JPS61194171A - Method for producing a laminated material in which boron nitride is deposited on the surface of a MoBN film formed on a substrate - Google Patents
Method for producing a laminated material in which boron nitride is deposited on the surface of a MoBN film formed on a substrateInfo
- Publication number
- JPS61194171A JPS61194171A JP3457285A JP3457285A JPS61194171A JP S61194171 A JPS61194171 A JP S61194171A JP 3457285 A JP3457285 A JP 3457285A JP 3457285 A JP3457285 A JP 3457285A JP S61194171 A JPS61194171 A JP S61194171A
- Authority
- JP
- Japan
- Prior art keywords
- boron nitride
- film
- deposited
- producing
- substrate
- 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
- 229910052582 BN Inorganic materials 0.000 title claims description 22
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 22
- 229910015215 MoBN Inorganic materials 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000002648 laminated material Substances 0.000 title description 5
- 239000000758 substrate Substances 0.000 title description 4
- 239000000919 ceramic Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 229910052796 boron Inorganic materials 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
本発明はＭｏＢＮ膜の表面に窒化ボロンを析出させた金
属・セラミック積層材料の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing a metal-ceramic laminate material in which boron nitride is deposited on the surface of a MoBN film.
更に詳しくはＢＮ膜によりＭＯの高温における耐酸化性
を高め、ガスの吸着性を少なくした材料、またＢＮの絶
縁膜を持つ機能的性質を有する材料として有用な積層材
料の製造方法に関する。More specifically, the present invention relates to a material in which the oxidation resistance of MO at high temperatures is increased and gas adsorption is reduced by using a BN film, and a method for producing a laminated material useful as a material having functional properties and having a BN insulating film.
従来技術
一般に金属・セラミック積層材料はセラミックを保護膜
として内部金属を保護し、また、セラミック層自体に機
能上の役割を持たせた電子素子等に利用される。BACKGROUND OF THE INVENTION In general, metal-ceramic laminated materials are used in electronic devices, etc., in which the ceramic layer is used as a protective film to protect internal metals, and the ceramic layer itself has a functional role.
これらの材料においては金属とセラミックの界面での密
着性が良好であること、また電子素子等に利用する場合
は更に膜の一様性、膜厚の制御性が要求される。Ｌ７か
し、セラミックの融点は金属の融点に比べて高いこと（
窒化ボロンの融点は３０００ｒ）、金属の表面が反応性
に富むとして、金属の表面を化学的気相蒸着法によって
セラミックを被覆する方法は知られている。These materials are required to have good adhesion at the interface between metal and ceramic, and when used in electronic devices, etc., furthermore, uniformity of the film and controllability of the film thickness are required. L7 However, the melting point of ceramics is higher than that of metals (
Since the melting point of boron nitride is 3000 r) and the surface of the metal is highly reactive, a method is known in which the surface of the metal is coated with ceramic by chemical vapor deposition.
しかし、この方法で窒化はう素セラミック被覆を行うと
、膜に不純物が含有し、またＢＮの融点が高いため、金
属材料を１０００〜２０００Ｃと言う非常に高い温度に
加熱しなければならず、しかもその操作も面倒である欠
点があった。そのほか、物理的方法として、真空蒸着法
、イオンプレー型インク法、スパッタ法によりセラミッ
クよると、膜が不均一で密着性も悪く、母材を加熱して
おく必要がある等の欠点があった。However, when coating boron nitride ceramics using this method, the film contains impurities, and because BN has a high melting point, the metal material must be heated to a very high temperature of 1000 to 2000C. Moreover, there was a drawback that the operation was troublesome. In addition, physical methods such as vacuum evaporation, ion spray ink, and sputtering have been used to create ceramic films, which have disadvantages such as uneven film formation, poor adhesion, and the need to heat the base material. .
本発明者らはこの欠点がなく、比較的低温で、且つ容易
ＫＢＮ膜で被覆する方法について研究の結果、本発明者
らの一人がさきにチタンを含まないオーステナイト系ス
テンレス鋼の成分ＫＮを０．１〜０．３％、Ｂを０．０
０５〜０．０２％、Ｃｅを０．００１〜０．１％（ただ
し、俤は重量係を示す。）を添加した合金を作り、これ
を真空中で７ｏｏｃ程度に加熱すると、合金内部から表
面にＢＮが析出して膜を形成し得ることを究明し得た。As a result of our research into a method of coating with a KBN film that does not have this drawback, is relatively low temperature, and can be easily coated with KBN film, one of the inventors has previously found that the composition KN of austenitic stainless steel, which does not contain titanium, can be reduced to 0. .1-0.3%, B 0.0
By making an alloy containing 0.05 to 0.02% Ce and 0.001 to 0.1% Ce (however, the weight indicates weight) and heating it in a vacuum to about 70oC, the surface of the alloy will be removed from the inside of the alloy. It was found that BN can be precipitated to form a film.
（％願昭５８−１４４４１９号）しかし、この方法によ
ると、金属がチタンを含まないオーステナイト系ステン
レス鋼に限られ、また・セリウムを必須とする問題点が
あった。(% Application No. 58-144419) However, this method has the problem that the metal is limited to austenitic stainless steel that does not contain titanium, and also requires cerium.
発明の目的
本発明は前記問題点を解消しようとするものであり、そ
の目的はセリウムの添加を必要とせず、真空中での加熱
によりセラミックとなる成分（Ｂ、Ｎ）を合金内部から
表面に析出させてＢＮ＠を形成させることにより密着性
が優れ、かつ均一にセラミック鼻で被覆された金属・セ
ラの結果、モリブデン及び窒化ボロンをターゲットとし
て使用し、例えばモリブデンターゲット上に窒化ボロン
の小片を並べて、アルゴンガスｘ、ｙは原子係を表わす
、ｘ〉０、Ｙ＞Ｏ１ｘ＋ｙ（１００）の組成からなる膜
が得られ、Ｂ、Ｎを高濃度に含有させたものが容易に得
られること、及びこの生成膜を真空中で５００〜１００
０ｒｌＣ加熱すると、窒素、壷素が表面に拡散結合して
窒化ボロンを析出することを究明し得た。この知見に基
いて本発明を完成した。Purpose of the Invention The present invention attempts to solve the above-mentioned problems, and its purpose is to transfer components (B, N) that become ceramic by heating in vacuum from the inside of the alloy to the surface without the need for adding cerium. By depositing and forming BN@, the metal/cera has excellent adhesion and is uniformly coated with a ceramic nose. Molybdenum and boron nitride are used as targets, for example, small pieces of boron nitride are placed on a molybdenum target. Argon gases x and y represent atomic ratios, a film having a composition of x>0, Y>O1x+y (100) can be obtained, and a film containing B and N at a high concentration can be easily obtained; And this produced film was heated to 500 to 100 in vacuum.
It was found that when heated at 0rlC, nitrogen and nitride diffusely bond to the surface to precipitate boron nitride. The present invention was completed based on this knowledge.
本発明の要旨は、モリブデン及び窒化ボロン（ただし、
ｘ、ｙは前記と同じものを表わす）で示されるＭｏ Ｂ
Ｎ膜を作り、これを真空中で５００〜１０００ Ｄ Ｋ
加熱して表面に窒化ボロンを析ｔｂ −ｓ ＜’Ｉｔ□
よ、よオ、や。８、ワ。７つよ窒化ボロンを析出させた
金属拳セラミック積層材料の製造方法に漬る。The gist of the present invention is that molybdenum and boron nitride (however,
x, y are the same as above)
Create a N film and heat it in vacuum at 500 to 1000 DK.
Boron nitride is deposited on the surface by heating tb -s <'It□
Yo, yo, yo. 8. Wa. 7 We will discuss the manufacturing method of metal fist ceramic laminated material with boron nitride precipitated.
本発明において高周波スパッタ法を使用するのは、絶縁
体である窒化はう素をターゲラ）セして使用するからで
ある。高周波スパッタ法はプラズマ生成のため、１０−
２〜１０２Ｐａのアルゴン雰囲気下で行う。得られるス
パッタ膜の組成のｘ、ｙはモリブデンターゲット上に並
べる窒化ボロンの面積比に比例して増加し、またアルボ
化させることができる。ｘ＋ｙの値は５，８くｘ＋Ｙく
４０であることが適当である。The high frequency sputtering method is used in the present invention because boron nitride, which is an insulator, is used as a target. The high frequency sputtering method generates plasma, so 10-
It is carried out under an argon atmosphere of 2 to 102 Pa. The composition x and y of the resulting sputtered film increase in proportion to the area ratio of boron nitride arranged on the molybdenum target, and can also be albonized. It is appropriate that the value of x+y be 5.8×x+Y×40.
基板としては例えば、モリブデン、サファイア、ガラス
、シリコン、石英が挙げられる。Examples of the substrate include molybdenum, sapphire, glass, silicon, and quartz.
得られたＭｏＢＮ膜を真空中（Ｍｏ 、 Ｂを酸化させ
ないため）で５００〜１０００Ｃで１分以上加熱すると
膜の表面に窒化ボロンが析出する。加熱温度が５ｏｏｃ
より低いと窒素・はう素が表面に拡散しないので５ｏｏ
ｃ以上であることが必要であることが必要である。When the obtained MoBN film is heated at 500 to 1000 C for 1 minute or more in vacuum (to avoid oxidizing Mo and B), boron nitride is precipitated on the surface of the film. Heating temperature is 5ooc
If it is lower than 5oo, nitrogen/boron will not diffuse to the surface.
It is necessary that the value is greater than or equal to c.
中における加熱温度及び加熱時間、真空度、不純物量等
によって変化する。これらの制御によって析出ＢＮ膜厚
を変化させることができる。It varies depending on the heating temperature and time inside, the degree of vacuum, the amount of impurities, etc. Through these controls, the thickness of the deposited BN film can be changed.
実施例
ＭＯの４インチ−ターゲット上に、５×５−の窒化ボロ
ンの小片を並べて、アルゴン５ Ｘ １０ ”ｔｏｒｒ
下で２０分間高周波スパｙ ＩＩ＊ １５０ ｍＡ、
１８０ Ｗ ）モリブデン基板上に製膜した。得られた
膜を５Ｘ１０−’ｔｏｒｒ以下の真空下で７５０〜９５
０Ｃで１時間加熱した。その結果は第１図に示す通りで
あった。析出するＢＮ膜厚は加熱前の膜中に含まれるＢ
Ｎの濃度によって大きく変化す石。厚いＢＮ膜を得るに
は、Ｂ＋Ｎが８〜１２原子係、２０〜４０原子係である
ことがよい。Example MO 4 inch target was lined with 5 x 5 pieces of boron nitride and heated to 5 x 10'' torr of argon.
High frequency spay II* 150 mA for 20 minutes under
180 W) A film was formed on a molybdenum substrate. The obtained film was heated under a vacuum of 5×10-'torr or less at 750 to 95
Heated at 0C for 1 hour. The results were as shown in FIG. The thickness of the precipitated BN film is the B contained in the film before heating.
A stone that changes greatly depending on the concentration of N. In order to obtain a thick BN film, it is preferable that B+N be 8 to 12 atoms, or 20 to 40 atoms.
ＢＮり膜厚は、スパッタ膜厚、スパッタガス（Ａｒ）れ
を適当に選択することによって制御し得る。得られた窒
化ボロンを表面に析出させ７ｈＭｏＢＮζ宵ツタ幅膜の
表面汚染度（付着した酸素と炭素の合計量、原子％）を
オージェ電子分光法で調ベア）糾果は下記表−１に示す
通りであった。The BN film thickness can be controlled by appropriately selecting the sputter film thickness and the sputter gas (Ar). The obtained boron nitride was precipitated on the surface and the surface contamination degree (total amount of attached oxygen and carbon, atomic %) of the 7hMoBNζ ivy film was measured by Auger electron spectroscopy) The results are shown in Table 1 below. It was on the street.
表−１
表面に付着したＯとＣの合計ｆｉｌ（原子％）この結果
が示すように、高周波スパッタ後、大気中にさらしたも
のの表面は多量の酸素、炭素で覆われているが、加熱後
、窒化ボロンを析出させたものは、その量が数分の１に
減少することがわかる。Table 1 Total fil of O and C attached to the surface (atomic %) As shown in this result, the surface of the product exposed to the atmosphere after high-frequency sputtering is covered with a large amount of oxygen and carbon, but after heating , it can be seen that the amount of boron nitride precipitated is reduced to several times.
発明の効果
本発明の方法によると、 Ｍｏと窒化ボロンをターゲッ
トとして用い、基板上に高周波スパッタ法によってＭｏ
ＢＮ＠を形成するため、Ｂ、Ｎを高濃度に含有させたも
のが容易に得られ、これを加熱すものとなし得ると共Ｋ
、表面の窒化ボロンは非ガス吸着性であって、清浄面で
あるため、高真空装置等の材料として好適である。Effects of the Invention According to the method of the present invention, Mo and boron nitride are used as targets, and Mo is deposited on the substrate by high-frequency sputtering.
In order to form BN@, a product containing a high concentration of B and N can be easily obtained, and this can be heated.
Since boron nitride on the surface is non-gas adsorbent and has a clean surface, it is suitable as a material for high vacuum equipment and the like.
更にまた、窒化ボロンの高絶縁の特性を利用した、種々
の素子を構成する材料、例えばＭＩＳ接合素子（金属−
絶縁体一半導体）やジョゼフソン素子（超電導体−絶縁
体−超電導体）等の材料としても優れたものである。Furthermore, boron nitride's highly insulating properties can be used to create materials constituting various devices, such as MIS junction devices (metal-
It is also an excellent material for materials such as insulator-semiconductor) and Josephson elements (superconductor-insulator-superconductor).
第１図は本発明の方法における高周波スパッタ法によっ
て生成した膜を真空中で加熱した場合における加熱温度
と析出するＢＮ膜の厚さとの関係図である。
特許出願人 科学技術庁金属材料技術研究所長中用龍−
第１図
Ｏｔｏ ２０ ３０ ４０
’１０（ｘ＋ｙ）FIG. 1 is a diagram showing the relationship between the heating temperature and the thickness of the deposited BN film when a film produced by high-frequency sputtering in the method of the present invention is heated in vacuum. Patent applicant: Yoryu Nakaka, director of the Institute of Metals and Materials Technology, Science and Technology Agency - Figure 1 Oto 20 30 40 '10 (x+y)
Claims (1)
高周波スパッタ法によって基板上に一般式 Ｍｏ＿１＿０＿０＿−＿（＿Ｘ＿＋＿Ｙ＿）Ｂ＿ＸＮ＿
Ｙ（ただし、Ｘ＞０、Ｙ＞０、Ｘ＋Ｙ＜１００を表わす
）で示されるＭｏＢＮ膜を作り、これを真空中で５００
〜１０００℃に加熱して表面に窒化ボロンを析出させた
ことを特徴とするＭｏＢＮ膜の表面に窒化ボロンを析出
させた金属・セラミック積層材料の製造方法。[Claims] Using molybdenum and boron nitride as targets,
The general formula Mo_1_0_0_-_(_X_+_Y_)B_XN_
A MoBN film represented by Y (representing X > 0, Y > 0, X + Y < 100) was made and heated in vacuum for 500
A method for producing a metal-ceramic multilayer material in which boron nitride is precipitated on the surface of a MoBN film, characterized in that boron nitride is precipitated on the surface by heating to ~1000°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3457285A JPS61194171A (en) | 1985-02-25 | 1985-02-25 | Method for producing a laminated material in which boron nitride is deposited on the surface of a MoBN film formed on a substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3457285A JPS61194171A (en) | 1985-02-25 | 1985-02-25 | Method for producing a laminated material in which boron nitride is deposited on the surface of a MoBN film formed on a substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61194171A true JPS61194171A (en) | 1986-08-28 |
| JPS6316464B2 JPS6316464B2 (en) | 1988-04-08 |
Family
ID=12418041
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3457285A Granted JPS61194171A (en) | 1985-02-25 | 1985-02-25 | Method for producing a laminated material in which boron nitride is deposited on the surface of a MoBN film formed on a substrate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61194171A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6320446A (en) * | 1986-07-12 | 1988-01-28 | Nissin Electric Co Ltd | Formation of boron nitride film |
| JPH0575496U (en) * | 1992-03-11 | 1993-10-15 | 共栄電工株式会社 | Non-seal pump |
| US6112843A (en) * | 1996-11-07 | 2000-09-05 | California Institute Of Technology | High mobility vehicle |
| JP2009149940A (en) * | 2007-12-20 | 2009-07-09 | Hitachi Tool Engineering Ltd | Nitride-containing target |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02109393U (en) * | 1989-02-16 | 1990-08-31 |
-
1985
- 1985-02-25 JP JP3457285A patent/JPS61194171A/en active Granted
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6320446A (en) * | 1986-07-12 | 1988-01-28 | Nissin Electric Co Ltd | Formation of boron nitride film |
| JPH0811822B2 (en) * | 1986-07-12 | 1996-02-07 | 日新電機株式会社 | Method for forming boron nitride film |
| JPH0575496U (en) * | 1992-03-11 | 1993-10-15 | 共栄電工株式会社 | Non-seal pump |
| US6112843A (en) * | 1996-11-07 | 2000-09-05 | California Institute Of Technology | High mobility vehicle |
| US6267196B1 (en) * | 1996-11-07 | 2001-07-31 | California Institute Of Technology | High mobility vehicle |
| JP2009149940A (en) * | 2007-12-20 | 2009-07-09 | Hitachi Tool Engineering Ltd | Nitride-containing target |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6316464B2 (en) | 1988-04-08 |
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