JPH01205085A - Method for cleaning metal - Google Patents
Method for cleaning metalInfo
- Publication number
- JPH01205085A JPH01205085A JP3009788A JP3009788A JPH01205085A JP H01205085 A JPH01205085 A JP H01205085A JP 3009788 A JP3009788 A JP 3009788A JP 3009788 A JP3009788 A JP 3009788A JP H01205085 A JPH01205085 A JP H01205085A
- Authority
- JP
- Japan
- Prior art keywords
- substrate
- vacuum furnace
- inert gas
- coating
- molecules
- 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
- 229910052751 metal Inorganic materials 0.000 title claims description 22
- 239000002184 metal Substances 0.000 title claims description 22
- 238000004140 cleaning Methods 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 16
- 239000000758 substrate Substances 0.000 claims abstract description 57
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 13
- -1 hydrogen ions Chemical class 0.000 claims abstract description 9
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000004767 nitrides Chemical class 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 21
- 239000011248 coating agent Substances 0.000 abstract description 16
- 238000000576 coating method Methods 0.000 abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 230000004913 activation Effects 0.000 abstract description 3
- 239000011247 coating layer Substances 0.000 abstract description 3
- 238000007788 roughening Methods 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000002173 cutting fluid Substances 0.000 abstract 1
- 239000008246 gaseous mixture Substances 0.000 abstract 1
- 238000010849 ion bombardment Methods 0.000 description 10
- 239000010936 titanium Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 238000010894 electron beam technology Methods 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010730 cutting oil Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- ing And Chemical Polishing (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、イオンボンバードなる手法において金属表面
を荒すことなく金属表面の清浄を可能にした金属の清浄
化方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a metal cleaning method that makes it possible to clean a metal surface without roughening the metal surface using a technique called ion bombardment.
（従来の技術）
従来より金属材料にコーティングを施す場合、その前工
程として該金属材料の表面処理、即ち表面の清浄が一般
に行われている。該清浄の目的は金属材料（基体）の表
面に酸素分子や窒素分子あるいは水蒸気等の吸着ガス分
子およびその化合物等が存在すると、コーティングの密
着性が劣るためにそれらを除去することであって、今日
、種々な清浄方法（例えば酸、アルカリ溶液によるもの
や超音波によるもの）が行われている。(Prior Art) Conventionally, when applying a coating to a metal material, surface treatment of the metal material, that is, surface cleaning has generally been performed as a pre-process. The purpose of this cleaning is to remove oxygen molecules, nitrogen molecules, water vapor, and other adsorbed gas molecules and their compounds, because if they exist on the surface of the metal material (substrate), the adhesion of the coating will be poor. Various cleaning methods are in use today, such as with acid, alkaline solutions and with ultrasound.
そして、その清浄方法の一手段としてイオンボンバード
なるものがある。該イオンボンバードはイオンスパッタ
法とも呼ばれ、第６図にその概略図を示すように真空炉
ａ内に基体すおよび電極Ｃを配設し、該炉内に不活性ガ
スｄ（一般にＡｒが使用される）を送給すると共に、前
記基体すと電極Ｃの間に電圧を掛けることによってグロ
ー放電させ、前記不活性ガスｄをイオン化させる。該イ
オン化された不活性ガスの原子は帯電している甚板すの
表面に衝突し、該表面に吸着している分子（０２やＮ２
あるいはＮ２０）をはじき飛ばしく解離し）基体表面を
清浄するものである。また、このイオンボンバードは表
面の汚れの種類にかかわらず清浄可能なものである。こ
うしたイオンスパッタ法による金属の表面清浄化法とし
て１例えば特開昭６０−９８８８号公報に示されるもの
等がある。Ion bombardment is one of the cleaning methods. This ion bombardment is also called ion sputtering method, and as shown in the schematic diagram in FIG. At the same time, a voltage is applied between the substrate and the electrode C to cause a glow discharge and ionize the inert gas d. The atoms of the ionized inert gas collide with the surface of the charged plate, and the molecules (02 and N2) adsorbed on the surface are
Alternatively, it dissociates by repelling N20) and cleans the substrate surface. Moreover, this ion bombardment can clean any kind of dirt on the surface. An example of a metal surface cleaning method using ion sputtering is disclosed in Japanese Patent Application Laid-Open No. 60-9888.
（発明が解決しようとする課題）
しかし上述の如き従来のイオンボンバードによる清浄方
法にあっては、基体表面に付着した吸着ガス分子を取除
くことは可能であっても、基体表面の酸化および窒化さ
れた部分はその酸素および窒素の結合力が高いために不
活性ガスの原子では。(Problem to be Solved by the Invention) However, in the conventional cleaning method using ion bombardment as described above, although it is possible to remove adsorbed gas molecules attached to the substrate surface, it is possible to remove oxidation and nitridation of the substrate surface. The part that was formed is an inert gas atom due to its high bonding strength of oxygen and nitrogen.
解離させることが難しく、その効果を上げるために長時
間に渡って清浄させると、酸化および窒化されていない
基体表面において基体原子（ＦｅやＣｒ）が解離されて
該表面に荒れが発生し、コーティングの密着力が低下す
ることもある。It is difficult to dissociate, and if cleaning is carried out for a long time to increase the effectiveness, substrate atoms (Fe and Cr) will be dissociated on the substrate surface that has not been oxidized and nitrided, and the surface will become rough, causing the coating to deteriorate. The adhesion strength may be reduced.
上記の点を考慮し１本発明は基体の表面を荒らすことな
く該表面の清浄、特に基体表面の酸化および窒化された
部分をも清浄し、ひいてはコーティングの密着力を向上
させることを目的とするものである。In consideration of the above points, the present invention aims to clean the surface of the substrate without roughening the surface, and in particular to clean the oxidized and nitrided portions of the substrate surface, thereby improving the adhesion of the coating. It is something.
（課題を解決するための手段）
上記の点に鑑み本発明は金属基体を不活性ガスおよび水
素が導入可能な真空炉内に載置し、該金属基体を電極と
して上記不活性ガスをイオン化し、その不活性ガスイオ
ンで上記金属基体表面上の吸着ガス分子を解離させ、そ
の後、上記金属基体を電極として上記水素をイオン化し
、その水素イオンで上記金属基体表面上の酸化物または
窒化物のうち少なくともどちらか一方を還元させること
を特徴とする金属の清浄化方法に係るものである。(Means for Solving the Problems) In view of the above points, the present invention places a metal substrate in a vacuum furnace into which an inert gas and hydrogen can be introduced, and uses the metal substrate as an electrode to ionize the inert gas. , the adsorbed gas molecules on the surface of the metal substrate are dissociated with the inert gas ions, and then the hydrogen is ionized using the metal substrate as an electrode, and the hydrogen ions are used to ionize the oxide or nitride on the surface of the metal substrate. The present invention relates to a metal cleaning method characterized by reducing at least one of the metals.
（作用）
上記端成による本発明の作用は、不活性ガスイオンで金
属基体表面上の吸着ガス分子を解離させた後、水素イオ
ンで前記金属基体表面上の酸化物および窒化物を還元す
ることにより基体表面を清浄し、コーティングの密着力
が向上されるものである。(Function) The function of the present invention based on the above-mentioned structure is to dissociate the adsorbed gas molecules on the surface of the metal substrate with inert gas ions, and then reduce the oxides and nitrides on the surface of the metal substrate with hydrogen ions. This cleans the substrate surface and improves the adhesion of the coating.
（実施例） 次に本発明における一実施例を図面に沿って説明する。(Example) Next, one embodiment of the present invention will be described with reference to the drawings.
先ず、本発明に使用される装置に関し第１図を用いて説
明する。該装置１は基体２の表面を清浄すると共にＴｉ
Ｎ （窒化チタン）をコーティングするための装置であ
って、真空炉３内に具備された基体２、シャッタ４、チ
タンインゴット５、電子ビームガン６と前記真空炉３に
接続された真空排気装置７を主要部として成っている。First, the apparatus used in the present invention will be explained with reference to FIG. The device 1 cleans the surface of the substrate 2 and also cleans the surface of the substrate 2.
This is a device for coating N (titanium nitride), which includes a substrate 2, a shutter 4, a titanium ingot 5, an electron beam gun 6, and a vacuum evacuation device 7 connected to the vacuum furnace 3, which are provided in a vacuum furnace 3. It consists of the main part.
真空炉３は一般的な陰極スパッタリングなるメツキ方法
に使用される周知の炉であって、その上壁にはＡｒガス
およびＮ２の混合気体が送給される第１送給路１ａが、
また側壁にはＮ２が送給される第２送給路１ｂが各々接
続されている。一方。The vacuum furnace 3 is a well-known furnace used in a general plating method called cathode sputtering, and the upper wall thereof has a first feed path 1a through which a mixed gas of Ar gas and N2 is fed.
Further, second feed paths 1b through which N2 is fed are connected to the side walls. on the other hand.
該真空炉３の底部には後述する真空排気装置７が装備さ
れて真空炉３内の気体は排出自在とされている。The bottom of the vacuum furnace 3 is equipped with a vacuum evacuation device 7, which will be described later, so that the gas inside the vacuum furnace 3 can be freely exhausted.
基体２は前記真空炉３の内壁に固着された基体ホルダ２
ａに取付けられた鋼板であって、前記基体ホルダ２ａが
１ｉ源８に接続されていることにより、イオンボンバー
ド時およびコーティング加工時には負に帯電されるもの
となる。The substrate 2 is a substrate holder 2 fixed to the inner wall of the vacuum furnace 3.
Since the substrate holder 2a is connected to the 1i source 8, it becomes negatively charged during ion bombardment and coating processing.
シャッタ４はイオンボンバード時に解離された吸着ガス
分子が直接チタンインボッ１−５へ飛散することがない
よう両者を遮断しているものであって、その開閉は自在
となっている。The shutter 4 blocks the adsorbed gas molecules dissociated during ion bombardment from directly scattering to the titanium ingots 1-5, and can be opened and closed freely.
チタンインゴット５は前記真空炉３内の底部附近に設置
された水冷ルツボ５ａ内に載置されると共に、電子ビー
ムガン６から発せられる電子ビームによって溶融、蒸発
されて窒素と化合し、その後、基体２の表面にコーティ
ングされる部材である。The titanium ingot 5 is placed in a water-cooled crucible 5a installed near the bottom of the vacuum furnace 3, and is melted and evaporated by the electron beam emitted from the electron beam gun 6 to combine with nitrogen. It is a member that is coated on the surface of.
次に本発明の清浄化方法の原理を第２図および第３図（
模式図）に沿って説明する。Next, the principle of the cleaning method of the present invention is illustrated in Figures 2 and 3 (
(Schematic diagram)
先ず、基体表面に吸着している吸着ガス分子を解離させ
る際には第２図に示すように従来と同様にＡｒガスをグ
ロー放電によってイオン化し、該Ａｒガスイオンが基体
２の表面へ衝突することにより前記吸着ガス分子（Ｏｚ
＝ＮｚおよびＮ２０）を基体表面から解離させる。この
時のグロー放電を発生させるための電圧はＡｒの有効な
電離確率を得るべく設定（約４００Ｖ）してある。その
後、第３図に示すようにＮ２を上記と同様にグロー放電
によってイオン化させ、その水素イオンにより基体表面
の酸化部分あるいは窒化部分を還元して純粋な基体材料
（ＦｅやＣｒ等）に戻して清浄する。この時の°グロー
放電を発生させるための電圧はＮ２の有効な電離確率を
得るべきものとなっており（約６０Ｖ）、前述したＡｒ
のイオン化時とは異なっている。First, when dissociating adsorbed gas molecules adsorbed on the substrate surface, Ar gas is ionized by glow discharge as in the conventional method, and the Ar gas ions collide with the surface of the substrate 2, as shown in FIG. By this, the adsorbed gas molecules (Oz
=Nz and N20) are dissociated from the substrate surface. The voltage for generating glow discharge at this time is set (approximately 400 V) to obtain an effective ionization probability of Ar. Thereafter, as shown in Figure 3, N2 is ionized by glow discharge in the same manner as above, and the hydrogen ions reduce the oxidized or nitrided parts on the substrate surface to return it to pure substrate material (Fe, Cr, etc.). Clean. At this time, the voltage to generate the glow discharge is such that an effective probability of ionization of N2 can be obtained (approximately 60 V), and the voltage used to generate the glow discharge is the same as the one mentioned above (approximately 60 V).
It is different from the time of ionization.
次に、前述した装置１を用いて基体表面の清浄およびコ
ーティング工程を第４図のヒートサイクルに沿って説明
する。Next, the process of cleaning and coating the substrate surface using the above-mentioned apparatus 1 will be explained along the heat cycle shown in FIG. 4.
先ず、第１図に示すように装置１の基体ホルダ２ａへ基
体２を、水冷ルツボ５ａにチタンインボッｌ−５を各々
配置し、真空排気装置７によって真空炉３内の空気を排
気して内圧を５ Ｘ Ｉ ０−５ｔｏｒｒにする（第４
図排気工程）。その後、真空炉３を加熱しく５２０℃で
２時間）、基体２の表面に付着している切削油等を蒸発
、脱ガスする（第４図脱ガス工程）。続いてイオンボン
バード工程に入るが、その前に真空炉３内をグロー放電
を得易い真空度（本例では１ ｔｏｒｒ）に設定すると
共に、第１送給路１ａよりＡｒとＮ２（体積比率１％）
の混合気体を送給する。その後、前述した原理に述べた
ように４００Ｖの加電圧によるグロー放電によってＡｒ
をイオン化し該Ａｒガスイオンで吸着ガス分子（Ｏｚ、
Ｎｚ等）を基体表面から解離させる（５ｏＯ℃で５分間
）。該解離された吸着ガス分子は真空炉内を浮遊してい
るため、真空排気装置７を作動させて排気する（その時
、内圧はＩＸｌ ０−３ｔｏｒｒ）。また、本例では吸
着ガス分子の解離をより確実にするべく該工程を温度繰
り返すものである。First, as shown in FIG. 1, the substrate 2 is placed in the substrate holder 2a of the apparatus 1, and the titanium ingot 1-5 is placed in the water-cooled crucible 5a, and the air inside the vacuum furnace 3 is evacuated by the vacuum evacuation device 7 to reduce the internal pressure. 5 X I Set to 0-5 torr (4th
Fig. Exhaust process). Thereafter, the vacuum furnace 3 is heated to 520° C. for 2 hours) to evaporate and degas the cutting oil and the like adhering to the surface of the substrate 2 (FIG. 4 degassing step). Next, the ion bombardment process begins, but before that, the inside of the vacuum furnace 3 is set to a degree of vacuum (1 torr in this example) that makes it easy to obtain a glow discharge, and Ar and N2 (volume ratio 1 %)
A mixture of gases is supplied. Then, as described in the principle above, Ar
is ionized and the Ar gas ions absorb adsorbed gas molecules (Oz,
Nz, etc.) are dissociated from the substrate surface (5 minutes at 500°C). Since the dissociated adsorbed gas molecules are floating in the vacuum furnace, the vacuum evacuation device 7 is operated to exhaust them (at that time, the internal pressure is IXl 0-3 torr). Furthermore, in this example, this step is repeated at different temperatures in order to more reliably dissociate the adsorbed gas molecules.
次に、真空炉内の圧力を再び１ ｔｏｒｒに戻し、加電
圧６０Ｖで水素をイオン化させ、該水素イオンによって
基体表面の酸化部分および窒化部分を還元する。この時
に還元された酸素および窒素は水素イオンと反応して水
蒸気（Ｎ２０） 、アンモニア（ＮＨ３）となって真空
炉内を浮遊し、再び基体材料と結合することはないもの
である。そして前記と同様に真空排気装置７を作動させ
前記水蒸気やアンモニアを排気し、これで基体表面は清
浄され、活性化が促されたものとなる。Next, the pressure in the vacuum furnace is returned to 1 torr, hydrogen is ionized with an applied voltage of 60 V, and the oxidized portions and nitrided portions on the surface of the substrate are reduced by the hydrogen ions. The oxygen and nitrogen reduced at this time react with hydrogen ions to become water vapor (N20) and ammonia (NH3), which float in the vacuum furnace and do not combine with the base material again. Then, in the same manner as described above, the vacuum evacuation device 7 is operated to exhaust the water vapor and ammonia, thereby cleaning the surface of the substrate and promoting activation.
次に、該清浄された基体表面に窒化チタンをコーティン
グする際は、先ず真空炉３の内圧を９×１０”” ｔｏ
ｒｒとして温度を５００℃に保ったまま第２送給路１ｂ
より窒素（Ｎ２）を送給すると共に、電子ビームガン６
より発生される電子ビームによりチタンインゴット５を
溶融、蒸発させて窒素と化学反応させ窒化チタン（Ｔｉ
Ｎ）とし、帯電した基体側へ飛散させて基体表面をコー
ティングする（第４図ＴｉＮコーティング工程）。そし
て最後に真空度を下げて常圧とすると共に、冷却して基
体を取出し、作業を終了する（第４図冷却工程）。Next, when coating the cleaned substrate surface with titanium nitride, first the internal pressure of the vacuum furnace 3 is reduced to 9×10"" to
rr while maintaining the temperature at 500°C.
While supplying more nitrogen (N2), the electron beam gun 6
The titanium ingot 5 is melted and evaporated by the electron beam generated by the titanium ingot 5, and is chemically reacted with nitrogen to form titanium nitride (Ti).
TiN) is scattered onto the charged substrate side to coat the substrate surface (Fig. 4, TiN coating step). Finally, the degree of vacuum is lowered to normal pressure, and the substrate is cooled and taken out to complete the work (cooling step in Figure 4).
く実験〉
次に本発明によって得られたＴｉＮコーティングと従来
のＡｒのみによる清浄後にＴｉＮコーティングしたもの
との密着性テストの比較実験結果について述べる（第５
図）。尚、本実験に用いる本発明によって得られた試験
片は、従来のものと比較するために一定加電圧によって
清浄したものとする。従って、前述した実施例に示した
ように適宜加電圧を変換させた場合には、本実験で得ら
れた結果より更に優れたものとなっている（参考のため
に第５図の破線で示す）６
本密着性テストとしては一般的なスクラッチ試験を採用
し、頂角が９０’のダイヤモンド圧子でコーティング表
面を以下の表に示す条件で引掻き。Next, we will discuss the results of a comparative experiment of adhesion test between the TiN coating obtained by the present invention and the conventional TiN coating after cleaning with Ar alone.
figure). Note that the test piece obtained according to the present invention used in this experiment was cleaned by applying a constant applied voltage for comparison with a conventional test piece. Therefore, when the applied voltage is changed appropriately as shown in the example described above, the results are even better than those obtained in this experiment (for reference, the results are shown by the broken line in Figure 5). )6 For this adhesion test, a general scratch test was adopted, and the coating surface was scratched under the conditions shown in the table below using a diamond indenter with an apex angle of 90'.
コーティング層が剥離した荷重を臨界荷重として測定し
たものである。The load at which the coating layer peeled off was measured as the critical load.
表
第５図の如く、本発明による清浄後のコーティングにあ
っては、如何なるボンバード出力にあっても、従来の清
浄のものに比べて密着力（臨界荷重）が２５％程度向上
されたものとなっている。As shown in Table 5, with the coating after cleaning according to the present invention, the adhesion force (critical load) is improved by about 25% compared to the conventional cleaning coating, regardless of the bombardment output. It has become.
尚、本例にあってはイオンボンバード時に第１送給路よ
りＡｒとＨ２の混合気体を送給したが、本発明はこれに
限らず、真空炉にＡｒ送給路とＨ２送給路を設は適宜、
送給気体を切換え可能な構成とすることも可能である。In this example, a mixed gas of Ar and H2 was fed from the first feeding path during ion bombardment, but the present invention is not limited to this, and the vacuum furnace may be provided with an Ar feeding path and a H2 feeding path. The settings are as appropriate.
It is also possible to have a configuration in which the gas to be supplied can be switched.
（発明の効果）
上述の如く本発明によれば、不活性ガスイオンで金属基
体表面上の吸着ガス分子を解離させた後、水素イオンで
前記金属基体表面上の酸化物および窒化物を還元するこ
とにより基体表面の活性化が促され、該基体表面にコー
ティングされるコーティング層は、その密着力が向上さ
れるという効果を有する。(Effects of the Invention) As described above, according to the present invention, after the adsorbed gas molecules on the surface of a metal substrate are dissociated with inert gas ions, the oxides and nitrides on the surface of the metal substrate are reduced with hydrogen ions. This promotes activation of the substrate surface and has the effect that the adhesion of the coating layer coated on the substrate surface is improved.
第１図乃至第５図は本発明の実施例を示し、第１図は本
発明に用いられる装置の縦断面図、第２図および第３図
は清浄化方法の原理を示す模式図、第４図は本発明にお
ける工程を示すヒートサイクルを示す図、第５図は密着
性テストの結果を示す図であり、第６図は従来のイオン
ボンバードを示す模式図である。
１・・・・・・装置、２・・・・・・基体、３・・・・
・・真空炉。1 to 5 show embodiments of the present invention, FIG. 1 is a longitudinal sectional view of the apparatus used in the present invention, FIGS. 2 and 3 are schematic diagrams showing the principle of the cleaning method, and FIG. FIG. 4 is a diagram showing a heat cycle showing the steps in the present invention, FIG. 5 is a diagram showing the results of an adhesion test, and FIG. 6 is a schematic diagram showing a conventional ion bombardment. 1...device, 2...substrate, 3...
...Vacuum furnace.
Claims (1)
空炉内に載置し、該金属基体を電極として上記不活性ガ
スをイオン化し、その不活性ガスイオンで上記金属基体
表面上の吸着ガス分子を解離させ、その後、上記金属基
体を電極として上記水素をイオン化し、その水素イオン
で上記金属基体表面上の酸化物または窒化物のうち少な
くともどちらか一方を還元させることを特徴とする金属
の清浄化方法。(1) Place the metal substrate in a vacuum furnace into which an inert gas and hydrogen can be introduced, use the metal substrate as an electrode to ionize the inert gas, and use the inert gas ions to adsorb onto the surface of the metal substrate. A metal characterized by dissociating gas molecules, then ionizing the hydrogen using the metal substrate as an electrode, and reducing at least one of oxides and nitrides on the surface of the metal substrate with the hydrogen ions. cleaning method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3009788A JPH01205085A (en) | 1988-02-12 | 1988-02-12 | Method for cleaning metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3009788A JPH01205085A (en) | 1988-02-12 | 1988-02-12 | Method for cleaning metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01205085A true JPH01205085A (en) | 1989-08-17 |
Family
ID=12294275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3009788A Pending JPH01205085A (en) | 1988-02-12 | 1988-02-12 | Method for cleaning metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01205085A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995018880A1 (en) * | 1994-01-11 | 1995-07-13 | Tadahiro Ohmi | Method and apparatus for solid surface treatment, and apparatus for forming passivation film, and process apparatus |
| WO1997019204A1 (en) * | 1995-11-07 | 1997-05-29 | Seiko Epson Corporation | Method and apparatus for surface treatment |
| KR20040036977A (en) * | 2002-10-25 | 2004-05-04 | 한국수력원자력 주식회사 | electrochemical decontamination system for the removal of surface contamination in radioactive metal waste and method thereof |
| JP2004323977A (en) * | 2003-04-28 | 2004-11-18 | Air Products & Chemicals Inc | Method for removing metal oxide from substrate surface to be treated |
| EP1491643A3 (en) * | 2003-06-25 | 2005-11-23 | United Technologies Corporation | Heat treatment for workpieces |
-
1988
- 1988-02-12 JP JP3009788A patent/JPH01205085A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995018880A1 (en) * | 1994-01-11 | 1995-07-13 | Tadahiro Ohmi | Method and apparatus for solid surface treatment, and apparatus for forming passivation film, and process apparatus |
| WO1997019204A1 (en) * | 1995-11-07 | 1997-05-29 | Seiko Epson Corporation | Method and apparatus for surface treatment |
| KR20040036977A (en) * | 2002-10-25 | 2004-05-04 | 한국수력원자력 주식회사 | electrochemical decontamination system for the removal of surface contamination in radioactive metal waste and method thereof |
| JP2004323977A (en) * | 2003-04-28 | 2004-11-18 | Air Products & Chemicals Inc | Method for removing metal oxide from substrate surface to be treated |
| EP1491643A3 (en) * | 2003-06-25 | 2005-11-23 | United Technologies Corporation | Heat treatment for workpieces |
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