to the susceptor 5. Furthermore, an exhaust station 11 is connected to the chamber 2 .
かかる構成の合成装置により、ｃ−ＢＮの合成を行うに
は、排気装置１１によりチャンバ２内を減圧にし、プラ
ズマ光源用ガスとしてＮ２ガスをフローさせた。マイク
ロ波出力は１ｋＷ、Ｎ２ガスの流量は２０ｃｃ／ｍｉｎ
とした。基板６の位置はマイクロ波プラズマの中心より
５００ｍｍの位置に設定した。In order to synthesize c-BN using the synthesizer having such a configuration, the pressure inside the chamber 2 was reduced by the exhaust device 11, and N2 gas was flowed as a plasma light source gas. Microwave output is 1kW, N2 gas flow rate is 20cc/min
And so. The position of the substrate 6 was set at a position 500 mm from the center of the microwave plasma.
Ｓｉウェハを基板６として、原料ガス供給装置７よりＢ
Ｃｆ２．およびＮ２ガスをそれぞれ０．２ Ｃｃ／ｍｉ
ｎおよび１Ｏｃｃ／ｍｉｎの流量としてチャンバ２内に
導入し、圧力をＩ Ｔｏｒｒとし、高周波出力を４００
Ｗとしてプラズマを発生させた。基板６に５００ｗの高
周波を加え、２００℃以下に加熱して、３時間の成膜を
行い、２μｍの厚さのｃ−ＢＮ膜を形成した。Using the Si wafer as the substrate 6, B is supplied from the raw material gas supply device 7.
Cf2. and N2 gas at 0.2 Cc/mi, respectively.
n and a flow rate of 1 Occ/min into the chamber 2, the pressure was I Torr, and the high frequency output was 400 Occ/min.
Plasma was generated using W. A high frequency wave of 500 W was applied to the substrate 6, and the substrate was heated to 200° C. or lower to form a film for 3 hours to form a c-BN film with a thickness of 2 μm.
この膜をＦＴ−ＩＲ（フーリエ変換赤外線吸収スペクト
ル）で調べたところ、１０５０ｃ＋ｎ−’に顕著な吸収
を示し、ｃ−ＢＮ膜の形成を確認できた。When this film was examined by FT-IR (Fourier transform infrared absorption spectrum), it showed remarkable absorption at 1050c+n-', confirming the formation of a c-BN film.
（第２実施例）
図に示す合成装置を用いて、Ｓｉウェハを基板６として
、原料ガス供給装置７よりＢＣｌ２３およびＮＨ，ガス
をそれぞれ０．２ ｃｃ／ｍｉｎおよび１０ｃｃ／ｍｉ
ｎの流量としてチャンバ２内に導入し、圧力をＩ Ｔｏ
ｒｒとし、高周波出力を４００Ｗとしてプラズマを発生
させた。(Second Example) Using the synthesis apparatus shown in the figure, using a Si wafer as the substrate 6, BCl23 and NH gas were supplied from the raw material gas supply device 7 at 0.2 cc/min and 10 cc/min, respectively.
n into the chamber 2 with a flow rate of I To
rr, and a high frequency output of 400W to generate plasma.
プラズマ光源用ガスとしては、Ｈｅガスをプラズマ光源
用ガス供給装置ｌよりフローさせた。マイクロ波出力は
１ｋＷ、Ｈｅガスの流量は２０ｃｃ／ｍｉｎとした。基
板６の位置はマイクロ波プラズマの中心より５００闘の
ところに設置し、基板６に４００Ｗの高周波を加え、２
００℃以下に加熱して、３時間の成膜を行って、２μｍ
の厚さのｃ−ＢＮ膜を形成した。As the plasma light source gas, He gas was flowed from the plasma light source gas supply device 1. The microwave output was 1 kW, and the He gas flow rate was 20 cc/min. The position of the substrate 6 is set at 500 mm from the center of the microwave plasma, and a high frequency of 400 W is applied to the substrate 6.
Heated to 00℃ or less and formed a film for 3 hours to form a film with a thickness of 2 μm.
A c-BN film with a thickness of .
この膜をＦＴ−ＩＲ（フーリエ変換赤外線吸収スペクト
ル）で調べたことろ、１０５１０５Ｏ’に顕著な吸収を
示し、ｃ−ＢＮ膜の形成を確認できた。When this film was examined by FT-IR (Fourier transform infrared absorption spectrum), it showed remarkable absorption at 105105O', confirming the formation of a c-BN film.
（第３実施例）
図に示す合成装置を用いて、Ｓｉウェハを基板６として
、原料ガス供給装置７よりＢＣｌ２３およびＮ２ガスを
それぞれ０．２ ｃｃ／ｍｉｎおよび１０ｃｃ／ｍｉｎ
の流量としてチャンバ２内に導入し、圧力をＩ Ｔｏｒ
ｒとし、高周波出力を４００Ｗとしてプラズマを発生さ
せた。(Third Example) Using the synthesis apparatus shown in the figure, using a Si wafer as the substrate 6, BCl23 and N2 gas were supplied from the raw material gas supply device 7 at 0.2 cc/min and 10 cc/min, respectively.
is introduced into the chamber 2 with a flow rate of I Tor
r, and the high frequency output was set to 400 W to generate plasma.
プラズマ光源用ガスとしては、Ｘｅガスをプラズマ光源
用ガス供給装置１よりフローさせた。マイクロ波出力は
１ｋＷ、Ｘｅガスの流量は２０ｃｃ／ｍｉｎとした。基
板６の位置はマイクロ波プラズマの中心より ５００
ｍｍのところに設置し、基板６に３５０ｗの高周波を加
え、２００℃以下に加熱して、３時間の成膜を行って、
２μｍの厚さのｃ−ＢＮ膜を形成した。As the plasma light source gas, Xe gas was flowed from the plasma light source gas supply device 1. The microwave output was 1 kW, and the Xe gas flow rate was 20 cc/min. The position of the substrate 6 is 500 mm from the center of the microwave plasma.
350 W of high frequency was applied to the substrate 6, heated to 200° C. or less, and formed a film for 3 hours.
A c-BN film with a thickness of 2 μm was formed.
この膜をＦＴ−ＩＲ（フーリエ変換赤外線吸収スペクト
ル）で調べたところ、１０５１０５Ｏ’に顕著な吸収を
示し、ｃ−ＢＮ膜の形成を確認できた。When this film was examined by FT-IR (Fourier transform infrared absorption spectrum), it showed remarkable absorption at 105105O', confirming the formation of a c-BN film.
（第４実施例）
図に示す合成装置を用いて、Ｓｉウェハを基板６として
、原料ガス供給装置７よりＢＣｌ２３およびＮ２ガスを
それぞれ０．２ ｃｃ／ｍｉｎおよび１０ｃｃ／ｍｉｎ
の流量としてチャンバ２内に導入し、圧力をＩ Ｔｏｒ
ｒとし、高周波出力を５００Ｗとしてプラズマを発生さ
せた。(Fourth Example) Using the synthesis apparatus shown in the figure, using a Si wafer as the substrate 6, BCl23 and N2 gas were supplied from the source gas supply device 7 at 0.2 cc/min and 10 cc/min, respectively.
is introduced into the chamber 2 with a flow rate of I Tor
r, and the high frequency output was set to 500 W to generate plasma.
プラズマ光源用ガスとしては、Ａｒガスをプラズマ光源
用ガス供給装置ｌよりフローさせた。マイクロ波出力は
１ｋＷ、Ａｒガスの流量は２０ｃｃ／ｍｉｎとした。基
板６の位置はマイクロ波プラズマの中心より ５００
ｍｍのところに設置し、基板６に３００Ｗの高周波を加
え、２００℃以下に加熱して、３時間の成膜を行って、
２μｍの厚さのｃ−ＢＮ膜を形成した。As the plasma light source gas, Ar gas was flowed from the plasma light source gas supply device 1. The microwave output was 1 kW, and the Ar gas flow rate was 20 cc/min. The position of the substrate 6 is 500 mm from the center of the microwave plasma.
300 W of high frequency was applied to the substrate 6, heated to 200° C. or less, and formed a film for 3 hours.
A c-BN film with a thickness of 2 μm was formed.
この膜をＦＴ−ＩＲ（フーリエ変換赤外線吸収スペクト
ル）で調べたところ、１０５１０５Ｏ’に顕著な吸収を
示し、ｃ−ＢＮ膜の形成を確認できた。When this film was examined by FT-IR (Fourier transform infrared absorption spectrum), it showed remarkable absorption at 105105O', confirming the formation of a c-BN film.
（第５実施例）
図に示す合成装置を用いて、Ｓｉウェハを基板６として
、原料ガス供給装置７よりＢ２Ｈ−およびＮＨ３ガスを
それぞれ０．２ ｃｃ／ｍｉｎおよび１０ｃｃ／ｍｉｎ
の流量としてチャンバ２内に導入し、圧力をＩ Ｔｏｒ
ｒとし、高周波出力を６００Ｗとしてプラズマを発生さ
せた。(Fifth Example) Using the synthesis apparatus shown in the figure, using a Si wafer as the substrate 6, B2H- and NH3 gases were supplied from the raw material gas supply device 7 at 0.2 cc/min and 10 cc/min, respectively.
is introduced into the chamber 2 with a flow rate of I Tor
r, and the high frequency output was set to 600 W to generate plasma.
プラズマ光源用ガスとしては、Ｎ２ガスおよびＡｒガス
をプラズマ光源用ガス供給装置１よりフローさせた。マ
イクロ波出力は１ｋＷ、ＨｚガスおよびＡｒガスの流量
はそれぞれ１Ｏｃｃ／ｍｉｎおよび２０ｃｃ７ｍｉｎと
した。基板６の位置はマイクロ波プラズマの中心より５
００ ｍｍのところに設置し、基板６に３００Ｗの高周
波を加え、２００℃に加熱して、３時間の成膜を行って
、２μｍの厚さのｃ−ＢＮ膜を形成した。As the plasma light source gas, N2 gas and Ar gas were flowed from the plasma light source gas supply device 1. The microwave output was 1 kW, and the flow rates of Hz gas and Ar gas were 1 Occ/min and 20 cc/min, respectively. The position of the substrate 6 is 5 points from the center of the microwave plasma.
00 mm, a high frequency of 300 W was applied to the substrate 6, the substrate 6 was heated to 200° C., and film formation was performed for 3 hours to form a c-BN film with a thickness of 2 μm.
この膜をＦＴ−ＩＲ（フーリエ変換赤外線吸収スペクト
ル）で調べたところ、１０５１０５Ｏ’に顕著な吸収を
示し、ｃ−ＢＮ膜の形成を確認できた。When this film was examined by FT-IR (Fourier transform infrared absorption spectrum), it showed remarkable absorption at 105105O', confirming the formation of a c-BN film.
［発明の効果］
以上のように、本発明のｃ−ＢＮの合成方法および装置
によれば、マイクロ波プラズマを光源とした光および高
周波プラズマにより原料ガスを分解、励起させ、高周波
を加えた基板上にｃ−ＢＮを形成することとしたので、
低温で、しかも安価にしてｃ−ＢＮを合成することがで
きる。[Effects of the Invention] As described above, according to the c-BN synthesis method and apparatus of the present invention, a material gas is decomposed and excited by light using microwave plasma as a light source and high-frequency plasma, and a substrate to which high-frequency waves are applied is produced. Since we decided to form c-BN on top,
c-BN can be synthesized at low temperatures and at low cost.
図は本発明のｃ−ＢＮ合成装置の一実施例を示す概略構
成図である。
１・・・・・・プラズマ光源用ガス供給装置２・・・・
・・チャンバ
３・・・・・・マイクロ波導波管
４・・・・・・マイクロ波発振装置
６・・・・・・基板
７・・・・・・原料ガス供給装置
８・・・・・・原料ガス導入口
９・・・・・・高周波プラズマ発生用コイル１０・・・
・・・高周波電源
特許出願人 オリンパス光学工業株式会社２・・・・
・・チャンバ
３・−・・・・マイクロ波導波管
４・・・・・・マイクロ波発振ＨＲ
６・・・・・・基板
７・・・・・・原料ガス供給装置
８・・・・−・原料ガス導入口
くThe figure is a schematic configuration diagram showing an embodiment of the c-BN synthesis apparatus of the present invention. 1... Gas supply device for plasma light source 2...
... Chamber 3 ... Microwave waveguide 4 ... Microwave oscillation device 6 ... Substrate 7 ... Raw material gas supply device 8 ... - Raw material gas inlet 9... High frequency plasma generation coil 10...
...High frequency power supply patent applicant Olympus Optical Industry Co., Ltd.2...
... Chamber 3 ... Microwave waveguide 4 ... Microwave oscillation HR 6 ... Substrate 7 ... Raw material gas supply device 8 ... -・Raw material gas inlet
Claims (2)
ガスとして用い、真空チャンバ内に希ガス，Ｈ＿２ガス
またはＮ＿２ガスの少なくとも１種をプラズマ光源用ガ
スとして導入し、このガスをマイクロ波で励起させたプ
ラズマを光源として原料ガスを分解励起させるとともに
、原料ガスを３００Ｗ以上の高周波プラズマ中を通過さ
せ、３００Ｗ以上の高周波を加えた基板上に立方晶窒化
硼素膜を形成することを特徴とする立方晶窒化硼素の合
成方法。(1) Using a boron atom-containing gas and a nitrogen atom-containing gas as source gases, at least one of rare gas, H_2 gas, or N_2 gas is introduced into the vacuum chamber as a plasma light source gas, and this gas is excited with microwaves. The material gas is decomposed and excited using the generated plasma as a light source, and the material gas is passed through a high frequency plasma of 300 W or more to form a cubic boron nitride film on a substrate to which a high frequency of 300 W or more is applied. Synthesis method of cubic boron nitride.
源と成膜室とを同一チャンバ内に配置し、マイクロ波プ
ラズマ発生機構よりも基板側でかつ原料ガスの導入部と
基板との間に高周波プラズマ発生機構を備え、基板外周
に高周波発生機構を備えたことを特徴とする立方晶窒化
硼素の合成装置。(2) Equipped with a microwave plasma generation mechanism, the plasma light source and the film forming chamber are placed in the same chamber, and high-frequency plasma is generated closer to the substrate than the microwave plasma generation mechanism and between the raw material gas introduction part and the substrate. A synthesis device for cubic boron nitride, characterized in that it is equipped with a generation mechanism and a high frequency generation mechanism is provided on the outer periphery of a substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28307190A JPH04157159A (en) | 1990-10-19 | 1990-10-19 | Method and device for synthesis of cubic boron nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28307190A JPH04157159A (en) | 1990-10-19 | 1990-10-19 | Method and device for synthesis of cubic boron nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04157159A true JPH04157159A (en) | 1992-05-29 |
Family
ID=17660832
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28307190A Pending JPH04157159A (en) | 1990-10-19 | 1990-10-19 | Method and device for synthesis of cubic boron nitride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04157159A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006042328B4 (en) * | 2006-09-01 | 2012-07-05 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for forming thin layers on substrate surfaces |
-
1990
- 1990-10-19 JP JP28307190A patent/JPH04157159A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006042328B4 (en) * | 2006-09-01 | 2012-07-05 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Method for forming thin layers on substrate surfaces |
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