JPH03183774A - Surface treatment of sintered hard alloy substrate for depositing diamond - Google Patents
Surface treatment of sintered hard alloy substrate for depositing diamondInfo
- Publication number
- JPH03183774A JPH03183774A JP32251689A JP32251689A JPH03183774A JP H03183774 A JPH03183774 A JP H03183774A JP 32251689 A JP32251689 A JP 32251689A JP 32251689 A JP32251689 A JP 32251689A JP H03183774 A JPH03183774 A JP H03183774A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- diamond
- protrusions
- diamond film
- cemented carbide
- 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
- 239000010432 diamond Substances 0.000 title claims abstract description 57
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 56
- 239000000758 substrate Substances 0.000 title claims abstract description 43
- 238000004381 surface treatment Methods 0.000 title claims description 6
- 238000000151 deposition Methods 0.000 title abstract description 5
- 229910045601 alloy Inorganic materials 0.000 title abstract description 4
- 239000000956 alloy Substances 0.000 title abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000012808 vapor phase Substances 0.000 claims abstract description 7
- 239000006061 abrasive grain Substances 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 9
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 229910009043 WC-Co Inorganic materials 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000005498 polishing Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000004873 anchoring Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035485 pulse pressure Effects 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- 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製造のために、超硬合金基体に気
相法ダイヤモンド合成法によりダイヤモンド膜を析出さ
せるに際し、該基体と析出ダイヤモンド膜との付着力を
高めるための該基体の前処理方法に関する。[Detailed Description of the Invention] <Industrial Application Field> The present invention is applied to depositing a diamond film on a cemented carbide substrate by a vapor phase diamond synthesis method in order to manufacture cutting tools, etc. The present invention relates to a method for pre-treating the substrate to enhance adhesion to the membrane.
（従来の技術〉
超硬合金基体に気相法によりダイヤモンド膜を析出させ
るに際し、析出ダイヤモンド膜と基体との付着力を高め
るための処理方法としては、酸、アルカリ等の化学薬品
によるエツチング（第４８回応用物理学会学術講演会、
１８ａ−Ｔ−４）、ダイヤモンドパウダー等による傷付
は処理（第４８回応用物理学会学術講演会、１８ａ−Ｔ
−５）、またアルコール等を含む特定のガス中でエツチ
ング（特開平１−１４５３９６号）等が知られている。(Prior art) When depositing a diamond film on a cemented carbide substrate by a vapor phase method, etching (etching) using chemicals such as acids and alkalis is a treatment method to increase the adhesion between the precipitated diamond film and the substrate. 48th Japan Society of Applied Physics Academic Conference,
18a-T-4), treatment of scratches caused by diamond powder, etc. (48th Japan Society of Applied Physics Academic Conference, 18a-T
-5), etching in a specific gas containing alcohol or the like (Japanese Unexamined Patent Publication No. 1-145396) is known.
しかし例えばこのような方法を利用して処理した旋盤用
の超硬合金チップにダイヤモンド膜を形成させた工具を
実際に旋削に用いて゛も、短時間でダイヤモンド膜が剥
離し、実用可能なレベルでの付着強度は得られなかった
。However, even if a tool with a diamond film formed on a cemented carbide tip for a lathe treated using this method is actually used for turning, the diamond film will peel off in a short period of time, making it difficult to use at a practical level. Adhesive strength was not obtained.
本発明者は前記方法よりも析出ダイヤモンド曲と析出基
体との間の接着力を高める手段について研究の結果、基
体面にアンカーの役目をする突起を設ければよいこと、
そして基体を電解研摩す酌ば容易に突起が生成すること
を知り、特願平１−２４５２００として出願した。この
方法により基体表面と、その表面に形成されたダイヤモ
ンド膜との密着強度を高めることができ、ダイヤモンド
膜を形成させた工具を旋削等に実際に供することが可能
となった。As a result of research into a means for increasing the adhesion between the precipitated diamond curve and the precipitated substrate compared to the above method, the present inventor found that it is sufficient to provide a protrusion that serves as an anchor on the substrate surface.
Then, he learned that protrusions are easily generated when the substrate is electrolytically polished, and filed a patent application as Japanese Patent Application No. 1-245200. This method makes it possible to increase the adhesion strength between the surface of the substrate and the diamond film formed on the surface, making it possible to actually use a tool on which a diamond film is formed for turning, etc.
（発明が解決しようとする課題〉 然し実用的には更に密着強度が求められている。(Problem to be solved by the invention) However, for practical purposes, even higher adhesion strength is required.
本発明者らは、前記特願平１−２４５２００に開示され
ている方法について、ダイヤモンド膜と基体の付着力を
基体の表面状態を変化させて測定した所、付着力は突起
の大きさ、密度に依存していることが明らかになった。The present inventors measured the adhesion force between the diamond film and the substrate by changing the surface condition of the substrate using the method disclosed in the above-mentioned Japanese Patent Application No. 1-245200. It has become clear that it depends on
即ち、突起が太く、長く、又密度が高くなるとダイヤモ
ンド膜の付着力は高まった。That is, the thicker, longer, and denser the protrusions, the greater the adhesion of the diamond film.
しかし、一般的に、突起が太く、長くなると基体の寸法
精度が低下する傾向が有るため、ダイヤモンドコーテイ
ング材の使用目的に合わせて、基体表面の突起の大きさ
、密度を制御する表面処理方法の開発が必要となった。However, in general, as the protrusions become thicker and longer, the dimensional accuracy of the substrate tends to decrease. Therefore, surface treatment methods that control the size and density of the protrusions on the substrate surface are used depending on the intended use of the diamond coating material. Development was necessary.
〈課題を解決するための手段〉
本発明者らは前記方法を開発すべく研究の結果、超硬合
金基体を研摩液中でパルス電圧を用いて電解研摩すると
、印加するパルス状電圧の周波数、パルス幅の変化に応
じて超硬合金基体表面に形成される突起の大きさ、密度
が変化すること、そして前記特願平１−２４５２００に
記載の方法に比し、更に高いアンカー効果を示す表面状
態、即ち太く長い突起が密度高く生成した状態を容易に
得られることを知り本発明を完成した。<Means for Solving the Problems> As a result of research to develop the method, the present inventors found that when a cemented carbide substrate is electrolytically polished using a pulsed voltage in a polishing liquid, the frequency of the applied pulsed voltage, The size and density of protrusions formed on the surface of the cemented carbide substrate change according to changes in pulse width, and the surface exhibits a higher anchoring effect than the method described in the above-mentioned Japanese Patent Application No. 1-245200. The present invention was completed after realizing that a state in which thick and long protrusions are densely formed can be easily obtained.
本発明は超硬合金基体の表面をパルス電圧により、電解
研摩して表面に突起群を形成させて、該表面に気相法に
よ、リダイヤモンド膜゛を析出させ、該膜と該表面との
付着力を高めるダイヤモンド析出用超硬合金基体の表面
処理法に関する。In the present invention, the surface of a cemented carbide substrate is electrolytically polished using pulsed voltage to form a group of protrusions on the surface, a diamond film is deposited on the surface by a vapor phase method, and the film and the surface are bonded together. This invention relates to a surface treatment method for cemented carbide substrates for diamond deposition to increase the adhesion of diamond.
次ぎに本発明について詳しく説明する。Next, the present invention will be explained in detail.
超硬合金は周期律表のＩＶ、Ｖ、Ｖｌ族の金属の炭化物
、窒化物、ホウ化物、ケイ化物をＣｏ、Ｎｉ、Ｆｅ金属
、又はこれらの合金を結合材として焼結したものである
が、代表的なものとしてはＷＣ−Ｃｏ系のものがあげら
れる。この超硬合金基体を陽極とし、電解液中でパルス
状電圧を用いて電解研摩すると、表面が溶解し無数の突
起が形成される。この場合主としてＣＯが溶解されるが
、一部のＷＣも溶解して、適度な突起群が形成される。Cemented carbide is made by sintering carbides, nitrides, borides, and silicides of metals in groups IV, V, and Vl of the periodic table with Co, Ni, Fe metals, or alloys of these as binders. A typical example is a WC-Co type. When this cemented carbide substrate is used as an anode and electrolytically polished using a pulsed voltage in an electrolytic solution, the surface is dissolved and countless protrusions are formed. In this case, mainly CO is dissolved, but some WC is also dissolved to form a suitable group of protrusions.
用いる電解液としてｕｃｘ 、 Ｈ，ＳＯ４，ＮａＯＨ
、ＫＯＨ等の水溶液が好ましく、濃度は１〜５０％程度
が好ましい。又ＮａＯＨ、ＫＯＨとアンモニア水との混
合液でも良い結果が得られている。又電解研摩時の電流
密度は０．１＾／ｃ１〜２Ａ／Ｃ１の範囲が好ましい。The electrolyte used is ucx, H, SO4, NaOH
, KOH and the like are preferred, and the concentration is preferably about 1 to 50%. Good results have also been obtained with a mixture of NaOH, KOH and aqueous ammonia. Further, the current density during electrolytic polishing is preferably in the range of 0.1^/c1 to 2 A/c1.
次ぎにパルス状電圧の周波数、パルス幅についｓｐ−・
〒１１ａ４＝＊Ｊ、＜Ｗｂ６ｈ１ｍｍ２４粘九宜／１ｒ
ｅＬ”？＋ｋｌコ【を狭くすると超硬合金表面上に形成
する突起の大きさ、密度が増加する傾向が見られた。こ
の結果は用いる超硬合金の種類、電流密度等の条件によ
って若干異なるがＷＣ−６％Ｃｏの超硬合金を２０℃、
２０％ＨＣ鷹水溶液中で、電流密度０．５Ａ／ｃ＋ｍ”
の条件で電解研摩した場合、印加電圧を１７２Ｈｚ 。Next, regarding the frequency and pulse width of the pulsed voltage, sp-・
〒11a4=*J, <Wb6h1mm24 viscosity/1r
There was a tendency for the size and density of protrusions formed on the cemented carbide surface to increase as the value of eL"?+kl was narrowed. This result differs slightly depending on the type of cemented carbide used, current density, and other conditions. is WC-6%Co cemented carbide at 20℃,
In 20% HC hawk solution, current density 0.5A/c+m”
When performing electrolytic polishing under the following conditions, the applied voltage was 172Hz.
パルス幅１２０■Ｓでは突起の太さ２μ鳳、長さ３μ麿
、密度５ Ｘ １０”個／ａ−で形成された。これに対
し、印加するパルス状電圧を２Ｈｚ、 ８０ｍ５とした
場合、突起の太さ４μ園、長さ６μ■、密度１ｘ１０４
個／ｍｔａ”と突起の大きさ、密度が増加し、付着力は
前述の１／２Ｈｚのパルス電圧を用いた場合の１．５倍
であった。When the pulse width was 120 μS, the protrusions were formed with a thickness of 2 μm, a length of 3 μm, and a density of 5 × 10” pieces/a-.On the other hand, when the pulsed voltage applied was 2 Hz and 80 m5, the protrusions were formed. Thickness: 4μ, length: 6μ, density: 1x104
The size and density of the protrusions increased by 1/mta'', and the adhesion force was 1.5 times that of the case using the 1/2 Hz pulse voltage described above.
尚、特願平１−２４５２００に開示されている定常電圧
を用いた電解研摩法では、突起の太さ２μ−１長さ２μ
園、密度２Ｘ１０”個／ｒａｙｓ”で、ダイヤモンド膜
の付着力は前述の２Ｈｚのパルス電圧を用いた場合の約
１７２であった。In addition, in the electrolytic polishing method using a steady voltage disclosed in Japanese Patent Application No. 1-245200, the thickness of the protrusion is 2μ-1 and the length is 2μ.
At a density of 2.times.10"pieces/rays", the adhesion force of the diamond film was about 172 using the 2 Hz pulse voltage described above.
本発明方法において、パルスの電圧印加時間がｋｇ −
Ａｓ ＋＃’ ｊＬし 木幻冨６虐１啼見吠隙ル萌ナス
ワ電圧印加時間が長ずざると一定電圧による電解研摩
と等しくなってしまう、更に周波数が大きすぎると電解
液中のイオンの泳動が追従できなくなり、パルス効果が
なくなる。In the method of the present invention, the pulse voltage application time is kg −
As ＋＃' jL し 木Genfu 6 郎 1 啼みょう る もえん わ If the voltage application time is not long, it will be equivalent to electrolytic polishing with a constant voltage, and if the frequency is too high, ions in the electrolyte will be removed. The electrophoresis becomes impossible to follow, and the pulse effect disappears.
本発明の方法で得られる突起の太さは２００μｍ以下、
長さは１５０μｍ以下、密度はｌＸｌ０”個／ｍｍ”で
あるが、ダイヤモンドコーティング超硬基体として用い
る望ましい突起の太さは１〜５０μｍ、長さは１〜５０
μｍ、密度はｌＸｌ０”個／ｍｍ”であり、そのための
パルス電圧はパルス幅１ ｍ５ｅｃ〜ｌ ｓｅｃ 、パ
ルスの周波数は５００Ｈｚ−１／１ＯＨｚである。The thickness of the protrusions obtained by the method of the present invention is 200 μm or less,
The length is 150 μm or less, and the density is 1×10 “pieces/mm”, but the desirable thickness of the protrusions used as the diamond-coated carbide substrate is 1 to 50 μm, and the length is 1 to 50 μm.
μm, the density is 1×10” pieces/mm, the pulse voltage for this has a pulse width of 1 m5ec to lsec, and the pulse frequency is 500Hz-1/1OHz.
尚、本発明方法においてパルス電解後の基体表面な砥粒
で傷付は処理を行ってもよい。砥粒としてはダイヤモン
ド、ｃＢＮ 、 Ａ１＊Ｏｓ 、ＳｉＣ等が挙げられる
が、とりわけダイヤモンドが好ましい。この場合、表面
に形成している突起が失われない程度に研摩する事が好
ましい。このため砥粒による研摩はダイヤモンド粒をペ
ースト状にした、いわゆるダイヤモンドペーストの使用
や、ダイヤモンド粒その他の砥粒をアルコール等の溶液
に懸濁させたものを超音波振動させるのも効果的である
。In the method of the present invention, scratches on the surface of the substrate after pulse electrolysis may be treated with abrasive grains. Examples of the abrasive grain include diamond, cBN, A1*Os, SiC, etc., but diamond is particularly preferred. In this case, it is preferable to polish the surface to such an extent that the protrusions formed on the surface are not lost. For this reason, polishing with abrasive grains is effective by using so-called diamond paste, which is a paste made of diamond grains, or by ultrasonically vibrating diamond grains or other abrasive grains suspended in a solution such as alcohol. .
このような処理によりダイヤモンドの核発生が均一とな
り、ダイヤモンド膜が均質となるばかりか、付着力も高
まる。この処理を行なわない場合は突起の上の部分で選
択的にダイヤモンド核の発生が生成し易く、ダイヤモン
ド膜表面の均一性が欠けた状態となり、突起のアンカー
効果が低下する可能性がある。Such treatment not only makes diamond nucleation uniform and makes the diamond film homogeneous, but also increases adhesion. If this treatment is not performed, diamond nuclei are likely to be generated selectively in the upper portions of the protrusions, resulting in a state in which the diamond film surface lacks uniformity, and the anchoring effect of the protrusions may be reduced.
以上の如く本発明の方法により超硬合金表面の処理を行
なうと従来に比べ強度が大きく、密度の高い突起がダイ
ヤモンド膜の内部に入り込むため、付着強度の高いダイ
ヤモンドコーティングが可能となると共に、突起の大き
さ密度が自由に制御できるため、その基体の利用目的に
合わせた強度のダイヤモンドコーティングが可能である
。As described above, when a cemented carbide surface is treated by the method of the present invention, protrusions with greater strength and density than before penetrate into the diamond film, making it possible to form a diamond coating with high adhesion strength. Since the size and density of the diamond can be freely controlled, it is possible to form a diamond coating with a strength that matches the intended use of the substrate.
〈効 果〉
本発明により超硬合金基体にダイヤモンド膜を付着強度
が極めて高い状態で析出が可能となり過酷な状況で使用
に耐えるダイヤモンド膜のついた工具の製造が可能とな
った。<Effects> According to the present invention, it is possible to deposit a diamond film on a cemented carbide substrate with extremely high adhesion strength, and it has become possible to manufacture a tool with a diamond film that can withstand use under harsh conditions.
次ぎに実施例、比較例により本発明を説明する。Next, the present invention will be explained with reference to Examples and Comparative Examples.
く実 施 例〉
ＷＣに６％のＧｏを含有した超硬合金基板（１２＋ａｍ
ｘ１２ｍｍＸ ２ ｍｆｆ１）を陽極、炭素棒を陰極と
して、ＨＣｌ１０％水溶液中を電解液とし、電圧は３Ｖ
、電流は０．５Ａ、パルスの周波数はｌ／２Ｈｚ 、パ
ルス幅１２０ｍ５で３０分間電解研摩を行なった。電解
研摩後、超硬合金表面は酸化物で覆われているため、Ｎ
、０Ｈ１Ｏ％水溶液で洗浄し、酸化物を除去した。次い
で基板表面を平均粒径１１．Ｌｍのダイヤモンドを含む
ペーストにより傷付は処理を行ない、更にアルコールで
洗浄した０次ぎにこのように処置された基板に、図に示
す装置を用い熱フイラメント合成法によりダイヤモンド
を析出させた。図においてｌは直径２５ｃｍφ、高さ２
０ｃｍの反応炉で、内部に熱フィラメント２、前記処理
した超硬合金基板４を支持する基板支持台３が設けられ
ている。５はダイヤ壬ンド新出田Ｈ鯨ガｆａｔ鎖ロー６
け境蕾■ヤある。基板と熱フィラメントとの距離を５Ｉ
ＩＩ＋１とし、原料としてガス化したエタノールを３
ｃｃ／分、水素を１００ｃｃ／分で供給口５より反応炉
内に導入し、圧力９０Ｔｏｒｒで３時間、ダイヤモンド
析出反応を続けた。基板上に平均１５μｍのダイヤモン
ド膜が析出した。ダイヤモンドは光学顕微鏡とラマン分
光により確認した。Example of implementation> Cemented carbide substrate containing 6% Go in WC (12+am
x12mm
Electrolytic polishing was performed for 30 minutes at a current of 0.5 A, a pulse frequency of 1/2 Hz, and a pulse width of 120 m5. After electrolytic polishing, the cemented carbide surface is covered with oxides, so N
, 0H1O% aqueous solution to remove oxides. Next, the substrate surface was coated with an average grain size of 11. Scratches were treated with a paste containing diamond of Lm, and then diamond was deposited on the thus treated substrate, which was further cleaned with alcohol, by thermal filament synthesis using the apparatus shown in the figure. In the figure, l is diameter 25cmφ and height 2
A 0 cm reactor was provided with a hot filament 2 and a substrate support 3 for supporting the treated cemented carbide substrate 4 inside. 5 is Diamond Jindo Niideta H Kujiraga fat chain low 6
There are border buds. The distance between the board and the hot filament is 5I.
II+1, and gasified ethanol as raw material is 3
cc/min, hydrogen was introduced into the reactor from the supply port 5 at a rate of 100 cc/min, and the diamond precipitation reaction was continued at a pressure of 90 Torr for 3 hours. A diamond film with an average thickness of 15 μm was deposited on the substrate. Diamonds were confirmed using an optical microscope and Raman spectroscopy.
次いで基板とダイヤモンド膜の付着強度を調べるため、
先端が半径０．２ｍｍの球面で頂角１２０°のダイヤモ
ンド製ロックウェル圧子を用い、ダイヤモンド膜に圧入
してダイヤモンド膜が剥離する迄の荷重を求めた。その
結果２５ｋｇでダイヤモンド膜が剥離した。Next, to examine the adhesion strength between the substrate and the diamond film,
A diamond Rockwell indenter having a spherical tip with a radius of 0.2 mm and an apex angle of 120° was used to press fit into the diamond film, and the load required until the diamond film peeled off was determined. As a result, the diamond film peeled off at 25 kg.
（比較例〉
実施例においてパルス定圧の代わりに定常電圧を用いた
以外、全く同様に処理して超硬合金基板にダイヤモンド
膜を形成させた実施例と同様にしてダイヤモンドの剥離
荷重を求めた。その結果１２ｋｇでダイヤモンドは剥離
した。(Comparative Example) The diamond peeling load was determined in the same manner as in the example in which a diamond film was formed on a cemented carbide substrate using the same process as in the example except that a steady voltage was used instead of the constant pulse pressure. As a result, the diamond peeled off at 12 kg.
図面は実施例、比較例に用いた熱フィラメント法ダイヤ
モンド合成装置を示す。
図において、１：反応炉、２：熱フィラメント、３：基
体支持台、４：超硬合金基体、５：ダイヤモンド析出用
原料ガス供給口、６：排気口を示す。The drawing shows a hot filament diamond synthesis apparatus used in Examples and Comparative Examples. In the figure, 1: reactor, 2: hot filament, 3: substrate support, 4: cemented carbide substrate, 5: raw material gas supply port for diamond precipitation, 6: exhaust port.
Claims (3)
して、表面に突起群を形成させて、該表面に気相法によ
りダイヤモンド膜を析出させ、該膜と該表面との付着力
を高めるダイヤモンド析出用超硬合金基体の表面処理法
。(1) The surface of the cemented carbide substrate is electrolytically polished using pulsed voltage to form a group of protrusions on the surface, and a diamond film is deposited on the surface by a vapor phase method to increase the adhesion between the film and the surface. Surface treatment method for cemented carbide substrates for diamond precipitation.
して、表面に突起群を形成させ、更にその表面を砥粒で
傷付け処理を施して該表面に気相法によりダイヤモンド
膜を析出させ、該膜と該表面との付着力を高めるダイヤ
モンド析出用超硬合金基体の表面処理法。(2) The surface of the cemented carbide substrate is electrolytically polished using a pulsed voltage to form a group of protrusions on the surface, and the surface is further scratched with abrasive grains, and a diamond film is deposited on the surface by a vapor phase method. , a method for surface treatment of a cemented carbide substrate for diamond precipitation to increase adhesion between the film and the surface.
り、パルスの周波数が５００Ｈｚ〜１／１０Ｈｚである
請求項１又は２の表面処理法。(3) The surface treatment method according to claim 1 or 2, wherein the pulse voltage has a pulse width of 1 msec to 1 sec and a pulse frequency of 500 Hz to 1/10 Hz.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32251689A JP2794601B2 (en) | 1989-12-14 | 1989-12-14 | Surface treatment of cemented carbide substrate for diamond deposition |
| DE69018243T DE69018243T2 (en) | 1989-09-22 | 1990-09-20 | METHOD FOR PRODUCING DIAMOND BY MEANS OF VAPOR DEPOSITION ON ELECTROCHEMICALLY TREATED SUBSTRATE. |
| EP90913889A EP0445305B1 (en) | 1989-09-22 | 1990-09-20 | Vapor deposited diamond synthesizing method on electrochemically treated substrate |
| PCT/JP1990/001209 WO1991004353A1 (en) | 1989-09-22 | 1990-09-20 | Vapor deposited diamond synthesizing method on electrochemically treated substrate |
| US07/700,168 US5164051A (en) | 1989-09-22 | 1990-09-20 | Method for vapor phase synthesis of diamond on electrochemically treated substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32251689A JP2794601B2 (en) | 1989-12-14 | 1989-12-14 | Surface treatment of cemented carbide substrate for diamond deposition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03183774A true JPH03183774A (en) | 1991-08-09 |
| JP2794601B2 JP2794601B2 (en) | 1998-09-10 |
Family
ID=18144530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32251689A Expired - Fee Related JP2794601B2 (en) | 1989-09-22 | 1989-12-14 | Surface treatment of cemented carbide substrate for diamond deposition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2794601B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6110240A (en) * | 1996-05-31 | 2000-08-29 | Ngk Spark Plug Co., Ltd. | Superhard article with diamond coat and method of manufacturing same |
| US6387502B1 (en) | 1998-09-04 | 2002-05-14 | Ngk Spark Plug Co., Ltd. | Diamond-coated hard metal member |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4851376B2 (en) * | 2007-03-23 | 2012-01-11 | 東海旅客鉄道株式会社 | Pretreatment method of conductive substrate used for synthesis of diamond film and method of manufacturing diamond film |
-
1989
- 1989-12-14 JP JP32251689A patent/JP2794601B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6110240A (en) * | 1996-05-31 | 2000-08-29 | Ngk Spark Plug Co., Ltd. | Superhard article with diamond coat and method of manufacturing same |
| US6387502B1 (en) | 1998-09-04 | 2002-05-14 | Ngk Spark Plug Co., Ltd. | Diamond-coated hard metal member |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2794601B2 (en) | 1998-09-10 |
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