CN103619778A - 陶瓷颗粒混合物，以及从这种混合物制备陶瓷部件的方法 - Google Patents
陶瓷颗粒混合物，以及从这种混合物制备陶瓷部件的方法 Download PDFInfo
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- CN103619778A CN103619778A CN201280030007.7A CN201280030007A CN103619778A CN 103619778 A CN103619778 A CN 103619778A CN 201280030007 A CN201280030007 A CN 201280030007A CN 103619778 A CN103619778 A CN 103619778A
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Abstract
本发明涉及陶瓷颗粒混合物，所述陶瓷颗粒混合物按重量计主要包含陶瓷材料制成的可烧结颗粒和至少一种添加剂的颗粒，所述至少一种添加剂是分散态吸收性无机固体材料，所述分散态吸收性无机固体材料对预定波长发射的激光束有比吸收度，所述比吸收度高于所述陶瓷混合物的其他组分的吸收度，并且在激光束存在下，所述分散态吸收性无机固体材料迅速降解，并放出气体，所述添加剂存在的比例是小于干重的5%。本发明也涉及从这种混合物生产的陶瓷部件。
Description
本发明涉及陶瓷颗粒混合物，所述陶瓷颗粒混合物按重量计主要包含陶瓷材料制成的可烧结颗粒和至少一种添加剂的颗粒，所述至少一种添加剂中的至少一种是无机固体材料。本发明也涉及基于这种陶瓷颗粒混合物的、处于生坯状态或者处于烧结状态的陶瓷坯件和陶瓷部件，以及从这种陶瓷混合物制备陶瓷部件的方法。
通过侵蚀的激光加工方法由Pham D.T.等描述在Laser milling（激光铣削）,Proclnstn Mech Engrs,卷216，B部分:J.Engineering Manufacture（工程加工杂志）,第657-667页(2002)。就加工而言，激光辐射通常在非常短的时期内递送到减损维度（reduced dimension）的表面。这造成了极高的峰值功率密度(1012W/m2)，这造成了经辐照材料中的一系列的转变。
能以这种方法获得所述材料的熔融和蒸发，这造成局部的加工微腔。逐渐造成了一系列的这种空腔(特别是由于检流计的偏转器（deflector）或电动轴的移动)，使其可构建表面的形貌并且逐步重新生成复杂的形状。然而，这种名为“激光铣削”的为人所熟知的方法有很多缺点：
-为了使所述方法有效，所述材料对激光束波长必需有吸收性，这需要激光源适应要加工的材料。
-加工时间会非常长久(数十小时)，并且对于小体积或有限体积的消除材料(例如数十mm3)也是如此。
-部件中光束产生的热造成了"热影响区域"，在所述区域对所述材料的性质造成局部损坏(形成玻璃相、开裂、生成不需要的新相等)。这方面对于陶瓷材料特别重要，认为所述陶瓷材料非常脆弱，并且例如生成裂纹对其机械稳定性方面而言特别有害。
由于这些局限，这种方法经常只用于生产单个组分并且是非常小的数量(压制模具、构建模具等)。
在专利申请WO2006/079459中，描述了一种从材料流或例如激光的能量流来加工生坯体的方法。提出的加工是在生坯陶瓷或由通过有机粘合剂粘合把颗粒组装在一起构成的金属部件上进行的。生坯部件的成形是由传统粉末冶金法进行，所述方法也由陶瓷技师使用并且在文献中有广泛记载(压制、挤压等)。粘合剂的掺入（incorporation）同样为现有技术已知，这能提高颗粒组装的内聚性。通过由于能量流或材料流对生坯物体的连续切割或“剪接"来获得现有技术文献中所述的加工。
专利申请DE19501279公开了使用UV脉冲激光以获得材料的选择性消除。
然而，这个文件强调了这个技术仅可能将材料少量除去，这是由于快速形成熔融材料层，所述熔融材料层再沉积在表面上。为了适应这个缺点，这个文件提供了液体存在下加工表面的方案，从而避免了这种除去的材料再沉积下来。
在A.Kruusing，Underwater and water-assisted laser processing（水下和水辅助的激光加工）:第1部分-general features,steam cleaning and shock processing（常见特性、蒸气清洁和冲击加工）Optics and Lasers in Engineering（光学和激光工程）41(2004),第307-327页中，也描述了在液体膜(经常是水)存在下使用激光表面加工。激光辐射期间，所述液体膜在局部剧烈受热，并且爆炸性地蒸发，从材料表面喷出矿渣和熔融颗粒。
在国际专利申请WO2010/055277中，将液体介质中的加工原理应用到生坯陶瓷或金属组分的示例中。所述加工在(由有机粘合剂粘合在一起的)金属或陶瓷的颗粒组装部件上进行，所述颗粒组装部件浸没在液体(水或醇)中，和/或其表面喷洒上这种液体。需要可变化的浸没时期(半小时到24小时)，从而使得所述液体通过开放孔隙侵入到生坯部件的核。
激光辐射期间，在生坯材料的表面，对所述材料中包含的液体发生了非常快速的加热。所述液体的极快蒸发(“爆炸性蒸发”)造成所述生坯部件结构的局部爆破。某些陶瓷材料(氧化铝和滑石)上成功实施了所述方法，但是不能用于加工例如堇青石。作者指出不是所有的陶瓷都适合这种类型的加工。另外，由于所述部件的分散加热会很快造成不希望的液体蒸发，所以加工深度仍然比较小(通常小于1mm)。持续这种加工需要把所述部件的重复地（renewed）浸没，或者将所述液体持续喷洒到要加工的表面。使用所述方法似乎特别繁琐，因为有至少三个原因：
溶剂的快速蒸发把加工深度限定在mm的程度。对某些陶瓷材料不能应用所述方法。因为由于所用液体会自然蒸发，应该避免中间存储，所以需要在组分出现后立即加工。
专利申请US2010/0032417中提到了就用于微电子装置中的“焊接垫”的脱模/清洁或者打孔而言，通过UV激光(波长小于400nm)进行生坯加工。一个实施方式提供了加工方法，所述方法通过使生坯团块（mass）中存在的有机粘合剂爆炸性蒸发来进行。高温下有机蒸气快速膨胀，并且通过材料出坯来把生坯材料局部降解。在这个文件中，能生坯加工的有机相是陶瓷技师熟知的粘合剂，所述粘合剂能确保颗粒相互之间的内聚性，并且增加所述部件的机械抗性。
在J.Gurauskis等，Laser drilling of Ni-YSZ Cements（Ni-YSZ水泥的激光打孔），Journal of the European Ceramic Society(欧洲陶瓷协会杂志)28(2008)，第2673-2680页，作者详细描述了生坯陶瓷部件的激光穿孔的过程。陶瓷材料的颗粒吸收了激光辐射，造成其温度的快速升高。然后热转移到所述有机粘合剂，所述粘合剂热解，生成气体喷射。气体爆炸将处理位点周围的材料带走。
在Kamran Imen等，Pulse CO2Laser Drilling of Green Alumina Ceramic（生坯氧化铝陶瓷的脉冲CO2激光打孔），IEEE Transactions on Advanced Packaging（IEEE先进封装学报），卷22，第4期，1999年11月中描述了相似的方法。此处在压力下接受激光辐射。
现有技术的这个检测显示了在由陶瓷颗粒混合物成形的生坯陶瓷部件的激光辐射的作用下，侵蚀造成的加工方法的情况中，总是出现陶瓷材料颗粒的快速加热。为了蒸发液体相（同时试图保护陶瓷材料免于过度加热），或者为了对所述陶瓷颗粒粘合在一起的有机粘合剂以气体喷射的形式进行热解，使用这种加热是有优势的。
所述陶瓷材料并不特别适合于吸收波长200nm－3μm的激光辐射。在这种波长范围内所述陶瓷材料（特别是氧化物类型）的吸收度通常比较普通（mediocre）。因此在这个范围内发射的任何激光辐射必需充分强力并持久，从而从所述陶瓷材料吸收的能量向液体相或向粘合剂的热量转移会产生这些相的爆炸性蒸发，并且撕裂材料。这造成了在控制不良的方法中有发生陶瓷颗粒的部分熔融的风险（这应该避免）和所述加工方法中的某些延缓。另外，在使用有机粘合剂聚合物的情况中，后者的缺点是热影响区域中不可控的蠕变和熔解。另外，在延伸超出3μm的波长范围(远红外)中，陶瓷材料的吸收度以及所述粘合剂的吸收度或所述液体相的吸收度要更高地多，这造成所述两种材料的合并加热，以及产生上述缺点。
也已知包含大量的结合的造孔（porogenic）剂的陶瓷混合物，其中之一可以由碳制成。这些混合物被成形并且焙烧，特别是为了生成处理车废气的多孔系统(见US2007/0006561)，并且其没有经过任何由激光处理进行的生坯加工。
本发明的目的是开发陶瓷颗粒混合物，所述混合物能对简单形状的陶瓷部件进行生坯加工，使其形成复杂形状。这种加工应该非常灵活（flexible）并且非常快速地进行，没有现有技术中处理的缺点。
根据本发明，通过使用例如开始时所述的陶瓷颗粒混合物能解决这些问题。在这种混合物中，所述无机固体材料对在预定波长发射预定能量流的激光辐射有吸收性，并且在这种预定波长下，所述无机固体材料的比吸收度（specific absorptivity）高于所述陶瓷混合物其他组分的比吸收度，并且所述陶瓷混合物包含小于干混合物的5重量%且大于0重量%的分散状态的吸收性无机固体材料颗粒，所述吸收性无机固体材料颗粒在所述激光辐射存在下能够迅速降解，并放出气体。
因此在将这种陶瓷颗粒混合物接受上述激光辐射的情况下，所述混合物并非是能直接吸收或优先吸收所述能量流的陶瓷材料的可烧结颗粒，而是能直接吸收或优先吸收所述能量流的矿物添加剂颗粒，所述矿物添加剂颗粒下文称为分散态吸收性固体材料（法文缩写MSDA）。由所述激光辐射接触的这些颗粒能在极短时间（特别是短于1微秒）内以气体形式降解。特别地，纳秒类型的脉冲激光(脉冲持续低于150ns)非常适合于这个目的，所述纳秒类型的脉冲激光在1μm附近发射并且有平均功率(通常平均功率5－100W)。因此，避免了陶瓷材料周围（即使是局部）的任何不合时宜加热的风险，并且所述加工时间会是非常短暂的。
吸收系数A或吸收度是决定电磁辐射和受其影响的表面之间相关作用的基本特性。用下式表示：
A=1-R
其中，R是受辐射材料表面的反射率。
这个无单位量取决于入射辐射的波长。其在0(没有吸收)到1(完全吸收)之间。(见：Ready J.F.(编)，LIA handbook of laser materials processing（LIA激光材料加工手册），Laser Institute of America（美国激光研究所），木兰出版公司（Magnolia PublishingInc.），2001，以及Oliveira C.等，Etude de l'absorption du rayonnement IR en vue dutraitement laser d'alliages ferreux（对用于铁合金激光处理的辐射IR的吸收性的研究），J.Phys.III France（法国），2(1992),2203-2223)。
通过掺入质量分数小于干混合物5重量%的MSDA，从而确保两个目标：如上述的有效加工，以及尽可能地将要加工的部件完全致密化，优选是100%的理论密度。
优选，如本发明的陶瓷颗粒混合物中，相对于其他组分，分散态吸收性无机固体材料有激光辐射的吸收度差异，所述差异大于0.2，优选等于或大于0.4，优选等于或大于0.5。优选，所述分散态吸收性固体材料是非粘性(non-binding)的材料。应该注意到本发明所述的陶瓷颗粒混合物能包含对陶瓷材料颗粒而言作为另一种添加剂的至少一种粘合剂。可以考虑本领域已知的任何类型的粘合剂，特别是无机粘合剂，其可以是分布在陶瓷材料的可烧结颗粒之间的、本身具有粘性的颗粒的形式，或者是这些颗粒的涂层的形式。根据本发明掺入到所述混合物的有机粘合剂的含量优选小于干混合物的5重量%，特别小于3重量%。
根据本发明的一个实施方式，所述分散态吸收性固体材料在没有热压力和/或光学压力的条件下是稳定的。因此所述陶瓷颗粒混合物能在正常条件下存储而没有问题，特别是在环境温度和没有接受激光辐射的条件下。其能是粉末形式，优选完全干的粉末，或者是液体悬浮液介质中的颗粒悬浮液形式，所述液体悬浮液介质是例如水性介质（如水）。优选MSDA在高于400℃的受控制的热条件下可以全部降解。因此在对由陶瓷颗粒混合物成形的陶瓷部件进行生坯加工之后，在烧结所述部件的步骤之前，可将任何痕量的所述分散态吸收性无机固体材料全部除去。
根据本发明，所述分散态吸收性无机固体材料可以全部或至少部分是碳。优选碳可以选自石墨、无烟煤、炭黑、活性炭、碳纳米管、石墨烯箔和其混合物。也可以考虑充满碳分散体的有机相，例如石墨或炭黑。
就生坯陶瓷部件加工而选择的MSDA是碳及其衍生物。碳在可用于现代激光源的宽范围频率(特别是200nm－3μm)内有高吸收系数或高吸收度。在脉冲模式中辐射，碳剧烈降解，并放出气体，其使得生坯材料周围的结构发生爆炸，造成陶瓷材料的颗粒出坯。由于其使得所述生坯材料具备极好的均匀性，优选微米或亚微米大小(d90<5μm，优选<1μm)的碳分散体。通常，不考虑分散的MSDA的性质，其粒度越小，所述生坯材料可以达到的均匀性就越小并且越好。有更小粒度的分散体时，有效生坯加工所需的碳的数量也更小。
碳的优点是在延伸的波长范围(从UV到远IR)内能极好地吸收激光能量，并且因此与纳秒类型脉冲激光的加工兼容，所述纳秒类型脉冲激光例如准分子、Nd:YAG、Nd:YVO4或者纤维激光等。在200nm－3μm的波长范围内，碳的吸收系数值超过值0.7。
优选所述陶瓷材料的可烧结颗粒全部或至少部分是氧化物类型的陶瓷材料。特别地，可以列举出的陶瓷材料有氧化铝、锆石、二氧化硅、氧化镁、氧化锌、氧化钛、混合的氧化物如PZT、钛酸钡、硅酸盐、羟基磷灰石、磷酸三钙及其混合物。
优选所述陶瓷材料的可烧结材料的粒度可以是微米或亚微米的级别。
根据本发明，掺入到所述陶瓷颗粒混合物的MSDA质量分数可以优选是干混合物的1重量%－3重量%之间。
本发明也涉及基于本发明的陶瓷颗粒混合物的生坯状态加工的陶瓷坯件和陶瓷部件。其也涉及根据本发明将生坯状态加工的陶瓷部件进行烧结之后，获得的经烧结的陶瓷部件。本发明也涉及根据本发明，从陶瓷颗粒混合物中制备生坯状态和经烧结状态的陶瓷部件的方法。
根据本发明加工的陶瓷部件可以特别是某种组件，所述组件用于电子、电机械器件、生物医药领域(假牙、骨替代品等)、制备挤压模头、珠宝、精密机械、过滤、催化支持物等。
根据本发明，这种方法包含使用陶瓷颗粒混合物，根据本发明所述陶瓷颗粒混合物按重量计主要包含陶瓷材料的可烧结颗粒和至少一种添加剂的颗粒，所述至少一种添加剂中的至少一种是无机固体材料。
在根据本发明的所述方法中，所述无机固体材料对在预定波长发射预定能量流的激光辐射是有吸收性，并且在这种波长下，所述无机固体材料的比吸收度（specificabsorptivity）高于所述陶瓷混合物其他组分的比吸收度，并且所述陶瓷混合物包含小于干混合物的5重量%且大于0重量%的分散状态的吸收性无机固体材料颗粒。根据本发明所述的方法还包括：
-由所述陶瓷混合物经生坯成形获得干的生坯陶瓷坯件，
-对所述生坯陶瓷坯件进行生坯加工，所述生坯加工通过将所述陶瓷材料接受在预定波长发射预定能量流的所述脉冲激光辐射来除去所述陶瓷材料来进行，和
-在接受这种激光辐射期间，选择性地使得分散态的吸收性固体材料颗粒吸收激光辐射能量，所述分散态的吸收性固体材料颗粒迅速降解并放出气体，所述生坯陶瓷坯件的陶瓷材料发生局部脱位，脱位的陶瓷材料出坯，由此获得经加工的生坯状态的陶瓷部件。
为了生成所述陶瓷颗粒混合物，其组分，和因而其必要的陶瓷材料颗粒和分散态吸收性无机固体材料能通过干法混合，所述方法生成干粉末。也能通过液体方法使其混合，所述液体方法通过将组分置于悬浮液中进行。在这个情况中，能考虑使用已知方式在成形前将悬浮液中的混合物干燥从而同样获得用于成形的干粉末，所述方式例如在烘箱中、炉子中、通过冷冻干燥或雾化。
优选，所述生坯成形通过本领域技术人员已知的技术（例如挤压、浇铸或压制）来实现。在挤压或浇铸的情况中，以糊料或悬浮液的形式使用陶瓷混合物，并且在这个情况中，在成形后进行上述干燥步骤。在所有情况中，获得用于加工的干生坯陶瓷坯件。在将这种干生坯陶瓷坯件成形之后，所述生坯团块（mass）能易于通过激光来加工。所述激光辐射是脉冲的，并且可以来自UV、IR或可见光范围内的任何合适的激光源发射。优选激光辐射的波长是200nm－3μm，特别是900nm－1100nm。优选提供的脉冲持续时间小于150ns。当在氧化气氛存在下进行加工时，接受激光辐射的所述分散态吸收性固体材料能以气体形式受到氧化。在特定优选的方式中，可以在环境压力、在空气中进行加工。
所述方法也可以包括生坯加工之后，将所述生坯加工的陶瓷部件的陶瓷材料颗粒进行烧结。烧结温度取决于陶瓷材料颗粒的特性。
可以优选考虑在烧结之前，在这种材料的降解温度，通过对其施加热力将分散态吸收性固体材料从经生坯加工的陶瓷部件中除去。这种情况下，所述经烧结的陶瓷部件完全避免了MSDA，这与根据现有技术的经烧结的陶瓷部件相似，但是没有显示后者的缺点，例如微裂纹、玻璃材料的沉积等。现在在以下非限制性的实施例帮助下更详细地描述本发明。
附图2和5显示了根据本发明加工的烧结前的部件，图1、4和6显示了根据本发明加工的烧结后的部件，以及图3显示了没有MSDA的生坯加工部件。
实施例1
通过Nd:YVO4激光生坯加工细氧化铝
称量限定量的氧化铝(来自派奇尼公司(Pechiney)的P172SB)(100g)，并且置于中性pH的去矿物质水的悬浮液中(100g)。把1质量%的聚乙二醇PEG加入到所述悬浮液中(如1g)，从而作为有机粘合剂。把23.5g的胶体石墨的水性悬浮液(导电敷层(Aquadag)18%-艾奇逊工业有限公司(Acheson Industries Ltd))加入到氧化铝颗粒的悬浮液中，把所有成分混合30分钟，然后通过冷冻干燥或旋转蒸发仪进行干燥。因此，获得的干混合物包含相对于混合物总重量的4.2重量%的石墨。所述石墨颗粒的粒度d90<5μm，并且所述氧化铝颗粒的粒度是d50=0.4μm。
因此获得的混合粉末通过单轴压制(40MPa用于25mm直径的片状物(tablet))，然后通过均衡压坯后(170MPa，2分钟)成形。
获得的片状物形式的生坯坯件然后在环境压力下通过激光进行加工，所述激光来自Trumark市售标记站(Trumpf)，所述标记站装配有由Q-Switch提供的20W标称功率的固体Nd:YVO4激光，这使得激光能以脉冲模式工作，所述激光具有移动表格XY和检流计头，使得光束扫描（sweep）要加工的表面。163mm焦距的光学器件能获得45μm的点。根据参数研究获得的最优激光参数是标称功率的40%-80%、40-80kHz的工作频率、100-6000mm/s的扫描速度、1－5μs的脉冲间隔和8－17ns的脉冲持续时间。根据例如格式为.dxf的CAD文件进行加工。
所述激光发射的辐射波长是1.06μm。在这个波长下，氧化铝的吸收度是约0.1，而碳的吸收度高达约0.9。
图1显示烧结后获得的结果，揭示了加工中能精细打孔网格的可能性(孔直径100μm，间隔60μm)，所述网格能以1mm等级的深度进行，也揭示了非常深的加工的可能性，所述深度容易超过5mm。加工深度中确定的唯一的局限是孔宽度/深度的纵横比，其就使用的聚集光学器件而言接近1/10。记录的除去材料的速率是每分钟10－100mm3的级别。加工的生坯部件然后在空气中按照下面两个步骤进行热处理：第一个步骤涉及全部除去所述部件中残留的碳；第二个步骤涉及烧结氧化铝。热处理循环包括在600℃(上升速率5℃/分钟)下1小时的阶段，然后是在1550℃(上升速率5℃/分钟)下1小时的阶段，和最后降低到环境温度(以5℃/分钟)，这使得能获得极好的致密部件，避免了可见的缺陷(孔或裂纹)。在扫描电子显微镜下观察到的经加工的表面显示了没有裂纹、没有孔隙、也没有任何再沉积的熔融材料层。
在用这种氧化铝对有或没有MSDA的生坯坯件进行类似的比较测试。根据本发明加工的生坯坯件示于图2。其空腔边缘干净，并且所述空腔的底部极为清洁。所述坯件的浅灰色是由存在作为MSDA的石墨造成。在将所述石墨烧结和降解之后，所述部件的颜色会与图1坯件获得的颜色一致。没有MSDA的生坯坯件揭示了实现生坯加工(见图3)的可能性。然而，然后需要的峰值功率要高于对有MSDA的生坯加工提供的峰值功率(通常>标称功率的60－80%)。另外，除去材料的速率比存在MSDA下获得的速率低得多(最小降低到1/3)。同样，能加工的深度明显下降，并且无法超过2mm：在光束提供的能量的作用下，氧化铝颗粒很快开始烧结，或甚至熔融，这中止了生坯加工过程。有光束辐射的区域中的氧化铝颗粒发生浅表蒸发，造成压力使得所述结构局部爆炸，这解释了没有MSDA情况下的生坯加工情况。
实施例2
通过Nd:YVO4激光生坯加工细锆石
与前一实施例使用的氧化铝P172不同，对压制的锆石片状物进行生坯加工的测试(东曹公司(Tosoh)Y-TZP)揭示了没有MSDA而进行加工的可能性。
通过掺入石墨类型的MSDA来加工锆石。
实现生坯加工的配方与氧化铝类似：100g锆石(d50=200nm)分散在100g去矿物质水中，所述水预先溶解了1g的PEG2000。然后14g导电敷层(d90<5μm)加入到悬浮液中，再将全部混合物在研磨介质存在下均化30分钟。所述悬浮液然后通过冷冻干燥或者旋转蒸发仪干燥，产生相对于干混合物2.4重量%的碳。所得的粉末在40MPa单轴压力下，以25mm直径的片状物形式压制，然后所述片状物在175MPa下均衡压坯。
所得的生坯片状物然后通过激光加工，所述激光来自前面实施例中相同的标记站。根据参数研究获得的最优激光参数与氧化铝相似，其为标称功率的40%－80%、40－80kHz的工作频率、100－6000mm/s的扫描速度、1－5μs的脉冲间隔和8－17ns的脉冲持续时间。根据例如格式为.dxf的CAD文件进行加工。
在波长1.06μm的激光辐射下，锆石的吸收度是0.2，同时石墨的吸收度是0.9的级别。
再次，能记录下非常高的除去材料的速率(>50mm3/分钟)，深度为数个mm。
同样，在这个情况中，注意到除了加工区域的纵横比之外，没有明显的关于深度的局限。施行了数种加工模式，涉及到生成精细和/或粗糙的细节。证明了所述加工精度是焦距处激光束大小的级别。
在空气中消除残留的碳和经加工部件的自然烧结之后，没有注意到明显的缺陷。。
在扫描电子显微镜下观察到的经加工的表面显示了没有裂纹、没有孔隙、也没有任何再沉积的熔融材料层。
某些未处理的片状物在空气中存储数天，然后加工。注意到加工中其表现与初始片状物相同－这证明了所述片状物没有老化。另一方面，就长时间存储压制部件而言，所述部件可以置于有干燥剂的气密空间中，从而避免其受到环境空气的湿润。
实施例3
通过3D激光生坯加工细氧化铝
根据实施例1中所示方法，制备来自派奇尼公司(Pechiney)的细氧化铝P172SB的混合粉末，所述粉末包含10体积%(或约4重量%)的碳(导电敷层)。25mm直径的片状物通过加载40MPa的单轴压力来压制。这些片状物然后用纳秒类型的脉冲Nd:YAG激光进行处理，所述激光设置有检流计头和5个电动轴(3个笛卡尔（cartesian）轴和2个可旋转轴)。将辐射微涡轮的CAD方案（plan）进行修改，并且所述对象通过使用实施例1详述的参数进行微加工来再生产。各涡轮叶片相继由所述片状物的连续旋转来生成。在这个示例中，微涡轮的加工时间是20分钟的级别。根据实施例1的方法来实现消除石墨和烧结对象。
所得结果示于图4，图4显示了消除MSDA和烧结之后，经加工的微涡轮。所得对象没有明显的缺陷(裂纹、孔隙等)，并且烧结之后的部件是完全致密的。
实施例4
3D生坯激光加工锆石
根据实施例2的方法获得的压制片状物逐层地进行加工，各层对应特定的加工方案。图5显示的金字塔形状的加工花费了20分钟。在字母Z和E下面方尖碑形状（obelisk）顶部的截面是50μm级别，勉强多于焦距处光束的大小。
图6显示了消除MSDA和烧结之后，经加工的片状物。可以看到，烧结之后，注意到所述部件没有几何结构扭曲。所述经加工的金字塔以及方尖碑形状（obelisk）保持完整，并且没有明显的缺陷。
应该理解本发明不以任何方式限制上述实施方式，并且在所附权利要求范围内可以进行修改。
Claims (27)
1.一种陶瓷颗粒混合物，所述陶瓷颗粒混合物按重量计主要包含陶瓷材料的可烧结颗粒和至少一种添加剂的颗粒，所述至少一种添加剂中的至少一种是无机固体材料，其特征在于，对在预定波长发射预定能量流的激光辐射有吸收性，并且在这种预定波长下其比吸收度高于所述陶瓷混合物其他组分的比吸收度，并且所述陶瓷混合物包含小于干混合物的5重量%且大于0重量%的处于分散状态下的所述吸收性无机固体材料颗粒，所述吸收性无机固体材料颗粒在所述激光辐射的存在下能够迅速降解，并放出气体。
2.如权利要求1所述的陶瓷颗粒混合物，其特征在于，相对于其他组分，所述分散态吸收性无机固体材料有激光辐射的吸收度差异，所述差异大于0.2，优选等于或大于0.4，优选等于或大于0.5。
3.如权利要求1或2所述的陶瓷混合物，其特征在于，所述分散态吸收性无机固体材料是非粘性的材料。
4.如权利要求1-3中任一项所述的陶瓷混合物，其特征在于，所述分散态吸收性无机固体材料在没有热压力和/或光学压力的条件下是稳定的。
5.如权利要求1-4中任一项所述的陶瓷混合物，其特征在于，所述分散态吸收性无机固体材料在高于400℃的受控制的热条件下可全部降解的。
6.如权利要求1-5中任一项所述的陶瓷混合物，其特征在于，所述陶瓷混合物包含的其他添加剂是至少一种陶瓷材料颗粒的粘合剂，其比例是小于干混合物的5重量%且大于0重量%。
7.如权利要求1-6中任一项所述的陶瓷混合物，其特征在于，所述分散态吸收性无机固体材料至少部分是碳。
8.如权利要求7所述的陶瓷混合物，其特征在于，所使用的碳优先选自石墨、无烟煤、炭黑、活性炭、碳纳米管、石墨烯箔及其混合物。
9.如权利要求1-8中任一项所述的陶瓷混合物，其特征在于，所述陶瓷材料的可烧结颗粒至少部分是氧化物类型的陶瓷材料。
10.如权利要求1-9中任一项所述的陶瓷混合物，其特征在于，所述陶瓷材料选自氧化铝、锆石、二氧化硅、氧化镁、氧化锌、氧化钛、混合的氧化物、钛酸钡、硅酸盐、羟基磷灰石、磷酸三钙及其混合物。
11.如权利要求1-10中任一项所述的陶瓷混合物，其特征在于，所述陶瓷混合物是粉末形式。
12.如权利要求1-10中任一项所述的陶瓷混合物，其特征在于，所述陶瓷混合物是所述颗粒在液体悬浮液介质中的悬浮液形式。
13.如权利要求1-12中任一项所述的陶瓷混合物，其特征在于，所述分散态吸收性无机固体材料颗粒的d90粒度小于5μm。
14.如权利要求1-13中任一项所述的陶瓷混合物，其特征在于，所述陶瓷材料颗粒的粒度是微米或亚微米。
15.经成形的生坯状态的陶瓷坯件，所述陶瓷坯件是基于如权利要求1-14中任一项所述的陶瓷混合物。
16.经加工的生坯状态的陶瓷坯件，所述陶瓷坯件是基于如权利要求1-14中任一项所述的陶瓷混合物。
17.经加工的陶瓷部件，所述陶瓷部件是如权利要求16所述的陶瓷部件的经烧结的状态。
18.一种制造陶瓷部件的方法，所述方法包括以下步骤：
-使用陶瓷颗粒混合物，所述陶瓷颗粒混合物按重量计主要包含陶瓷材料的可烧结颗粒和至少一种添加剂的颗粒，所述至少一种添加剂中的至少一种是无机固体材料，
其特征在于，所述无机固体材料对在预定波长发射预定能量流的激光辐射有吸收性，并且在所述波长下，所述无机固体材料的比吸收度高于所述陶瓷混合物其他组分的比吸收度，以及所述陶瓷混合物包含小于干混合物的5重量%且大于0重量%的处于分散状态下的所述吸收性无机固体材料颗粒，并且所述方法还包括
-由所述陶瓷混合物经生坯成形获得干的生坯陶瓷坯件，
-对所述生坯陶瓷坯件进行生坯加工，所述生坯加工通过将所述陶瓷材料接受脉冲激光辐射来除去所述陶瓷材料来进行，所述脉冲激光辐射在预定波长发射预定能量流，和
-在接受所述激光辐射期间，选择性地使得分散态的吸收性固体材料颗粒吸收激光辐射能量，所述分散态的吸收性固体材料颗粒迅速降解并放出气体，陶瓷材料从生坯陶瓷坯件发生局部脱位，脱位的陶瓷材料出胚，由此获得经加工的生坯状态的陶瓷部件。
19.如权利要求18所述的方法，其特征在于，所述组分的颗粒通过干法混合，形成粉末。
20.如权利要求18所述的方法，其特征在于，所述方法包括将所述组分的颗粒置于液体悬浮液介质中，形成悬浮液。
21.如权利要求18-20中任一项所述的方法，其特征在于，所述生坯成形是通过对使用的陶瓷混合物挤压、浇铸或压制来实现。
22.如权利要求18-21中任一项所述的方法，其特征在于，所述脉冲激光辐射的波长是200nm－3μm。
23.如权利要求22所述的方法，其特征在于，所述脉冲激光辐射的波长是900nm－1100nm。
24.如权利要求18-23中任一项所述的方法，其特征在于，所述脉冲激光辐射的脉冲持续时间小于150ns。
25.如权利要求18-24中任一项所述的方法，其特征在于，所述方法还包括在生坯加工之后，对经生坯加工的陶瓷部件的陶瓷材料颗粒进行烧结。
26.如权利要求25所述的方法，其特征在于，所述方法包括烧结之前，在分散态吸收性固体材料的降解温度，通过对其施加热力将分散态吸收性固体材料从经生坯加工的陶瓷部件中除去。
27.如权利要求18-26中任一项所述的方法，其特征在于，所述生坯加工在环境压力、在空气下进行。
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| US20140179511A1 (en) | 2014-06-26 |
| WO2012164025A1 (fr) | 2012-12-06 |
| EA024987B1 (ru) | 2016-11-30 |
| AU2012264687B2 (en) | 2016-05-26 |
| EA201391654A1 (ru) | 2014-03-31 |
| CN103619778B (zh) | 2016-06-15 |
| IL229731A0 (en) | 2014-01-30 |
| CA2837659A1 (en) | 2012-12-06 |
| EP2714621B1 (fr) | 2018-11-14 |
| BR112013030870A2 (pt) | 2017-02-21 |
| ZA201309615B (en) | 2015-04-29 |
| JP6149332B2 (ja) | 2017-06-21 |
| EA024987B8 (ru) | 2017-03-31 |
| KR20140046422A (ko) | 2014-04-18 |
| EP2714621B8 (fr) | 2019-03-06 |
| CH706791B1 (fr) | 2016-10-31 |
| US9115034B2 (en) | 2015-08-25 |
| MX2013014073A (es) | 2014-03-21 |
| AU2012264687A1 (en) | 2014-01-16 |
| JP2014516000A (ja) | 2014-07-07 |
| EP2714621A1 (fr) | 2014-04-09 |
| NZ618857A (en) | 2016-03-31 |
| KR101935446B1 (ko) | 2019-01-04 |
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