TWI554650B - A cooling functional electrochemical mold - Google Patents
A cooling functional electrochemical mold Download PDFInfo
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- TWI554650B TWI554650B TW104111191A TW104111191A TWI554650B TW I554650 B TWI554650 B TW I554650B TW 104111191 A TW104111191 A TW 104111191A TW 104111191 A TW104111191 A TW 104111191A TW I554650 B TWI554650 B TW I554650B
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Description
本發明是關於一種適用於工作樣品表面或局部表面之電化學處理用模具,此模具可使待處理樣品之特定表面裸露,並使工作樣品在進行電化學加工時保持特定的溫度,此具有冷卻功能的電化學治具可提供需特定裸露之樣品表面進行電解、電解拋光、電鍍、陽極處理、蝕刻、浸鍍、酸洗、鹼洗、等綠能相關產業之製程。 The invention relates to an electrochemical treatment mold suitable for working on a surface or a partial surface of a working sample, which can expose a specific surface of a sample to be treated and maintain a specific temperature of the working sample during electrochemical processing, which has cooling The functional electrochemical fixture can provide processes for the green energy-related industries such as electrolysis, electropolishing, electroplating, anodizing, etching, immersion plating, pickling, caustic washing, etc. on the surface of a specific exposed sample.
學術或研究單位在製作電化學小試片時可簡單地控制所需的實驗條件,但是當樣品尺寸與數量放大至工業界量產時卻常常面臨到電流密度和溫度不穩定的問題。 Academic or research units can simply control the experimental conditions required when making electrochemical small test strips, but often suffer from current density and temperature instability when the sample size and quantity are scaled up to industrial mass production.
一般教科書對於電化學的反應,常以簡單的示意圖解釋之,其中陽極又稱為氧化極,於反應過程中易失去電子、或產生離子化,陰極又稱為還原極,於反應過程中易得到電子或接受正離子,而外加電壓/電流值與電解液的成份、濃度、溫度、與攪伴乃是控制反應速率的重要參數,由於示意圖為一簡便且眾所容易接受之反應機構圖,因此,學界之基 本電化學實驗,或業界之量產製程中設備,均以此示意圖為標準設計的參考,然而,此圖乃是一理想化之示意圖,該設計於電化學反應中將產生如反應面積不易估算、電極邊緣反應速率較快等缺點。 The general textbook's reaction to electrochemistry is often explained by a simple diagram. The anode is also called the oxidation pole. It is easy to lose electrons or ionize during the reaction. The cathode is also called the reduction pole. It is easy to get in the reaction process. Electron or accept positive ions, and the applied voltage/current value and electrolyte composition, concentration, temperature, and stirring are important parameters for controlling the reaction rate. Since the schematic diagram is a simple and easily accepted reaction mechanism diagram, Foundation of the academic world This electrochemical experiment, or the equipment in the mass production process of the industry, is based on this schematic diagram as a standard design reference. However, this figure is an idealized schematic diagram, which will produce an easy estimation of the reaction area in the electrochemical reaction. , the electrode edge reaction rate is faster and other shortcomings.
為了改善以上示意圖於實際電化學反應中所產生之缺點,一些較精密的電化學量測實驗常以管罩式為設計,即工作電極(working electrode)表面利用一個已知表面積之玻璃管罩住,管內裝有電解液,而對極(counter electrode)電極則由管之上端開口處置入管內,並於管內形成一電化學反應系統,此設計可改善反應面積的量測與局部反應速率不均勻的問題,但是管內之電解液容量有限,易造成長時間反應後之濃度下降的情形。槽狀式為另一種電化學反應設計,乃是將工作樣品固定於電解槽外,而電解槽壁之開口面積即為樣品之反應面積,再將對極電極置於電解槽內,此設計可解決電解液濃度下降的問題,然而此設計之缺點在於裝卸工作電極時易造成電解液洩漏,或是需將電解液事先由反應槽內取出的缺點。 In order to improve the shortcomings of the above schematic diagram in the actual electrochemical reaction, some more precise electrochemical measurement experiments are often designed with a tube cover type, that is, the working electrode surface is covered with a glass tube of a known surface area. The tube is filled with electrolyte, and the counter electrode is disposed in the tube from the upper end of the tube, and an electrochemical reaction system is formed in the tube. This design can improve the measurement of the reaction area and the local reaction rate. The problem of unevenness, but the electrolyte capacity in the tube is limited, which tends to cause a decrease in the concentration after a long period of reaction. The groove type is another electrochemical reaction design, which is to fix the working sample outside the electrolytic cell, and the opening area of the wall of the electrolytic cell is the reaction area of the sample, and then the counter electrode is placed in the electrolytic cell. The problem of lowering the concentration of the electrolyte is solved. However, the disadvantage of this design is that the electrolyte is easily leaked when the working electrode is loaded or unloaded, or the electrolyte is required to be taken out from the reaction tank in advance.
針對以上工件在反應過程中的電流密度與溫度控制的穩定性,本發明專利將提出不同設計之電化學處理用治具設計來提升量產形電化學製程的穩定性。 In view of the current density and temperature control stability of the above workpiece during the reaction process, the present invention will propose a design of an electrochemical treatment jig of different designs to improve the stability of the mass production electrochemical process.
本發明之目的在於提供一種具有冷卻功能的電化學治具,藉由治具的輔助使樣品的特定區域可進行電化學反應與加工等化學反應。本發明專利考量了模具的操作方便性、使用壽命延長、與商業價值,因此利用低材料成本的聚合物、金屬、金屬表面經絕緣處理等絕緣材料聚 合物、工程塑膠、聚合物、或壓克力製造一種化學處理用的治具並應用濕式化學處理環境中,此化學處理用的治具結構具有生產簡單性與面積變化性大等特性,適用於工業量產上。此一種具有冷卻功能的電化學治具之分解圖10結構如第1圖所示,包含:治具群組10a;噴灑式同軸線水冷式電極群組10b;與導電棒群組所組合10c,其中,治具群組10a包含:治具下座101;下座第一表面螺牙孔102;下座第二表面螺牙孔103;導電棒螺牙孔104;治具上蓋105;治具下蓋106;上蓋防水墊圈107;下蓋防水墊圈108;導電片109;工作樣品110;試片防水墊圈111,噴灑式同軸線水冷式電極群組10b包含:電極腔體座112;電極蓋113;電極蓋防水墊圈114;進水管115;出水管116;進水導管117;出水導管118;此噴灑式同軸線水冷式電極群組10b的特點在於;進出水口在於同一軸線上,入水口將冷卻水噴灑致電極管內後,出水口讓冷卻水在同軸線上流出,達到快速冷卻的效果;導電棒群組10c包含:彎頭管119;彎頭管螺牙120;彎頭管蓋121;彎頭管銜接軟管122;矽膠塞123;絕緣套管124;導電棒125;導電柱126;彎頭管防水墊圈127。 It is an object of the present invention to provide an electrochemical jig having a cooling function, wherein a specific region of a sample can be subjected to a chemical reaction such as electrochemical reaction and processing by the aid of a jig. The invention patent considers the convenience of the operation of the mold, the service life is prolonged, and the commercial value, so the polymer, the metal, the metal surface of the low material cost is insulated, the insulating material polymer, the engineering plastic, the polymer, or the acrylic The company manufactures a jig for chemical treatment and applies it in a wet chemical treatment environment. The jig structure for chemical treatment has characteristics such as simple production and large area variability, and is suitable for industrial mass production. This structure of the one shown in exploded view 10 of the electrochemical jig having a cooling function as FIG. 1, comprising: a fixture 10a group; spray type water-cooled coaxial electrode group 10B; and the combined group 1OC conductive rod, Wherein, the fixture group 10a comprises: a fixture lower seat 101 ; a lower seat first surface screw hole 102 ; a lower seat second surface screw hole 103 ; a conductive rod screw hole 104 ; a fixture upper cover 105 ; Cover 106 ; upper cover waterproof gasket 107 ; lower cover waterproof gasket 108 ; conductive sheet 109 ; working sample 110 ; test strip waterproof gasket 111 , spray coaxial water-cooled electrode group 10b : electrode cavity seat 112 ; electrode cover 113 ; Electrode cover waterproof gasket 114 ; inlet pipe 115 ; outlet pipe 116 ; inlet conduit 117 ; outlet conduit 118 ; the spray-type coaxial water-cooled electrode group 10b is characterized in that the inlet and outlet are on the same axis, and the inlet is cooled. After spraying into the electrode tube, the water outlet allows the cooling water to flow out on the coaxial line to achieve rapid cooling effect; the conductive rod group 10c includes: elbow tube 119 ; elbow tube thread 120 ; elbow tube cover 121 ; elbow Pipe connection hose 1 22 ; silicone plug 123 ; insulating sleeve 124 ; conductive rod 125 ; conductive column 126 ; elbow tube waterproof gasket 127 .
第2圖更說明了具有冷卻功能的電化學治具立體組合圖20,其結構包括一中空之治具下座201;用於與治具下座201相結合之治具上蓋202與治具下蓋203;設置於冷卻電極端之進水管204與出水管205;用於延伸進水管204與出水管205之進水導管206與出水導管207;設置於中空治具下座201側邊之彎頭管208;彎頭管208下方設置有彎頭管蓋209;並於彎頭管208與彎頭管蓋209之間插入用於防止滲水之彎頭管銜接軟管210;彎頭管銜接軟管210之另一端設置有用於防止滲水之矽膠塞211;將 絕緣套管213插入矽膠塞211、彎頭管銜接軟管210、與彎頭管208內;再將導電棒214插入絕緣套管213內並與冷卻電極之側邊互相接觸;彎頭管208與中空治具下座201之接觸面設置有彎頭管防水墊圈212用於防止滲水。 FIG. 2 further illustrates a three-dimensional combination diagram 20 of an electrochemical fixture having a cooling function, the structure comprising a hollow fixture lower seat 201 ; and a fixture upper cover 202 and a fixture under the fixture lower seat 201 a cover 203 ; an inlet pipe 204 and an outlet pipe 205 disposed at the end of the cooling electrode; a water inlet pipe 206 and a water outlet pipe 207 for extending the inlet pipe 204 and the outlet pipe 205 ; and an elbow disposed at the side of the lower seat 201 of the hollow jig a tube 208 ; an elbow tube cover 209 is disposed under the elbow tube 208 ; and an elbow tube connecting hose 210 for preventing water seepage is inserted between the elbow tube 208 and the elbow tube cover 209 ; the elbow tube is connected to the hose The other end of the 210 is provided with a rubber stopper 211 for preventing water seepage; the insulating sleeve 213 is inserted into the rubber stopper 211 , the elbow pipe connecting hose 210 , and the elbow pipe 208 ; and the conductive bar 214 is inserted into the insulating sleeve 213 . And contacting the side of the cooling electrode with each other; the contact surface of the elbow pipe 208 and the hollow fixture lower seat 201 is provided with an elbow pipe waterproof gasket 212 for preventing water seepage.
第3圖說明了工作樣品置於具有冷卻功能的電化學治具立體組合圖30,用於與治具下座303相結合之治具上蓋304與治具下蓋306;設置於中空之治具下座303與治具上蓋304之間之上蓋防水墊圈305;工作樣品301裝置於治具下座303之一表面並利用治具上蓋304鎖緊; 工作樣品301之一表面與治具上蓋304之間設置有試片防水墊圈302;進水導管307與出水導管308設置於冷卻電極下端並由治具下座303之第二表面伸出;;設置於中空治具下座201側邊之彎頭管309;彎頭管309;彎頭管蓋310;彎頭管銜接軟管311;矽膠塞312;絕緣套管314;導電棒315;彎頭管防水墊圈313;彎頭管309下方設置有彎頭管蓋310;並於彎頭管309與彎頭管蓋310之間插入用於防止滲水之彎頭管銜接軟管311;彎頭管銜接軟管311之另一端設置有用於防止滲水之矽膠塞312;將絕緣套管314插入矽膠塞312、彎頭管銜接軟管311、與彎頭管內309;再將導電棒315插入絕緣套管314內並與冷卻電極之側邊互相接觸;彎頭管309與中空治具下座303之接觸面設置有彎頭管防水墊圈313用於防止滲水。 Figure 3 illustrates a three-dimensional assembly diagram 30 of an electrochemical fixture having a cooling function, a fixture upper cover 304 and a fixture lower cover 306 combined with the fixture lower seat 303 ; the lower seat 303 and the fixture 305 between the upper cover cover the waterproof packing 304; means to a work sample 301 of a jig lower seat surface 303 using a jig upper lid 304 and the locking; one work fixture 301 and the surface 304 of the sample cover A test piece waterproof gasket 302 is disposed between; the water inlet conduit 307 and the water outlet conduit 308 are disposed at a lower end of the cooling electrode and protrude from a second surface of the fixture lower seat 303 ; and an elbow disposed at a side of the hollow fixture lower seat 201 Tube 309 ; elbow tube 309 ; elbow tube cover 310 ; elbow tube connection hose 311 ; silicone plug 312 ; insulating sleeve 314 ; conductive rod 315 ; elbow tube waterproof gasket 313 ; elbow tube 309 is provided with a bend The head pipe cover 310 ; and an elbow pipe connecting hose 311 for preventing water seepage is inserted between the elbow pipe 309 and the elbow pipe cover 310 ; the other end of the elbow pipe connecting hose 311 is provided with a silicone rubber for preventing water seepage. Plug 312 ; insert the insulating sleeve 314 into the silicone plug 312 , elbow pipe Connect the hose 311 and the elbow tube 309 ; then insert the conductive rod 315 into the insulating sleeve 314 and contact the side of the cooling electrode; the contact surface of the elbow tube 309 and the hollow fixture lower seat 303 is curved. The head pipe waterproof gasket 313 is used to prevent water seepage.
第4圖說明了水冷式電極分解結構圖40,包含中空之電極腔體座401用於進行水冷卻之熱交換用;電極腔體座401之第一表面為電極接觸面402;電極腔體座401之第二表面為母螺牙403結構;電極蓋防水墊圈404設置於電極腔體座401之第二表面與電極蓋405之間;電極蓋405之第一表面為公螺牙406結構;電極蓋405之第二表面設置 有進水管407與出水管408且進水管伸入中空之電極腔體座401內。 Figure 4 is a diagram showing a water-cooled electrode decomposition structure 40 , including a hollow electrode cavity holder 401 for heat exchange for water cooling; a first surface of the electrode cavity holder 401 is an electrode contact surface 402 ; an electrode cavity holder The second surface of the 401 is a female screw 403 structure; the electrode cover waterproof gasket 404 is disposed between the second surface of the electrode cavity holder 401 and the electrode cover 405 ; the first surface of the electrode cover 405 is a male screw 406 structure; The second surface of the cover 405 is provided with an inlet pipe 407 and an outlet pipe 408 and the inlet pipe extends into the hollow electrode cavity seat 401 .
第5圖說明了水冷式電極立體組合圖50,包含一中空之電極腔體座501用於進行水冷卻之熱交換用;電極腔體座501之第一表面為電極接觸面502;電極蓋與503與電極腔體座501之第二表面相結合;電極蓋503之一表面設置有進水管504與出水管505;用於延伸進水管與出水管之進水導管506與出水導管507。 Figure 5 illustrates a water-cooled electrode three-dimensional assembly diagram 50 , including a hollow electrode cavity holder 501 for heat exchange for water cooling; the first surface of the electrode cavity holder 501 is an electrode contact surface 502 ; the electrode cover and 503 combined with the second surface of the electrode chamber, 501; 503, one surface of the electrode cover 504 is provided with a water inlet pipe 505 and outlet pipe; means for extending into the inlet and outlet pipe of the outlet conduit 506 and conduit 507.
以下,茲使用第1圖~第9圖來詳細說明本發明相關之具有冷卻功能的電化學治具之各實施例。此外,在圖面的說明中,同一要素或具有同一機能的要素係使用同一符號,並省略重複的說明。 Hereinafter, each embodiment of the electrochemical jig having a cooling function according to the present invention will be described in detail using Figs. 1 to 9 . In the description of the drawings, the same elements or elements having the same function are denoted by the same reference numerals, and the description thereof will not be repeated.
以第1圖之模具實體進行鋁材表面之電解拋光,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過酸洗與鹼洗後之鋁材進行電解拋光使鋁材表面具有鏡面反射效果。利用模具之開口範圍限定鋁片表面之待處理面積,並利用外加電壓與電解液成份來控制電解拋光的品質,電解拋光的條件為:5~20%過氯酸(HClO4)+5~20%單丁醚乙二脂(CH3(CH2)3OCH2CH2OH)+85~95%乙醇(C2H6O),電解液溫度為2~40℃,電解電壓為5~50伏特,電解拋光時間為1~10分鐘,第6圖顯示較佳的電解拋光操作條件為15%過氯酸(HClO4)+15%單丁醚乙二脂(CH3(CH2)3OCH2CH2OH)+70%乙醇(C2H6O),電解液溫度為25℃,電解電壓為40伏特,電解拋光時 間為1.5分鐘,利用本模具處理後的鋁板表面具有光學級的反射平面,其樣品照片如如第7圖所示。 The surface of the aluminum material was electropolished by the mold body of Fig. 1, and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the aluminum material after pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the applied voltage and electrolyte composition are used to control the quality of the electropolishing. The conditions of the electropolishing are: 5-20% perchloric acid (HClO 4 ) + 5~20 % monobutyl ether ethylene diester (CH 3 (CH 2 ) 3 OCH 2 CH 2 OH) + 85 ~ 95% ethanol (C 2 H 6 O), electrolyte temperature is 2 ~ 40 ° C, electrolysis voltage is 5 ~ 50 Volt, electropolishing time is 1~10 minutes, Figure 6 shows the best electropolishing operation condition is 15% perchloric acid (HClO 4 ) + 15% monobutyl ether ethylene diester (CH 3 (CH 2 ) 3 OCH 2 CH 2 OH)+70% ethanol (C 2 H 6 O), the electrolyte temperature is 25 ° C, the electrolysis voltage is 40 volts, the electropolishing time is 1.5 minutes, and the surface of the aluminum plate treated with the mold has an optical grade reflection. The plane, the sample photo is as shown in Figure 7 .
以第1圖之模具實體進行鋁材表面之電解拋光,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過酸洗與鹼洗後之鋁材進行電解拋光使鋁材表面具有鏡面反射效果。利用模具之開口範圍限定鋁片表面之待處理面積,並利用外加電壓與電解液成份來控制電解拋光的品質,電解拋光操作條件為15%過氯酸(HClO4)+15%單丁醚乙二脂(CH3(CH2)3OCH2CH2OH)+70%乙醇(C2H6O),電解液溫度為5℃,電解電壓為50伏特,電解拋光時間為3分鐘,利用本模具處理後的鋁板表面具有光學級的反射平面。 The surface of the aluminum material was electropolished by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the aluminum material after pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the quality of the electropolishing is controlled by the applied voltage and the electrolyte composition. The electropolishing operation condition is 15% perchloric acid (HClO 4 ) + 15% monobutyl ether B Diester (CH 3 (CH 2 ) 3 OCH 2 CH 2 OH) + 70% ethanol (C 2 H 6 O), electrolyte temperature 5 ° C, electrolysis voltage 50 volts, electropolishing time 3 minutes, using this The surface of the aluminum plate after the mold treatment has an optical level of reflection plane.
以第1圖之模具實體進行鋁材表面之電解拋光,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過酸洗與鹼洗後之鋁材進行電解拋光使鋁材表面具有鏡面反射效果。利用模具之開口範圍限定鋁片表面之待處理面積,並利用外加電壓與電解液成份來控制電解拋光的品質,電解拋光操作條件為15%過氯酸(HClO4)+15%單丁醚乙二脂(CH3(CH2)3OCH2CH2OH)+70%乙醇(C2H6O),電解液溫度為40℃,電解電壓為20伏特,電解拋光時間為0.5分鐘,利用本模具處理後的鋁板表面具有光學級的反射平面,此平整的表面具有光學級的反射平面。 The surface of the aluminum material was electropolished by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the aluminum material after pickling and alkali washing is electropolished to give a specular reflection effect on the surface of the aluminum. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the quality of the electropolishing is controlled by the applied voltage and the electrolyte composition. The electropolishing operation condition is 15% perchloric acid (HClO 4 ) + 15% monobutyl ether B Diester (CH 3 (CH 2 ) 3 OCH 2 CH 2 OH) + 70% ethanol (C 2 H 6 O), electrolyte temperature 40 ° C, electrolysis voltage 20 volts, electropolishing time 0.5 minutes, using this The surface of the aluminum plate after the mold treatment has an optical level of reflection plane having an optical level of reflection plane.
以第1圖之模具實體進行鋁材之表面之陽極處理處理,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過機械研磨之鋁片再經陽極處理後可使鋁片反應成多孔性之三氧化二鋁薄膜。利用模具之開口範圍限定鋁片表面之待處理面積,使鋁片表面與經陽極處理後產生多孔性之三氧化二鋁薄膜,並利用外加電壓與電解液成份來控制孔密度的分佈與孔洞的大小,陽極處理的電解液主要以硫酸、磷酸、或草酸為主。利用3wt.%(重量百分比)草酸水溶液為電解液、外加40伏特直流電壓、陽極處理時間1小時、電解液溫度為25℃、可使金屬鋁片表面反應產生半透明的三氧化二鋁薄膜,再利用飽和氯化銅溶液將殘留的鋁基材移除後可得多孔性透明的三氧化二鋁薄膜。 The surface of the aluminum material was anodized by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the mechanically ground aluminum sheet is anodized to react the aluminum sheet into a porous aluminum oxide film. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the surface of the aluminum sheet is treated with anodized aluminum oxide film, and the applied voltage and electrolyte composition are used to control the distribution of pore density and the pores. The size and anode treated electrolyte are mainly sulfuric acid, phosphoric acid, or oxalic acid. Using a 3wt.% (by weight) aqueous solution of oxalic acid as the electrolyte, an external DC voltage of 40 volts, an anodic treatment time of 1 hour, and an electrolyte temperature of 25 ° C, the surface of the metal aluminum sheet can be reacted to produce a translucent aluminum oxide film. The porous aluminum substrate is removed by using a saturated copper chloride solution to obtain a porous transparent aluminum oxide film.
以第1圖之模具實體進行鋁材之表面之陽極處理處理,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過機械研磨之鋁片再經陽極處理後可使鋁片反應成多孔性之三氧化二鋁薄膜。利用模具之開口範圍限定鋁片表面之待處理面積,使鋁片表面與經陽極處理後產生多孔性之三氧化二鋁薄膜,並利用外加電壓與電解液成份來控制孔密度的分佈與孔洞的大小,陽極處理的電解液主要以硫酸、磷酸、或草酸為主,利用10vol.%(體積百分比)硫酸水溶液為電解液、外加20伏特直流電壓、陽極處理時間1小時、電解液溫度為15℃、可使金屬鋁片表面反應產生半透明的三氧化二鋁薄膜,再利用飽和氯化銅溶液將殘留的鋁基材移除 後可得透明的三氧化二鋁薄膜。 The surface of the aluminum material was anodized by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the mechanically ground aluminum sheet is anodized to react the aluminum sheet into a porous aluminum oxide film. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the surface of the aluminum sheet is treated with anodized aluminum oxide film, and the applied voltage and electrolyte composition are used to control the distribution of pore density and the pores. The size, anode treated electrolyte is mainly sulfuric acid, phosphoric acid, or oxalic acid, using 10vol.% (by volume) sulfuric acid aqueous solution as electrolyte, plus 20 volts DC voltage, anode treatment time 1 hour, electrolyte temperature 15 °C The surface of the metal aluminum sheet can be reacted to produce a translucent aluminum oxide film, and the residual aluminum substrate can be removed by using a saturated copper chloride solution to obtain a transparent aluminum oxide film.
以第1圖之模具實體進行鋁材之表面之陽極處理處理,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過機械研磨之鋁片再經陽極處理後可使鋁片反應成多孔性之三氧化二鋁薄膜。利用模具之開口範圍限定鋁片表面之待處理面積,使鋁片表面與經陽極處理後產生多孔性之三氧化二鋁薄膜,並利用外加電壓與電解液成份來控制孔密度的分佈與孔洞的大小,陽極處理的電解液主要以硫酸、磷酸、或草酸為主,利用1vol.%(體積百分比)磷酸水溶液為電解液、外加200伏特直流電壓、陽極處理時間5小時、電解液溫度為1℃、可使金屬鋁片表面反應產生透明的三氧化二鋁薄膜,再利用飽和氯化銅溶液將殘留的鋁基材移除後可得半透明的三氧化二鋁薄膜,其樣品照片如第8(a)圖所示,顯微結構圖如第8(b)圖所示。 The surface of the aluminum material was anodized by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the mechanically ground aluminum sheet is anodized to react the aluminum sheet into a porous aluminum oxide film. The opening area of the mold is used to define the area to be treated on the surface of the aluminum sheet, and the surface of the aluminum sheet is treated with anodized aluminum oxide film, and the applied voltage and electrolyte composition are used to control the distribution of pore density and the pores. The size, anode treated electrolyte is mainly sulfuric acid, phosphoric acid, or oxalic acid, using 1vol.% (volume percent) phosphoric acid aqueous solution as electrolyte, plus 200 volts DC voltage, anode treatment time 5 hours, electrolyte temperature 1 °C The surface of the metal aluminum sheet can be reacted to produce a transparent aluminum oxide film, and the residual aluminum substrate is removed by using a saturated copper chloride solution to obtain a translucent aluminum oxide film, and the sample photo is as shown in the eighth. (a) As shown in the figure, the microstructure diagram is shown in Figure 8(b) .
以第1圖之模具實體進行鈦材之表面之陽極處理處理,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過機械研磨之鈦片再經陽極處理後可使鈦片反應成多孔性之二氧化鈦薄膜。利用模具之開口範圍限定鈦片表面之待處理面積,使鈦片表面與經陽極處理後產生多孔性之二氧化鈦薄膜,並利用外加電壓與電解液成份來控制孔密度的分佈與孔洞的大小,陽極處理的電解液主要以氟化氨或氫氟酸主,利用0.4 vol.%HF(氫氟酸)水溶液為電解液、外加60伏特直流電壓、陽極處理時間1小時、電解液溫度為25℃、可使金屬鈦片表面反應產生多孔性透明的二氧化鈦薄膜,樣品之顯微結構如第9圖顯示。 The surface of the titanium material was anodized by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the mechanically ground titanium sheet is anodized to react the titanium sheet into a porous titanium dioxide film. The opening area of the mold is used to define the area to be treated on the surface of the titanium sheet, and the surface of the titanium sheet and the titanium oxide film which is porous after the anode treatment are used, and the distribution of the pore density and the size of the pore are controlled by the applied voltage and the electrolyte composition, and the anode is used. The treated electrolyte is mainly fluorinated ammonia or hydrofluoric acid, using 0.4 vol.% HF (hydrofluoric acid) aqueous solution as electrolyte, plus 60 volt DC voltage, anode treatment time 1 hour, electrolyte temperature 25 ° C, The surface of the titanium metal sheet can be reacted to produce a porous transparent titanium oxide film, and the microstructure of the sample is shown in Fig . 9 .
以第1圖之模具實體進行鈦材之表面之陽極處理處理,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過機械研磨之鈦片再經陽極處理後可使鈦片反應成多孔性之二氧化鈦薄膜。利用模具之開口範圍限定鈦片表面之待處理面積,使鈦片表面與經陽極處理後產生多孔性之二氧化鈦薄膜,並利用外加電壓與電解液成份來控制孔密度的分佈與孔洞的大小,陽極處理的電解液主要以氟化氨或氫氟酸主,利用0.4vol.%HF(氫氟酸)水溶液為電解液、外加80伏特直流電壓、陽極處理時間1小時、電解液溫度為25℃、可使金屬鈦片表面反應產生多孔性透明的二氧化鈦薄膜。 The surface of the titanium material was anodized by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the mechanically ground titanium sheet is anodized to react the titanium sheet into a porous titanium dioxide film. The opening area of the mold is used to define the area to be treated on the surface of the titanium sheet, and the surface of the titanium sheet and the titanium oxide film which is porous after the anode treatment are used, and the distribution of the pore density and the size of the pore are controlled by the applied voltage and the electrolyte composition, and the anode is used. The treated electrolyte is mainly fluorinated ammonia or hydrofluoric acid, using 0.4 vol.% HF (hydrofluoric acid) aqueous solution as electrolyte, plus 80 volt DC voltage, anode treatment time 1 hour, electrolyte temperature 25 ° C, The surface of the titanium metal sheet can be reacted to produce a porous transparent titanium oxide film.
以第1圖之模具實體進行鈦材之表面之陽極處理處理,具有冷卻功能的電化學治具照片如第6圖所示。此範例將表面經過機械研磨之鈦片再經陽極處理後可使鈦片反應成多孔性之二氧化鈦薄膜。利用模具之開口範圍限定鈦片表面之待處理面積,使鈦片表面與經陽極處理後產生多孔性之二氧化鈦薄膜,並利用外加電壓與電解液成份來控制孔密度的分佈與孔洞的大小,陽極處理的電解液主要以氟化氨或氫氟酸主,利用0.4 vol.%HF(氫氟酸)水溶液為電解液、外加40伏特直流電壓、陽極處理時間1小時、電解液溫度為30℃、可使金屬鈦片表面反應產生多孔性透明的二氧化鈦薄膜。 The surface of the titanium material was anodized by the mold body of Fig. 1 , and the photo of the electrochemical fixture having the cooling function is shown in Fig. 6 . In this example, the surface of the mechanically ground titanium sheet is anodized to react the titanium sheet into a porous titanium dioxide film. The opening area of the mold is used to define the area to be treated on the surface of the titanium sheet, and the surface of the titanium sheet and the titanium oxide film which is porous after the anode treatment are used, and the distribution of the pore density and the size of the pore are controlled by the applied voltage and the electrolyte composition, and the anode is used. The treated electrolyte is mainly made up of ammonium fluoride or hydrofluoric acid, using 0.4 vol.% HF (hydrofluoric acid) aqueous solution as electrolyte, plus 40 volt DC voltage, anode treatment time 1 hour, electrolyte temperature 30 ° C, The surface of the titanium metal sheet can be reacted to produce a porous transparent titanium oxide film.
10‧‧‧具有冷卻功能的電化學治具分解結構圖 10‧‧‧Decomposition diagram of electrochemical fixture with cooling function
20‧‧‧具有冷卻功能的電化學治具立體組合圖 20‧‧‧Three-dimensional combination of electrochemical fixtures with cooling function
30‧‧‧工作樣品置於具有冷卻功能的電化學治具立體組合圖 30‧‧‧Working samples placed on a stereoscopic combination of electrochemical fixtures with cooling function
40‧‧‧水冷式電極分解結構圖 40‧‧‧Water-cooled electrode decomposition structure
50‧‧‧水冷式電極立體組合圖 50‧‧‧Water-cooled electrode three-dimensional combination diagram
10a‧‧‧治具群組 10a‧‧‧ fixture group
101、201、303‧‧‧治具下座 101, 201, 303‧‧ ‧ fixtures
102‧‧‧下座第一表面螺牙孔 102‧‧‧The first surface screw hole in the lower seat
103‧‧‧下座第二表面螺牙孔 103‧‧‧Second surface screw hole
104‧‧‧導電棒螺牙孔 104‧‧‧ Conductor rod screw hole
105、202、304‧‧‧治具上蓋 105, 202, 304‧‧ ‧ fixture cover
106、203、306‧‧‧治具下蓋 106, 203, 306‧‧ ‧ fixture under cover
107、305‧‧‧上蓋防水墊圈 107, 305‧‧‧Top cover waterproof gasket
108‧‧‧下蓋防水墊圈 108‧‧‧Underwaterproof gasket
109‧‧‧導電片 109‧‧‧Conductor
110、301‧‧‧工作樣品 110, 301‧‧‧ working samples
111、302‧‧‧試片防水墊圈 111, 302‧‧‧ test strip waterproof gasket
10b‧‧‧噴灑式同軸線水冷式電極群組 10b‧‧‧Spray coaxial water-cooled electrode group
112、401、501‧‧‧電極腔體座 112, 401, 501‧‧‧ electrode cavity seat
113、405、503‧‧‧電極蓋 113, 405, 503‧‧ ‧ electrode cover
114、404‧‧‧電極蓋防水墊圈 114, 404‧‧‧ electrode cover waterproof gasket
115、204、407、504‧‧‧進水管 115, 204, 407, 504 ‧ ‧ water inlet
116、205、408、505‧‧‧出水管 116, 205, 408, 505‧‧‧ water outlet
117、206、307、506‧‧‧進水導管 117, 206, 307, 506‧‧ water inlet conduit
118、207、308、507‧‧‧出水導管 118, 207, 308, 507‧‧ ‧ water conduit
10c‧‧‧導電棒群組 10c‧‧‧ Conductor rod group
119、208、309‧‧‧彎頭管 119, 208, 309‧‧‧ elbow tube
120‧‧‧彎頭管螺牙 120‧‧‧ elbow thread
121、209、310‧‧‧彎頭管蓋 121, 209, 310‧‧‧ elbow cover
122、210、311‧‧‧彎頭管銜接軟管 122, 210, 311‧‧‧ elbow pipe connection hose
123、211、312‧‧‧矽膠塞 123, 211, 312‧‧ ‧ rubber stopper
124、213、314‧‧‧絕緣套管 124,213,314‧‧‧Insulation casing
125、214、315‧‧‧導電棒 125, 214, 315‧‧‧ conductive rods
126‧‧‧導電柱 126‧‧‧conductive column
127、212、313‧‧‧彎頭管防水墊圈 127, 212, 313‧‧‧ elbow pipe waterproof gasket
402、502‧‧‧電極接觸面 402, 502‧‧‧electrode contact surface
403‧‧‧電極腔體座母螺牙 403‧‧‧Electro-cavity seat female thread
406‧‧‧電極蓋公螺牙 406‧‧‧electrode cover male screw
第1圖 具有冷卻功能的電化學治具分解結構圖。 Figure 1 is an exploded view of an electrochemical fixture with a cooling function.
第2圖 具有冷卻功能的電化學治具立體組合圖。 Figure 2 is a three-dimensional combination of electrochemical fixtures with cooling function.
第3圖 工作樣品置於具有冷卻功能的電化學治具立體組合圖。 Figure 3 The working sample is placed in a stereoscopic combination of electrochemical fixtures with cooling function.
第4圖 水冷式電極分解結構圖。 Figure 4 Water-cooled electrode decomposition structure diagram.
第5圖 水冷式電極立體組合圖。 Figure 5 is a three-dimensional combination of water-cooled electrodes.
第6圖 具有冷卻功能的電化學治具照片。 Figure 6 Photograph of an electrochemical fixture with a cooling function.
第7圖 鋁樣品經電解拋光後的照片。 Figure 7 Photograph of the aluminum sample after electropolishing.
第8圖 鋁陽極處理薄膜照片與顯微影像。 Figure 8 Photographs and microscopic images of aluminum anodized films.
第9圖 多孔性二氧化鈦薄膜顯微影像。 Figure 9 Microscopic image of porous titanium dioxide film.
10‧‧‧具有冷卻功能的電化學治具分解結構圖 10‧‧‧Decomposition diagram of electrochemical fixture with cooling function
10a‧‧‧治具群組 10a‧‧‧ fixture group
101‧‧‧治具下座 101‧‧‧There is a seat
102‧‧‧下座第一表面螺牙孔 102‧‧‧The first surface screw hole in the lower seat
103‧‧‧下座第二表面螺牙孔 103‧‧‧Second surface screw hole
104‧‧‧導電棒螺牙孔 104‧‧‧ Conductor rod screw hole
105‧‧‧治具上蓋 105‧‧ ‧ fixture cover
106‧‧‧治具下蓋 106‧‧‧The lower cover of the fixture
107‧‧‧上蓋防水墊圈 107‧‧‧Upper cover waterproof gasket
108‧‧‧下蓋防水墊圈 108‧‧‧Underwaterproof gasket
109‧‧‧導電片 109‧‧‧Conductor
110‧‧‧試片 110‧‧‧ test strips
111‧‧‧試片防水墊圈 111‧‧‧Test strip waterproof gasket
10b‧‧‧噴灑式同軸線水冷式電極群組 10b‧‧‧Spray coaxial water-cooled electrode group
112‧‧‧電極腔體座 112‧‧‧Electrode cavity seat
113‧‧‧電極蓋 113‧‧‧electrode cover
114‧‧‧電極蓋防水墊圈 114‧‧‧Electrode cover waterproof gasket
115‧‧‧進水管 115‧‧‧ water inlet
116‧‧‧出水管 116‧‧‧Outlet pipe
117‧‧‧進水導管 117‧‧‧ water inlet conduit
118‧‧‧出水導管 118‧‧‧Water conduit
10c‧‧‧導電棒群組 10c‧‧‧ Conductor rod group
119‧‧‧彎頭管 119‧‧‧ elbow tube
120‧‧‧彎頭管螺牙 120‧‧‧ elbow thread
121‧‧‧彎頭管蓋 121‧‧‧ elbow cover
122‧‧‧彎頭管銜接軟管 122‧‧‧ elbow pipe connection hose
123‧‧‧矽膠塞 123‧‧‧矽 rubber stopper
124‧‧‧絕緣套管 124‧‧‧Insulation casing
125‧‧‧導電棒 125‧‧‧ Conductive rod
126‧‧‧導電柱 126‧‧‧conductive column
127‧‧‧彎頭管防水墊圈 127‧‧‧ elbow pipe waterproof gasket
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TW104111191A TWI554650B (en) | 2015-04-08 | 2015-04-08 | A cooling functional electrochemical mold |
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TW200923136A (en) * | 2007-11-16 | 2009-06-01 | Univ Nat Chiao Tung | Electrochemistry mold |
CN102445478A (en) * | 2011-09-22 | 2012-05-09 | 中国科学院金属研究所 | Working electrode for realizing electrochemical test of high-temperature high-pressure water system |
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TW200923136A (en) * | 2007-11-16 | 2009-06-01 | Univ Nat Chiao Tung | Electrochemistry mold |
CN102445478A (en) * | 2011-09-22 | 2012-05-09 | 中国科学院金属研究所 | Working electrode for realizing electrochemical test of high-temperature high-pressure water system |
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