TW201105827A - Pretreatment method - Google Patents

Pretreatment method Download PDF

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TW201105827A
TW201105827A TW98127242A TW98127242A TW201105827A TW 201105827 A TW201105827 A TW 201105827A TW 98127242 A TW98127242 A TW 98127242A TW 98127242 A TW98127242 A TW 98127242A TW 201105827 A TW201105827 A TW 201105827A
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graphite substrate
graphite
substrate
remove
cleaning
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TW98127242A
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Chinese (zh)
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TWI391537B (en
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guo-zhen Zhang
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guo-zhen Zhang
Li wei rong
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Abstract

A pretreatment method is disclosed, and more particularly a surface treatment method carried out before performing an electroplating process of a graphite substrate. The method takes a sorbitan based activator of pH value between 3 and 9, and nitric acid with concentration between 3% and 50%, as the activator and the solvent used in the surface treatment method carried out before performing the electroplating process of the graphite substrate, so as to prevent the surface of the graphite substrate from being eroded and damaged due to the surface treatment, allowing the metal layer attached to the surface of the graphite substrate to have better binding force, thereby increasing the service life of metal layer.

Description

201105827 六、發明說明: 【發明所屬之技術領域】 一種前處理方法’尤指石墨基板於進行電鍍工程前,所進行 之表面處理方法,钵使石墨基板於電鍍後,附著於石墨基板表面 之金屬層為可具有較佳之結合力’並可使金屬層之壽命增加。 【先前技術】201105827 VI. Description of the invention: [Technical field of invention] A pretreatment method, in particular, a surface treatment method performed before a plating process on a graphite substrate, and a metal attached to the surface of the graphite substrate after electroplating of the graphite substrate The layer can have a better bonding force' and can increase the life of the metal layer. [Prior Art]

按’電子元件的體積趨於微小化,而且單位面積上的密集度 也愈來愈高,使電子元件的總發熱量則幾乎逐年升高,倘若沒有 良好的散熱方式來排除電子元件所產生的熱,這些過高的溫度將 導致電子7C件產生電子雜與誠力等縣造絲體的穩定性靖 低’以及驗電子元件本身的壽命,然而,就當前的散熱方式, 是以純銅雜合金來當熱擴散的基礎材料,或是更進—步的將靜 管埋入基礎,以加快熱擴散的速度,但此槪法所需之成 本也相對的提高了許多,而關、_導熱係數約為棚驗及 2_/=,在發熱量不斷升高的電子元件上,已漸漸的不敷使用, 而目前,碳為自然界卜種豐富含量的物質,且碳經由石墨化處 =後,可成為良好的電導體及熱導體,但是,由於石墨表面在後 蝕^時其表面所形成之金屬層,在短時間内即會產生腐 Γ製Γ二金屬層與石墨表面之結合力較差,進而導致後段加 用石墨較低’且成品使用壽命較短,因此,業界即排除使 問題與1作為導熱體’但本案之發明人,遂顿研究上述之 …之發生顧’進而發現石墨基板在進行紐工程前, 201105827 為必須先進彳了表Φ處理,以將石墨基絲面之油脂清除,但在清 除油脂時’都會利用ΗPM 4之溶劑來溶解油脂,但此種作法 為會造成;5,基板表面產生魏,而讓輔朗於石墨裡,且當 油脂清除後’騎濃度7 Q%摘酸,清洗石墨基板表面, 以去除石墨基板表面所產生之氧化物,此時,濃度7 Q%之硝酸 又會再-人大量的彳㈤石墨基板表面,而讓〃練殘留在石墨裡,使 石墨基板於電鑛金屬層後’金屬層與石墨基板之結合力較差,且 段時間後’殘留於石墨裡的硝酸與溶劑會造成金屬層腐飯、剝 落疋以本案之發明人即針對上述作法所產生之問題不斷的研 究以及試做’遂發展出本案之前處理方法。 【發明内容】 本發月之主要目的乃在於,细p Η值介於p Η 3至p Η 9 之間的山梨轉酐系活性劑與濃度介於3%至5〇%之間之硝 酸’作為石墨基板於進行電鑛I程前,所進行之表面處理方法所 使用之溶劑,以讓石墨基板於電錢後,附著於基 屬層為可騎擁找合力,射使金顧之壽命增加。 【實施方式】 造請=第-圖卿,_中可清楚看出,#石墨基板於電命 刖進仃表面處理時,係依照下列步驟進行: — 表面清洗^用溶劑清洗石墨基板表面,以去除石墨基相 髒/亏與顆粒,且溶劑在清洗石墨基 音波振频械力,糊恤_輪紐^ = 201105827 氣泡在形成生長和閉合產生強大振蘯力,使石墨基板表面沾附 的髒污與顆粒迅速脫離,進而更加徹底的清潔石墨基板表面。 (B) 脫脂:利用ph值介於PH3至PHg之間的山梨醣 * 醇酐系活性劑,來清除石墨基板表面所吸附的油脂,由於此有機 溶劑之PΗ值較為接近t性,因此較為不會侵蝕石墨基板表面。 (C) 水洗.清洗石墨基板表面於進行脫酯後,表面所殘留 之溶劑,且因步驟B所使用之溶劑不會對石墨基板表面侵蝕,進 • 而可讓此水洗步驟可更加的將溶劑清除乾淨。 (D) 活化:利用濃度介於3%至5 〇%之間之稀釋硝酸清 洗石墨基板表面,以去除石墨基板表面因脫酯及水洗所產生之氧 化物,並使石墨基板表面露出結晶組織,以讓石墨基板表面電鍍 金屬層後,金屬層於石墨基板表面可具有更佳之結合力,且此濃 度範圍之硝酸較為不會侵蝕石墨基板表面。 (E) 水洗·清除石墨基板表面因活化所殘留之確酸,且因 瞻步驟D所㈣之猶不會對石墨基板表面冊,進而可讓此水洗 步驟可更加的將硝酸清除乾淨。 當完成上述步驟後,即可對石墨基板進行電鍍工程,以讓石 墨基板表面鍍上金屬層,且由於石墨基板在進行電鍍前之表面處 理時’並未對石墨基板表面造成侵钱破壞,也未殘留山梨酶醇肝 系活性劑綱酸,因此,附著於石墨基板表面之麵層為可具有 較佳之結合力,且石墨内也未殘留溶劑汹酸,進而可使金屬層 之壽命增加。 201105827 再者,若 進行-次或一次以上之步驟D與步驟E,二: 表面 :材質ΓΓ=示’由圖中可清當石墨基板含有銘 =時’其观·繼冑行⑽叫魏照下列步驟 (Α)清洗:利用溶劑清洗石墨基板表面,以去除 ♦表面之髒污與赚,且溶齡親石墨基板表叫,為可_超 音波振盪的機械力,使溶劑中產生數以萬計的小氣泡,而這些小 氧泡在形成生長和閉合時產生強大振盪力,使石墨基板表面沾附 的髒污無粒迅速雌,進而更加徹底的清潔石墨基板表面。 。⑻脫脂:利用印值介於ΡΗ3至ΡΗ9之間的山梨酶 2軒系活性劑,來清除石墨基板表面所吸_油脂,由於此有機 鲁确之ρ Η錄為接近十性’因此較為不會侵餘石墨基板表面。 (C) 水洗·清洗石墨基板表面於進行脫酯後,表面所殘留 之溶劑’且因步驟Β所額之溶劑不會對石墨基板表面絲,進 -而可讓此水洗步驟可更加的將溶劑清除乾淨。 (D) 活化·利用濃度介於3 %至5 〇 %之ρ《之;ε肖酸清洗石 墨基板表面,以去除石墨基板表面因脫酯及水洗所產生之氧化 物’並使石墨基板表面露出結晶組織,以讓石墨基板表面電鑛金 屬層後,金屬層於石墨基板表面可具有更佳之結合力,且此濃度 範園之硝酸較為不會侵蝕石墨基板表面。 201105827 ⑻水洗:練石墨絲表_活倾㈣之猶,且因 步驟D所使狀_不會對石墨基板表面,進而可讓此水洗 步驟可更加的將靖酸清除乾淨。According to the 'electronic components, the volume tends to be miniaturized, and the density per unit area is getting higher and higher, so that the total heat generation of electronic components is almost increased year by year, if there is no good heat dissipation method to eliminate the electronic components. Heat, these excessive temperatures will cause the electronic 7C parts to produce electronic impurities and the stability of the silk fabrics of Chengli County and the life of the electronic components themselves. However, the current heat dissipation method is pure copper alloy. To be the base material for thermal diffusion, or to further embed the static tube into the foundation to speed up the heat diffusion, but the cost of this method is also relatively improved, and the thermal conductivity About the shed inspection and 2_/=, on the electronic components with increasing heat generation, it has gradually disappeared. At present, carbon is a natural substance rich in content, and carbon can pass through the graphitization = It becomes a good electrical conductor and a thermal conductor. However, due to the metal layer formed on the surface of the graphite surface after the back etching, the bonding force between the two metal layers and the graphite surface is poor in a short time. In turn, the graphite added in the latter stage is lower and the service life of the finished product is shorter. Therefore, the industry has ruled out the problem with 1 as the heat conductor. However, the inventor of the case, the research of the above-mentioned... Before the New Zealand project, 201105827 must be advanced to the table Φ treatment to remove the grease on the graphite base surface, but in the removal of grease, 'the solvent of PM 4 will be used to dissolve the grease, but this will cause; 5 The surface of the substrate is produced by Wei, and the auxiliary is applied to the graphite, and when the grease is removed, the concentration is 7 Q%, and the surface of the graphite substrate is cleaned to remove the oxide generated on the surface of the graphite substrate. At this time, the concentration is 7 Q. % of nitric acid will be again - a large number of bismuth (five) graphite substrate surface, and let the sputum remain in the graphite, so that the graphite substrate in the electro-mineral metal layer 'metal layer and graphite substrate bonding is poor, and after a period of time' The nitric acid and solvent remaining in the graphite will cause the metal layer to be rotted and peeled off. The inventor of this case is constantly researching and solving the problems caused by the above-mentioned practices. Pre-treatment method. SUMMARY OF THE INVENTION The main purpose of this month is to have a fine p Η value between p Η 3 and p Η 9 of sorbic acid-based active agent and a concentration of between 3% and 5% by weight of nitric acid. As a graphite substrate, the solvent used in the surface treatment method before the electro-metal I process is performed, so that the graphite substrate can be attached to the basal layer after the electricity is charged, and the life of the gyro can be increased. . [Embodiment] It is clear that the #石图, _ can clearly see that the #graph substrate is treated in the following steps: - Surface cleaning ^ Clean the surface of the graphite substrate with a solvent to Remove the graphite-based phase dirty/deficient and particles, and the solvent is cleaning the graphite-based sound waves. The paste _ wheel ^ ^ ^ 201105827 Bubbles in the formation of growth and closure produce strong vibrating force, so that the surface of the graphite substrate is dirty The dirt and particles are quickly detached, thereby further cleaning the surface of the graphite substrate. (B) Degreasing: The sorbose* alcoholic acid active agent having a pH between pH 3 and PHg is used to remove the grease adsorbed on the surface of the graphite substrate. Since the P Η value of the organic solvent is relatively close to t, it is not Will erode the surface of the graphite substrate. (C) Washing. Cleaning the surface of the graphite substrate after de-esterification, the solvent remaining on the surface, and the solvent used in step B does not erode the surface of the graphite substrate, so that the water washing step can further solvent Clean up. (D) Activation: The surface of the graphite substrate is cleaned by dilute nitric acid at a concentration between 3% and 5% by weight to remove oxides from the surface of the graphite substrate due to de-esterification and water washing, and to expose the surface of the graphite substrate to crystal structure. After the metal layer is plated on the surface of the graphite substrate, the metal layer can have a better bonding force on the surface of the graphite substrate, and the nitric acid in the concentration range does not corrode the surface of the graphite substrate. (E) Washing and removing the acid residue remaining on the surface of the graphite substrate due to activation, and the surface of the graphite substrate is not covered by the step (4), so that the water washing step can further remove the nitric acid. After the above steps are completed, the graphite substrate can be electroplated to plate the surface of the graphite substrate with a metal layer, and since the graphite substrate is subjected to surface treatment before electroplating, it does not cause damage to the surface of the graphite substrate. Since the sorbitan liver active agent acid is not left, the surface layer adhering to the surface of the graphite substrate has a good binding force, and the solvent does not remain in the graphite, and the life of the metal layer can be increased. 201105827 Furthermore, if step-D and step E are performed one or more times, two: surface: material ΓΓ = show 'can be clear from the figure when the graphite substrate contains the inscription = when it's view · the next step (10) called Wei Zhao The following steps (Α) cleaning: cleaning the surface of the graphite substrate with a solvent to remove the dirt and profit of the surface of the ♦, and the surface of the pro-graphite substrate is called a mechanical force that can oscillate, causing tens of thousands of solvents. The small bubbles are counted, and these small oxygen bubbles generate a strong oscillating force when forming growth and closure, so that the surface of the graphite substrate is stained with no particles and quickly, and the surface of the graphite substrate is more thoroughly cleaned. . (8) Degreasing: using the sorbic acid 2 Xuan active agent with a value between ΡΗ3 and ΡΗ9 to remove the _ grease from the surface of the graphite substrate, since this organic ruthenium ρ Η is close to the ten-sex' Residual graphite substrate surface. (C) Washing and cleaning the surface of the graphite substrate after the de-esterification, the solvent remaining on the surface' and the solvent due to the step does not affect the surface of the graphite substrate, so that the water washing step can further solvent Clean up. (D) Activation·Using a concentration of 3% to 5% of ρ"; ε-chamoic acid cleans the surface of the graphite substrate to remove oxides from the surface of the graphite substrate due to de-esterification and water washing' and expose the surface of the graphite substrate After crystallizing the structure to make the surface of the graphite substrate electro-mineral metal layer, the metal layer can have better bonding force on the surface of the graphite substrate, and the nitric acid of the concentration is not corroded on the surface of the graphite substrate. 201105827 (8) Washing: Practicing graphite wire table _ live tilting (four), and because of step D, it will not be on the surface of the graphite substrate, so that this washing step can further remove the acid.

I (F )#置換i程:彻鋅置紐,麟離子置翻銘表面 形成-層鋅金屬薄膜,以利含崎f之石墨基板進行電鑛工程。 (G)水洗.清除石墨基板表面殘留之鋅置換液。 當完成上述步驟後,即可對石墨基板進行電錢工程,以讓含 有鋁材質之石墨基板表面鍍上金屬層,且由於石墨基板在進行電 鑛前之表面處辦,並未對石墨基板表面造成侵触壞,也未殘 留山梨醣醇酐系活性劑或硝酸,因此,附著於石墨基板表面之金 層為了具有較佳之結合力,且石墨内也未殘留溶劑或硝酸,進 而可使金屬層之壽命增加。 再者’若要增加金屬層與石墨基板表面之結合力,為可重覆 進订一次或一次以上之步驟D至步驟G,以更加的活化石墨基板 表面。 【圖式簡單說明】 第圖係為本發明較佳實施方式之流程圖。 曾一 一圖係為本發明再一較佳實施方式之流程圖。 【主要元件符號說明】I (F )# Replacement i: The zinc is placed in the nucleus, and the lining of the lining is placed on the surface of the surface. A zinc-based metal film is formed to facilitate the electro-mineral engineering of the graphite substrate containing the saki. (G) Washing. Remove the zinc replacement liquid remaining on the surface of the graphite substrate. After the above steps are completed, the graphite substrate can be subjected to an electric money project to plate the surface of the graphite substrate containing the aluminum material with a metal layer, and since the graphite substrate is disposed on the surface before the electric ore, the surface of the graphite substrate is not Intrusion is caused, and no sorbitan-based active agent or nitric acid remains. Therefore, the gold layer attached to the surface of the graphite substrate has a good bonding force, and no solvent or nitric acid remains in the graphite, and the metal layer can be further Life expectancy increases. Further, if the bonding force between the metal layer and the surface of the graphite substrate is to be increased, step D to step G can be repeated one or more times to further activate the surface of the graphite substrate. BRIEF DESCRIPTION OF THE DRAWINGS The drawings are a flow chart of a preferred embodiment of the invention. The prior art is a flow chart of still another preferred embodiment of the present invention. [Main component symbol description]

Claims (1)

201105827 七、申請專利範圍: 1、一種前處理方法’尤指石墨基板於電鍍前所使用之表面 處理方法,該處理方法係依照下列步驟進行: (A)清洗:利用溶劑清洗石墨基板表面,以去除石墨基板 表面之髒污與顆粒; (B) 脫醋:利用ρη值介於PH3至PΗ9之間的脂肪族 酯類有機溶劑,來清除石墨基板表面所吸附的油脂; (C) 水洗:清洗石墨基板表面於進行脫酯後,表面所殘留 之溶劑; (D) 活化:利用濃度介於3%至5 〇%之間之罐酸清洗石 i基板表φ ’以去除;g墨基板表關細旨及水洗所產生之化 物,並使石墨基板表面露出結晶組織; / E )水洗··清除石墨基板表面因活化所殘留之硝酸; ^上’即可將石墨基板進行電鑛工程,以讓石墨基板表 上金屬層。 申請專利範圍第1項所述之前處理方法 D與步驟E材重覆進行—次或—次以上。 3、 如申請專利範圍第工項所述之前處理 A利用溶劑清洗 4、 w 為可簡音波清洗方式為之 所使用的表面Γ處理方法,尤指含有練f之石墨基板於電鑛 (Ah方法,該處理方法係依照下列步戰進行: 先利用落劑清洗石墨基板表面,以去除石墨基1 201105827 表面之辭污與顆粒; (B) 脫酯:利用ρη值介於ρη3至PΗ9之間的脂肪族 酉曰類有機溶劑,來清除石墨基板表面所吸附的油脂; » (C) 水洗:清洗石墨基板表面於進行脫酯後,表面所殘留 之溶劑; (D)活化:利用濃度介於3%至5 〇%之間之硝酸清洗石 墨基板表面,以去除石墨基板表面因脫酯及水洗所產生之氧化 •物,並使石墨基板表面露出結晶組織; (Ε )水洗· ’月除石墨基板表面因活化所殘留之石肖酸; (F)鋅置換工程:利用鋅置換液,將鋅離子置換到鋁表面 形成一層鋅金屬薄膜; G)水洗:清除石墨基板表面殘留之辞置換液; 上金屬層 藉上’即可將石墨基板進行電鍍工程,以讓石墨基板表面鑛 D至步驟處理方法’該步驟 A利4項所述之前處理方法’其中該步驟 先石墨基板表面時,為可以超音波清洗方式為之。201105827 VII. Patent application scope: 1. A pretreatment method, especially the surface treatment method used for the graphite substrate before electroplating. The treatment method is carried out according to the following steps: (A) Cleaning: cleaning the surface of the graphite substrate with a solvent to Remove the dirt and particles on the surface of the graphite substrate; (B) De-acetalization: remove the grease adsorbed on the surface of the graphite substrate by using an aliphatic ester organic solvent having a pη value between PH3 and PΗ9; (C) Washing: cleaning The surface of the graphite substrate after the de-esterification, the solvent remaining on the surface; (D) Activation: using a tank acid cleaning solution with a concentration between 3% and 5 〇% to remove the substrate φ ' to remove; g ink substrate surface The purpose of the product and the product produced by washing, and the surface of the graphite substrate is exposed to the crystal structure; / E) water washing · removing the residual nitric acid on the surface of the graphite substrate due to activation; ^ on the graphite substrate can be electro-mine engineering, so that A metal layer on the graphite substrate. Prior to the application of the patent scope, the treatment method D and the step E material are repeated for one or more times. 3. Before the application of the scope of the patent application, the treatment A uses solvent cleaning. 4, w is the surface enthalpy treatment method used for the simple sound wave cleaning method, especially the graphite substrate containing the modified f in the electric ore (Ah method). The treatment method is carried out according to the following steps: firstly, the surface of the graphite substrate is cleaned by using a falling agent to remove the smudges and particles on the surface of the graphite base 1 201105827; (B) De-esterification: using a ρη value between ρη3 and PΗ9 An aliphatic terpene organic solvent to remove grease adsorbed on the surface of the graphite substrate; » (C) Washing: cleaning the surface of the graphite substrate after de-esterification, the solvent remaining on the surface; (D) Activation: using a concentration of 3 Nitric acid cleans the surface of the graphite substrate between 5% and 5% to remove oxides from the surface of the graphite substrate due to de-esterification and water washing, and expose the surface of the graphite substrate to the crystal structure; (Ε) Washing · 'Month removal graphite substrate (D) zinc replacement engineering: using zinc replacement liquid, replacing zinc ions with aluminum surface to form a zinc metal film; G) washing: removing graphite substrate Residual residue replacement liquid; the upper metal layer can be used to electroplating the graphite substrate to allow the graphite substrate surface to be D to the step processing method. When the surface of the graphite substrate is used, it can be ultrasonically cleaned.
TW98127242A 2009-08-13 2009-08-13 Pretreatment method TW201105827A (en)

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