CN114630853A - 抛光垫的增材制造 - Google Patents
抛光垫的增材制造 Download PDFInfo
- Publication number
- CN114630853A CN114630853A CN202080074378.XA CN202080074378A CN114630853A CN 114630853 A CN114630853 A CN 114630853A CN 202080074378 A CN202080074378 A CN 202080074378A CN 114630853 A CN114630853 A CN 114630853A
- Authority
- CN
- China
- Prior art keywords
- difunctional
- urethane acrylate
- oligomer
- acrylate oligomer
- polishing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
一种用于抛光垫的抛光层的增材制造的系统、配方和方法。所述配方包括基于双官能多元醇或双官能多硫醇的聚氨酯丙烯酸酯低聚物。所述技术包括选择所述双官能多元醇或所述双官能多硫醇以影响所述抛光层的性质。所述配方还包括单体和光敏引发剂。所述配方的黏度适用于所述抛光层的3D打印。
Description
技术领域
本公开内容涉及用于化学机械抛光中的抛光垫。
背景技术
集成电路典型地通过在硅晶片上顺序地沉积导电层、半导体层或绝缘层来形成在基板上。多种制造技术采用在基板上的层的平坦化。例如,对于某些应用(例如,抛光金属层以在图案化层的沟槽中形成过孔、插塞和线),平坦化上覆层(overlying layer),直到暴露图案化层的顶表面。在其他应用(例如,用于光刻的介电层的平坦化)中,抛光上覆层,直到在下层(underlying layer)之上保留所期望的厚度。
化学机械抛光(CMP)是一种公认的平坦化技术。在应用中,该平坦化技术可将基板安装在承载头上。基板的暴露表面典型地抵靠旋转的抛光垫放置。承载头在基板上提供可控制负载以将基板推靠在抛光垫上。可向抛光垫的表面供应抛光液(诸如具有磨粒的浆料)。化学机械抛光的一个目标可以是抛光均匀性。如果基板上的不同区域以不同速率进行抛光,则基板的某些区域可能去除的材料过多(“抛光过度”)或去除的材料过少(“抛光不足”)。除了平坦化之外,抛光垫还可用于修整(finishing)操作(诸如擦光(buffing))。
用于CMP的抛光垫可包括“标准”垫和固定研磨垫(fixed-abrasive pad)。标准垫可具有带有耐用粗糙表面的聚氨酯抛光层,并且还可包括可压缩背衬层(backing layer)。相比之下,固定研磨垫具有保持在容纳介质中的磨粒,并且可被支撑在一般不可压缩的背衬层上。
抛光垫典型地通过模制、铸造或烧结聚氨酯材料制成。在模制的情况下,抛光垫可一次一个地制成,例如通过注射成型(injection molding)制成。在铸造的情况下,将液态前驱物铸造和固化成饼状件(cake),随后,将其切分成单独垫件(pad piece)。然后,可将这些垫件机加工成最终厚度。可将槽(groove)机加工到抛光表面中,或者可使其作为注射成型工艺的一部分形成。
发明内容
一个方面涉及一种用于抛光垫的抛光层的三维(3D)打印的配方(formulation)。所述配方包括基于(例如,掺入)双官能多元醇或双官能多硫醇的聚氨酯丙烯酸酯低聚物。所述配方还包括单体(例如,多个单体)、添加剂和光敏引发剂。所述配方的黏度(viscosity)适用于所述抛光层的3D打印。
另一方面涉及一种合成用于抛光垫的增材制造的聚氨酯丙烯酸酯低聚物的方法。所述方法包括选择双官能多元醇或双官能多硫醇以影响所述抛光垫的抛光层的性质。所述方法包括执行所述双官能多元醇或所述双官能多硫醇与双官能异氰酸酯的催化反应,以得到聚氨酯低聚物。所述方法包括用丙烯酸酯将所述聚氨酯低聚物封端,以得到所述聚氨酯丙烯酸酯低聚物,其中在所述增材制造中所应用的所述聚氨酯丙烯酸酯低聚物影响所述性质。
又一方面涉及一种合成用于抛光垫的增材制造的聚氨酯丙烯酸酯低聚物的方法。所述方法包括选择双官能多元醇或双官能多硫醇以影响在所述增材制造中具有所述聚氨酯丙烯酸酯低聚物的3D打印配方的黏度和影响所述抛光垫的抛光层的性质。所述方法包括在催化剂的存在下使所述双官能多元醇或所述双官能多硫醇与双官能异氰酸酯反应,以得到聚氨酯低聚物预聚物。所述方法包括在所述聚氨酯低聚物预聚物上掺入丙烯酸酯作为封端物(end cap),以得到所述聚氨酯丙烯酸酯低聚物,其中在所述增材制造中的所述聚氨酯丙烯酸酯低聚物影响所述性质。
又一方面涉及一种制造抛光垫的方法。所述方法包括通过喷嘴注射具有聚氨酯丙烯酸酯低聚物的配方以形成所述抛光垫的抛光层。所述聚氨酯丙烯酸酯低聚物是用丙烯酸酯封端的聚氨酯低聚物。所述聚氨酯低聚物是基于双官能多元醇和双官能异氰酸酯或基于双官能多硫醇和所述双官能异氰酸酯。所述方法包括向所述配方施加光以固化所注射的所述聚氨酯丙烯酸酯低聚物,其中所述双官能多元醇或所述双官能多硫醇经选择以影响所述抛光层的性质。
以下的附图和描述中阐述了一个或多个实现方式的细节。其他特征和优点将从说明书和附图中以及从权利要求书中显而易见。
附图说明
图1A是示例性抛光垫的示意性截面侧视图。
图1B是另一个示例性抛光垫的示意性截面侧视图。
图1C是又一个示例性抛光垫的示意性截面侧视图。
图2是化学机械抛光站的部分截面的示意性侧视图。
图3是例示与图1A的抛光垫接触的基板的示意性侧视图。
图4是包括在用于抛光垫的3D打印的配方中的聚氨酯丙烯酸酯低聚物的方法的流程框图。
图5至图7是可合成的示例性聚氨酯丙烯酸酯低聚物的图。
图8是聚氨酯丙烯酸酯低聚物的示例性合成的图。
图9是可用于形成聚氨酯丙烯酸酯低聚物的示例性双官能多元醇/多硫醇和双官能异氰酸酯的图。
在各图中,相似的附图标记指示相似的元件。
具体实施方式
本公开内容的一些方面涉及一种用于抛光垫的抛光层的3D打印的配方。所述配方包括用双官能多元醇或双官能多硫醇合成的聚氨酯丙烯酸酯低聚物。多元醇是含有多个羟基基团的有机化合物。多硫醇是具有若干硫醇官能团的化合物。所述配方可进一步包括单体(例如,单体的混合物)、添加剂、光敏引发剂等。所述配方的黏度适用于抛光层的3D打印。
聚氨酯丙烯酸酯低聚物可以是半结晶聚酯基聚氨酯丙烯酸酯,其为通过双官能多元醇(或双官能多硫醇)和双官能异氰酸酯的催化反应合成的紫外线(UV)可固化低聚物。双官能多元醇可以是例如半结晶聚酯多元醇。特别是对于合成,双官能多元醇(或双官能多硫醇)和双官能异氰酸酯的催化反应可得到聚氨酯低聚物作为预聚物。然后,通过使用丙烯酸酯将预聚物封端来产生聚氨酯丙烯酸酯低聚物作为UV可固化低聚物。由异氰酸酯基团形成的聚氨酯可赋予低聚物韧性,而由多元醇形成的聚氨酯可赋予柔性。本技术的实现方式可包括选择双官能多元醇或双官能多硫醇以影响抛光垫的抛光层的性质。双官能多元醇可以是例如聚酯多元醇、聚碳酸酯多元醇、聚(酯-醚)多元醇、聚(碳酸酯-酯)多元醇或它们的混合物。多硫醇可以是其中-SH基团代替-OH基团的对应结构。
多元醇(例如,半结晶聚酯)或多硫醇在用于封端的低聚物的预聚物的合成中的化学结构在赋予低聚物所期望的性质以及因此抛光层的性质的特定值方面发挥作用。具有类似的骨架化学(backbone chemistry)但具有不同官能团的两种多元醇可导致低聚物和抛光层的不同性质。类似地,具有类似的骨架化学但具有不同官能团的两种多硫醇可导致低聚物和抛光层的不同性质。
用半结晶聚酯多元醇(或对应多硫醇)形成的这些低聚物可具有高结晶度,并且因此在光致聚合之后赋予材料良好的韧性。在实现方式中,这些聚氨酯丙烯酸酯低聚物可合成为具有所期望的最终性质。在某些实现方式中,低聚物合成可在相对低的温度下是无溶剂的并且在惰性气氛下执行。
该技术可包括制备聚氨酯丙烯酸酯低聚物与其他单体、添加剂和光敏引发剂的配方。通过本技术的聚氨酯丙烯酸酯低聚物,该配方可具有相对低的黏度以促成用于制造CMP垫的配方的3D打印。配方可被制备为聚氨酯丙烯酸酯低聚物、单体(例如,丙烯酸单体)、添加剂和光敏引发剂的均质混合物。然后,可将配方3D打印以制造CMP垫。这些CMP垫对于半导体应用可具有高模量和良好弹性。
参照图1A至图1C,抛光垫18包括抛光层22。如图1A所示,抛光垫可以是由抛光层22组成的单层垫,或者如图1C所示,抛光垫可以是包括抛光层22和至少一个背衬层20的多层垫。
抛光层22可以是在抛光中呈惰性的材料。抛光层22的材料可以是塑料,例如聚氨酯。在一些实现方式中,抛光层22是相对耐用且坚硬的材料。例如,抛光层22可具有约40至80(例如,50至65)的肖氏D级硬度。抛光层22可由聚氨酯丙烯酸酯低聚物形成。
如图1A所示,抛光层22可以是具有均质组成的层,或者如图1B所示,抛光层22可包括保持在塑料材料(例如,聚氨酯)的基体29中的磨粒28。磨粒28比基体29的材料更硬。磨粒28可占抛光层的0.05重量百分比(重量%)至75重量%。例如,磨粒28可小于抛光层22的1重量%,例如小于0.1重量%。或者,磨粒28可大于抛光层22的10重量%,例如大于50重量%。磨粒的材料可以是金属氧化物,诸如二氧化铈(ceria)、氧化铝或二氧化硅,或者它们的任何组合。此外,在一些实现方式中,抛光层包括孔,例如小空隙。孔可以是50至100微米宽。
抛光层22可具有80密耳或更小、50密耳或更小或25密耳或更小的厚度D1。由于整修工艺(conditioning process)趋向于磨损覆盖层,因此抛光层22的厚度可经选择以使抛光垫18具有有用寿命,例如3000个抛光和整修循环。
在微观尺度上,抛光层22的抛光表面24可具有粗糙表面纹理,例如2至4微米的均方根(rms)表面粗糙度。例如,抛光层22可经受研磨或整修工艺以产生粗糙表面纹理。另外,3D打印可提供小而均匀的特征,例如低至200微米。
尽管抛光表面24在微观尺度上可以是粗糙的,但是抛光层22在抛光垫本身的宏观尺度上可具有良好的厚度均匀性。这种均匀性可指抛光表面24相对于抛光层的底表面的高度的全局变化,并且不包括有意地形成在抛光层中的任何宏观槽或穿孔。厚度不均匀性可小于1密尔。
在一些实施方式中,抛光表面24的至少一部分可包括形成在其中的多个槽26,以用于承载浆料。槽26可以是几乎任何图案,诸如同心圆、直线、交叉影线、螺旋和类似者。在存在槽、然后槽存在于抛光表面24上的实施方式中,在槽26之间的平台(plateaus)可以是例如抛光垫18的总水平表面积的25%至90%。因此,槽26可占据抛光垫18的总水平表面积的10%至75%。在槽26之间的平台可具有约0.1mm至2.5mm的横向宽度(lateral width)。
在一些实现方式中,例如,如果存在背衬层20,则槽26可完全地延伸穿过抛光层22。在一些实现方式中,槽26可延伸穿过抛光层22的厚度的约20%至80%,例如40%至60%。槽26的深度可以是0.25mm至1mm。例如,在具有40密耳至60密耳厚(例如,50密耳厚)的抛光层22的抛光垫18中,槽26可具有约15密耳至25密耳(例如,20密耳)的深度D2。
背衬层20可比抛光层22更软且更可压缩。背衬层20的肖氏A级硬度可为80或更小,例如,肖氏A级硬度为约60或更小。背衬层20可比抛光层22更厚或更薄(或厚度相同)。
在某些实现方式中,背衬层20可以是开孔(open-cell)或闭孔(closed-cell)泡沫,诸如具有空隙的聚氨酯或聚硅氧烷,使得在压力下,小孔塌缩,并且背衬层压缩。用于背衬层的材料的示例是来自康涅狄格州罗杰斯(Rogers,Conn.)的Rogers Corporation的PORON 4701-30,或来自Rohm&Haas的SUBA-IV。背衬层20的硬度通常可通过选择层材料和孔隙率来调节。或者,背衬层20可由与抛光层相同的前驱物形成并且具有与抛光层相同的孔隙率,但是具有不同的固化程度以便具有不同的硬度。
现在转到图2,可在CMP设备的抛光站10处抛光一个或多个基板14。适用的抛光设备的描述可在美国专利号5,738,574中找到,该专利的全部公开内容以引用方式并入本文。
抛光站10可包括可旋转压板(rotatable platen)16,抛光垫18放置在该可旋转压板上。在抛光期间,抛光液30(例如,磨料浆)可通过浆料供应端口或组合的浆料/冲洗臂32供应到抛光垫18的表面。抛光液30可包含磨粒、pH调节剂或化学活性组分。
基板14通过承载头34保持抵靠在抛光垫18上。承载头34悬挂在支撑结构(诸如转盘)上,并且通过承载头驱动轴36连接至承载头旋转马达,使得承载头可围绕轴38旋转。在抛光液30的存在下,抛光垫18和基板14的相对运动导致基板14的抛光。
参照图3,至少抛光垫18的抛光层22是利用3D打印制造的。在制造中,薄材料层逐渐地沉积和融合(fuse)。例如,垫前驱物材料的配方的液滴52可从液滴喷射打印机55的喷嘴54喷射以形成层50。液滴喷射打印机类似于喷墨打印机,但采用的是垫前驱物材料而不是墨水。喷嘴54平移(如箭头A所示)跨过支撑件51。
对于沉积的第一层50a,喷嘴54可喷射到支撑件51上。对于随后沉积的层50b,喷嘴54可喷射到已经凝固的材料56上。在每个层50凝固之后,然后在先前沉积的层上沉积新的层,直到制造出完整3维抛光层22。每个层由喷嘴54以存储在于计算机60上运行的3D绘图计算机程序中的图案施加。每个层50小于抛光层22的总厚度的50%,例如小于10%,例如小于5%,例如小于1%。
支撑件51可以是刚性基部,或者是柔性膜,例如聚四氟乙烯(PTFE)层。如果支撑件51是膜,则支撑件51可形成抛光垫18的一部分。例如,支撑件51可以是背衬层20或在背衬层20与抛光层22之间的层。或者,可从支撑件51移除抛光层22。
凝固可通过聚合来完成。例如,垫前驱物材料的层50可以是包括单体的配方,并且单体可通过紫外线(UV)固化原位聚合。垫前驱物材料可在沉积后立即有效地固化,或者整个垫前驱物材料的层50可沉积,并且然后整个层50同时地固化。
然而,有替代技术来完成3D打印。例如,液滴52可以是在冷却时凝固的聚合物熔体。或者,打印机通过散布粉末层并将粘合剂材料的液滴喷射到粉末层上来产生抛光层22。在这种情况下,粉末可包括添加剂,例如磨粒28。
3D打印通常避免了制作模具的需要,模具可能相对昂贵,并且它们的使用增加了制造时间。3D打印可消除若干常规垫制造步骤,诸如模制、铸造和机械加工。另外地,由于逐层打印,通常可在3D打印中实现紧密公差(tight tolerance)。而且,在某些实施方式中,通过简单地改变存储在3D绘图计算机程序中的图案,可采用一个打印系统(具有打印机55和计算机60)来制造多种不同的抛光垫。
在一些实现方式中,背衬层20也可通过3D打印来制造。例如,背衬层20和抛光层22可由打印机55在不间断操作中制造。通过施加不同量的固化,例如不同强度的UV辐射,可使背衬层20具有与抛光层22不同的硬度。
在其他实现方式中,背衬层20通过常规工艺制造,并且然后固定到抛光层22。例如,抛光层22可通过薄粘合剂层(例如,作为压敏粘合剂)固定到背衬层20。
图4是合成聚氨酯丙烯酸酯低聚物以包括在用于抛光垫的抛光层的3D打印的配方中的方法400。抛光垫可以是CMP垫。聚氨酯丙烯酸酯低聚物在性质上可以是黏性的。具有聚氨酯丙烯酸酯低聚物和单体(例如,丙烯酸单体)的3D打印配方可以是在70℃温度下黏度在10cP至20cP范围内的自由流动的黏性液体。
在框402处,所述方法包括将具有不同结构的多个双官能多元醇(例如,不同的聚酯多元醇)与经由增材制造所制造的抛光垫的抛光层的不同物理性质的值相关。同样地,不同结构的对应双官能多硫醇可被包括在与物理性质的值的相关中。
不同双官能多元醇/多硫醇可与在增材制造(例如,3D打印)中由具有由双官能多元醇或双官能多硫醇形成的聚氨酯丙烯酸酯低聚物的配方制造的抛光层的性质相关。物理性质可以是例如断裂伸长率、在较高温度(例如,40℃至90℃)下的储能模量、玻璃化转变温度、熔点或极限抗拉强度(UTS)。这些形成的低聚物可在较高温度下维持储能模量,同时维持断裂伸长率和UTS。
由双官能多元醇(或多硫醇)合成的聚氨酯丙烯酸酯低聚物的确切化学组成和结构影响在增材制造中制造的抛光垫的物理性质。通过3D打印机喷嘴喷射的具有聚氨酯丙烯酸酯低聚物的配方可经受光致聚合以形成抛光层。所应用的聚氨酯丙烯酸酯低聚物可以是经受UV光以固化或交联聚氨酯丙烯酸酯低聚物以及其他丙烯酸单体、光敏引发剂和添加剂的聚氨酯丙烯酸酯低聚物。添加剂可调节配方的黏度和可固化性以及抛光层的机械性质。
在框404处,所述方法包括选择双官能多元醇或双官能多硫醇以影响抛光层的性质(例如,伸长率、UTS等)。对物理性质的影响可能是性质的值的增加,例如,断裂伸长率或UTS的增加。双官能多元醇可经选择以满足抛光层的性质的指定数值范围。
所述方法可包括选择双官能多元醇(或双官能多硫醇)以降低具有用双官能多元醇合成的聚氨酯丙烯酸酯低聚物的3D打印机配方的黏度,或者满足配方的黏度的指定数值范围,或者使得黏度低于最大值。在一些实现方式中,在增材制造中通过3D打印机喷嘴喷射的配方的黏度的最大值为20厘泊(cP)。
在框406处,所述方法包括执行选择的双官能多元醇或双官能多硫醇与双官能异氰酸酯的催化反应以得到聚氨酯低聚物(例如,作为预聚物)。双官能异氰酸酯可以是例如二异氰酸酯。在一种实现方式中,催化反应中的催化剂是二月桂酸二丁基锡(DBTDL)。
在框408,所述方法包括用丙烯酸酯将聚氨酯低聚物封端以得到聚氨酯丙烯酸酯低聚物410。丙烯酸酯可以是例如丙烯酸-2-羟乙酯。
一个实现方式是用于抛光垫的抛光层的3D打印的配方。通过利用所述配方的3D打印制造的抛光层可具有至少8%的断裂伸长率和至少30兆帕(MPa)的UTS。
所述配方包括聚氨酯丙烯酸酯低聚物、单体、添加剂和光敏引发剂。添加剂可以是例如硅氧烷、聚醚硅氧烷或表面活性剂。在实现方式中,配方不需要包括溶剂,因为溶剂可充当增塑剂以降低或不利地影响机械性质。
单体通常可以是单体的混合物。单体可以是丙烯酸单体。丙烯酸单体可包括甲基丙烯酸单体。单体可以是带有具有可聚合烯基基团的部分的单体。
单体可以是例如丙烯酸异冰片酯、丙烯酸环己酯、丙烯酸三甲基环己酯、二丙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、四氢糠基丙烯酸酯、N,N-二甲基丙烯酰胺、N,N-二乙基丙烯酰胺、丁二醇二丙烯酸酯、己二醇二丙烯酸酯、季戊四醇三丙烯酸酯和季戊四醇四丙烯酸酯、乙烯基吡咯烷酮和类似者。其他单体也适用。
光敏引发剂可以是例如OmniradTM 819、OmniradTM 184或OmniradTM4265,它们都可从总部位于美国北卡罗来纳州夏洛特(Charlotte,North Carolina)的IGM Resins USAInc.获得。光敏引发剂的另一个示例是从总部位于美国伊利诺伊州奥罗拉(Aurora,Illinois)的RAHN USA Corp.获得的GenocureTM*PBZ(4-苯基二苯甲酮)。光敏引发剂的另一个示例是可从总部位于瑞士巴塞尔的BASF Schweiz AG获得的TPO or TPO-L(或混合物)。光敏引发剂可具有叔氨基化合物(例如,三乙醇胺或类似者),其可结合II型光敏引发剂具有可能的去质子作用以产生自由基。
如所讨论的,聚氨酯丙烯酸酯低聚物可用双官能多元醇合成。双官能多元醇的两种实现方式具有以下相应结构:
图5至图7是可在本技术中合成的聚氨酯丙烯酸酯低聚物的示例,并且可赋予3D打印配方和抛光垫的抛光层的所期望的性质。图5是通用结构A,它可以是至少三种类型:1型、2型和3型。图6是通用结构B,它可以是至少两种类型:4型和5型。图7是通用结构C,它可以是至少6型。用于通用结构B的R′的选项与用于通用结构A和C的R′的相同。如图5至图7所示,对于类型结构中的两个R,该给定结构中的每个R都是不同的。1型用于链烷二醇和聚酯二醇。2型用于链烷二醇和聚碳酸酯二醇。
图8是根据某些实现方式的聚氨酯丙烯酸酯低聚物的示例性合成。合成从多元醇(1摩尔当量)和二异氰酸酯(2摩尔当量)开始。包括催化剂DBTDL,并且将混合物加热至在40℃至100℃的范围内的温度,以得到多元醇-二异氰酸酯预聚物。最后,在该例示的实现方式中,将丙烯酸-2-羟乙酯(2摩尔当量)与预聚物在40℃至100℃的范围内的温度下混合,以用丙烯酸酯将预聚物在两端封端,以得到聚氨酯丙烯酸酯低聚物。
图9是可用于形成聚氨酯丙烯酸酯低聚物的双官能多元醇/多硫醇和双官能异氰酸酯的示例。在这些例示的示例中,示例性多元醇包括聚醚多元醇、聚酯多元醇和聚碳酸酯多元醇。对应多硫醇(未描绘)与所描绘的多元醇相同但是将-OH基团替换为-SH基团。示例性双官能异氰酸酯(OCN-R′-NCO)是分别标记为TDI、IPDI、4,4′-MDI、HMDI和HDI的结构。
所述配方的黏度适用于抛光层的3D打印。例如,配方的黏度在70℃下小于20cP。配方可具有一定黏度,以用于通过3D打印喷嘴喷射配方。黏度在70℃的温度下可在10cP至20cP的范围内。
在一些实现方式中,配方中聚氨酯丙烯酸酯低聚物的浓度可在10重量%至35重量%的范围内,例如20重量%至25重量%。配方中单体的浓度可在例如60重量%至85重量%的范围内,例如70重量%至75重量%。配方中光敏引发剂的浓度可在例如1重量%至5重量%或1重量%至7.5重量%的范围内。
制造抛光垫(诸如CMP垫)的方法包括通过喷嘴注射(例如,在3D打印中)具有聚氨酯丙烯酸酯低聚物的配方以形成抛光垫的抛光层。聚氨酯丙烯酸酯低聚物是用丙烯酸酯封端的聚氨酯低聚物。聚氨酯低聚物是双官能多元醇(或双官能多硫醇)和双官能异氰酸酯的催化反应的产物。
光被施加到配方以固化喷射的聚氨酯丙烯酸酯低聚物来形成抛光层。选择双官能多元醇(或双官能多硫醇)以影响抛光层的物理性质。物理性质可以是例如断裂伸长率、UTS或储能模量,并且多元醇可经选择以使得性质满足最小值或满足指定数值范围。双官能多元醇(或双官能多硫醇)还可经选择以降低具有由双官能多元醇(或双官能多硫醇)合成的聚氨酯丙烯酸酯低聚物的配方的黏度。
如所讨论的,所述配方可包括单体、添加剂和光敏引发剂。配方中的组分浓度可包括小于35重量%的聚氨酯丙烯酸酯低聚物、大于60重量%的单体和小于5重量%的光敏引发剂。在实现方式中,配方在70℃的温度下具有在10cP至20cP范围内的黏度,以用于通过喷嘴喷射配方。
实施例
这些实施例仅作为示例给出,并且不意味着限制本技术。实施例包括实施例1和实施例2。实施例1中的双官能多元醇不同于实施例2中的双官能多元醇。实施例证明多元醇影响低聚物和具有该低聚物的相关联固化配方(例如,作为抛光垫的抛光层的固化配方)的最终性质。实施例比较了赋予了低聚物和具有该低聚物的固化材料的不同性质的两种不同多元醇(具有类似的化学性质或结构)。
因此,在本技术的实现方式中,可基于双官能多元醇的选择来合成具有所期望的最终性质的低聚物。在某些实现方式中,低聚物合成可在相对低的温度下是无溶剂的并且在惰性气氛下执行。低聚物合成可涉及利用用于易于处理和以受控方式进行的反应的单体(共聚单体)中的一者进行合成。
如所指出的,实施例1和实施例2中的聚氨酯丙烯酸酯低聚物分别使用两种不同的半结晶聚酯多元醇合成。通过用连续吹扫氮气在三颈圆底烧瓶中称量1摩尔当量的多元醇来合成低聚物。两个侧颈分别用于氮气(N2)入口和出口,而中间的颈用于机械搅拌。除了多元醇之外,将2摩尔当量的二异氰酸酯添加到三颈圆底烧瓶中。搅拌烧瓶中的反应混合物并加入催化剂(二月桂酸二丁基锡,DBTDL)。将反应混合物在55℃搅拌6小时之后得到预聚物。然后,将反应混合物冷却至45℃并且向反应混合物加入2摩尔当量的丙烯酸-2-羟乙酯作为封端剂以形成最终低聚物。最终低聚物(聚氨酯丙烯酸酯低聚物)是自由流动的黏性液体。
然后,通过制作聚氨酯丙烯酸酯低聚物、单体和光敏引发剂的均匀混合物来制备配方。具体地,配方包括聚氨酯丙烯酸酯低聚物(15重量%至25重量%)、单体(70重量%至80重量%)、添加剂(2重量%至5重量%)和光敏引发剂(2重量%)。通过以18英尺/分钟在Heraeus UV固化站中暴露于多达1140mJ/cm2的UV光3遍(每遍暴露在380mJ/cm2下),配方在V型狗骨状硅胶模具(厚度为2mm)中体固化(cured bulk)。在实践中,这些配方可被3D打印,然后被固化以制作CMP垫,包括用于半导体应用的具有高模量和良好弹性的CMP垫。因此,可根据样品的厚度减少UV剂量。
实施例1:
在实施例1中,双官能多元醇是可从总部位于美国伊利诺伊州诺斯菲尔德(Northfield,Illinois)的Stepan公司获得的PC-1040-55。PC-1040-55是线状脂肪族聚酯多元醇,具体是2,000分子量聚乙烯/聚己二酸丁二醇酯二醇(polyethylene/polybutylene adipate diol)。如所讨论的,多元醇用于合成聚氨酯丙烯酸酯低聚物。
对于具有约18重量%低聚物、约78重量%单体和约2重量%光敏引发剂的配方,黏度在70℃下为在15cP至17cP的范围内。固化配方具有以下在表1中列出的性质。
表1.实施例1中的固化配方的性质
伸长率(%) | 18-21 |
UTS(MPa) | 39-42 |
在30℃下的储能模量(MPa) | 1200-1400 |
在90℃下的储能模量(MPa) | 100-300 |
实施例2:
在实施例2中,双官能多元醇是也可从Stepan公司获得的PC-101P-55,并且是无溶剂饱和聚酯树脂。PC-101P-55是线状脂肪族聚酯多元醇,并且是产生聚氨酯弹性体的通用聚酯。如所讨论的,多元醇用于合成聚氨酯丙烯酸酯低聚物。
对于具有约18重量%低聚物、约78重量%单体和约2重量%光敏引发剂的配方,黏度在70℃下为在12cP至14cP的范围内。固化配方具有以下在表2中列出的性质。
表2.实施例2中的固化配方的性质
伸长率(%) | 10-12 |
UTS(MPa) | 35-45 |
在30℃下的储能模量(MPa) | 1200-1400 |
在90℃下的储能模量(MPa) | 200-300 |
一个实现方式是用于抛光垫的抛光层的3D打印的配方。抛光层可具有至少8%的伸长率和至少30MPa的UTS。所述配方包括基于双官能多元醇或双官能多硫醇的聚氨酯丙烯酸酯低聚物。聚氨酯丙烯酸酯低聚物可以是结晶度在1%至50%范围内的半结晶的。所述配方还包括单体(例如,多个单体)、添加剂和光敏引发剂。添加剂可包括例如硅氧烷、聚醚硅氧烷或表面活性剂,或者它们的任何组合。配方中聚氨酯丙烯酸酯低聚物的浓度可在例如10重量%至35重量%的范围内。配方中单体的浓度可在例如60重量%至85重量%的范围内。配方中光敏引发剂的浓度可在例如1重量%至5重量%的范围内。多个单体可包括丙烯酸单体或多个丙烯酸单体。丙烯酸单体可以是甲基丙烯酸单体。单体可以是带有具有可聚合烯基基团的部分的单体。在一些情况下,单体可包括丙烯酸异冰片酯、丙烯酸环己酯、丙烯酸三甲基环己酯、二丙二醇二丙烯酸酯、三丙二醇二丙烯酸酯、四氢糠基丙烯酸酯、N,N-二甲基丙烯酰胺、N,N-二乙基丙烯酰胺、丁二醇二丙烯酸酯、己二醇二丙烯酸酯、季戊四醇三丙烯酸酯和季戊四醇四丙烯酸酯、乙烯基吡咯烷酮或它们的任何组合。所述配方的黏度适用于抛光层的3D打印。配方可具有一定黏度,以用于通过3D打印喷嘴喷射配方。黏度在70℃下可小于20cP。黏度在70℃的温度下可在10cP至20cP的范围内。
另一个实现方式是一种合成用于抛光垫的增材制造的聚氨酯丙烯酸酯低聚物的方法。所述方法包括选择双官能多元醇或双官能多硫醇以影响抛光垫的抛光层的性质(例如,断裂伸长率、UTS、储能模量、玻璃化转变温度或熔点)。双官能多元醇可以是半结晶聚酯、聚碳酸酯或聚乙烯和类似者。双官能多硫醇可以是对应的双官能多硫醇。双官能异氰酸酯可以是例如二异氰酸酯。影响性质可涉及选择双官能多元醇或双官能多硫醇以满足性质的指定数值范围。在某些情况下,影响性质可以是增加抛光层的伸长性质或UTS。所述方法可包括将包括双官能多元醇的多个双官能多元醇与性质相关或将包括双官能多硫醇的多个双官能多硫醇与性质相关。所述方法可进一步包括选择双官能多元醇或双官能多硫醇以影响具有聚氨酯丙烯酸酯低聚物的3D打印配方的黏度(例如,降低黏度或满足指定数值范围)。该选择可使得黏度低于在增材制造中通过3D打印机喷嘴喷射的最大值(例如,20cP)。
所述方法包括执行双官能多元醇或双官能多硫醇与双官能异氰酸酯的催化反应(例如,聚合),以得到聚氨酯低聚物(例如,作为预聚物)。催化剂的一个示例是DBTDL。所述方法包括用丙烯酸酯(例如,丙烯酸-2-羟乙酯)将聚氨酯低聚物封端,以得到聚氨酯丙烯酸酯低聚物(例如,作为UV可固化低聚物)。在增材制造中所应用的聚氨酯丙烯酸酯低聚物影响性质。所应用的聚氨酯丙烯酸酯低聚物可包括经受紫外线(UV)光以固化或交联聚氨酯丙烯酸酯低聚物的聚氨酯丙烯酸酯低聚物。所应用的聚氨酯丙烯酸酯低聚物可涉及经受光致聚合的聚氨酯丙烯酸酯低聚物。
又一个实现方式涉及一种合成用于抛光垫的增材制造的聚氨酯丙烯酸酯低聚物(例如,UV可固化低聚物)的方法。所述方法包括选择双官能多元醇或双官能多硫醇以影响在增材制造中具有聚氨酯丙烯酸酯低聚物的3D打印配方的黏度和影响抛光垫的抛光层的性质。所述性质可以是断裂伸长率、UTS、储能模量、玻璃化转变温度或熔点,或者它们的任何组合。影响黏度可以是使3D打印配方的黏度低于20cP。所述方法包括在催化剂的存在下使双官能多元醇或双官能多硫醇与双官能异氰酸酯反应,以得到聚氨酯低聚物预聚物。所述方法包括在聚氨酯低聚物预聚物上掺入丙烯酸酯作为封端物,以得到聚氨酯丙烯酸酯低聚物,其中在增材制造中的聚氨酯丙烯酸酯低聚物影响性质。
又一个实现方式是一种制造抛光垫(诸如CMP垫)的方法。所述方法包括通过喷嘴(例如,3D打印机喷嘴)注射具有聚氨酯丙烯酸酯低聚物的配方以形成所述抛光垫的抛光层。在一些情况下,配方可在70℃的温度下具有在10cP至20cP的范围内的黏度,以用于通过喷嘴喷射所述配方。所述配方还可包括单体(例如,丙烯酸单体)、添加剂和光敏引发剂。在一些示例中,配方中的组分浓度可以是小于35重量%的聚氨酯丙烯酸酯低聚物、大于60重量%的单体和小于5重量%的光敏引发剂。聚氨酯丙烯酸酯低聚物是用丙烯酸酯封端的聚氨酯低聚物。聚氨酯低聚物是基于双官能多元醇和双官能异氰酸酯或基于双官能多硫醇和双官能异氰酸酯。聚氨酯低聚物可以是双官能多元醇和双官能异氰酸酯的催化反应的产物,或者是双官能多硫醇和双官能异氰酸酯的催化反应的产物。所述方法包括向所述配方施加光以固化所注射的聚氨酯丙烯酸酯低聚物,其中双官能多元醇或双官能多硫醇经选择以影响抛光层的性质,并且其中双官能多元醇或双官能多硫醇可另外地经选择以降低配方的黏度。该性质可以是伸长率、UTS或储能模量。影响性质可以是满足该性质的最小值。影响性质可以是满足该性质的指定数值范围。
已经描述了多个实现方式。然而,将理解,可在不背离本公开内容的精神和范围的情况下做出各种修改。例如,抛光垫或承载头或两者可移动以提供抛光表面与基板之间的相对运动。抛光垫可以是圆形的或一些其他形状。粘合剂层可被施加到抛光垫的底表面以将垫固定到压板,并且在抛光垫被放置在压板上之前,粘合剂层可以被可移除衬里覆盖。另外,尽管使用了竖直定位的术语,但是应当理解,抛光表面和基板可保持倒置、保持在竖直取向上或保持在一些其他取向上。因此,其他实现方式在所附权利要求书的范围内。
Claims (15)
1.一种用于合成用于抛光垫的增材制造的聚氨酯丙烯酸酯低聚物的方法,包括:
选择双官能多元醇或双官能多硫醇以影响所述抛光垫的抛光层的性质;
执行所述双官能多元醇或所述双官能多硫醇与双官能异氰酸酯的催化反应,以得到聚氨酯低聚物;和
用丙烯酸酯将所述聚氨酯低聚物封端,以得到所述聚氨酯丙烯酸酯低聚物,其中在所述增材制造中所应用的所述聚氨酯丙烯酸酯低聚物影响所述性质。
2.如权利要求1所述的方法,其中所述聚氨酯低聚物包括预聚物,并且其中所述聚氨酯丙烯酸酯低聚物包括紫外线(UV)可固化低聚物。
3.如权利要求1所述的方法,其中所述性质包括断裂伸长率、极限抗拉强度(UTS)、储能模量、玻璃化转变温度或熔点,或者它们的任何组合。
4.如权利要求1所述的方法,其中所述双官能多元醇包括半结晶聚酯、聚碳酸酯或聚乙烯。
5.如权利要求1所述的方法,其中所述双官能异氰酸酯包括二异氰酸酯。
7.如权利要求1所述的方法,其中所述催化反应中的催化剂包括二月桂酸二丁基锡(DBTDL),并且其中所述催化反应包括聚合。
8.如权利要求1所述的方法,其中所述丙烯酸酯包括丙烯酸-2-羟乙酯。
9.如权利要求1所述的方法,其中影响所述性质包括增加所述抛光层的伸长性质、UTS或储能模量。
10.如权利要求1所述的方法,其中影响所述性质包括选择所述双官能多元醇或所述双官能多硫醇以满足所述性质的指定数值范围。
11.如权利要求1所述的方法,包括:将包括所述双官能多元醇的多个双官能多元醇与所述性质相关或将包括所述双官能多硫醇的多个双官能多硫醇与所述性质相关。
12.如权利要求1所述的方法,其中所应用的所述聚氨酯丙烯酸酯低聚物包括经受UV光以固化或交联所述聚氨酯丙烯酸酯低聚物的所述聚氨酯丙烯酸酯低聚物,或者其中所应用的所述聚氨酯丙烯酸酯低聚物包括经受光致聚合的所述聚氨酯丙烯酸酯低聚物。
13.如权利要求1所述的方法,其中选择所述双官能多元醇或所述双官能多硫醇进一步包括选择所述双官能多元醇或所述双官能多硫醇以实现以下一者或多者:降低包括所述聚氨酯丙烯酸酯低聚物的三维(3D)打印配方的黏度,满足包括所述聚氨酯丙烯酸酯低聚物的3D打印机配方的黏度的指定数值范围,或者使得包括所述聚氨酯丙烯酸酯低聚物的配方的黏度低于最大值。
14.如权利要求1所述的方法,其中在所述增材制造中通过3D打印机喷嘴所喷射的所述配方的所述黏度的所述最大值包括20厘泊(cP)。
15.一种用于合成用于抛光垫的增材制造的聚氨酯丙烯酸酯低聚物的方法,包括:
选择双官能多元醇或双官能多硫醇以影响在所述增材制造中具有所述聚氨酯丙烯酸酯低聚物的三维(3D)打印配方的黏度和影响所述抛光垫的抛光层的性质;
在催化剂的存在下使所述双官能多元醇或所述双官能多硫醇与双官能异氰酸酯反应,以得到聚氨酯低聚物预聚物;和
在所述聚氨酯低聚物预聚物上掺入丙烯酸酯作为封端物,以得到所述聚氨酯丙烯酸酯低聚物,其中在所述增材制造中的所述聚氨酯丙烯酸酯低聚物影响所述性质。
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US12006442B2 (en) | 2024-06-11 |
US20210071017A1 (en) | 2021-03-11 |
EP4028440A1 (en) | 2022-07-20 |
EP4028440A4 (en) | 2023-09-27 |
WO2021050761A1 (en) | 2021-03-18 |
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