TWI831199B - 用於產生立體印刷物件之方法 - Google Patents
用於產生立體印刷物件之方法 Download PDFInfo
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- TWI831199B TWI831199B TW111117695A TW111117695A TWI831199B TW I831199 B TWI831199 B TW I831199B TW 111117695 A TW111117695 A TW 111117695A TW 111117695 A TW111117695 A TW 111117695A TW I831199 B TWI831199 B TW I831199B
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- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229960001156 mitoxantrone Drugs 0.000 description 1
- WKWOFMSUGVVZIV-UHFFFAOYSA-N n-bis(ethenyl)silyl-n-trimethylsilylmethanamine Chemical compound C[Si](C)(C)N(C)[SiH](C=C)C=C WKWOFMSUGVVZIV-UHFFFAOYSA-N 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
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- 239000000049 pigment Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000671 polyethylene glycol diacrylate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
本發明係關於一種使用涉及含有作為末端基(甲基)丙烯酸基團之聚矽氧之一光可固化聚矽氧組合物產生一立體(3D)印刷物件之方法。
Description
本發明係關於一種使用包括(甲基)丙烯酸聚矽氧聚合物之一光可固化組合物產生一立體(3D)印刷物件之方法。
3D印刷技術(亦稱為積層製造(AM)、快速原型製造或分層製造)涵蓋多種不同技術且用於產生幾乎任何形狀或幾何形狀之立體物件而無需模具或加工。如今,歸因於大量可能商業應用,積層製造正經歷非常強之發展且具有重要增長潛力。為允許增加其使用,必須拓寬可與一積層製造設備一起使用之材料範圍。
一重要種類之可固化聚矽氧組合物透過熱固性交聯固化,其與一3D列印機之配合使用較複雜且幾乎與積層製造程序不相容。事實上,在一逐層3D印刷程序中,各層必須保持其形狀。隨著產品高度增加,下層不保持其形狀及流動以導致建築結構之變形或崩塌。因此,獲得聚矽氧部分之不適當形狀。
已提出若干解決方案來阻止此印刷適性問題。例如,在WO2018/206689中,經由一3D液相沈積模型化程序實現聚矽氧3D印刷物件,其中可固化聚矽氧組合物具有足夠流變性質以允許避免在完全固化之
前印刷物件在室溫下崩塌或變形。此方法之主要缺點係缺乏程序之精確度(>100微米/層)且需要對成品物件實施一後處理以確保固化程序完全完成。
基於光聚合之3D印刷技術現正受到越來越多之關注。其等自一液體材料開始局部沈積且固化或自一液體桶選擇性地固化。此等技術之實例係UV立體光微影(SLA)、UV數位光處理(DLP)、連續液體介面生產(CLIP)及噴墨沈積。
例如,WO2015197495中揭示UV立體光微影(SLA)。例如,UV立體光微影(SLA)使用通常由一掃描器系統在X-Y(水平)平面中移動之雷射光束。由來自所產生之資料源之資訊引導之馬達驅動將雷射光束發送於表面上之反射鏡。
例如,WO 2016181149及US20140131908中揭示UV數位光處理(DLP)。在一UV數位光處理(DLP)中,將一3D模型發送至列印機,且一桶液體聚合物在安全光條件下曝露於來自一DLP投影儀之光。DLP投影儀將3D模型之影像顯示在液體聚合物上。DLP投影儀可安裝在由透明彈性膜製成之視窗下面,其中來自DLP投影儀之UV光可穿透該視窗。
例如,WO2014126837及WO2016140891中揭示連續液體介面生產(CLIP,最初係連續液體中間相印刷),其(例如)使用光聚合來產生多種形狀之平滑側面固體物件。
例如,WO2015107333、WO2016109819及WO2016134972中揭示擠壓3D印刷程序。例如,在此程序中,材料透過一噴嘴擠壓以印刷一物件之一個截面,其可對於各層重複。可將一能源直
接附接至噴嘴使得其在擠壓之後立即固化或可與噴嘴分離以延遲固化。一旦各層完成,噴嘴或構建平台即通常在Z軸(垂直)平面中移動之前在X-Y(水平)平面中移動。UV固化可在沈積之後立即進行或可在UV光下移動板以在沈積與UV固化之間提供延遲。一支撐材料可用於避免在空氣中擠壓一細絲材料。一些後處理處理可用於改良印刷表面之品質。
例如,WO201740874、WO2016071241、WO20 16134972、WO2016188930、WO2016044547及WO2014108364中揭示噴墨沈積,其(例如)使用具有在一印刷區域周圍移動之一列印頭之材料噴射列印機以(例如)由UV聚合噴射特定液體可固化組合物。噴墨噴嘴形成一液滴之能力以及其體積及速度受材料之表面張力影響。
由於3D光聚合基於在可在曝露於特定波長之光源之後固化/光聚合之一液態中使用單體/低聚物,因此光可固化聚矽氧組合物更易於其固化材料之許多優點(諸如撓性、生物相容性、電氣及電子組件之絕緣性質及良好化學性質、溫度及耐氣候性)而備受關注。
目前用於3D印刷之光可固化液體聚矽氧組合物主要係耦合至一光可激活催化劑之複加成可固化聚矽氧組合物。此技術之問題係反應之催化作用並非瞬時,且當使用(例如)3D噴墨印刷時,固化產品通常需要後固化。
US2020071525中描述另一新方法,其中描述一種用於製作立體光微影3D印刷聚矽氧結構之光可固化聚(矽氧烷)組合物,其包括:
(a)一第一可聚合聚(矽氧烷),其具有一第一末端基有機功能及一第二末端基有機功能,各末端基包括丙烯酸酯或甲基丙烯醯氧丙基,
(b)一第二可聚合聚(矽氧烷),其包括重複單元,該等重複單元之至
少一些重複單元具有一側鏈可聚合基團。
(c)一光起始劑,其較佳地係乙基(2,4,6-三甲基苯甲醯)苯基膦酸酯(TPO-L),及
(d)一敏化劑,其較佳地係異丙基噻噸酮(ITX)。
其具有自約10kDa至約60kDa之一較佳分子量。其被描述為適合於構建微器件且3D印刷結構較佳地具有約0.5-1MPa之一低楊氏模數及約140%之一斷裂伸長率。藉由將光起始劑濃度之含量提高至約0.8%(組合物之總重量之重量%)而獲得一最大值約160%之斷裂伸長率。然而,在此含量下,光起始劑在固化之後誘發一黃色材料,其在許多應用中非所欲。此外,所有實例包含使用異丙基噻噸酮(ITX)作為敏化劑。
因此,仍需要自給出固化產品之較高斷裂伸長率(特定言之遠高於上述參考中所描述之140%)之聚矽氧光聚合物組合物獲得一3D物件,其經調適以支援3D-UV印刷技術,諸如UV立體光微影(SLA)、UV數位光處理(DLP)、連續液體介面生產(CLIP)、UV擠壓及噴墨沈積。此外,亦需要改良抗拉強度及其他物理性質使得其開放用途於各種領域,諸如健康照護、電子學、航空太空、運輸、構造、工業備件、密封及與墊片之接合。
本發明之一目的係提供一種用於使用給出良好硬度性質之一光可固化聚矽氧組合物產生一立體印刷物件之方法。
本發明之另一目的係提供一種用於使用不一定需要使用一敏化劑(諸如異丙基噻噸酮(ITX))之一光可固化聚矽氧組合物產生一立體印刷物件之方法。
本發明之又一目的係提供一種根據本發明之方法形成之立體(3D)印刷物件。
此等目的尤其由本發明(其係關於一種產生一立體印刷物件之方法)實現,該方法包括
(a)對於100重量份之至少一種具有以下化學式(1)之有機聚矽氧烷聚合物CE:M*DxM* (1)
其中:.M*係:R1(R)2SiO1/2;.D係(R)2SiO2/2;.x係1至小於60,且較佳地x係自3至50,.R係選自由甲基、乙基、丙基、三氟丙基及苯基組成之群組之烷基,且最較佳地R係甲基,.R1係通式-CnH2nO-CH2CHR2(CH2)m-OCOCH=CHR3之一部分,其中n係3或4且m係0或1,較佳地m係1,R2係H、OH或-CzH2z-CH2OH,z係1、2或3且R3係H或-CH3;(b)自0重量份至20重量份、較佳地自1重量份至20重量份且甚至更佳
地自1重量份至10重量份之至少一種具有以下化學式(2)之有機聚矽氧烷聚合物XL:M Dv(DACR)w M (2)
其中.M係:R2(R)2SiO1/2;(R)3SiO1/2或R4(R)2SiO1/2.D係(R)2SiO2/2;.DACR係(R2)(R)SiO2/2;.y係自0至500,較佳地自10至500,且最佳地自50至400,.w係自0至50,較佳地自1至25,且最佳地自3至20,且當w=0時,y係自1至500且M表示:R2(R)2SiO1/2或R4(R)2SiO1/2;.R係選自由甲基、乙基、丙基、三氟丙基及苯基組成之群組之烷基,且最佳地R係甲基,.R2係以下通式之一部分:○-CnH2nO-CH2CHR2(CH2)m-OCOCH=CHR3,其中n係3或4且m係0或1,R2係H、OH或-CzH2z-CH2OH,z係1、2或3,R3係H或-CH3;或○-CnH2nO COCH=CHR3,其中n係3或4,R3係H或-CH3;.R4係化學式(3)之一部分:
(c)自0.01重量份至10重量份之至少一種光起始劑PI,較佳地自0.01
重量份至3重量份,(d)至少15重量份、較佳地自20重量份至100重量份、甚至更佳地自20重量份至50重量份之至少一種無機填料F,(e)自0重量份至10重量份之至少一種敏化劑PS,(f)自0重量份至10000重量份之至少一種光可固化有機(甲基)丙烯酸單體/低聚物M,及(g)自0重量份至10重量份之至少一種添加劑I;2)使該光可固化組合物X曝露於光化輻射以在一板或支撐件上形成一固化截面,及3)在具有新層之先前固化截面上重複步驟1)及2)以構建該立體印刷物件。
為實現此等目標,值得讚揚的係,申請人完全令人吃驚及出乎意料地證明藉由使用特定丙烯酸封端聚矽氧(根據本發明之3-丙烯氧基-2-羥基丙氧基丙基末端基)相對於根據先前技術之標準丙烯酸封端聚矽氧((甲基)丙烯基氧丙基末端基)組合該光可固化材料組合物X中之一無機填料之至少15重量份(對於100重量份之丙烯酸封端聚矽氧),可經由3D-UV印刷獲得具有良好硬度性質之一固化材料使得其開放用於各種領域(諸如健康照護、電子學、航空太空、運輸、構造、工業備件、密封及與墊片之接合及其類似者)之3D印刷中之光可固化聚矽氧組合物之用途。結果係在不使用允許可使用一更廣泛範圍之3D-UV列印機之3D印刷程序具有更大靈活性之一敏化劑(諸如異丙基噻噸酮(ITX))之情況下獲得。
在另一較佳實施例中,選擇組分及組分之數量以使組合物X在25℃時具有低於50Pa.s之一動態黏度且較佳地在25℃時具有低於20
Pa.s之一動態黏度。在此情況中,組合物X可由普通SLA列印機或DLP列印機(諸如一ASIGA MAX)處理。
術語「動態黏度」意欲表示伴隨材料中之一流率梯度之存在之剪切應力。本報告中引用之所有黏度均對應於在25℃下或根據標準ASTM D445以本身已知之一方式量測之動態黏度之一量值。通常使用一布氏(Brookfield)黏度計來量測黏度。
在一較佳實施例中,其中該有機聚矽氧烷聚合物CE包括作為末端基之甲基(丙烯酸)部分,該甲基(丙烯酸)部分包括羥基且具有廣義平均通式:M*DxM*
其中.M*係:R1(R)2SiO1/2;.D係(R)2SiO2/2;.x係自1至小於60,且較佳地x係自3至50,.R係選自由甲基、乙基、丙基、三氟丙基及苯基組成之群組之烷基,且最佳地R係甲基,.R1係通式-CnH2nO-CH2CHR2(CH2)m-OCOCH=CHR3之一部分,其中n係3或4且m係0或1,R2係OH或-CzH2z-CH2OH,z係1、2或3且R3係H或-CH3。
其中a係自1至20,且較佳地a係自1至10,b係自1至500,且較佳地b係自10至500。
其中n係自10至400,較佳地n係自50至200,且甚至更佳地n係自50至150。
其中n係自1至500,且較佳地n係自1至200。
其中a係自2至50,且較佳地a係自2至20;b係自0至500,且較佳地b係自10至400。
光起始劑之適合實例包含醯基磷氧化物或醯基膦氧化物。一溶劑可與光起始劑(諸如異丙醇(IPA))組合使用以將其溶解於聚矽氧組合物中。
CPO-1及CPO-2可根據Molecules 2020,25(7),1671,New Phosphine Oxides as High Performance Near UV Type I Photoinitiators of Radical Polymerization中描述的協定來製備。
其他適合光起始劑係液體雙醯基膦氧化物(諸如US2016/0168177 A1中所描述)或醯基膦(諸如US2008/0004464中所描述)。
最佳光起始劑係乙基(2,4,6-三甲基苯甲醯)苯基膦酸酯
(10)(TPO-L)。
適合無機填料F可選自增強無機填料F1、導熱無機填料F2、導電無機填料F3及其等之混合物組成之群組。
在一些實施例中,增強無機填料F1選自二氧化矽及/或氧化鋁,較佳地選自二氧化矽。由於可使用二氧化矽,設想填料由通常小於或等於0.1μm之一精細顆粒大小及通常在約50平方米每克至300平方米每克以上之範圍內之比表面積與重量之一高比率特徵化。此類型之二氧化矽係市售產品且在聚矽氧組合物之製造技術中係眾所周知。此等二氧化矽可為矽酸膠、熱解製備之二氧化矽(稱為燃燒或氣相二氧化矽之二氧化矽)或藉由此等二氧化矽之混合物之濕式法製備之二氧化矽(沈澱二氧化矽)。對於本發明之目的而言,若二氧化矽對印刷產品具有一增強作用,則化學本質及製備能夠形成無機填料之二氧化矽之方法不重要。當然,亦可使用各種二氧化矽之切割。此等二氧化矽粉末具有通常接近或等於0.1μm之一平均顆粒大小及大於50m2/g、較佳地在50m2/g與400m2/g之間、尤其在150m2/g與350m2/g之間的一BET比表面積5。此等二氧化矽可視情況藉助選自滿足至少兩個準則之分子之群組之至少一種相容劑進行預處理:a)在二氧化矽與自身及周圍聚矽氧油之其氫鍵區域中與二氧化矽發生一高度交互作用;及b)藉由在一氣流中在真空下加熱,其本身或其降解產物容易自最終混合物移除,且低分子量之化合物係較佳的。
亦可藉由添加一未經處理之二氧化矽及類似於可在預處理中使用且如上文所界定之至少一種增容劑來原位處理此等二氧化矽。
增容劑根據處理方法(預處理或原位)選擇且可(例如)自選
自包括以下之群組:氯矽烷、聚有機環矽氧烷(諸如八甲基環矽氧烷(D4))、矽氮烷(較佳地二矽氮烷)或其等之混合物、係較佳矽氮烷且可與二乙烯基四甲基-二矽氨烷相關聯之六甲基二矽氮烷(HMDZ)、每分子具有鏈接至矽之一或多個羥基之聚有機矽氧烷、胺(諸如氨)或具有一低分子量之烷基胺(諸如二乙胺)、烷氧矽烷(諸如甲基丙烯醯氧基丙基三甲氧基矽烷)、具有一低分子量之有機酸(諸如甲酸或乙酸,或丙烯酸及其等之混合物)。在原位處理之情況中,增容劑較佳地在水之存在下使用。對於此方面之更多細節,可參考(例如)專利FR-B-2 764 894。
可能使用由矽氮烷提供早期處理(例如FR-A-2 320 324)或一延遲處理(例如EP-A-462 032)之先前技術之增容方法,應記住根據本發明根據所使用之二氧化矽,其用途通常不可能就藉由根據本發明之對兩種時機進行處理而獲得之機械性質(特定言之延伸性)而言獲得最佳結果。
在一較佳實施例中,無機填料F選自由矽酸膠、氣相式二氧化矽、沈澱矽石或其等之混合物組成之群組。
作為一增強無機填料F1之實例,可使用氧化鋁且特定言之摻雜或未以一已知方式有利地採用一高度分散氧化鋁。當然,亦可使用各種氧化鋁之切割。較佳地,所使用之增強填料係單獨使用或與氧化鋁混合之一燃燒二氧化矽。
根據本發明,可設想使用一互補填料,諸如一導熱無機填料F2及/或一導電無機填料F3。兩者均可由用於控制填料形狀之形態及/或填充填料之內部空隙/孔隙之一表面積改良劑進行表面處理。表面積改良劑之引入降低填料之總表面積。
適合導熱無機填料F2包含氮化硼、氮化鋁、銅、銀、鋁、
鎂、黃銅、金、鎳、氧化鋁、氧化鋅、氧化鎂、氧化鐵、氧化銀、氧化銅、金屬塗佈有機顆粒、鍍銀鎳、鍍銀銅、鍍銀鋁、鍍銀玻璃、銀片、銀粉、炭黑、石墨、金剛石、碳奈米管、二氧化矽及其等之混合物。較佳地,導熱無機填料F2係氮化硼。
適合導電無機填料F3包含一金屬或其他組分。特定言之,其可包含(例如)填料(諸如炭黑、石墨)、金屬組件(例如鋁、銅、黃銅、青銅、鎳或鐵)、導電無機顏料(諸如氧化錫、氧化鐵及二氧化鈦)、無機鹽及其等之組合。石墨且特定言之合成石墨係特別有用。亦可包含合成石墨、天然石墨及其等之組合。一具體實施例亦可包含銀粒子、塗覆銀核心粒子及碳奈米管。
當存在時,敏化劑PS在1ppm至高達10重量份之範圍內。一最佳使用量在組合物X之總含量之10ppm至100ppm之範圍內。
就敏化劑而言,其意謂吸收光之能量之分子且充當將此能量傳送至受體分子之供體。
適合敏化劑PS之實例包含由二苯甲酮及其衍生物、噻噸酮及其衍生物、蒽醌及其衍生物、甲酸苄酯、樟腦醌、二苯乙二酮、菲醌、香豆素及鯨油酚及其等之混合物組成之群組。
就二苯甲酮衍生物而言,其意謂取代二苯甲酮及二苯甲酮之聚合版本。術語「噻噸酮衍生物」係指取代噻噸酮及蒽醌衍生物、取代蒽醌,特定言之蒽醌磺酸及丙烯醯胺基胺取代蒽醌。
作為適合敏化劑PS之具體實例,可提及(特定言之)以下產品:異丙基噻噸酮;二苯甲酮;樟腦醌;9-蒽酮;蒽醌;1-4-二羥基蒽醌;2-甲基蒽醌;2,2’-雙(3-羥基-1,4-萘醌);2,6-二羥基蒽醌;1-羥基環
己基苯基酮;1,5-二羥基蒽醌;1,3-二苯基-1,3-丙烷二酮;5,7-二羥基黃酮;二苯甲醯過氧化物;2-苯甲醯苯甲酸;2-羥基-2-甲基丙酮酮;2-苯乙酮;蒽酮;4,4’-二甲氧基安息香;菲醌;2-乙基蒽醌;2-甲基蒽醌;2-乙基蒽醌;1,8-二羥基蒽醌酮;二苯甲醯過氧化物;2,2-二甲氧基-2-苯乙酮;安息香;2-羥基-2-甲基丙苯酮;苯甲醛;4-(2-羥基乙氧基)苯基-(2-羥基-2-甲基丙基)酮;苯甲醯丙酮;乙基(2,4,6-三甲基苯甲醯基)苯基膦酸鹽及其等之混合物。
作為敏化劑PS之商業產品之實例,可提及以下產品:Esacure® TZT、Speedcure® MBP、Omnipol® BP及噻噸酮衍生物、Irgacure® 907、Omnipol® TX及Genopol® TX-1產品。
此化合物對應於產物Ebecryl P36(CAS:85340-63-2)。
當存在一光可固化有機(甲基)丙烯酸單體/低聚物M時,如上文所描述,添加一敏化劑可有用。
適合光可固化有機(甲基)丙烯酸單體/低聚物M之實例包含(但不限於)以下,聚乙二醇二丙烯酸酯(PEGDA)、1,6-雙-(金屬矽氧基-2-乙氧基氨基)-2,4,4-三甲基Exane(UDMA)、二甲基丙烯酸三乙二醇酯(TEGDMA)、甲基丙烯酸雙酚A-縮水甘油酯或2,2-雙-4-2-(羥基-3-異丙氧基-1-氧基)丙烷(雙GMA),三羥甲基丙烷三丙烯酸酯(TTA)及雙酚A乙氧基二丙烯酸酯(Bis-EDA)。
本發明可固化聚矽氧組合物可視情況包括至少一種添加劑I,只要其等不干擾固化機制或對目標性質產生不利影響。該添加劑之選
擇取決於其中使用該等組合物及所要性質的應用。其可以包含單獨使用或作為一混合物使用之各種類型之添加劑,諸如顏料、退光劑、消光劑、熱及/或光穩定劑、抗靜電劑、阻燃劑、抗菌劑、抗真菌劑及觸變減黏劑。
在一較佳實施例中,選擇組分及組分(a)至(g)之量以使組合物X在25℃時具有低於50Pa.s之一動態黏度且較佳地在25℃時具有低於20Pa.s之一動態黏度以允許容易與標準UV-3D列印機一起使用。
在一較佳實施例中,光可固化組合物X經由使用選自由UV立體光微影(SLA)、UV數位光處理(DLP)、連續液體介面生產(CLIP)、UV擠壓及噴墨沈積組成之群組之一技術之一3D列印機提供。此等技術及相關3D印刷設備係熟習技術者所熟知。
為構建物件,可(例如)經由CAD軟體(諸如SolidWorks、Sculpt或SelfCAD)使用一3D數位檔案。此等檔案(通常係STL檔案)由將模型切割成薄層進行印刷之一切片機處理。接著,將指令發送至一3D列印機。
本發明之其他優點及特徵將在閱讀以圖解方式給出且無任何限制之以下實例時出現。
實例
I)用於實例中之原材料:
1)具有雙(3-丙烯氧基2-羥丙氧基丙基)末端基之聚二甲基矽氧烷CE:
聚二甲基矽氧烷聚合物CE-1(發明):n=6;在25℃下,黏度係170mPa.s。
聚二甲基矽氧烷聚合物CE-2(發明):n=45,在25℃下,黏度係200mPa.s。
聚二甲基矽氧烷聚合物CE-3(比較):n係自250至280;在25℃下,黏度係1200mPa.s。
3)具有鏈XL中之(丙烯氧基-2-羥丙氧基丙基)基團之聚二甲基矽氧烷:
聚二甲基矽氧烷聚合物XL-1;a係自3至4且b係約220。
4)無機填料F1:由Wacker以商品名HDK® H2000出售之熱解二氧化矽表面處理(三甲基矽氧基)。
5)光起始劑PI:TPO-L:2,4,6-三甲基苯甲醯-苯基膦酸酯。
II)物理性質
黏度:根據ASTM D445或ISO3104,在25℃下量測樣品之黏度。
硬度:根據ASTM D2240或ISO868,在25℃下量測固化樣品之硬度。
II)配方(使用一3D列印機Asiga固化及3D印刷)
根據表1製備配方。
接著,手動或使用一快速混合器將其混合。接著將所得混合物倒入具有1升之一容量且具有XYZ:119×67×75mm之一印刷板之Asiga 3D列印機之桶中。接著,設計一H2樣品之一「.stl」檔案(長度40mm +/-0.5,厚度2mm +/-0.2)。使用「.stl」檔案及27層之一構建程序製備2mm厚之樣品。各層具有75微米之一厚度。第一層在30s期間進行輻照以實現與平台之一良好黏附,且以下層在385nm及5.8mW/cm2下在20s期間對於各層進行輻照。在3D印刷之後,樣品可在180s期間在一UV箱/右頁/左頁中,在405nm處後固化。
下表1中引用物理性質。
根據本發明之實例1及2與實例3(比較)之比較展示當使用根據本發明之聚合物時,很好地改良肖氏硬度(超過3倍)。
Claims (7)
- 一種用於產生一立體印刷物件之方法,其包括(a)對於100重量份之至少一種具有以下化學式(1)之有機聚矽氧烷聚合物CE:M*DxM* (1)其中:M*係:R1(R)2SiO1/2;D係(R)2SiO2/2;x係1至小於60,R係選自由甲基、乙基、丙基、三氟丙基及苯基組成之群組之烷基,R1係通式-CnH2nO-CH2CHR2(CH2)m-OCOCH=CHR3之一部分,其中n係3或4且m係0或1,R2係H、OH或-CzH2z-CH2OH,z係1、2或3且R3係H或-CH3;(b)自1重量份至20重量份之至少一種具有以下化學式(2)之有機聚矽氧烷聚合物XL:M Dy(DACR)w M (2)其中M係:R2(R)2SiO1/2;(R)3SiO1/2或R4(R)2SiO1/2 D係(R)2SiO2/2;DACR係(R2)(R)SiO2/2;y係自0至500, w係自0至50,且當w=0時,y係自1至500且M表示:R2(R)2SiO1/2或R4(R)2SiO1/2;R係選自由甲基、乙基、丙基、三氟丙基及苯基組成之群組之烷基,R2係以下通式之一部分:-CnH2nO-CH2CHR2(CH2)m-OCOCH=CHR3,其中n係3或4且m係0或1,R2係H、OH或-CzH2z-CH2OH,z係1、2或3,R3係H或-CH3;或-CnH2nO-COCH=CHR3,其中n係3或4且R3係H或-CH3;R4係化學式(3)之一部分:
- 如請求項1之方法,其中該有機聚矽氧烷聚合物CE包括作為末端基之甲基(丙烯酸)部分,該甲基(丙烯酸)部分包括羥基且具有廣義平均通式:M*DxM*其中M*係:R1(R)2SiO1/2;D係(R)2SiO2/2;x係自1至小於60,R係選自由甲基、乙基、丙基、三氟丙基及苯基組成之群組之烷基,R1係通式-CnH2nO-CH2CHR2(CH2)m-OCOCH=CHR3之一部分,其中n係3或4且m係0或1,R2係OH或-CzH2z-CH2OH,z係1、2或3且R3係H或-CH3。
- 如請求項1之方法,其中該無機填料F選自由矽酸膠、氣相式二氧化矽、沈澱矽石或其等之混合物組成之群組。
- 如請求項1之方法,其中選擇該等組分及該等組分之數量以使該組合 物X在25℃時具有低於50Pa.s之一動態黏度。
- 如請求項1之方法,其中該光可固化組合物X經由使用選自由UV立體光微影(SLA)、UV數位光處理(DLP)、連續液體介面生產(CLIP)、噴墨沈積及UV擠壓組成之群組之一技術之一3D列印機提供。
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