TW201714982A - 雷射可標記之聚合物及塗料 - Google Patents
雷射可標記之聚合物及塗料 Download PDFInfo
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Abstract
本發明係關於雷射可標記之聚合物及塗料,其特徵在於以下事實:其包含具有經界定粒度之錫/銻氧化物塗佈之球形TiO2粒子作為雷射添加劑。
Description
本發明係關於雷射可標記之聚合物及塗料,其特徵在於以下事實:其包含具有經界定粒度之錫/銻氧化物塗佈之球形TiO2粒子作為雷射添加劑。
製成品之標示在幾乎所有工業部門中變得日益重要。因此,例如,經常必須將製造日期、批號、失效日期、條碼、2D碼、公司標誌及序號施加至塑膠零件。就此而言,日益重要的是使用雷射之非接觸、極快速及靈活標記。使用此技術,可以高速度、甚至對非同平面表面施加刻印。由於刻印位於塑膠體或聚合塗料自身內,故其永久地耐磨損。
由於許多塑膠及聚合塗料對雷射光透明,雷射敏感劑由於在塑膠材料內吸收雷射能量(由於直接地與聚合物或聚合塗料或間接地與添加材料相互作用)而引起局部高度可見之變色,故通常將其添加至塑膠及聚合塗料。雷射敏感劑可係吸收雷射光之有機染料或顏料。可給出變色之多種原因,例如聚合物之分解或吸收劑自身自不可見形式轉化為可見形式。塑膠之色彩變深通常係由於因所引入之雷射能量發生碳化而發生。
已知眾多用於雷射標記塑膠及聚合材料之雷射添加劑(吸收劑)。使用Nd-YAG雷射(釹摻雜之釔鋁石榴石雷射)、YVO4雷射(釩酸釔雷射)及1064nm光纖雷射標記之適宜材料較佳係吸收波長1064nm之光
且本身僅具有輕微的固有色彩之彼等。實例係磷酸銅、氧化鉍、氯氧化鉍、雲母上之銻摻雜氧化錫或金屬。
EP 1 377 522 A2闡述(例如)由經煅燒之銻/錫混合氧化物組成之用於塑膠之雷射標記之添加劑,其中銻在表面處之濃度大於總體上在粒子中之銻濃度。粒度係0.1μm至10μm、較佳0.5μm至5μm。利用添加劑,在主要數量之聚合物中獲得深色雷射標記。然而,該等添加劑具有其僅展現聚合物依賴性標記且因此標記製程極為緩慢之缺點。
存在雷射標記僅在彩色或淺色塑膠零件上極困難地可見之問題。淺色或彩色塑膠零件之實例係電纜絕緣物、鍵盤或彩色鍵帽、管線或殼體材料。此處期望深色、儘可能黑色之刻印,此乃因相對於彩色背景此顯示顯著高於灰色標記之對比度。深色標記可藉助雷射輻射使塑膠碳化來產生。然而,此限於少數聚合物類型且通常由於粗糙化而導致表面之改變。在薄層及膜的情況下,此尤其引起機械強度之損失。
因此業內仍需要雷射添加劑,其尤其在彩色基材上及薄塗層或膜中由於雷射轟擊而導致深色、聚合物獨立性、平滑且快速標記,其耐久且經長時期保持,即使在機械應力下。
因此,本發明之目標係尋找尤其在白色或彩色塑膠物品上或在白色、淺色或彩色塗層及膜中產生高對比度及機械穩定之深色標記之方法。本發明之另一目標在於提供用於雷射標記之雷射顏料或添加劑,其僅具有輕微的固有色彩或完全沒有色彩,且在雷射光之作用下在摻雜有其之聚合物或聚合塗料中產生極好之標記結果,尤其得到高對比度及清晰的深色標記且可應用於廣泛範圍之塑膠中。
本發明之又一目標係提供製備此一雷射添加劑之方法。
令人驚訝地,已發現若塑膠或聚合物包含具有錫/銻氧化物塗層之精細二氧化鈦作為雷射添加劑,則藉由雷射轟擊可為彩色塑膠物品
及聚合物層提供深色標記。借助於本發明之雷射添加劑,亦可藉由雷射轟擊為通常不與雷射添加劑反應之塑膠物品或聚合物層提供深色標記。此等包括(例如)不能展現碳化之聚矽氧。然而,借助於本發明之添加劑,原本僅對雷射光極緩慢起反應且亦僅可困難地碳化之聚合物(例如PA、PE、PP、PMMA、POM)亦可快速且以高對比度標記。
因此,本發明係關於雷射可標記之聚合物及塗料,其特徵在於其包含球形TiO2粒子作為雷射顏料或添加劑,其中TiO2粒子表面上塗佈有銻摻雜之二氧化錫層(Sn,Sb)O2且雷射顏料之數量加權粒度<15μm,其藉助雷射繞射以D95量測。此處銻摻雜之二氧化錫層(Sn,Sb)O2用作雷射能量之吸收劑。在雷射轟擊時,雷射添加劑之TiO2經還原為以深色為特徵之TixOy。
除化學組成之外,尤其粒度分佈對本發明之雷射顏料之作用而言甚為重要。雷射顏料具有極窄之粒度分佈,除深色標記之外,其與先前技術相比能夠增加邊緣清晰度。
此外,球形TiO2粒子之粒度亦可影響標記結果。若TiO2球體之直徑係0.05μm至10μm、較佳0.1μm至2μm且尤其0.15μm至1μm,則較佳獲得具有高邊緣清晰度之高對比度深色標記。適宜TiO2粒子可(例如)以商品名Kronos(Kronos)及Hombitec(Sachtleben)自市面購得。
若藉助雷射繞射以D95所量測之顏料之質量加權粒度係15μm或以下、較佳10μm或以下且尤佳4μm或以下,則獲得具有高邊緣清晰度之標記。
本發明之較佳添加劑具有0.05μm、尤其0.1μm且極佳0.15μm之D25值。
本發明添加劑之D50值較佳係0.05μm至10μm、尤其0.1μm至5μm且極佳0.15μm至1μm。
在此申請案中,雷射添加劑之粒度係藉助雷射繞射(Malvern Mastersizer 2000)測定。
特定適宜之雷射添加劑之特徵在於以下事實:其具有較佳<100歐姆*cm之粉末比電阻。
在此專利申請案中,粉末比電阻係如以下測定。在直徑為d之丙烯酸玻璃管中,藉助於10kg砝碼,將1.5g添加劑壓縮於兩個金屬撞錘之間並量測產生之電阻R。根據以下自經壓縮添加劑之層厚度L(對應於金屬撞錘之間隔)獲得粉末比電阻
球形TiO2粒子利用銻摻雜之二氧化錫層在表面上塗佈。基於SnO2,摻雜係0.1mol%至60mol%、較佳1mol%至40mol%、尤其2mol%至30mol%。
(Sn,Sb)O2塗層之比例基於添加劑較佳係0.1重量%至99重量%、尤其5重量%至80重量%且極佳10重量%至70重量%。
本發明雷射添加劑適宜性之基本特徵係於塑膠及塗料應用中之淺固有色彩。
基於欲標記之聚合物或塗料材料,用於雷射標記之本發明添加劑之使用濃度係0.005%至30%、較佳0.015%至20%且極佳0.1%至15%。由於添加劑之低固有色彩,塑膠物品之色彩性質因添加劑而輕微地或僅在極小程度上受損。
在雷射光之作用下,經摻雜之聚合物展現具有高對比度及明顯邊緣清晰度之深色標記。未觀察到在用於深色標記之其他方法中發生之起泡及表面之相關粗糙化。
除優良的光學性質、對比度及邊緣清晰度外,本發明之雷射添加劑能夠利用高脈衝速率來快速標記並具有基於雷射設定之大的製程
窗口。另外,標記之亮度可藉由調整雷射參數具體地控制降至極深色標記。高度細節化彩色半色調影像可僅經由控制雷射參數(功率、曝光持續時間、焦點)而獲得。本發明同樣係關於影像生成之方法。
本發明添加劑之製備相對簡單且可藉由本身已知之方法實施。將球形TiO2粒子用銻摻雜之二氧化錫層塗佈。塗佈較佳藉由以下步驟實施:使TiO2球體懸浮於水中並在適宜pH下使金屬氧化物或金屬氧化物水合物沈澱出及使氫氧化物或氧化物水合物轉化為金屬氧化物。一般而言,將呈溶解形式之銻或錫之金屬鹽(例如SnCl4或SbCl3)添加至水性懸浮液且通常在適宜pH下以金屬氧化物水合物之形式沈澱。隨後藉由在升高之溫度下處理將金屬氧化物水合物轉化為相應氧化物。將所得產物濾出,洗滌,乾燥,煅燒且最後篩分。
二氧化鈦與(Sn,Sb)O2層之組合在若干方面中具有有利效應。即使在極小粒子之情況下,(Sn,Sb)O2存在亦引起雷射光之顯著吸收。因此,本發明之雷射添加劑即使在極低濃度下亦有效作為用於雷射標記之添加劑。極精細之粒度有利於形成深色標記。本發明之產物展現窄粒度分佈、良好分散性、低磨損性、高亮度及透明度。
雷射添加劑可類似於標準工業方法(例如)作為乾燥顏料混合物、作為液體製劑或糊劑或經由基於塑膠或蠟之濃縮物(即,所謂的母料)引入塑膠或聚合物中。亦可藉由擠出複合物(compound)引入本發明之雷射添加劑。此由於其不需要進一步稀釋用於後續處理中而不同於母料,此乃因在期望之塑膠中已包含最終濃度之期望添加劑。除雷射活性顏料之外,亦可在所有該等添加劑添加過程期間添加著色顏料及其他添加劑。
在有利的實施例中,首先製備具有相對高濃度之本發明雷射添加劑之塑膠母料,然後在塑膠加工期間將其作為顆粒以少量添加至塑膠之主要組合物。
此外,可將著色劑添加至聚合物,此允許寬色彩變化、特定地紅色、綠色及藍色。適宜著色劑尤其係有機顏料及染料。
可用於雷射標記之聚合材料尤其係所有已知之塑膠、尤其熱塑性塑膠、此外熱固性塑膠及彈性體,其闡述於(例如)Ullmann,第15卷,第457頁及其後,Verlag VCH中。適宜熱塑性聚合物係(例如)聚乙烯、聚丙烯,聚醯胺、聚酯、聚醚酯、聚伸苯基醚、聚縮醛、聚對苯一甲酸丁二酯(PBT)、聚對苯二甲酸乙二酯(PET)、聚甲基丙烯酸甲酯、聚乙烯醇縮醛、聚苯乙烯、丙烯腈-丁二烯-苯乙烯(ABS)、丙烯腈-苯乙烯-丙烯酸酯(ASA)、苯乙烯-丙烯腈(SAN)、聚碳酸酯、聚醚碸及聚醚酮及其共聚物、混合物及/或聚合物摻和物,例如PC/ABS、MABS。
適宜熱固性聚合物係(例如)聚胺基甲酸酯、三聚氰胺樹脂、聚酯及環氧樹脂。
本發明雷射添加劑之併入可(例如)藉由複合經母料、經由糊劑或藉由在成型加工步驟期間直接添加(直接著色)來實施。可視情況將其他添加劑(例如加工助劑、穩定劑、阻燃劑、填充劑及著色顏料)在雷射添加劑併入期間添加至聚合物、較佳地塑膠顆粒或粉末。經摻雜之塑膠顆粒或粉末之實驗室製備通常藉由以下實施:首先將塑膠顆粒引入適宜混合器中,利用分散助劑將其潤濕及然後添加並合併所需之雷射添加劑及彩色顏料。在工業實踐中,聚合物之著色及添加劑至其之添加通常經由彩色濃縮物(母料)或複合物來實施。出於此目的,將彩色顏料及添加劑在擠出機(通常共軸旋轉雙螺桿擠出機)中利用高剪力分散於熔融塑膠中。塑膠熔體穿過擠出機頭上之多孔板離開並藉助適宜下游裝置轉化為顆粒(例如股線造粒方法或水下製粒)。由此獲得之顆粒可直接於擠出機或注射模製機中進一步加工。在加工期間所形成之模製物展現雷射添加劑之極均勻分佈。隨後,使用適宜雷射實施雷
射標記。
在彩色或白色雷射可標記之聚合物或塑膠之情況下,除本發明之雷射添加劑之外,聚合物或塑膠包含一或多種著色劑。在無著色劑之情形下,塑膠係透明至不透明的。即使在無著色劑之情形下,在本發明之雷射添加劑之存在下在聚合物中亦獲得深色標記。
聚合物、較佳熱塑性聚合物、熱固性聚合物或彈性體中之雷射添加劑之濃度通常取決於所用之聚合物材料。
基於塑膠或塗料,用於雷射標記之本發明添加劑之使用濃度較佳係0.01%至30%、尤其0.015%至20%且極佳0.1%至15%。由於本發明雷射顏料之淺固有色彩,故經標記之塑膠或聚合物之光學性質僅因雷射添加劑而輕微程度地受損。雷射添加劑之低比例輕微地改變聚合物系統而不影響其加工性。
在雷射光之作用下,本發明之添加劑在聚合物中展現具有高對比度及明顯邊緣清晰度之深色標記。未觀察到在用於深色標記之其他方法中發生之起泡及表面之相關粗糙化。
本發明亦關於製備本發明經摻雜之聚合材料之方法,其特徵在於將聚合材料與本發明之雷射添加劑混合且然後在熱作用下成型。
使用雷射刻印聚合物係藉由使試樣進入脈衝雷射、較佳Nd:YAG雷射之射線路徑來實施。此外,使用準分子雷射刻印係可能的。然而,使用其他習用類型之雷射(其具有在所用顏料具有高吸收或反應性之範圍內之波長),良好至極佳之標記結果亦係可能的。所得標記係由輻射時間(或在脈衝雷射之情況下的脈衝計數)及雷射之輻射功率以及所用之塑膠系統來確定。所用雷射之功率取決於特定應用且可由熟習此項技術者按不同情況容易地確定。
所用雷射通常具有157nm至10.6μm之範圍內、較佳532nm至10.6μm範圍內之波長。在此可提及(例如)CO2雷射(10.6μm)及
Nd:YAG雷射(1064nm或532nm)或UV雷射。準分子雷射具有以下波長:F2準分子雷射(157nm)、ArF準分子雷射(193nm)、KrCl準分子雷射(222nm)、KrF準分子雷射(248nm)、XeCl準分子雷射(308nm)、XeF準分子雷射(351nm)、具有355nm(三倍頻)或265nm(四倍頻)波長之倍頻Nd:YAG雷射。尤佳者係使用Nd:YAG雷射(1064nm或532nm)、光纖雷射(1060nm至1070nm)或二極體雷射(940nm至980nm)。所用雷射之能量密度通常在1J/cim2至2000J/cm2、較佳10J/cm2至2000J/cm2之範圍內。在使用脈衝雷射時,脈衝頻率通常在1kHz至100kHz之範圍內。可用於本發明方法中之相應雷射可自市面購得。
根據本發明經摻雜之聚合物及塗料可用於迄今將習用印刷方法用於刻印之所有領域。舉例而言,由本發明之聚合物製成之模製組合物、半製成品及成品零件可用於電氣、電子及汽車工業。在由根據本發明經摻雜之聚合物組成之(例如)加熱、通風及冷卻部分中之電纜、管道、裝飾條或功能零件或開關、插頭、桿及手柄之標示及刻印即使係在難以接近的地方亦可藉助雷射光來實施。
此外,本發明之聚合物系統可用於食品行業或玩具行業中之包裝。包裝上標記之特徵在於以下事實:其耐擦拭及耐劃痕,在隨後殺菌製程期間穩定並在標記製程期間可以衛生上純淨之方式施加。完整的標示影像可永久地施加至可再用系統之包裝。此外,本發明之聚合物系統用於醫學技術,例如用於標記皮氏培養皿(von Petri dish)、微量滴定板、導管、可棄式注射器、安瓿、樣品容器、供給管及醫學收集袋或儲存袋。
用於雷射刻印之另一重要應用領域係用於動物之個別標示之塑膠標籤,所謂的家畜標籤或耳標。條碼系統用於儲存具體地屬動物之資訊。此可視需要借助掃描儀讀出。由於耳標有時在動物身上保持若干年,故刻印必須極耐久。
因此由本發明之聚合物組成之模製組合物、半製成品及成品零件之雷射標記係可能的。
以下實例意欲解釋本發明而非對其加以限制。所指示百分比係重量百分比。
本申請案中之所有D25、D50及D95值係使用Malvern Mastersizer 2000儀器藉助雷射繞射測定。
在攪拌的同時,將直徑D95為700nm至900nm(使用來自Malvern Ltd.,UK,Malvern 2000之量測儀器量測)之100g球形TiO2(Kronos 2900,KRONOS Inc.)於2l去礦物質水中加熱至75℃。使用10%鹽酸將懸浮液之pH調整至2.0之值。隨後緩慢計量加入由264.5g 50%SnCl4溶液、60.4g 35%SbCl3溶液及440g 10%鹽酸組成之於鹽酸中之氯化錫銻溶液,在此期間藉由同時添加32%氫氧化鈉溶液使懸浮液之pH保持恆定。當添加完成時,將混合物再攪拌15min。隨後藉由添加32%氫氧化鈉溶液將pH調整至3.0之值,並將混合物再攪拌30min。
將產物濾出,洗滌,乾燥,在500℃至900℃之溫度下煅燒30min並藉助100μm篩進行篩分。
在轉筒混合器中利用2g分散助劑(Process-Aid 24,Colormatrix)將1kg PP顆粒(Metocene 648T,Basell)潤濕。添加3g實例1之雷射添加劑、1g有機黃色顏料(PV Fast Yellow HG,Clariant)及0.25g綠色顏料(PV Fast Green GNX,Clariant)並在轉筒混合器中合併2min。將所得混合物在200℃至220℃之夾套溫度下在共軸旋轉雙螺桿擠出機中利用高剪力複合,藉助造粒模成型以得到股線,在水浴中冷卻並藉助旋轉
刀製粒。在注射成型機上將所得複合物轉換為尺寸為60mm×90mm×1.5mm(w×h×d)之板。然後使用波長為1064nm且最大輸出功率為10.5W之脈衝YVO4雷射來雷射標記塑膠板。測試格柵之速度在500mm/s與5000mm/s之間且頻率在20kHz與100kHz之間變化。對具有50μm之線間隔以及線文字之填充區域進行雷射,以高達3000mm/s之速度獲得穩定深色雷射標記。線標記極其明確且具有精確細節。標記之平滑表面證實添加劑與較少的周圍聚合物之反應。
類似於A1,將3g實例1之添加劑併入PMMA中,使用2g TiO2 Kronos 2220代替有機彩色顏料。隨後使用波長為1064nm且最大輸出功率為10.5W之脈衝YVO4雷射來雷射標記塑膠板。測試格柵之速度在500mm/s與5000mm/s之間且頻率在20kHz與100kHz之間變化。對具有50μm之線間隔及另外線腳本之填充區域進行雷射。以高達5000mm/s之速度(其對應於雷射之最大標記速度)達成穩定深色雷射標記。
液體聚矽氧橡膠(LSR)係在熱作用下易於聚合之雙組份系統。將兩個液體組份以1:1比率混合以得到聚矽氧橡膠。在實例中,使用來自Shin-Etsu之LSR類型:KEG 2000/50。將6g實例1之雷射添加劑添加至500g LSR之組份1並劇烈混合。隨後添加500g組份2並再次劇烈混合。將此液體混合物傾倒至模具中並置於實驗室烘箱中在180℃下固化20分鐘。固化後,將模製物冷卻並類似於實例A1進行雷射標記。
將560.5g Crylcoat 2689-0(Allnex)、29.5g Primid XL-552(Ems Chemie AG)、8.0g BYK 364P(BYK-Chemie GmbH)、2.0g Benzoin(DSM)及400g Kronos 2160(Kronos Titan GmbH)以及60g實例1之添加劑在實驗室混合器中劇烈混合5min。將所得混合物在70℃與100℃
之溫度下在適宜擠出機中擠出。將所得擠出物冷卻,破碎並研磨。添加2.0g Aeroxide Alu C(Evonik)後,使用網格寬度為125μm之篩來篩分粉末。藉助電暈或摩擦方法將所得粉末塗料材料施加至測試金屬片並在180℃(試樣溫度)下烘烤10min。
類似於實例A1及實例A2,使用IR雷射標記測試金屬片上之塗料。
Claims (11)
- 一種雷射可標記之聚合物及塗料,其特徵在於其包含球形TiO2粒子作為雷射添加劑,其中該等TiO2粒子在表面上經銻摻雜之二氧化錫層(Sn,Sb)O2塗佈,且該等TiO2粒子具有藉助雷射繞射以D95量測<15μm之數量加權粒度。
- 如請求項1之雷射可標記之聚合物及塗料,其中該二氧化錫層中之銻含量基於該二氧化錫係0.1mol%至60mol%。
- 如請求項1或2之雷射可標記之聚合物及塗料,其中該雷射添加劑具有藉助雷射繞射以D25量測0.05μm之數量加權粒度。
- 如請求項1至3中任一項之雷射可標記之聚合物及塗料,其中該雷射添加劑係基於該欲標記之聚合物或塗料材料以0.005重量%至30重量%之濃度應用。
- 如請求項1至4中任一項之雷射可標記之聚合物及塗料,其中該聚合物係熱塑性聚合物、熱固性聚合物、彈性體或聚矽氧。
- 如請求項1至5中任一項之雷射可標記之聚合物及塗料,其中該聚合物另外包含一或多種彩色顏料及/或染料。
- 一種製備如請求項1至6中任一項之雷射可標記之聚合物及塗料之方法,其特徵在於該雷射添加劑之添加係藉由複合、經由母料或經由糊劑或藉由直接添加至該聚合物來同時或依序地實施,並視情況添加一或多種添加劑,且然後在熱作用下使該聚合物成型。
- 一種如請求項1至6中任一項之雷射可標記之聚合物及塗料之用途,其係作為用於生產模製組合物、半製成品、成品零件及用於成像之材料。
- 一種由如請求項1至6中任一項之雷射可標記之聚合物組成之模 製組合物、半製成品、成品零件及膜。
- 一種由如請求項1至6中任一項之雷射可標記之聚合物組成之粉末塗料。
- 一種經銻摻雜之二氧化錫層(Sn,Sb)O2塗佈之球形TiO2粒子,其特徵在於該等TiO2粒子在表面上經銻摻雜之二氧化錫層(Sn,Sb)O2塗佈且該等TiO2粒子具有藉助雷射繞射以D95量測<15μm之數量加權粒度,且該二氧化錫層中之銻含量基於該二氧化錫係2mol%至15mol%。
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