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公开(公告)号：US4449780A
公开(公告)日：1984-05-22
申请号：US397553
申请日：1982-07-12
申请人： Carl F. Swinehart
发明人： Carl F. Swinehart
摘要： The addition of a getter consisting essentially of reactive oxides of boron and silicon, to a melt of an alkali metal halide serves to overcome problems of unacceptable color, afterglow and hardness attributable to trace impurities present in the melt. These trace impurities are generally metals present in a concentration less than 1 part per million (ppm) parts of melt. An ingot melt-grown from charge stock treated with the getter provides high quality optical bodies such as light pipes, laser windows and scintillators. Specific problems characteristic of a scintillator ingot grown from a highly purified alkali metal halide "remelt", such as is obtained by crushing and melting portions of a melt-grown ingot, are overcome by adding to the remelt a portion of fresh powder stock in which the getter has been uniformly distributed.A process is taught for the Stockbarger growth of a scintillator ingot from a charge stock treated to include a getter consisting essentially of the combined reactive oxides of boron and silicon, comprising superheating a melt of treated charge stock for a period of time sufficient to react at least some of the reactive oxides with deleterious trace impurities present in the melt, and growing a scintillator ingot free from discoloration, afterglow or undue hardness due to the presence of the impurities.
摘要翻译： 将基本上由硼和硅的活性氧化物组成的吸气剂加入到碱金属卤化物的熔体中用于克服存在于熔体中的微量杂质引起的不可接受的颜色，余辉和硬度的问题。 这些痕量杂质通常是以小于1ppm（ppm）份熔体的浓度存在的金属。 用吸气剂处理的电荷材料熔融生长的锭子提供了高质量的光学体，如光管，激光窗和闪烁体。 通过将熔融生长的锭的部分破碎和熔化获得的高纯度碱金属卤化物“重熔”生长的闪烁体锭的特征的特征是通过加入一部分新鲜粉末原料来克服，其中 吸气剂是均匀分布的。 教导了一种从经处理的电荷原料的闪烁体锭的Stockbarger生长的过程，其包括基本上由硼和硅的组合的活性氧化物组成的吸气剂，包括将经处理的电荷原料的熔体过热一段足以在 至少一些具有有害微量杂质的活性氧化物存在于熔体中，并且由于杂质的存在而生长闪烁体锭没有变色，余辉或不适当的硬度。
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2.发明授权Method of making an ionic fluoride optical body with reduction of absorption bands 失效制造具有减少吸收带的离子氟化物光学体的方法
公开(公告)号：US4089937A
公开(公告)日：1978-05-16
申请号：US779623
申请日：1977-03-21
申请人： Carl F. Swinehart , Herbert Packer
发明人： Carl F. Swinehart , Herbert Packer
CPC分类号： G02B1/00 , C04B35/553
摘要： A hot-pressed optical body which is free from absorption bands due to carbon dioxide, water, hydroxyl ion and acid fluorides in the ultraviolet, visible and near-infrared wavelength regions. Typically, the optical body is formed from a powder of an alkaline earth metal fluoride, alkali metal fluoride, or rare earth metal fluoride. One or more absorption bands due to a single impurity may be reduced or eliminated, or bands due to plural impurities may be reduced or eliminated sequentially, or simultaneously. The optical body is made by flowing a reactive, reducing gas, optionally, in combination with hydrogen fluoride gas, directly into the die cavity containing a pressable ionic fluoride powder, and either hot-pressing or extruding the powder.
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公开(公告)号：US4055457A
公开(公告)日：1977-10-25
申请号：US716051
申请日：1976-08-20
申请人： Carl F. Swinehart
发明人： Carl F. Swinehart
摘要： Large ultra-pure, prism-quality essentially single crystal boules and ingots of alkali metal chlorides and alkali metal bromides are grown by the methods of Kyropoulos and Stockbarger. Optically single crystals of these alkali metal halides are clear optical bodies free of haze throughout. A typical Kyropoulos grown boule of KBr of this invention is also absorption-free, and has cleavage or crystallographic planes which deviate from parallel by 1.degree. to 3.degree. per inch. By `absorption-free` is meant freedom of absorption at 7.2 microns (.mu.) due to nitrate, at 9.5-11 .mu. due to silicate, and at between 8 and 9 .mu. due to sulfate, which are the most difficult to control but as the term implies the bodies are also free of infrared absorption for impurities such as CO.sub.3.sup.-2, PO.sub.4.sup.-3, OH.sup.-, BO.sub.2.sup.-, SH.sup.-, CNO.sup.-, HCO.sub.3.sup.-, etc., which are easily avoided by use of good commercially available growth stock.A particular process for growth for either of the foregoing methods in a silica or quartz crucible, comprises growing an ultrapure ingot of KBr from a relatively impure melt containing silicate, sulfate, nitrate and nitrite ions, and includes maintaining the sodium content of the melt during growth to less than about 20 ppm (parts per million) and the barium content less than 10 ppm, adding barium bromide to the melt if necessary, and, contacting the melt with a trace of free bromine in a covered, but not air-tight, pot.
摘要翻译： 通过Kyropoulos和Stockbarger的方法生长大型超纯，棱柱质量的碱性金属氯化物和碱金属溴化物。 这些碱金属卤化物的光学单晶是透明的光学体。 本发明的KBr的典型的Kyropoulos生长的棒也是无吸收的，并且具有相对于每平方英寸1°至3°的切割或结晶平面。 “无吸收”是指由于硝酸盐在7.2微米（μm）下的吸收自由度，由于硅酸盐而在9.5-11微米处，并且由于硫酸盐而在8至9微米之间，这是最难控制的，但是作为 该术语意味着物体对于诸如CO 3 -2，PO 4 -3，OH-，BO 2 - ，SH-，CNO-，HCO 3 - 等杂质也没有红外吸收，这些容易通过使用商业上很好地避免 可用成长股。
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4.发明授权Getter for melt-grown scintillator ingot and method for growing the ingot 失效吸收剂用于熔融生长的闪烁体锭和用于生长锭的方法
公开(公告)号：US4277303A
公开(公告)日：1981-07-07
申请号：US931323
申请日：1978-08-07
申请人： Carl F. Swinehart
发明人： Carl F. Swinehart
摘要： The addition of a getter consisting essentially of reactive oxides of boron and silicon, to a melt of an alkali metal halide serves to overcome problems of unacceptable color, afterglow and hardness attributable to trace impurities present in the melt. These trace impurities are generally metals present in a concentration less than 1 part per million (ppm) parts of melt. An ingot melt-grown from charge stock treated with the getter provides high quality optical bodies such as light pipes, laser windows and scintillators. Specific problems characteristic of a scintillator ingot grown from a highly purified alkali metal halide "remelt", such as is obtained by crushing and melting portions of a melt-grown ingot, are overcome by adding to the remelt a portion of fresh powder stock in which the getter has been uniformly distributed.A process is taught for the Stockbarger growth of a scintillator ingot from a charge stock treated to include a getter consisting essentially of the combined reactive oxides of boron and silicon, comprising superheating a melt of treated charge stock for a period of time sufficient to react at least some of the reactive oxides with deleterious trace impurities present in the melt, and growing a scintillator ingot free from discoloration, afterglow or undue hardness due to the presence of the impurities.
摘要翻译： 将基本上由硼和硅的活性氧化物组成的吸气剂加入到碱金属卤化物的熔体中用于克服存在于熔体中的微量杂质引起的不可接受的颜色，余辉和硬度的问题。 这些痕量杂质通常是以小于1ppm（ppm）份熔体的浓度存在的金属。 用吸气剂处理的电荷材料熔融生长的锭子提供了高质量的光学体，如光管，激光窗和闪烁体。 通过将熔融生长的锭的部分破碎和熔化获得的高纯度碱金属卤化物“重熔”生长的闪烁体锭的特征的特征是通过加入一部分新鲜粉末原料来克服，其中 吸气剂是均匀分布的。 教导了一种从经处理的电荷原料的闪烁体锭的Stockbarger生长的过程，其包括基本上由硼和硅的组合的活性氧化物组成的吸气剂，包括将经处理的电荷原料的熔体过热一段足以在 至少一些具有有害微量杂质的活性氧化物存在于熔体中，并且由于杂质的存在而生长闪烁体锭没有变色，余辉或不适当的硬度。
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公开(公告)号：US4586785A
公开(公告)日：1986-05-06
申请号：US603018
申请日：1984-06-25
申请人： Carl F. Swinehart
发明人： Carl F. Swinehart
摘要： The addition of a getter consisting essentially of reactive oxides of boron and silicon, to a melt of an alkali metal halide serves to overcome problems of unacceptable color, afterglow and hardness attributable to trace impurities present in the melt. These trace impurities are generally metals present in a concentration less than 1 part per million (ppm) parts of melt. An ingot melt-grown from charge stock treated with the getter provides high quality optical bodies such as light pipes, laser windows and scintillators. Specific problems characteristic of a scintillator ingot grown from a highly purified alkali metal halide "remelt", such as is obtained by crushing and melting portions of a melt-grown ingot, are overcome by adding to the remelt a portion of fresh powder stock in which the getter has been uniformly distributed. A process is taught for the Stockbarger growth of a scintillator ingot from a charge stock treated to include a getter consisting essentially of the combined reactive oxides of boron and silicon, comprising superheating a melt of treated charge stock for a period of time sufficient to react at least some of the reactive oxides with deleterious trace impurities present in the melt, and growing a scintillator ingot free from discoloration, afterglow or undue hardness due to the presence of the impurities.
摘要翻译： 将基本上由硼和硅的活性氧化物组成的吸气剂加入到碱金属卤化物的熔体中用于克服存在于熔体中的微量杂质引起的不可接受的颜色，余辉和硬度的问题。 这些痕量杂质通常是以小于1ppm（ppm）份熔体的浓度存在的金属。 用吸气剂处理的电荷材料熔融生长的锭子提供了高质量的光学体，如光管，激光窗和闪烁体。 通过将熔融生长的锭的部分破碎和熔化获得的高纯度碱金属卤化物“重熔”生长的闪烁体锭的特征的特征是通过加入一部分新鲜粉末原料来克服，其中 吸气剂是均匀分布的。 教导了一种从经处理的电荷原料的闪烁体锭的Stockbarger生长的过程，其包括基本上由硼和硅的组合的活性氧化物组成的吸气剂，包括将经处理的电荷原料的熔体过热一段足以在 至少一些具有有害微量杂质的活性氧化物存在于熔体中，并且由于杂质的存在而生长闪烁体锭没有变色，余辉或不适当的硬度。
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公开(公告)号：US3981818A
公开(公告)日：1976-09-21
申请号：US406585
申请日：1973-10-15
申请人： Carl F. Swinehart , Marko Sfiligoj
发明人： Carl F. Swinehart , Marko Sfiligoj
CPC分类号： C30B21/02
摘要： A composition of matter transparent to infrared rays and shock resistant which is a directionally grown, polycrystalline solidified melt of a eutectic composition comprising at least two components wherein the ratio of the index of refraction of one to the other is within the range of 1.2 to 1.0, the directionally oriented, polycrystalline mass is grown in a controlled manner by adding heat to the melt and removing the same from the solids during the solidification step, the amount of heat being added to the melt and conducted through the solidified melt being 10.sup.3 to 10.sup.5 times the latent heat of fusion of the eutectic mixture.
摘要翻译： 包含至少两种组分的共晶组合物的定向生长的多晶固化熔体的红外线透光性和耐冲击性的组合物，其中一种与另一种之间的折射率之比在1.2至1.0的范围内 ，通过向熔体中加热并在固化步骤中将其从固体中除去，以有控制的方式生长定向取向的多晶质量，加入到熔体中并通过固化熔体传导的热量为103至105 倍的共晶混合物的融合潜热。
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公开(公告)号：US4050905A
公开(公告)日：1977-09-27
申请号：US581233
申请日：1975-05-27
申请人： Carl F. Swinehart
发明人： Carl F. Swinehart
CPC分类号： C30B11/006 , C30B11/00 , C30B29/12
摘要： Large, doped crystal ingots are grown in a Stockbarger furnace from a melt of an alkali metal or alkaline earth metal salt using very slow oscillation (1 - 2 cycles per minute) of the ingot through a small arc of 5.degree. -20.degree. to produce an ingot having a more even distribution of dopant and an absence of open boundaries between macrocrystals within the ingot.
摘要翻译： 大量掺杂的晶锭通过碱金属或碱土金属盐的熔体在库存式加热炉中生长，使用非常慢的振荡（每分钟1-2次循环）通过5°-20°的小弧度产生 具有更均匀分布的掺杂剂的晶锭和在晶锭内的大量晶体之间不存在开放的边界。
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8.发明授权Hot-pressed ionic fluoride optical bodies free of absorption bands and method of making them 失效热压离子氟化物光学体，不含吸收剂及其制备方法
公开(公告)号：US4013796A
公开(公告)日：1977-03-22
申请号：US391890
申请日：1973-08-27
申请人： Carl F. Swinehart , Herbert Packer
发明人： Carl F. Swinehart , Herbert Packer
CPC分类号： G02B1/00 , C04B35/553
摘要： A hot-pressed optical body is disclosed which is free from absorption bands due to carbon dioxide, water, hydroxyl ion and acid fluorides in the ultraviolet, visible and near-infrared wavelength regions. Typically, the optical body is formed from a powder of an alkaline earth metal fluoride, alkali metal fluoride, or rare earth metal fluoride. One or more absorption bands due to a single impurity may be reduced or eliminated, or bands due to plural impurities may be reduced or eliminated sequentially, or simultaneously. The optical body is made by flowing a reactive, reducing gas, optionally, in combination with hydrogen fluoride gas, directly into the die cavity containing a pressable powder, and either hot-pressing or extruding the powder.
摘要翻译： 一种热紫外线，可见光和近红外波长区域中由于二氧化碳，水，羟基离子和酸性氟化物而没有吸收带的热压光学体。 通常，光学体由碱土金属氟化物，碱金属氟化物或稀土金属氟化物的粉末形成。 可以减少或消除由于单一杂质引起的一个或多个吸收带，或者由于多种杂质导致的带可能被顺序地或同时地消除或消除。 光学体通过任选地与氟化氢气体组合的反应性还原气体直接流入含有可加压的离子性氟化物粉末的模腔，以及热压或挤出粉末而制成。
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公开(公告)号：US4341654A
公开(公告)日：1982-07-27
申请号：US241566
申请日：1981-03-09
申请人： Carl F. Swinehart
发明人： Carl F. Swinehart
摘要： The addition of a getter consisting essentially of reactive oxides of boron and silicon, to a melt of an alkali metal halide serves to overcome problems of unacceptable color, afterglow and hardness attributable to trace impurities present in the melt. These trace impurities are generally metals present in a concentration less than 1 part per million (ppm) parts of melt. An ingot melt-grown from charge stock treated with the getter provides high quality optical bodies such as light pipes, laser windows and scintillators. Specific problems characteristic of a scintillator ingot grown from a highly purified alkali metal halide "remelt", such as is obtained by crushing and melting portions of a melt-grown ingot, are overcome by adding to the remelt a portion of fresh powder stock in which the getter has been uniformly distributed.A process is taught for the Stockbarger growth of a scintillator ingot from a charge stock treated to include a getter consisting essentially of the combined reactive oxides of boron and silicon, comprising superheating a melt of treated charge stock for a period of time sufficient to react at least some of the reactive oxides with deleterious trace impurities present in the melt, and growing a scintillator ingot free from discoloration, afterglow or undue hardness due to the presence of the impurities.
摘要翻译： 将基本上由硼和硅的活性氧化物组成的吸气剂加入到碱金属卤化物的熔体中用于克服存在于熔体中的微量杂质引起的不可接受的颜色，余辉和硬度的问题。 这些痕量杂质通常是以小于1ppm（ppm）份熔体的浓度存在的金属。 用吸气剂处理的电荷材料熔融生长的锭子提供了高质量的光学体，如光管，激光窗和闪烁体。 通过将熔融生长的锭的部分破碎和熔化获得的高纯度碱金属卤化物“重熔”生长的闪烁体锭的特征的特征是通过加入一部分新鲜粉末原料来克服，其中 吸气剂是均匀分布的。 教导了一种从经处理的电荷原料的闪烁体锭的Stockbarger生长的过程，其包括基本上由硼和硅的组合的活性氧化物组成的吸气剂，包括将经处理的电荷原料的熔体过热一段足以在 至少一些具有有害微量杂质的活性氧化物存在于熔体中，并且由于杂质的存在而生长闪烁体锭没有变色，余辉或不适当的硬度。
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公开(公告)号：US4044112A
公开(公告)日：1977-08-23
申请号：US632059
申请日：1975-11-14
CPC分类号： C01F5/28 , G02B1/00 , C01P2002/01 , C01P2002/82 , C01P2004/51 , C01P2004/61
摘要： A process is disclosed for converting basic magnesium carbonate into pure hot-pressable magnesium fluoride such as is used for the hot-pressing of infra-red radiation transmitting optical bodies. The process includes contacting a slurry of basic magnesium carbonate with carbon dioxide to form enough magnesium bicarbonate or hydrates of magnesium carbonate, in situ, to alter the particles in the slurry. Carbonation of the slurry increases solubility of the solids by establishing an equilibrium relationship in solution between the unstable magnesium bicarbonate and hydrates of magnesium carbonate particles. When the carbonated slurry is contacted with a slight excess of hydrofluoric acid it precipitates solid particles of fine hydrous magnesium fluoride. Neutralization of excess hydrofluoric acid is effected with ammonium hydroxide. The solid particulate precipitate is dried and calcined to yield hot-pressable magnesium fluoride powder of exceptional purity and consistent quality.A hot-pressable magnesium fluoride powder has been prepared which has a specific and uniform refractive index, n.sub.D = 1.3850 at 20.degree. C; the powder is made up of primary particles the majority of which have an average particle diameter of greater than 5 .mu. (microns). These physical properties and a characteristic ill-defined X-ray diffraction pattern suggestive of an amorphous structure, allow the powder to be hot-pressed into an optical body without grinding the powder.
摘要翻译： 公开了用于将碱式碳酸镁转化为纯热压氟化镁的方法，例如用于热压红外辐射透射光学体的方法。 该方法包括将碱式碳酸镁的浆料与二氧化碳接触以形成足够的碳酸氢镁或碳酸镁的水合物，以便改变浆料中的颗粒。 浆料的碳酸化通过在不稳定的碳酸氢镁和碳酸镁颗粒的水合物之间的溶液中建立平衡关系来增加固体的溶解度。 当碳酸化浆液与略过量的氢氟酸接触时，会沉淀出含水氟化镁的固体颗粒。 过量氢氟酸的中和是用氢氧化铵进行的。 将固体颗粒沉淀物干燥并煅烧，得到纯度高，质量一致的热压氟化镁粉末。
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