CN1856590A - 金属蒸发容器及其制造方法 - Google Patents

金属蒸发容器及其制造方法 Download PDF

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CN1856590A
CN1856590A CNA2004800275653A CN200480027565A CN1856590A CN 1856590 A CN1856590 A CN 1856590A CN A2004800275653 A CNA2004800275653 A CN A2004800275653A CN 200480027565 A CN200480027565 A CN 200480027565A CN 1856590 A CN1856590 A CN 1856590A
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weight
oxide
boat
nitride
compound
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D·M·小鲁辛科
A·萨恩
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General Electric Co
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General Electric Co
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Abstract

一种用于蒸发金属的耐火容器，具有显著提高的使用寿命和抗腐蚀性能，所述容器主要由耐火硼化物、氮化硼和约0.10－10重量％的选自氧化物、碳化物、氮化物和其混合物的稀土金属化合物构成。

Description

金属蒸发容器及其制造方法
              相关申请相互参照
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                  发明领域
本发明涉及一种改进的金属真空蒸发容器。
                  发明背景
真空沉积是一种常用的在金属、玻璃和塑料等各种基板上涂覆金属如铝、铜、锌和锡的方法。金属一般在本领域中通称为″舟″或涂覆金属舟的金属或陶瓷容器或器皿中借助于电阻加热被蒸发。舟被连接到真空室内的电源上并被加热到足以导致放入的与舟接触的金属装料蒸发的受控工作温度。
在真空涂覆金属工艺中，涂覆金属舟中的金属熔体被加热到一个非常高的温度，在很多情况下被加热到高于通常在浇铸操作中所遇到的温度，高达1200℃和1200℃之上。这意味着所述金属熔体即铝熔体的腐蚀性将更强并将相当于腐蚀性酸，缩短涂覆金属舟的寿命。
除了涂覆金属条件之外，影响舟寿命的一个因素是舟表面的润湿性。如果舟表面对熔融金属是基本上不可润湿的，则由于较小的蒸发表面积，蒸发单位量的铝将需要更高的舟温度。更高的工作温度将从而导致更高的腐蚀速率，从而缩短舟的使用寿命。除舟表面的润湿性之外，对更长的/有效舟寿命来说另一个重要因素是在舟凹槽内积累的熔渣的润湿性。在几个小时的金属涂覆操作之后，围绕舟内的金属熔池边缘开始有熔渣积累。熔渣是熔融金属与耐火舟反应的副产物。熔渣对涂覆金属一般不润湿并能阻止金属熔池扩展，由此提高工作温度并进一步缩短舟的使用寿命。舟和/或熔渣表面的改进的润湿性被认为是提高涂覆金属舟平均寿命的一个重要因素。
还有一个对更长和有效的舟寿命来说非常重要的性能/因素；就是舟的抗热降解能力。如果舟的工作温度超过某一临界值例如超过1600℃，舟将会热分解，使得熔融金属渗入舟内从而缩短舟的使用寿命。当线材没有均匀地输送到舟表面上时通常就会发生这种现象，导致在舟内部产生局部的热点。
在现有技术的范围内，涂覆金属舟的平均寿命大约为10小时，根据涂覆金属条件的不同能提供从约600000英尺的敷金属基板到约1000,000英尺的基板。人们一直试图使用各种耐火舟组成来提高涂覆金属舟的使用寿命。美国专利4528120公开了一种舟，它包含10-60重量％的氮化硼(“BN”)、0-60％的氮化铝与氮化硅中的至少一种、和30-70重量％的选自钛、锆、铝和铬的硼化物以及硅、钛和铬的碳化合物中的至少一种。公布号JP 06-298566公开了一种组成，它包括0.3-10重量％的碱土金属氧化物、稀土氧化物或碱土金属硼酸盐，15-50重量％的BN，和余量的比例为1∶1.5到1∶4的氮化铝与二硼化钛。
Montgomery的专利US 5604164中公开了“通过向二硼化钛和氮化硼的陶瓷复合材料组成中添加一种单质金属如钼和一种氧化物添加剂如Y2O3，可以大大改进舟的性能，特别是其润湿特性，并降低舟凹槽被铝腐蚀的速率”，Montgomery公开了一种主要由二硼化钛；氮化硼；至少3重量％的选自Mo、W、Ta和Nb的金属；以及至少0.7重量％的选自CaO和Y2O3的氧化物构成的耐火舟。
现在仍存在对提高涂覆金属舟的使用寿命的需要。申请人意外发现，一种具有改进的性能包括改进的抗热降解性、润湿性和耐腐蚀性的耐火舟组成能提供更长的使用寿命。在一个实施方案中所述令人吃惊的改进的耐火舟组成显示出以下性能：a)舟表面的较少腐蚀；b)更高程度的抗热降解性；c)润湿性更好的舟表面；和d)润湿性更好的熔渣，而不要求在组成中掺杂至少3重量％的金属元素Mo、Ta、W和/或Nb。
                      发明概述
一种用于蒸发金属的耐火容器，它主要由耐火硼化物、氮化硼和约0.10-10重量％的选自氧化物、碳化物、氮化物或其混合物的稀土金属化合物构成。在本发明的一个实施方案中，所述稀土金属化合物主要由氧化钇构成。
本发明还涉及制造用于蒸发金属的耐火容器的方法，该方法的步骤包括：a)形成一种均匀粉末混合物，其组成主要由耐火硼化物、氮化硼和约0.10-10重量％的选自氧化物、碳化物、氮化物或其混合物的稀土金属化合物构成；b)形成密度为粉末混合物理论密度的至少50％的生坯；d)在足够高的温度和压力下加热生坯，形成至少为理论密度的约85％的致密坯；和e)冷却并回收坯。
                      发明详述
在本文中，“主要由...组成”的表达方式容许包含不会显著影响所考虑的耐火组成的基本特性和新特性的物质。
本发明耐火舟的组成
在本发明的一个实施方案中，耐火组合物主要由耐火硼化物、氮化硼和约0.10-10重量％的选自氧化物、碳化物、氮化物或其混合物的稀土金属化合物构成。
稀土金属的例子包括但不限于钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱和镥。稀土金属氧化物的例子包括但不限于氧化钇、氧化镧、二氧化铈、氧化镨、氧化钕、氧化钐、氧化铕、氧化钆、氧化铽、氧化镝、氧化钬、氧化铒、氧化铥、氧化镱和氧化镥。
在本发明的一个实施方案中，耐火组合物主要由约35-65重量％的耐火硼化物、45-65重量％的氮化硼和约0.10-10重量％的包括稀土金属氧化物的稀土金属化合物构成。在一个实施例中，所述包括稀土金属氧化物的稀土金属化合物的量在组合物的0.10-7重量％的范围的。
所述耐火硼化物的例子包括但不限于耐火硬金属如Ta、Zr和过渡金属如Ti的硼化物，例如二硼化钛、二硼化锆或其混合物。
在本发明的第二实施方案中，组合物内进一步包括小于约10重量％的平均粒度为约15微米或更小的氮化铝或氮化硅粉末。在一个实施例中，氮化铝或氮化硅的量小于5％。在另一实施例中，其小于3％。
在本发明的第三实施方案中，组合物内进一步包括氧化钙或氧化铝和/或这些氧化物与稀土氧化物的化合物，其中氧化物的总含量小于10重量％。
在本发明的第四实施方案中，组合物内进一步包括0.2-5重量％的选自元素Al、Si、Ti、Fe、Co、Ni的碳化物和氮化物及其混合物的元素或化合物。
在本发明的第五实施方案中，不是含有稀土金属氧化物，或者是除稀土金属氧化物之外，在起始组成中包含了一种稀土金属氮化物例如氮化钇，使得所述氮化物在对含稀土金属氧化物的耐火舟的热压处理中被部分或完全转化成氧化物。
在本发明的第六实施方案中，不是含有稀土金属氧化物，或者是除含有稀土金属氧化物之外，在起始组成中包含了一种稀土金属碳化物例如碳化镧，用于在热压处理中部分或完全转化成稀土金属氧化物或氧化物复合物。
在本发明的另一实施方案中，氮化硼粉末组分具有约2-40m2/g(通过本领域已知的BET法测得)的比表面积且纯度为至少96重量％。96％的纯度是指通过分析所发现的硼和氮的总量为至少96重量％；粘附的氧化硼和氮氧化硼形式的氧的含量可以高达3.8重量％；并且在组成中可以存在总量达约0.1重量％的碳和0.5重量％的金属杂质。
在一个实施方案中，发射光谱分析表明二硼化钛粉末组分中基本上没有不期望的金属杂质，即该粉末基本上是纯的。如果存在金属杂质(如单质金属)，其含量通常小于5000份每百万份硼化物粉末(ppm)，即小于TiB2总重的0.5重量％，其中所述金属杂质包括但不限于铝、钡、钙、铬、钴、铜、铁、钾、锂、镁、锰、钠、镍、硅、钒、钨和锌。硼化物粉末产品中的这些金属杂质(如果存在的话)的来源通常是用于制备所述产品的反应物或设备。还可能存在最高达1重量％的选自元素钛和硼的氧化物、碳化物和氮化物的杂质。
在本发明的一个实施方案中，稀土金属化合物是氧化钇或氧化镧。在实施例中，申请人意外发现主要由氧化钇Y2O3构成的钇化合物能提高耐火舟和其中形成的熔渣的润湿性，使涂覆金属舟具有显著提高的有效寿命。
在一个实施方案中，其中稀土金属氧化物是氧化钇，所述三氧化二钇或氧化钇组分的纯度为至少95％且平均粒度为约15微米或更小。
在另一个实施方案中，包括CaO、MgO、Al2O3、TiO2、这些氧化物和稀土氧化物的化合物在内的任选的氧化物可以与稀土金属氧化物例如Y2O3以约0.10-10重量％的总量结合使用。稀土氧化物的化合物的例子包括YAG(Al5Y3O12)、YAP(AlYO3)和YAM(Al2Y4O7)。
在一个实施方案中，任选的金属氧化物的总量为约0.75-5重量％。在另一个实施方案中，所述量为约1-3重量％。
制造涂覆金属舟的方法
在一个实施方案中，通过使用混合工具提供均匀混合物例如通过高剪切混合、球磨、立式球磨、喷射研磨等等制备了BN、TiB2、稀土金属氧化物粉末和任选的AIN和/或CaO、Al2O3和TiO2的粉末混合物。混合可以在湿润或干燥条件下完成，例如在空气中、在惰性气体如氩气或氮气下、或者在水或有机溶剂如丙酮、甲醇或异丙醇中。然后通过模具如干压模、冷等静压机(CIP)模、注射模等等将混合物粉末模压以获得压坯。
随后，在非氧化气氛如真空、惰性气体气氛例如氮气和氩气、或还原性气氛例如氢气中，通过利用某种烧结方式如大气压烧结、真空烧结、气氛加压烧结、热压烧结或热等静压(HIP)烧结将压坯烧结至理论密度的至少85％。所述非氧化气氛是为了防止非氧化陶瓷粉末氧化。HIP烧结的步骤通常包括将压坯密封到金属或玻璃密封舱中，然后将密封舱保持在热等静压力下。在一个实施例中，致密化温度在约1300-2100℃的范围内，且外加压力在大约5-300MPa的范围内。
由烧结工艺可以获得密度为材料理论密度(TD)的至少约85-98％的致密化坯段。所述密度取决于工艺中所用的压力、温度和停留时间。由致密化的坯段可以在任何期望的方向上机械加工出蒸发舟。
                      实施例
这里所提供的实施例是用于说明本发明的，而非用于限制本发明的范围。
实施例1-5：
在实施例1-5中，具有以下分析的粉末被用作起始材料，其中稀土金属氧化物为Y2O3。实施例5包括Montgomery的参考文献中的等级Mo-21P，因此包括“Montgomery”实施例。
表1
实施例 ％TD 组成(重量％)
BN TiB2 CaO Y2O3 Al2O3 Mo
1 90％ 53.9 45.0 1.1 - - -
2 87％ 52.3 46.4 0.32 0.37 0.56 -
3 85％ 52.0 46.4 0.16 1.09 0.29 -
4 84％ 52.1 46.4 0.13 0.68 0.64 -
5 86％ 44.6 44.6 - 5.41 - 5.42
在每个实施例中，包含各组分的粉末混合物在高剪切搅拌器中均匀干燥。然后粉末混合物被冷压形成直径2英寸高2-5英寸的圆柱形生坯。生坯被引入热压机中并在一种还原气氛中和氩气吹扫条件下于1450℃-2000℃被致密化。
由坯段切削出约100mm×20mm×6mm的蒸发舟，并形成约60mm×15mm×2mm的凹陷或凹槽。不管它们在坯段中的位置如何，由实施例1-5的组成制成的蒸发舟都具有为理论密度(TD)的84％-90％的密度和400-1200μohm×cm的比电阻。
对蒸发舟1-5的测试：
在下列的铝真空蒸发条件下测试由实施例1-5制造的蒸发舟。在真空室中通过直接通电对舟进行加热。通过由凹槽的一端附近供给的铝线连续提供铝，在舟的远端感生出一个热点。热点的最高温度为约1715-1781℃。
随着测试的进行，可以注意到铝完全浸透实施例5的舟(“Montgomery”舟)，在舟中心的下方形成裂缝。实施例1-4的铝渗透要少得多。30分钟之后，观察到Montgomery舟已经热破坏到裂缝可见的程度，相比之下本发明的舟(无金属掺杂)仍然可用。
实施例6-10：
重复实施例1-5，只不过改为使用纯度约95-99％的氧化镧粉末。实验结果与实施例1-5的结果相似，本发明的实施例只有很小的或与现有技术的Montgomery实施例相比少得多的铝渗透。
实施例11-19：
在这些实施例中，形成包含表2所列组成的坯段，然后测量导电性以及进行润湿性测试。表2中的所有组分都是以重量％表示的。
所述坯段是通过在高剪切搅拌器中均匀干燥各组分的粉末混合物而形成的。混合的粉末然后被冷压形成直径2英寸高4-6英寸的圆柱形生坯。生坯被引入热压机并在还原气氛中和氩气吹扫条件下于1450-2100℃被致密化。对于实施例15，为保证ZrO2粉末小于0.7μm，在与其它组分均匀混合之前将含有ZrO2的预混合粉末湿球磨和干燥。
在润湿性测试中，通过将质量已知的铝锭放在抛光的坯段试样表面上来测量坯段试样对熔融铝的润湿性。在小于0.001毫巴的真空下将试样和铝迅速加热，直到铝熔融、展开、然后蒸发。蒸发之后，铝展开的面积可见并可利用数字图象分析进行测量。通过用铝的展开面积除以铝锭的质量，可以获得润湿性值，单位为mm2/g。
表2
实施例 BN TiB2 CaO Y2O3 Al2O3 ZrO2 AlN Mo
11 52.3 44.3 0.1 0.7 0.6 2.0
12 54.0 44.3 1.7
13 45.9 44.4 1.7 8.0
14 54.3 44.3 0.8 0.7
15 52.9 44.3 2.8
16 39.3 44.3 0.1 0.7 0.6 15.0
17 54.3 44.3 0.8 0.7
18 54.3 44.3 0.1 0.7 0.6
19 54.6 44.3 1.1
对坯段的润湿性能、密度和电阻率的测试结果列在表3中：
表3
实施例 理论密度(g/cc) 润湿面积(mm2/g) 质量(g) 密度(g/cc) ％理论密度 电阻率(u-ohm-cm)
11 2.98 4770 22.3 2.2 75％ 2986
12 2.97 5758 23.9 2.4 81％ 19028
13 3.23 5007 21.1 2.7 83％ 6395
14 2.96 5165 21.4 2.5 84％ 2059
15 2.99 4989 21.8 2.5 84％ 4436
16 3.14 5616 21.0 2.7 86％ 959
17 2.96 4973 22.3 2.6 87％ 4228
8 2.96 3482 22.1 2.6 88％ 1994
9 2.94 854 21.9 2.7 92％ 3966
实施例20-22：
在这些实施例中，形成了涂覆金属舟并以形成敷金属膜对这些涂覆金属舟进行了测试。将含有本发明所述组成的舟与市场上可商购的金属舟即购自Cleveland，Ohio的GE Advanced Ceramics的“经典”舟进行了对比。实施例20采用经典舟组成，已知为一种“2部分舟”，或包含TiB2和BN为主要组分的组成。实施例21代表一种“3部分舟”组成，可从GE Advanced Ceramics以“AC-6000”商购。“3部分”组成通常定义为含有TiB2、BN和AIN作为主要组分的组成。实施例22是本发明的一个实施例。所有组分都是以重量％表示的。
表4
实施例 类型 BN TiB2 CaO Y2O3 Al2O3 AIN
20 2-部分 45到60 40到55 1-2
21 3-部分 25-35 40-55 1-3 10-30
22 2-部分 53.6 45.0 0.1 0.7 0.6
在E.Josephson等人的题为“The Effects of Boat and WireParameters on Boat Life and Coating Quality in Vacuum Metallizationof an OPP Web”(1995 SVC会议录)的论文中，对2部分舟(BN/TiB2-实施例20中所述类型的舟)和3部分舟(BN/AlN/TiB2-实施例21中所述类型的舟)的有效舟寿命进行了对比。作者在结论部分指出：“使用两种常规的方法测量舟寿命，两相舟显示了较长的寿命。据统计舟组成在周期数上具有惊人的90％的可信度，用于线性英尺涂覆金属时具有75％的可信度”。另外，“通过肉眼观察可以发现两相舟具有较少的沉积和更好的耐腐蚀性”。
腐蚀和润湿性测试的结果表明，实施例21和22相比实施例20的经典舟具有显著提高的性能。不过，实施例22又比使用实施例21的舟表现好得多，在润湿性和耐腐蚀性能方面都显示了改善。在本领域中已知在润湿性和耐腐蚀性之间存在一种折衷。三部分舟通常润湿性更好；而两部分舟耐腐蚀性更强。本发明的实施例22产生了令人意外的改进和平衡的性能，所提供的舟润湿性更好同时也更耐腐蚀。
尽管已经参照优选实施方案对本发明进行了说明，但本领域技术人员能够理解，在不脱离本发明的范围的基础上可以作出各种改变或等效替换其中的要素。本发明并不限于所公开的作为实施本发明的最佳方式的具体实施方案，而是包括落入附加权利要求书范围之内的所有实施方案。
在此申请中，除非特别指出，所有单位都是公制的且所有含量和百分比都以重量计。此外，文中所引用的所有文献也都在此清楚地引入作为参考。

Claims (15)

1.一种用于蒸发金属的耐火容器，所述耐火容器主要由以下材料构成：约45-6重量％的氮化硼；
约35-65量％的耐火硼化物；
和约0.10-10重量％的选自氧化物、碳化物、氮化物和其混合物的稀土金属化合物。
2.根据权利要求1的耐火容器，其中稀土金属化合物选自氧化钇、氧化镧及其混合物。
3.根据权利要求1-2中任何一项的耐火容器，其中稀土金属化合物是纯度为至少95％且平均粒度为约15微米或更小的氧化钇。
4.根据权利要求1-3中任何一项的耐火容器，还包含直到10重量％的平均粒度为约15微米或更小的氮化铝或氮化硅。
5.根据权利要求1-4中任何一项的耐火容器，还包含氧化钙、氧化铝、氧化镁和二氧化钛中的至少一种。
6.根据权利要求1-5中任何一项的耐火容器，还包含一种选自YAG(Al5Y3O12)、YAP(AlYO3)、YAM(Al2Y4O7)及其组合的化合物。
7.根据权利要求1-6中任何一项的耐火容器，还包含0.2-5重量％的选自元素Al、Si、Ti、Fe、Co、Ni的碳化物和氮化物及其混合物的元素或化合物。
8.一种提高用于蒸发金属的耐火舟的使用寿命的方法，所述方法包括在主要由45-65重量％的氮化硼和35-65重量％的耐火硼化物构成的组成中掺杂约0.10-10重量％的选自氧化物、碳化物、氮化物或其混合物的稀土金属化合物。
9.根据权利要求8的方法，进一步包括在所述组成中掺杂0.2-5重量％的选自元素Al、Si、Ti、Fe、Co、Ni的碳化物和氮化物及其混合物的元素或化合物。
10.一种制造用于蒸发金属的耐火舟的方法，所述方法包括以下步骤：形成的一个成型体，所述成型体包含主要由45-65重量％的氮化硼、约35-65重量％的耐火硼化物和约0.10-10重量％的选自氧化物、碳化物、氮化物或其混合物的稀土金属化合物构成的均匀粉末混合物，并由所述成型体制成耐火舟。
11.根据权利要求10的方法，其中稀土金属氧化物是纯度为至少95％且平均粒度为约15微米或更小的氧化钇。
12.根据权利要求10-11中任何一项的方法，其中成型体还包含直到10重量％的平均粒度为约15微米或更小的氮化铝或氮化硅。
13.根据权利要求10-12中任何一项的方法，其中成型体还包含氧化钙、氧化铝、氧化镁和二氧化钛中的至少一种。
14.根据权利要求10-13中任何一项的方法，其中成型体还包含一种选自YAG(Al5Y3O12)、YAP(AlYO3)、YAM(Al2Y4O7)及其组合的化合物。
15.根据权利要求10-14中任何一项的方法，其中成型体还包含0.2-5重量％的选自元素Al、Si、Ti、Fe、Co、Ni的碳化物和氮化物及其混合物的元素或化合物。
CNA2004800275653A 2003-09-24 2004-09-24 金属蒸发容器及其制造方法 Pending CN1856590A (zh)

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