公开(公告)号：US20080292535A1

公开(公告)日：2008-11-27

申请号：US12116995

申请日：2008-05-08

申请人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Von Der Goenna

发明人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Von Der Goenna

IPC分类号： C01F11/22

CPC分类号： C01F11/22 ,  C01B9/08 ,  C01P2006/80 ,  C30B11/00 ,  C30B29/12

摘要： The method provides CaF2 single crystals with low scattering, small refractive index differences and few small angle grain boundaries, which can be tempered at elevated temperatures. In the method a CaF2 starting material is heat-treated for at least five hours at temperatures between 1000° C. and 1250° C. and then vaporized at a temperature of at least 1100° C. in a vacuum of at most 5*10−4 mbar to form a vapor. The vapor is condensed at a temperature between 500° C. to 1280° C. to form a condensate. Then a melt formed from the condensate is cooled in a controlled manner to obtain the single crystal, which is subsequently tempered. The method is preferably performed with a CaF2 starting material including waste material and cuttings from previously used melts.

摘要翻译： 该方法提供具有低散射，小折射率差异和几个小角度晶界的CaF 2单晶，其可以在升高的温度下回火。 在该方法中，将CaF 2起始材料在1000℃至1250℃之间的温度下热处理至少5小时，然后在至少为5×10 10的真空中在至少1100℃的温度下蒸发 -4毫巴形成蒸气。 蒸气在500℃至1280℃之间的温度下冷凝以形成冷凝物。 然后将由冷凝物形成的熔体以受控的方式冷却，得到随后回火的单晶。 该方法优选用包括废料的CaF 2起始材料和先前使用的熔体的切屑进行。

公开(公告)号：US07588637B2

公开(公告)日：2009-09-15

申请号：US11609626

申请日：2006-12-12

申请人： Andreas Weisleder ,  Matthias Mueller ,  Joerg Kandler ,  Andreas Menzel ,  Rainer Guett

发明人： Andreas Weisleder ,  Matthias Mueller ,  Joerg Kandler ,  Andreas Menzel ,  Rainer Guett

IPC分类号： C30B13/28

CPC分类号： C30B11/00 ,  C30B29/12

摘要： A method for producing high-purity, large-volume monocrystals that are especially radiation-resistant and have low intrinsic birefringence. From a melt of crystalline raw material, with controlled cooling and solidification, a crystal is generated. As the crystalline raw material, shards and/or waste from already-grown crystals is used, and the re-used raw material 1) upon visual observation in daylight has no color; and 2) upon illumination with a white-light lamp in a darkroom a) has no or at maximum a just barely perceivable reddish and/or bluish fluorescence; and b) has no or at maximum a just barely perceivable diffuse scattering; and c) has no or only slight discrete scattering of at maximum two visually perceivable scattering centers per dm3. In this way, crystals can be obtained which after tempering have a BSDF value of

摘要翻译： 一种生产高纯度，大容量单晶的方法，特别是耐辐射和具有低固有双折射。 从结晶原料的熔体中，通过控制冷却和固化，产生晶体。 作为结晶原料，使用已经生长的晶体的碎片和/或废物，并且在日光下目视观察时，再利用的原料1）没有颜色; 和2）在暗室中用白光灯照明时a）没有或最多只有几乎不可察觉的淡红色和/或蓝色荧光; 和b）没有或最多只有几乎不可察觉的漫射散射; 和c）没有或仅有最大两个视觉上可感知的散射中心/ dm 3的轻微离散散射。 以这种方式，可以获得晶体，其在回火之后BSDF值<7×10 -7，减去36 Zernike系数<15×10-8之后的RMS均匀性，111方向的±0.2nm的SDR-RMS值 /厘米。

公开(公告)号：US20090297430A1

公开(公告)日：2009-12-03

申请号：US12539795

申请日：2009-08-12

申请人： Andreas Weisleder ,  Matthias Mueller ,  Joerg Kandler ,  Andreas Menzel ,  Rainer Guett

发明人： Andreas Weisleder ,  Matthias Mueller ,  Joerg Kandler ,  Andreas Menzel ,  Rainer Guett

IPC分类号： C01F11/22 ,  C01F5/28

CPC分类号： C30B11/00 ,  C30B29/12

摘要： The high-purity alkaline earth halide crystals, especially CaF2, BaF2 or MgF2 crystals, have a diffuse scatter distribution function value of less than 7×10−7, an RMS uniformity of refractive index of less than 15×10−8 after subtraction of Zernike coefficients and an RMS value of birefringence in the (111) direction of less than 0.2 nm/cm. Preferably the crystals exhibit a loss coefficient of less than 5×10−4 cm−1 after irradiation with 10×109 laser pulses with an energy density of 10 mJ/cm2 at a wavelength of 193 nm. Also they have RMS birefringence in the (100) direction or the (111) direction that is less than 0.35 nm/cm.

摘要翻译： 高纯度碱土卤化物晶体，特别是CaF 2，BaF 2或MgF 2晶体具有小于7×10 -7的漫射散射分布函数值，减去Zernike系数后的折射率RMS均匀度小于15×10 -8， （111）方向的双折射的RMS值小于0.2nm / cm。 优选地，在193nm的能量密度为10mJ / cm 2的10×10 9个激光脉冲照射之后，晶体表现出小于5×10 -4 cm -1的损耗系数。 此外，它们在（100）方向或（111）方向上具有小于0.35nm / cm的RMS双折射。

公开(公告)号：US07534412B2

公开(公告)日：2009-05-19

申请号：US12116995

申请日：2008-05-08

申请人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Von Der Goenna

发明人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Von Der Goenna

IPC分类号： C01D3/02 ,  C01F11/22 ,  C30B23/00 ,  C30B25/00

CPC分类号： C01F11/22 ,  C01B9/08 ,  C01P2006/80 ,  C30B11/00 ,  C30B29/12

摘要： Single crystals with low scattering, small refractive index differences and few small angle grain boundaries have a bi-directional scattering distribution function value (BSDF) of less than 1.5*10−6 or 5*10−7.

摘要翻译： 具有低散射，小折射率差异和少量小角度晶界的单晶具有小于1.5×10-6或5×10-7的双向散射分布函数值（BSDF）。

公开(公告)号：US20050211160A1

公开(公告)日：2005-09-29

申请号：US11063147

申请日：2005-02-22

申请人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Goenna

发明人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Goenna

IPC分类号： G03F1/14 ,  C01B9/08 ,  C01F11/22 ,  C30B11/00 ,  C30B29/12 ,  G02B1/02 ,  G02B5/30 ,  G03F7/20 ,  H01L21/027 ,  C30B1/00 ,  C30B9/00 ,  C30B28/06

CPC分类号： C01F11/22 ,  C01B9/08 ,  C01P2006/80 ,  C30B11/00 ,  C30B29/12

摘要： The method provides CaF2 single crystals with low scattering, small refractive index differences and few small angle grain boundaries, which can be tempered at elevated temperatures. In the method a CaF2 starting material is heat-treated for at least five hours at temperatures between 1000° C. and 1250° C. and then vaporized at a temperature of at least 1100° C. in a vacuum of at most 5*10−4 mbar to form a vapor. The vapor is condensed at a temperature between 500° C. to 1280° C. to form a condensate. Then a melt formed from the condensate is cooled in a controlled manner to obtain the single crystal, which is subsequently tempered. The method is preferably performed with a CaF2 starting material including waste material and cuttings from previously used melts.

摘要翻译： 该方法提供具有低散射，小折射率差异和几个小角度晶界的CaF 2 N 2单晶，其可以在升高的温度下回火。 在该方法中，将CaF 2原料在1000℃至1250℃之间的温度下热处理至少5小时，然后在至少1100℃的温度下蒸发 真空度至多为5×10 -4毫巴以形成蒸汽。 蒸气在500℃至1280℃之间的温度下冷凝以形成冷凝物。 然后将由冷凝物形成的熔体以受控的方式冷却，得到随后回火的单晶。 该方法优选用包含废料的CaF 2原料和先前使用的熔体的切屑进行。

公开(公告)号：US20050178316A1

公开(公告)日：2005-08-18

申请号：US11042286

申请日：2005-01-24

申请人： Joerg Kandler ,  Lutz Parthier ,  Thomas Kaufhold ,  Gunther Wehrhan ,  Clemens Kunisch

发明人： Joerg Kandler ,  Lutz Parthier ,  Thomas Kaufhold ,  Gunther Wehrhan ,  Clemens Kunisch

IPC分类号： C30B11/02 ,  C30B11/00 ,  C30B29/12 ,  C30B33/00 ,  G02B1/02 ,  C30B15/00 ,  C30B21/06 ,  C30B27/02 ,  C30B28/10 ,  C30B30/04

CPC分类号： C30B11/00 ,  C30B29/12 ,  C30B33/00 ,  G02B1/02 ,  Y10T117/1072 ,  Y10T117/108

摘要： The method for producing single crystals includes drying crystal raw material by removing water, reaction of impurities with a scavenger, preferably a metal halide, and homogenizing the melt. The method is performed with the raw material in a melt vessel with a variable-sized through-going opening, in which drying occurs at 100° C. to 600° C. for at least 20 hours with a geometric conductance value for the through-going opening of 2.00 to 30.00 mm2; the reacting occurs at 600° C. to 1200° C. for at least nine hours with a geometric conductance value of 0.0020 to 0.300 mm2 and the homogenizing occurs at above 1400° C. for at least six hours with a geometric conductance value of 0.25 to 1.1 mm2. Alternatively the geometric conductance value is the same during drying, reacting and homogenizing and takes a value between 0.25 and 1 mm2.

公开(公告)号：US06740159B2

公开(公告)日：2004-05-25

申请号：US10230232

申请日：2002-08-28

申请人： Joerg Kandler ,  Ewald Moersen ,  Burkhard Speit ,  Harry Bauer ,  Thure Boehm ,  Eric Eva ,  Michael Thier ,  Hexin Wang ,  Frank Richter ,  Hans-Josef Paus

发明人： Joerg Kandler ,  Ewald Moersen ,  Burkhard Speit ,  Harry Bauer ,  Thure Boehm ,  Eric Eva ,  Michael Thier ,  Hexin Wang ,  Frank Richter ,  Hans-Josef Paus

IPC分类号： C30B15804

CPC分类号： G02B1/02 ,  C30B11/00 ,  C30B29/12

摘要： A method of making a fracture-resistant large-size calcium fluoride single crystal is described, which is suitable for an optical component for radiation in the far UV range. The calcium fluoride raw material for the single crystal is first melted and subsequently solidified by cooling the melt to form a single crystal. However the calcium fluoride raw material is doped with from 1 to 250, preferably 1 to 100, ppm of strontium, preferably added as strontium fluoride, and contains from 1 to 10 ppm of sodium as well as up to 100 ppm of other impurities.

摘要翻译： 描述了制造耐断裂大尺寸氟化钙单晶的方法，其适用于在远紫外范围内用于辐射的光学部件。 首先将用于单晶的氟化钙原料熔化并随后通过冷却熔体而固化形成单晶。 然而，氟化钙原料掺杂有1至250，优选1至100ppm的锶，优选以氟化锶加入，并且含有1至10ppm的钠以及至多100ppm的其它杂质。

公开(公告)号：US07393409B2

公开(公告)日：2008-07-01

申请号：US11063147

申请日：2005-02-22

申请人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Von der Goenna

发明人： Lars Ortmann ,  Joerg Kandler ,  Andreas Menzel ,  Matthias Mueller ,  Lutz Parthier ,  Gordon Von der Goenna

IPC分类号： C30B23/00 ,  C01B7/19

CPC分类号： C01F11/22 ,  C01B9/08 ,  C01P2006/80 ,  C30B11/00 ,  C30B29/12

摘要： The method provides CaF2 single crystals with low scattering, small refractive index differences and few small angle grain boundaries, which can be tempered at elevated temperatures. In the method a CaF2 starting material is heat-treated for at least five hours at temperatures between 1000° C. and 1250° C. and then sublimed at a sublimation temperature of at least 1100° C. in a vacuum of at most 5*10−4 mbar to form a vapor. The vapor is condensed at a condensation temperature of at least 500° C., which is at least 20° C. below the sublimitation temperature, to form a condensate. Then a melt formed from the condensate is cooled in a controlled manner to obtain the single crystal, which is subsequently tempered. The method is preferably performed with a CaF2 starting material including waste material and cuttings from previously used melts.

摘要翻译： 该方法提供具有低散射，小折射率差异和几个小角度晶界的CaF 2 N 2单晶，其可以在升高的温度下回火。 在该方法中，将CaF 2原料在1000℃和1250℃之间的温度下热处理至少5小时，然后在至少1100℃的升华温度升华。 在至多5×10 -4 Mbar的真空中，以形成蒸汽。 蒸气在至少500℃的冷凝温度下冷凝，其在亚临界温度以下至少20℃，以形成冷凝物。 然后将由冷凝物形成的熔体以受控的方式冷却，得到随后回火的单晶。 该方法优选用包含废料的CaF 2原料和先前使用的熔体的切屑进行。

公开(公告)号：US07344595B2

公开(公告)日：2008-03-18

申请号：US11042286

申请日：2005-01-24

申请人： Joerg Kandler ,  Lutz Parthier ,  Thomas Kaufhold ,  Gunther Wehrhan ,  Clemens Kunisch

发明人： Joerg Kandler ,  Lutz Parthier ,  Thomas Kaufhold ,  Gunther Wehrhan ,  Clemens Kunisch

IPC分类号： C30B11/02

CPC分类号： C30B11/00 ,  C30B29/12 ,  C30B33/00 ,  G02B1/02 ,  Y10T117/1072 ,  Y10T117/108

摘要： The method for producing single crystals includes drying crystal raw material by removing water, reaction of impurities with a scavenger, preferably a metal halide, and homogenizing the melt. The method is performed with the raw material in a melt vessel with a variable-sized through-going opening, in which drying occurs at 100° C. to 600° C. for at least 20 hours with a geometric conductance value for the through-going opening of 2.00 to 30.00 mm2; the reacting occurs at 600° C. to 1200° C. for at least nine hours with a geometric conductance value of 0.0020 to 0.300 mm2 and the homogenizing occurs at above 1400° C. for at least six hours with a geometric conductance value of 0.25 to 1.1 mm2. Alternatively the geometric conductance value is the same during drying, reacting and homogenizing and takes a value between 0.25 and 1 mm2.

摘要翻译： 单晶的制造方法包括通过除去水来干燥晶体原料，使杂质与清除剂反应，优选金属卤化物，使熔融物均质化。 该方法使用原料在具有可变尺寸的通孔的熔体容器中进行，其中在100℃至600℃下干燥至少20小时，其中通孔的几何电导值， 2.00〜30.00mm 2的开口; 反应在600℃至1200℃下发生至少9小时，几何电导值为0.0020至0.300mm 2，均质化在1400℃以上发生至少六次 几何电导值为0.25至1.1mm 2的小时。 或者，在干燥，反应和均化期间几何电导值相同，并且取0.25至1mm 2之间的值。

公开(公告)号：US20070186844A1

公开(公告)日：2007-08-16

申请号：US11609626

申请日：2006-12-12

申请人： Andreas Weisleder ,  Matthias Mueller ,  Joerg Kandler ,  Andreas Menzel ,  Rainer Guett

发明人： Andreas Weisleder ,  Matthias Mueller ,  Joerg Kandler ,  Andreas Menzel ,  Rainer Guett

IPC分类号： C30B15/00 ,  C30B19/00 ,  C30B23/00

CPC分类号： C30B11/00 ,  C30B29/12

摘要： A method for producing high-purity, large-volume monocrystals that are especially radiation-resistant and have low intrinsic birefringence. From a melt of crystalline raw material, with controlled cooling and solidification, a crystal is generated. As the crystalline raw material, shards and/or waste from already-grown crystals is used, and the re-used raw material 1) upon visual observation in daylight has no color; and 2) upon illumination with a white-light lamp in a darkroom a) has no or at maximum a just barely perceivable reddish and/or bluish fluorescence; and b) has no or at maximum a just barely perceivable diffuse scattering; and c) has no or only slight discrete scattering of at maximum two visually perceivable scattering centers per dm3. In this way, crystals can be obtained which after tempering have a BSDF value of

摘要翻译： 一种生产高纯度，大容量单晶的方法，特别是耐辐射和具有低固有双折射。 从结晶原料的熔体中，通过控制冷却和固化，产生晶体。 作为结晶原料，使用已经生长的晶体的碎片和/或废物，并且在日光下目视观察时，再利用的原料1）没有颜色; 和2）在暗室中用白光灯照明时a）没有或最多只有几乎不可察觉的淡红色和/或蓝色荧光; 和b）没有或最多只有几乎不可察觉的漫射散射; 和c）在dm 3处没有或仅有最大两个视觉上可感知的散射中心的轻微的离散散射。 以这种方式，可以获得晶体，其在回火之后具有<7×10 -7 -7的BSDF值，在减去36次泽尼克系数<15×10 -8 -8之后的RMS均匀性 ，111方向的SDR-RMS值<0.2nm / cm。