TWI583825B - 鏡面拋光層及其表面處理方法 - Google Patents

鏡面拋光層及其表面處理方法 Download PDF

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TWI583825B
TWI583825B TW104100572A TW104100572A TWI583825B TW I583825 B TWI583825 B TW I583825B TW 104100572 A TW104100572 A TW 104100572A TW 104100572 A TW104100572 A TW 104100572A TW I583825 B TWI583825 B TW I583825B
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substrate
treatment
placing
curing
mirror
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建英 繆
威 李
承亨 吳
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納米及先進材料研發院有限公司
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Description

鏡面拋光層及其表面處理方法 【相關申請的交叉參考】
本申請主張於2014年1月30日提交的美國臨時專利申請序號61/965,421、2014年1月30日提交的美國臨時專利申請序號61/965,417、2014年1月30日提交的美國臨時專利申請序號61/965,420、2014年1月9日提交的美國臨時專利申請序號61/964,586、2014年1月9日提交的美國臨時專利申請61/964,584、2014年12月8日提交的美國非臨時專利申請14/564,030的優先權，並引用全文將其公開內容併入本文。
本發明涉及一種形成在基材上的鏡面拋光層，尤其涉及一種在基材上形成鏡面拋光層的預處理方法。
金屬或者塑膠基材上的鏡面拋光層是經由若干傳統的方法(諸如電鍍、真空沉積和熱蒸鍍)來實現的。除了保護基材和裝飾金屬感功能外，該鏡面拋光層還可以提供其他性能或特性，諸如電或熱傳導性。然而，這些傳統的處理具有它們自身的缺點。
電鍍，工業中最常用的表面處理，由於大量有毒的副產物和廢料對環境有害。由於複雜的後處理程序，因此整個過程將以高成本操作。這限制並阻礙了電鍍工業的進一步發展。越來越多的國家經由許多政策禁止或限制電鍍工業。
真空沉積和熱蒸鍍使用無法連續生產的昂貴設備。該批量生產可使產量降低並使產品不穩定。在沒有執行產品預處理和後處理的其他輔助方法的情況下，利用上述方法的塗覆產品(尤其是塑膠產品)的性能可能不夠好，諸如黏附性。
US20060135281公開了一種包括經由電鑄(電鍍)形成的細晶粒金屬層的塗層，其展示了高硬度。US20060135282教導了具有2nm至5,000nm大小的小金屬材料晶粒的塗層。中國專利申請CN1944710A公開了經由硝酸銀溶液與氨水和氫氧化鈉的反應形成的鏡面狀塗層，之後該塗層用硼氫化物顯影。CN101469427A教導了經由噴塗硝酸銀和酒石酸鉀以及氫氧化鈉的溶液形成的銀鏡面，該塗層用亞硫酸鈉進行後處理。
在上述專利申請中，電鍍方法仍用於這兩個美國發明，其不能解決廢料的高成本和環境污染的問題。另外兩個發明僅僅報導了在沒有特殊改質情況下銀的傳統鏡面狀反應，這會導致銀鏡面狀塗層的不良黏附性和銀塗層的氧化問題。
因此，對在基材上形成具有良好黏附特性和低成本的鏡面拋光層，存在未得到滿足的需要。另外，可以以有效且環保的方式製造這種鏡面拋光層。
本發明開發了一種處理金屬或者塑膠基材以形成鏡面拋光層的方法。在改質基材表面狀況的幾個預處理步驟之後，不管是金屬還是塑膠材料，為了增加上面塗層的黏附性，將使用顯現金屬外觀且光滑的裝飾功能的鏡面拋光層。將塗覆可變外塗層，以保護下面的鏡面拋光層並實現色彩豐富的裝飾。所有塗層材料和處理步驟都是環保的，且無需昂貴的設備。在沒有較大改變的情況下可以使用普通噴塗系統，這能實現連續生產以得到更多一致且穩定的塗層產品，並增加產量。
因此，本發明的第一方面在於給基材提供多步預處理方法以形成鏡面拋光層。
根據本發明的實施方式，一種用於預處理以形成鏡面拋光層的基材的方法包括：將第一材料放置在基材上，其中第一材料包括第一環氧樹脂、第一流平劑、丁醇、丙酮、雙丙酮醇、第一固化劑和2,4,6-三(二甲氨基甲基)苯酚；固化該第一材料；將第二材料放置在固化的第一材料上，其中第二材料包括第二環氧樹脂、第二流平劑、2-甲基苯基縮水甘油醚、 雙丙酮醇、丁醇、第二固化劑和2,4,6-三(二甲氨基甲基)苯酚；固化該第二材料；和在固化的第二材料上塗覆鏡面拋光層。
優選地，該方法還包括用混合溶劑沖洗固化的第二材料。
優選地，該方法還包括用氯化錫(II)和鹽酸的混合溶液處理固化的第二材料。
優選地，該基材為金屬基材或者塑膠基材。
優選地，該方法還包括經由將後處理材料放置在鏡面拋光層上以後處理鏡面拋光層。
本發明的第二方面在於提供一種在用本發明所述的方法製備的塑膠或金屬基材上形成的鏡面拋光層。
11~17‧‧‧步驟
參考附圖，在下文中將更加詳細地描述本發明的實施方式，其中：圖1是根據本發明實施方式，示意在金屬/塑膠基材上製備鏡面拋光塗層的方法步驟的流程圖。
在以下的描述中，提出了在金屬/塑膠基材上形成的鏡面拋光層，和基材的預處理方法的對應實施方式作為優選實施例。對於本領域技術人員顯而易見的是，在不背離本發明的範圍和精神的情況下可以進行包括附加和/或替換的修改。可以省略具體細節以免使本發明模糊不清；然而，該公開被撰寫成使本領域的技術人員在沒有過多實驗的情況下能夠實踐本文的教導。
在該發明中，提供了處理塑膠或金屬基材以實現鏡面拋光層的整個過程，它不僅能用於批量生產，例如浸漬，而且還能用於連續生產，例如自動化生產線中的噴塗。
圖1是根據本發明實施方式，示意在金屬/塑膠基材上製備鏡面拋光塗層的方法步驟的流程圖。在步驟11中，首先經由初步預處理預先處理基材。對於金屬基材，用砂紙拋光該金屬基材。之後，用水、洗潔精、丙酮和乙醇清洗該拋光的金屬基材。對於塑膠基材，可以使用電漿處理、化學處理和/或物理處理來預處理該塑膠基材。在步驟12中，用第一材料改質預處理基材的表面以改善該基材的黏附性。經由浸漬或噴塗將第一材料放置在預處理基材上，之後在烤箱中固化。該第一材料包括環氧樹脂(諸如E-51)、流平劑(諸如BYK-361N、丁醇、丙酮、雙丙酮醇)、固化劑(諸如TZ-550和2,4,6-三(二甲氨基甲基)苯酚)。在步驟13中，用第二材料改質預處理基材的表面以改善鏡面拋光層的黏附性。經由浸漬或噴塗將第二材料放置在固化的第一材料上，之後在烤箱中固化。該第二材料包括環氧樹脂(諸如E-51)、流平劑(諸如BYK-361N、2-甲基苯基縮水甘油醚(CGE)、雙丙酮醇、丁醇)、固化劑(諸如TZ-550和2,4,6-三(-二甲氨基甲基)苯酚)。在步驟14中，用第三材料改質預處理基材的表面以增進鏡面拋光層的形成。用第三材料沖洗以第二材料處理的預處理基材的表面。該第三材料是包含混合溶劑(諸如1：1(體積比)的丙酮和乙醇)的一種溶液。在步驟15中，用第四材料改質預處理基材的表面以增進鏡面拋光層的形成。將第四材料應用在用第三材料處理的預處理基材的表面上，之後在室溫下使其乾燥。該第四材料是包含氯化錫(II)和酸的混合物的一種溶液。在步驟16中，在該預處理基材的表面上塗覆鏡面拋光層。在步驟17中，實施用於鏡面拋光層的後處理。
優選地，塑膠基材包括丙烯腈丁二烯苯乙烯(ABS)、聚丙烯(PP)或聚碳酸酯(PC)，且金屬基材包括鐵、鋅、鋁、鎂或它們的合金。
優選地，將執行在鏡面拋光層上放置透明或可變色材料(後處理材料)的步驟以保護它或增加一些特殊功能，其可以經由浸漬或噴塗來產生，之後在烤箱中進行熱處理。
因此，雖然金屬和塑膠兩種基材的表面具有不同特性，但是可將本發明的基材預處理方法應用於這兩種基材。該預處理方法能夠增強基材和鏡面拋光層之間的黏附性。在本發明中沒有使用有害且不環保的化 學品。另外，用本發明的該方法製備的鏡面拋光層提供了高的膜硬度、抗劃傷性和耐衝擊性。
實施例
塗覆金屬和塑膠基材的過程主要包括預處理、放置功能性塗覆和後處理。
1.基材的多步預處理
由於兩種類型基材的表面特性不同，因此對於金屬和塑膠基材，基材的預處理也是不同的。
1)處理金屬基材的主要步驟如下所示：
(1)表面拋光：分別用#240、#360和#800的砂紙拋光該金屬基材。也可以使用振動研磨機或者滾筒研磨機以用適當的研磨石拋光相同基材。對於軟金屬，諸如Al或Mg合金，如果拋光不適宜，則可以跳過該步驟。
(2)基材清洗：將該(拋光的)基材浸入到DI水和洗潔精的混合物中。音波震盪基材超過30分鐘。使用流動的DI水逐一地沖洗樣品。在1：1(體積比)的丙酮和乙醇中再次經由超音波震盪清洗基材超過30分鐘。用流動的乙醇沖洗基材，在空氣中乾燥它們。
(3)用材料1改質表面：經由浸漬或者噴塗將材料1放置在預處理基材上，之後在烤箱中固化。固化溫度可以根據基材材質在80~150℃的溫度範圍內變化，持溫至少10分鐘。通常，低溫適合塑膠基材，高溫適合金屬基材。材料1將用於改質基材表面以實現上面塗層的良好黏附性。
材料1的實施例是約10g E-51、0.1g BYK-361N、6g丁醇、1g丙酮、10g雙丙酮醇、2g TZ-550和1g 2,4,6-三(二甲氨基甲基)苯酚。經由在室溫中攪拌超過30分鐘將這些化學品加入並混合在一起。如果必要，在超音波浴中音波震盪混合物3分鐘。製備好之後，應將材料1保存在室溫或者諸如5~10℃的低溫中。然而，一旦加入固化劑TZ-550，材料1在室溫中應該在2小時內用完。
(4)用材料2改質表面：經由浸漬或者噴塗將材料2放置在塗有材料1的基材上，之後在烤箱中固化。固化溫度可以根據基材在80~150℃的溫度範圍變化，持溫至少10分鐘。通常，低溫適合塑膠基材，高溫適合金屬基材。該材料2將用於改質表面特性以實現上面塗層的良好黏附性。
材料2的實施例是約22g E-51、0.2g BYK-361N、2g GGE、12g雙丙酮醇、8g丁醇、5g TZ-550和1g 2,4,6-三(二甲氨基甲基)苯酚。經由在室溫中攪拌超過30分鐘將這些化學品加入並混合在一起。如果必要，在超音波浴中音波震盪混合物3分鐘。製備好之後，應將塗層材料2保存在室溫或者諸如5~10℃的低溫中。然而，一旦加入固化劑TZ-550，材料2在室溫中應該在1小時內用完。
2)處理塑膠基材的主要步驟如下所示：
(1)電漿處理：將等塑膠基材放入電漿室中，並使用電漿清洗機以高電平處理它們至少20分鐘。
(2)化學處理：使用不同的化學品處理不同的塑膠材料。實施例是濃酸對ABS處理5~7分鐘，或者高錳酸鉀的強氧化劑對PP在70℃處理24小時。
(3)物理處理：如果必要，可以在3.2巴的條件下使用噴砂物理處理超過1分鐘。
(4)用材料1改質表面：經由浸漬或者噴塗將材料1放置在預處理基材上，之後在烤箱中進行熱處理。熱處理溫度可以根據基材在80~150℃的溫度範圍內變化，持溫至少10分鐘。通常，低溫適合塑膠基材，高溫適合金屬基材。材料1將用於改質基材表面以實現上面塗層的良好黏附性。
材料1的實施例是約10g E-51、0.1g BYK-361N、6g丁醇、1g丙酮、10g雙丙酮醇、2g TZ-550和1g 2,4,6-三(二甲氨基甲基)苯酚。經由在室溫中攪拌超過30分鐘將這些化學品加入並混合在一起。如果必 要，在超音波浴中音波震盪混合物3分鐘。製備好之後，應將材料1保存在室溫或者諸如5~10℃的低溫中。然而，一旦加入成分TZ-550，材料1在室溫中應該在2小時內用完。
(5)用材料2改質表面：經由浸漬或者噴塗將材料2放置在塗有材料1的基材上，之後在烤箱中進行熱處理。熱處理溫度可以根據基材在80~150℃的溫度範圍變化，持溫至少10分鐘。通常，低溫適合塑膠基材，高溫適合金屬基材。材料2將用於改質表面特性以實現上面塗層的良好黏附性。
材料2的實施例是約22g E-51、0.2g BYK-361N、2g GGE、12g雙丙酮醇、8g丁醇、5g TZ-550和1g 2,4,6-三(二甲氨基甲基)苯酚。經由在室溫中攪拌超過30分鐘將這些化學品加入並混合在一起。如果必要，在超音波浴中音波震盪混合物3分鐘。製備好之後，應將材料2保存在室溫或者諸如5~10℃的低溫中。然而，一旦加入成分TZ-550，材料2在室溫中應該在1小時內用完。
(6)用材料3改質表面：用流動的混合溶劑(諸如1：1(體積比)的丙酮和乙醇)沖洗用以上材料處理的表面。這可以經由使用洗滌瓶來實現。此後，用流動的DI水沖洗表面，在室溫中乾燥表面。混合溶劑製備好之後，可以用能長時間(數天或數周)保持有效的密封蓋保存在室溫中。該步驟處理將使表面粗糙，以增強上面塗層的黏附性。
(7)用材料4改質表面：材料4是能經由浸漬或者噴塗使用的一種溶液。處理之後，將在室溫中乾燥基材。
材料4的實施例是約2g氯化錫(II)和2mL鹽酸(37%)。以約60℃的溫度加熱該溶液約10分鐘，直到形成澄清溶液。此後，在室溫中加入400mL的DI水，並徹底使溶液漩流。在使用之前，使溶液在室溫中用蓋密封至少4小時以使其陳化。將溶液保存在室溫中並用蓋密封。製備好之後，該溶液應該保持有效1-2周。該步驟處理可在下面基材的表面上形成一些活性位置，之後使形成鏡面拋光層的反應變得更容易。
2．在經上述步驟處理之後的基材上製備鏡面拋光層
經由浸漬或者噴塗將2種溶液放置在經上述步驟處理之後的基材上，之後在烤箱中固化。當浸漬時，立即將2種溶液混合物並應用在基材上。如果使用噴塗，在2個獨立容器中具有2種溶液的雙頭噴槍或者2個同時工作的單頭噴槍是必須的。固化溫度可以根據基材在80~150℃的溫度範圍變化，持溫至少10分鐘。通常，低溫適合塑膠基材，高溫適合金屬基材。該塗層將實現鏡面拋光層。
製備2種溶液的實施例如下所示：
2-1)用於鏡面拋光層的溶液1(其應在使用時製備且不應長時間保存)的製備如下：。
1)將20mL的DI水加入到空玻璃燒杯中；2)將6g氫氧化鈉慢慢地加入到上述玻璃燒杯中；3)在室溫中小心地攪拌上述溶液直到所有固體被溶解；4)將10g硝酸銀加入到空玻璃瓶中；5)將100mL的DI水加入到上述玻璃瓶中；6)在室溫中攪拌上述溶液直到所有固體被溶解；7)將溶液3)倒入溶液6)中；8)徹底攪拌上述溶液(將形成棕色沉澱物)；9)將20mL的28%氨水加入到另一空玻璃燒杯中；10)將50mL的DI水加入到上述玻璃燒杯中；11)徹底攪拌上述溶液；12)將溶液11)滴入溶液8)中，直到所有棕色沉澱物正好被再溶解(將使用大約60mL的氨溶液)並形成澄清溶液；13)用DI水將澄清溶液稀釋成總體積為1000mL的溶液；
2-2)將如下製備用於鏡面拋光層的溶液2，且將其保存在室溫中並用蓋密封。製備好之後，該溶液將保持數月有效。
1)將8g葡萄糖加入空玻璃瓶中；2)加入0.5g檸檬酸；3)加入20mL乙醇；4)加入980mL的DI水；5)徹底攪拌該溶液，直到所有固體都被溶解；
3．塗覆鏡面拋光層之後的後處理
將在鏡面拋光層上執行放置透明或者可變色材料(後處理材料)的步驟，以保護它或者增加一些特殊功能，其可以經由浸漬或者噴塗來實施，之後在烤箱中進行熱處理。熱處理溫度可以根據基材在80~150℃的溫度範圍變化，持溫至少10分鐘。通常，低溫適合塑膠基材，高溫適合金屬基材。該後處理在改變整個外觀成不同顏色或者提供其他特殊功能的同時，還將保護鏡面拋光的下面塗層。
後處理材料的實施例是約15g甲基三乙氧基矽烷(MTES)、2g γ-巰基丙基三甲氧基矽烷(A189)、6g乙醇、0.5g乙酸、5g丙酮、5g DI水、2g LUDOX® HS-30矽酸膠和15g雙丙酮醇。經由在室溫中攪拌超過30分鐘將這些化學品加入並混合在一起。如果必要，在超音波浴中音波震盪混合物45分鐘，直到獲得透明溶液。此後，在烤箱中以70℃加熱後處理材料18小時，之後冷卻至室溫並保持24小時。應將後處理材料保存在室溫或者諸如5~10℃的低溫中。
調整後處理材料顏色的實施例是首先使用聚四氟乙烯(PTFE)過濾器(450nm孔徑大小)過濾上述無色外塗層溶液。將50g的經過濾的無色後處理材料與11mg結晶紫混合以得到均勻溶液。
特性和性能試驗
根據本發明上述實施例中，實施關於丙烯腈丁二烯苯乙烯(ABS)和聚丙烯(PP)基材的鏡面拋光層的各種性能試驗。
實施關於標準ASTM D3363-05/ISO 15184：1998(ISO 15184：2012)的膜硬度試驗。在提供750g荷重的條件下，試驗結果顯示了沒有明顯變化的4H和沒有被損壞的6H。用市場中銷售的常規鏡面塗層實施相同試驗，試驗結果僅為2H。
實施關於標準ASTM D3359-02/ISO 2409：2007的膠帶試驗的黏附性。在具有百格紋路的條件下，試驗結果顯示了5B(100%沒有脫落)。用市場中銷售的常規鏡面塗層實施相同試驗，試驗結果顯示了100/100脫落。
實施關於標準ISO 1518-1：2011的抗劃傷性試驗。經由馬達使以面板支撐物固定的試驗面板相對於尖筆移動。尖筆移動的速度是(35±5)mm/s。選擇具有(0.50±0.01)mm半徑的半球形硬金屬尖的劃痕型尖筆，以用於該試驗。試驗結果顯示了對於ABS，表面塗層通過了150g試驗，對於PP，表面塗層通過了81g試驗。
實施關於API指導方針的REACH試驗。在高度關注物質(SVHC)的候選列表中的155個基材中沒有任何一個被檢測出。
實施關於標準ASTM F2357-04的抗磨損性試驗。在具有100個循環的磨損之後，ABS基材的鏡面拋光層的損耗是3.3mg，PP基材的鏡面拋光層的損耗是2.1mg。
本發明前面的描述提供了示例和說明，其並非想要窮舉或者侷限該發明在所公開的精確形式。對於本領域的技術人員而言，許多修改和變更將是顯而易見的。
為了最好地解釋本發明的精神和它的實際應用，選擇並描述了這些實施方式，進而使該領域的技術人員能夠理解該發明的各種實施方式以及適合特殊用途的各種變更。其旨在由所附申請專利範圍及其等效物以限定本發明的範圍。
11~17‧‧‧步驟

Claims (15)

  1. 一種用於預處理基材以形成鏡面拋光層的方法，包括：將第一材料放置在該基材上，其中該第一材料包括第一環氧樹脂、第一流平劑、丁醇、丙酮、雙丙酮醇、第一固化劑和2,4,6-三(二甲氨基甲基)苯酚；固化該第一材料；將第二材料放置在固化的該第一材料上，其中該第二材料包括第二環氧樹脂、第二流平劑、2-甲基苯基縮水甘油醚、雙丙酮醇、丁醇、第二固化劑和2,4,6-三(二甲氨基甲基)苯酚；固化該第二材料；和在固化的該第二材料上塗覆一鏡面拋光層。
  2. 如申請專利範圍第1項所述的方法，還包括：用氯化錫(II)和鹽酸的溶液混合物處理固化的該第二材料。
  3. 如申請專利範圍第1項所述的方法，其中將該第一材料放置在該基材上的步驟係經由浸漬或者噴塗來執行。
  4. 如申請專利範圍第1項所述的方法，其中將該第二材料放置在該基材上的步驟係經由浸漬或者噴塗來執行。
  5. 如申請專利範圍第1項所述的方法，其中固化該第一材料的步驟在80至150℃的溫度範圍執行。
  6. 如申請專利範圍第1項所述的方法，其中固化該第二材料的步驟在80至150℃的溫度範圍執行。
  7. 如申請專利範圍第1項所述的方法，還包括：經由將後處理材料放置在該鏡面拋光層上來後處理該鏡面拋光層，其中該後處理材料包括甲基三乙氧基矽烷、γ-巰基丙基三甲氧基矽烷、乙醇、乙酸、丙酮、DI水、矽酸膠和雙丙酮醇；和固化該後處理材料。
  8. 如申請專利範圍第1項所述的方法，還包括： 用混合溶劑沖洗固化的該第二材料。
  9. 如申請專利範圍第8項所述的方法，其中該混合溶劑包括體積比例為1比1的丙酮和乙醇。
  10. 如申請專利範圍第1項所述的方法，其中該基材為金屬基材或者塑膠基材。
  11. 如申請專利範圍第10項所述的方法，還包括：在將該第一材料放置在該基材上的步驟之前，利用一初步處理預處理該金屬基材。
  12. 如申請專利範圍第11項所述的方法，其中該初步處理包括：拋光該金屬基材；和用水和洗潔精清洗該金屬基材。
  13. 如申請專利範圍第10項所述的方法，還包括：在將該第一材料放置在該基材上的步驟之前，利用一初步處理預處理該塑膠基材。
  14. 如申請專利範圍第13項所述的方法，其中該初步處理是電漿處理、化學處理或者物理處理。
  15. 一種在用申請專利範圍第1項所述的方法製備的該基材上形成的鏡面拋光層。
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