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CN221752882U - Gas diffusion cascade for the preparation of silicon-28 isotope abundance above 99% using silane as medium - Google Patents

Gas diffusion cascade for the preparation of silicon-28 isotope abundance above 99% using silane as medium Download PDF

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CN221752882U
CN221752882U CN202322641995.7U CN202322641995U CN221752882U CN 221752882 U CN221752882 U CN 221752882U CN 202322641995 U CN202322641995 U CN 202322641995U CN 221752882 U CN221752882 U CN 221752882U
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gas diffusion
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diffusion cascade
silicon
silane
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周明胜
姜东君
孙旺
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Tsinghua University
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Abstract

The utility model relates to a gas diffusion cascade for preparing silicon-28 isotopes with abundance of more than 99% by taking silane as a medium. The gas diffusion cascade comprises: a plurality of gas diffusion and separation devices, and a high-speed magnetic levitation gas compressor located before each of the gas diffusion and separation devices in a flow direction of silane gas; and obtaining silicon-28 isotopes with the abundance of more than 99% by taking silane as a medium from the light fraction end of the gas diffusion cascade.

Description

用于以硅烷为介质制备丰度为99%以上的硅-28同位素的气 体扩散级联Gas diffusion cascade for the preparation of silicon-28 isotope abundance above 99% using silane as medium

技术领域Technical Field

本实用新型涉及一种用于以硅烷为介质制备丰度为99%以上的硅-28同位素的气体扩散级联,属于同位素分离技术领域。The utility model relates to a gas diffusion cascade for preparing silicon-28 isotope with an abundance of more than 99% by taking silane as a medium, and belongs to the technical field of isotope separation.

背景技术Background Art

稳定同位素目前在医疗、生物、农业、环境、工业制造、科研等领域有较为广泛的应用。硅元素在自然界有3种同位素,分别是硅-28(28Si)、硅-29(29Si)和硅-30(30Si),其天然丰度分别为92.22%、4.69%和3.09%。硅-28同位素主要应用于半导体、量子计算、计量学领域。使用99%以上丰度的硅-28材料制备半导体元件,可以减少硅-29和硅-30造成的晶格缺陷、降低声子散射、提高热导率;并且具有门电压更低、开关速度更快等优点,可用于制造高速CPU、大功率器件、高性能传感器等。硅-28同位素的核自旋为0,高丰度硅-28可用于制备量子信息设备中长自旋相干时间关键材料,去除29Si干扰。使用同位素纯的硅-28材料制备单晶球体,可以测量更精确的阿伏伽德罗常数值。Stable isotopes are currently widely used in the fields of medicine, biology, agriculture, environment, industrial manufacturing, scientific research, etc. There are three isotopes of silicon in nature, namely silicon-28 ( 28 Si), silicon-29 ( 29 Si) and silicon-30 ( 30 Si), with natural abundances of 92.22%, 4.69% and 3.09% respectively. Silicon-28 isotopes are mainly used in semiconductors, quantum computing, and metrology. The use of silicon-28 materials with an abundance of more than 99% to prepare semiconductor components can reduce lattice defects caused by silicon-29 and silicon-30, reduce phonon scattering, and improve thermal conductivity; and it has the advantages of lower gate voltage and faster switching speed, and can be used to manufacture high-speed CPUs, high-power devices, high-performance sensors, etc. The nuclear spin of silicon-28 isotopes is 0. High-abundance silicon-28 can be used to prepare key materials with long spin coherence time in quantum information devices to remove 29 Si interference. Using isotopically pure silicon-28 material to prepare single crystal spheres can measure more accurate values of Avogadro's constant.

在实际应用中,对于硅-28同位素材料的丰度要求很高,通常要求硅-28同位素的丰度高于99%,有时甚至要求达到99.7%以上。硅-28同位素的天然丰度为92.22%。目前国内外使用低温精馏法(SiH4、SiCl4或SiH3CH3体系)、气体离心法(介质为SiF4或SiHCl3)、化学交换法(SiF4与不同络合剂的分离体系)、激光法(Si2F6)分离硅同位素的研究取得了一定的成果,但是硅同位素的工业化生产研究尚未实现突破。硅同位素的低温精馏法分离系数较小,气体离心法分离轻气体的效率较低,激光分离法产量很低、成本较高,用于工业化生产的经济性均不佳。In practical applications, the abundance of silicon-28 isotope materials is very high, usually requiring the abundance of silicon-28 isotope to be higher than 99%, and sometimes even requiring it to reach more than 99.7%. The natural abundance of silicon-28 isotope is 92.22%. At present, the research on separation of silicon isotopes using cryogenic distillation (SiH 4 , SiCl 4 or SiH 3 CH 3 system), gas centrifugation (medium is SiF 4 or SiHCl 3 ), chemical exchange (separation system of SiF 4 and different complexing agents), and laser method (Si 2 F 6 ) at home and abroad has achieved certain results, but the research on industrial production of silicon isotopes has not yet achieved a breakthrough. The separation coefficient of silicon isotope cryogenic distillation method is small, the efficiency of gas centrifugation method in separating light gas is low, and the output of laser separation method is very low and the cost is high, and the economic efficiency of industrial production is not good.

早期金属多孔膜广泛应用于铀同位素扩散分离,但成本较高;有机高分子膜性能优良、成本极低,在工业制造中得到了大规模应用,但是在高丰度的硅-28同位素制造中的应用还缺少研究。Early metal porous membranes were widely used in the diffusion separation of uranium isotopes, but they were relatively expensive. Organic polymer membranes have excellent performance and extremely low cost, and have been widely used in industrial manufacturing. However, there is still a lack of research on their application in the manufacture of high-abundance silicon-28 isotopes.

另外,由于针对不同气体介质和/或不同目标同位素,气体扩散级联的设计与运行有很大的区别,因此,不能理所当然地认为可以将针对某一种气体介质和/或某一种目标同位素的气体扩散级联应用于另一种气体介质和/或另一种目标同位素。In addition, since the design and operation of gas diffusion cascades are very different for different gas media and/or different target isotopes, it cannot be taken for granted that a gas diffusion cascade for a certain gas medium and/or a certain target isotope can be applied to another gas medium and/or another target isotope.

实用新型内容Utility Model Content

实用新型要解决的问题Problems to be solved by utility models

本实用新型的目的在于提供一种用于以硅烷为介质制备高丰度硅-28同位素的气体扩散级联,该气体扩散级联的分离系数大、流量大、成本低,适于工业化应用,进一步地,还可同步地得到硅-30同位素副产品。The utility model aims to provide a gas diffusion cascade for preparing high-abundance silicon-28 isotope using silane as a medium. The gas diffusion cascade has a large separation coefficient, a large flow rate, and a low cost, and is suitable for industrial application. Furthermore, a silicon-30 isotope by-product can be obtained synchronously.

用于解决问题的方案Solutions for solving problems

根据潜心研究,发现通过以下技术方案的实施,能够解决上述技术问题:Through careful research, it is found that the above technical problems can be solved by implementing the following technical solutions:

[1].一种用于以硅烷为介质制备丰度为99%以上的硅-28同位素的气体扩散级联,其特征在于,包括:[1] A gas diffusion cascade for preparing silicon-28 isotope with an abundance of more than 99% using silane as a medium, characterized in that it comprises:

多个气体扩散分离装置,和a plurality of gas diffusion separation devices, and

在硅烷气体的流动方向上位于每个所述气体扩散分离装置之前的高速磁悬浮气体压缩机;a high-speed magnetically suspended gas compressor located before each of the gas diffusion separation devices in the flow direction of the silane gas;

从所述气体扩散级联的轻馏分端得到以天然丰度的硅烷为介质制备的丰度为99%以上的硅-28同位素。From the light fraction end of the gas diffusion cascade, silicon-28 isotope with an abundance of more than 99% is obtained, which is prepared using natural abundance silane as a medium.

[2].根据[1]所述的气体扩散级联,其中,所述气体扩散级联由通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数为1.009~1.011的气体扩散分离装置构成:将多个气体扩散分离装置并联以构成分离级,再将多个所述分离级串联。[2] A gas diffusion cascade according to [1], wherein the gas diffusion cascade is composed of a gas diffusion separation device having a silane basic total separation coefficient of 1.009 to 1.011 obtained by experimental measurement of a four-stage full reflux diffusion cascade: a plurality of gas diffusion separation devices are connected in parallel to form a separation stage, and a plurality of the separation stages are then connected in series.

[3].根据[2]所述的气体扩散级联,其中,通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数不小于1.010。[3] A gas diffusion cascade according to [2], wherein the silane-based total separation coefficient measured by a four-stage full reflux diffusion cascade experiment is not less than 1.010.

[4].根据[1]~[3]中任一项所述的气体扩散级联,其中,所述气体扩散级联的总级数为200~600级,优选地为280~300级。[4] The gas diffusion cascade according to any one of [1] to [3], wherein the total number of stages of the gas diffusion cascade is 200 to 600, preferably 280 to 300.

[5].根据[1]~[3]中任一项所述的气体扩散级联,其中,所述气体扩散级联的供料级位于距离重馏分端3~100级,优选地,5~50级的位置,所述气体扩散级联的轻馏分流量为所述供料级的供料流量的0.01~0.05倍,所述气体扩散级联的总流量为所述供料级的供料流量的1800~3500倍。[5] A gas diffusion cascade according to any one of [1] to [3], wherein the feed stage of the gas diffusion cascade is located 3 to 100 stages away from the heavy fraction end, preferably 5 to 50 stages away, the light fraction flow rate of the gas diffusion cascade is 0.01 to 0.05 times the feed flow rate of the feed stage, and the total flow rate of the gas diffusion cascade is 1800 to 3500 times the feed flow rate of the feed stage.

[6].根据[1]~[3]中任一项所述的气体扩散级联,其中,从所述气体扩散级联的重馏分端中得到的重馏分的硅-28同位素丰度小于92.1%,所述重馏分包含硅-30同位素副产品。[6] A gas diffusion cascade according to any one of [1] to [3], wherein the heavy fraction obtained from the heavy fraction end of the gas diffusion cascade has a silicon-28 isotope abundance of less than 92.1%, and the heavy fraction contains a silicon-30 isotope byproduct.

[7].根据[1]~[3]中任一项所述的气体扩散级联,其中,所述天然丰度的硅烷气体的纯度为高于99.9%。[7] A gas diffusion cascade according to any one of [1] to [3], wherein the purity of the naturally abundant silane gas is higher than 99.9%.

实用新型的效果Effect of utility model

本实用新型中,可以在气体扩散级联上利用气体扩散法以硅烷为介质分离硅-28同位素,分离系数大、流量大、成本低,适于工业化应用,进一步地,在重馏分端可以得到硅-30同位素副产品。In the utility model, the silicon-28 isotope can be separated by using the gas diffusion method in the gas diffusion cascade with silane as the medium, and the separation coefficient is large, the flow rate is large, and the cost is low, which is suitable for industrial application. Furthermore, the silicon-30 isotope byproduct can be obtained at the heavy fraction end.

具体地,作为分离介质的硅烷(SiH4),与其他潜在的可用于作为Si同位素分离介质的物质相比,相对分子质量小,气体扩散分离系数相对大。气体扩散分离过程为物理分离过程,不引入其它杂质。而且,高速磁悬浮压缩机能够有效压缩轻气体。因此,本实用新型的气体扩散级联,由于使用高速磁悬浮压缩机有效压缩轻气体,并采用分离系数相对大的硅烷作为分离介质,所以具有流量大、效率高、制备出的高丰度硅-28同位素纯度高等优点。Specifically, silane (SiH 4 ) as a separation medium has a smaller relative molecular mass and a relatively large gas diffusion separation coefficient compared to other potential substances that can be used as Si isotope separation media. The gas diffusion separation process is a physical separation process and does not introduce other impurities. Moreover, a high-speed magnetic levitation compressor can effectively compress light gases. Therefore, the gas diffusion cascade of the utility model has the advantages of large flow, high efficiency, and high purity of the prepared high-abundance silicon-28 isotope, because it uses a high-speed magnetic levitation compressor to effectively compress light gases and adopts silane with a relatively large separation coefficient as the separation medium.

在上述的基础上,本实用新型能够通过灵活调整气体扩散级联的长度(级数)和流量(轻馏分流量、总流量等)来调整目标同位素丰度(甚至可实现99.9%以上的丰度)。另一方面,本实用新型中,甚至在级联长度不超过600级的情况下,便可将硅-28同位素丰度浓缩到99%以上,具有良好的经济性。On the basis of the above, the utility model can adjust the target isotope abundance (even achieving an abundance of more than 99.9%) by flexibly adjusting the length (number of stages) and flow rate (light fraction flow rate, total flow rate, etc.) of the gas diffusion cascade. On the other hand, in the utility model, even when the cascade length does not exceed 600 stages, the silicon-28 isotope abundance can be concentrated to more than 99%, which has good economic efficiency.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1为依照本实用新型的实施方案的单级单个分离器内气体过膜原理示意图。FIG1 is a schematic diagram showing the principle of gas passing through a membrane in a single-stage single separator according to an embodiment of the present utility model.

图2为依照本实用新型的实施方案的气体扩散级联制备高丰度硅-28同位素的原理示意图。FIG. 2 is a schematic diagram showing the principle of preparing high-abundance silicon-28 isotope by gas diffusion cascade according to an embodiment of the present invention.

图3为依照本实用新型的实施例的以硅烷为介质制备高丰度硅-28同位素的制备中所使用的双管道扩散级联装置图。FIG. 3 is a diagram of a double-pipeline diffusion cascade device used in the preparation of high-abundance silicon-28 isotope using silane as a medium according to an embodiment of the present invention.

图4为示出本实用新型的实施方案的各分离级的串联形式的示意图。FIG. 4 is a schematic diagram showing a series connection of the separation stages according to an embodiment of the present invention.

图5为依照本实用新型的实施例的气体扩散级联各级硅-28同位素丰度分布图。FIG. 5 is a diagram showing the isotope abundance distribution of silicon-28 at each stage of the gas diffusion cascade according to an embodiment of the present invention.

具体实施方式DETAILED DESCRIPTION

以下将详细说明本实用新型的各种示例性实施例、特征和方面。在这里专用的词“示例性”意为“用作例子、实施例或说明性”。这里作为“示例性”所说明的任何实施例不必解释为优于或好于其它实施例。Various exemplary embodiments, features and aspects of the present invention will be described in detail below. The word "exemplary" used herein means "used as an example, embodiment or illustrative". Any embodiment described herein as "exemplary" is not necessarily to be interpreted as being superior or better than other embodiments.

另外,为了更好地说明本实用新型,在下文的具体实施方式中给出了众多的具体细节。本领域技术人员应当理解,没有某些具体细节,本实用新型同样可以实施。在另外一些实例中,对于本领域技术人员熟知的方法、手段、器材和步骤未作详细描述,以便于凸显本实用新型的主旨。In addition, in order to better illustrate the utility model, many specific details are given in the specific embodiments below. It should be understood by those skilled in the art that the utility model can also be implemented without certain specific details. In other examples, methods, means, equipment and steps well known to those skilled in the art are not described in detail in order to highlight the main purpose of the utility model.

如无特殊声明,本说明书中所使用的单位均为国际标准单位,并且本实用新型中出现的数值,数值范围,均应当理解为包含了工业生产中所不可避免的系统性误差或设计约束内近似于相应值。本文可提供包含特定值的参数的示范,但这些参数无需确切等于相应的值。Unless otherwise stated, the units used in this specification are all international standard units, and the numerical values and numerical ranges appearing in the utility model should be understood to include the inevitable systematic errors in industrial production or approximate corresponding values within the design constraints. This article may provide demonstrations of parameters containing specific values, but these parameters do not need to be exactly equal to the corresponding values.

本说明书中,实施例中提到的方向用语,例如“上”、“下”、“前”、“后”、“左”、“右”等,仅是参考附图的方向,并非用来限制本实用新型的保护范围。In this specification, directional terms mentioned in the embodiments, such as "upper", "lower", "front", "back", "left", "right", etc., are only used to refer to the directions of the drawings and are not intended to limit the scope of protection of the present utility model.

本说明书中,使用“可以”表示的含义包括了进行某种处理以及不进行某种处理两方面的含义。In this specification, the word "may" includes both performing a certain process and not performing a certain process.

本说明书中,所提及的“一些具体/优选的实施方案”、“另一些具体/优选的实施方案”、“实施方案”等是指所描述的与该实施方案有关的特定要素(例如,特征、结构、性质和/或特性)包括在此处所述的至少一种实施方案中,并且可存在于其它实施方案中或者可不存在于其它实施方案中。另外,应理解,所述要素可以任何合适的方式组合在各种实施方案中。In this specification, the references to "some specific/preferred embodiments", "other specific/preferred embodiments", "embodiments", etc., mean that the specific elements (e.g., features, structures, properties and/or characteristics) described in connection with the embodiments are included in at least one embodiment described herein, and may or may not exist in other embodiments. In addition, it should be understood that the elements may be combined in various embodiments in any suitable manner.

本说明书中,使用“数值A~数值B”表示的数值范围是指包含端点数值A、B的范围。In this specification, the numerical range expressed using "a numerical value A to a numerical value B" means a range including the endpoints A and B.

本实用新型的用于以硅烷为介质制备丰度为99%以上的硅-28同位素的气体扩散级联包括:多个气体扩散分离装置,和在硅烷气体的流动方向上位于每个所述气体扩散分离装置之前的高速磁悬浮气体压缩机;从所述气体扩散级联的轻馏分端得到以天然丰度的硅烷为介质制备的丰度为99%以上的硅-28同位素。The utility model discloses a gas diffusion cascade for preparing silicon-28 isotopes with an abundance of more than 99% by using silane as a medium, comprising: a plurality of gas diffusion separation devices, and a high-speed magnetic suspension gas compressor located before each of the gas diffusion separation devices in the flow direction of the silane gas; silicon-28 isotopes with an abundance of more than 99% prepared by using silane with natural abundance as a medium are obtained from the light fraction end of the gas diffusion cascade.

通过采用上述气体扩散级联,本实用新型提供了用于以硅烷为介质制备高丰度硅-28同位素的气体扩散级联,该气体扩散级联的分离系数大、流量大、成本低,适于工业化应用。By adopting the gas diffusion cascade, the utility model provides a gas diffusion cascade for preparing high-abundance silicon-28 isotope using silane as a medium. The gas diffusion cascade has a large separation coefficient, a large flow rate, and a low cost, and is suitable for industrial application.

图1为依照本实用新型的实施方案的气体扩散级联制备高丰度硅-28同位素的原理示意图。FIG1 is a schematic diagram showing the principle of preparing high-abundance silicon-28 isotope by gas diffusion cascade according to an embodiment of the present invention.

在本实用新型的实施方案中,气体扩散级联是由多个气体扩散分离装置串和/或并联构成,其具体串、并联构成方式的一个实例如图3所示。In the embodiment of the present utility model, the gas diffusion cascade is composed of a plurality of gas diffusion separation devices connected in series and/or in parallel. An example of a specific series and parallel configuration is shown in FIG3 .

气体扩散分离装置对工作介质的分离为相对分离,而非绝对分开,仅通过单个分离级通常无法得到最终产品所需的丰度,因此往往采用如图4所示的多个分离级串联的连接方式,组成气体扩散级联,其中,每个分离级内部可以由多个气体扩散分离装置并联构成,图4中未示出各分离级内部多个气体扩散分离装置的并联形式。在一些优选的实施方案中,将多个气体扩散分离装置并联构成分离级,再将多个分离级串联,能够实现目标同位素丰度的逐级递增,最终达到要求的产品丰度;多个气体扩散分离装置的并联,能够增加单级的流量,以达到工业生产所需的产量。在上述气体扩散分离装置并联的过程中,每台气体扩散分离装置在水力学参数方面不受同一分离级其它机器的干扰,从而在原理上便于进行生产上的放大设计。The separation of the working medium by the gas diffusion separation device is a relative separation, not an absolute separation. It is usually impossible to obtain the required abundance of the final product through only a single separation stage. Therefore, a plurality of separation stages are often connected in series as shown in FIG4 to form a gas diffusion cascade, wherein each separation stage can be composed of a plurality of gas diffusion separation devices in parallel. FIG4 does not show the parallel connection of the plurality of gas diffusion separation devices in each separation stage. In some preferred embodiments, a plurality of gas diffusion separation devices are connected in parallel to form a separation stage, and then the plurality of separation stages are connected in series, so that the target isotope abundance can be gradually increased, and the required product abundance can be finally achieved; the parallel connection of a plurality of gas diffusion separation devices can increase the flow rate of a single stage to achieve the output required for industrial production. In the process of connecting the above-mentioned gas diffusion separation devices in parallel, each gas diffusion separation device is not interfered with by other machines in the same separation stage in terms of hydraulic parameters, so that it is convenient to carry out a scaled-up design in production in principle.

各个气体扩散分离装置以SiH4通过多孔有机膜的同位素分离效应为基础进行分离。图2为依照本实用新型的实施例的单级单个分离器内气体过膜原理示意图。Each gas diffusion separation device performs separation based on the isotope separation effect of SiH 4 passing through a porous organic membrane. FIG2 is a schematic diagram of the principle of gas passing through a membrane in a single-stage single separator according to an embodiment of the utility model.

在一些优选的实施方案中,气体扩散分离装置的通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数为1.009~1.011。In some preferred embodiments, the silane-based total separation coefficient of the gas diffusion separation device measured through a four-stage total reflux diffusion cascade experiment is 1.009 to 1.011.

在一些特别优选的实施方案中,气体扩散级联由通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数为1.009~1.011的气体扩散分离装置构成:将多个气体扩散分离装置并联以构成分离级,再将多个所述分离级串联。In some particularly preferred embodiments, the gas diffusion cascade is composed of a gas diffusion separation device with a silane basic total separation coefficient of 1.009 to 1.011 obtained by measuring a four-stage full reflux diffusion cascade experiment: multiple gas diffusion separation devices are connected in parallel to form a separation stage, and then multiple of the separation stages are connected in series.

对于分离级,掌握了膜前压强、膜前后压比与分离系数的关系,发现分离系数随膜前压强减小而增大、随膜前后压比增大而增大。基于此,通过进一步合理设计,在一些优选的实施方案中,本实用新型的气体扩散级联中,通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数优选地不小于1.010。For the separation stage, the relationship between the pressure before the membrane, the pressure ratio before and after the membrane and the separation coefficient is mastered, and it is found that the separation coefficient increases with the decrease of the pressure before the membrane and increases with the increase of the pressure ratio before and after the membrane. Based on this, through further reasonable design, in some preferred embodiments, in the gas diffusion cascade of the utility model, the silane-based total separation coefficient obtained by the four-stage full reflux diffusion cascade experiment is preferably not less than 1.010.

本实用新型中,四级全回流扩散级联实验测量硅烷基本全分离系数通过本领域常见的质谱分析方法进行,具体实施途径不限。基本全分离系数的定义为单位摩尔质量的差对应的分离系数。In the present invention, the four-stage total reflux diffusion cascade experiment is performed to measure the basic total separation coefficient of silane by a mass spectrometry method commonly used in the art, and the specific implementation method is not limited. The basic total separation coefficient is defined as the separation coefficient corresponding to the difference in unit molar mass.

本实用新型中,对于气体扩散级联的总级数没有特别限制,可根据实际需要而适当调节。在一些优选的实施方案中,所述气体扩散级联的总级数可以为200~600级,所述气体扩散级联的总级数更优选地为280~300级。In the present invention, there is no particular restriction on the total number of gas diffusion cascades, which can be appropriately adjusted according to actual needs. In some preferred embodiments, the total number of gas diffusion cascades can be 200 to 600, and the total number of gas diffusion cascades is more preferably 280 to 300.

在一些优选的实施方案中,所述气体扩散级联中,优选地,供料级位于距离重馏分端3~100级的位置,更优选地,供料级位于距离重馏分端5~50级的位置,进一步优选地,供料级位于距离重馏分端5~30级的位置。In some preferred embodiments, in the gas diffusion cascade, preferably, the feed stage is located at a position 3 to 100 stages away from the heavy fraction end, more preferably, the feed stage is located at a position 5 to 50 stages away from the heavy fraction end, further preferably, the feed stage is located at a position 5 to 30 stages away from the heavy fraction end.

本实用新型中,对于气体扩散级联的轻馏分流量没有特别限制,可根据实际需要而适当调节。在一些优选的实施方案中,所述气体扩散级联的轻馏分流量优选地为所述供料级的供料流量的0.01~0.05倍,更优选地,0.015~0.045倍,进一步优选地,0.02~0.04倍。In the present invention, there is no particular restriction on the light fraction flow rate of the gas diffusion cascade, which can be appropriately adjusted according to actual needs. In some preferred embodiments, the light fraction flow rate of the gas diffusion cascade is preferably 0.01 to 0.05 times the feed flow rate of the feed stage, more preferably 0.015 to 0.045 times, and further preferably 0.02 to 0.04 times.

本实用新型中,对于气体扩散级联的总流量没有特别限制,可根据实际需要而适当调节。在一些优选的实施方案中,所述气体扩散级联的总流量为所述供料级的供料流量的1800~3500倍,更优选地为2000~3000倍。In the present invention, there is no particular restriction on the total flow rate of the gas diffusion cascade, which can be appropriately adjusted according to actual needs. In some preferred embodiments, the total flow rate of the gas diffusion cascade is 1800 to 3500 times the feed flow rate of the feed stage, and more preferably 2000 to 3000 times.

在一些优选的实施方案中,从所述气体扩散级联的重馏分端中得到的重馏分的硅-28同位素丰度小于92.1%,进一步地,所述重馏分包含硅-30同位素副产品。In some preferred embodiments, the heavy fraction obtained from the heavy fraction end of the gas diffusion cascade has a silicon-28 isotope abundance of less than 92.1%, and further, the heavy fraction contains a silicon-30 isotope byproduct.

在一些优选的实施方案中,天然丰度的硅烷气体的纯度为高于99.9%。天然丰度的硅烷气体可以为市售品。In some preferred embodiments, the purity of natural abundance silane gas is greater than 99.9%.Natural abundance silane gas can be commercially available.

在一些优选的实施方案中,所使用的高速磁悬浮压缩机优选地为可用于负压条件下的高速磁悬浮压缩机,例如,CN209510664U中记载的用于负压条件下的高速磁悬浮压缩机(该专利的内容作为参考全部地并入本文中)。In some preferred embodiments, the high-speed magnetic levitation compressor used is preferably a high-speed magnetic levitation compressor that can be used under negative pressure conditions, for example, the high-speed magnetic levitation compressor for use under negative pressure conditions described in CN209510664U (the contents of this patent are incorporated herein by reference in their entirety).

另外,每个气体扩散分离装置之前,可存在一个或多个(例如2~4个)高速磁悬浮压缩机。In addition, there may be one or more (eg, 2 to 4) high-speed magnetic levitation compressors before each gas diffusion separation device.

在另一些优选的实施方案中,经过高速磁悬浮压缩机压缩之后,硅烷气体经过气体扩散分离装置前后(即,过膜前后)的单级压比至少为4.5,更优选地为4.8以上,甚至高达5.0以上,例如,5.2。In other preferred embodiments, after compression by the high-speed magnetic levitation compressor, the single-stage pressure ratio of the silane gas before and after passing through the gas diffusion separation device (i.e., before and after passing through the membrane) is at least 4.5, more preferably above 4.8, or even as high as above 5.0, for example, 5.2.

以下参照图5并结合具体实施例对本实用新型提供的用于以硅烷为介质制备高丰度硅-28同位素的气体扩散级联进行详细说明。但是本领域技术人员将会理解,下列实施例仅用于说明本实用新型,而不应视为限定本实用新型的范围。实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规产品。The following is a detailed description of the gas diffusion cascade for preparing high-abundance silicon-28 isotopes using silane as a medium provided by the utility model with reference to FIG. 5 and in combination with specific embodiments. However, those skilled in the art will understand that the following embodiments are only used to illustrate the utility model and should not be regarded as limiting the scope of the utility model. If no specific conditions are specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturer are followed. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.

将化学纯度高于99.9%的天然丰度的硅烷供入气体扩散级联,在气体扩散级联轻馏分端得到硅-28同位素丰度为99%以上的硅烷。以SiH4通过多孔有机膜的同位素分离效应为基础,使用高速磁悬浮气体压缩机实现SiH4气体的有效压缩,利用气体扩散法进行硅-28同位素的生产制备。具体实施例如下。Silane with a chemical purity higher than 99.9% of natural abundance is fed into a gas diffusion cascade, and silane with a silicon-28 isotope abundance of more than 99% is obtained at the light fraction end of the gas diffusion cascade. Based on the isotope separation effect of SiH 4 passing through a porous organic membrane, a high-speed magnetically suspended gas compressor is used to achieve effective compression of SiH 4 gas, and the production and preparation of silicon-28 isotope is carried out by gas diffusion method. Specific embodiments are as follows.

图3为依照本实用新型的实施例的以硅烷为介质制备高丰度硅-28同位素的制备中所使用的双管道扩散级联装置图。FIG. 3 is a diagram of a double-pipeline diffusion cascade device used in the preparation of high-abundance silicon-28 isotope using silane as a medium according to an embodiment of the present invention.

气体扩散级联由硅烷基本全分离系数为1.010的气体扩散分离装置串、并联构成,总级数为291级,其中供料级位于距离重馏分端10级的位置。The gas diffusion cascade is composed of gas diffusion separation devices with a silane-based total separation coefficient of 1.010 connected in series and in parallel, with a total number of 291 stages, wherein the feed stage is located 10 stages away from the heavy fraction end.

气体扩散级联轻馏分流量为供料流量的0.0366倍,气体扩散级联总流量为供料流量的2716倍,重馏分中硅-28同位素丰度为91.96%。气体扩散级联中硅-28同位素在各级的丰度分布如图5所示。The light fraction flow rate of the gas diffusion cascade is 0.0366 times the feed flow rate, the total gas diffusion cascade flow rate is 2716 times the feed flow rate, and the silicon-28 isotope abundance in the heavy fraction is 91.96%. The abundance distribution of silicon-28 isotopes at each stage in the gas diffusion cascade is shown in Figure 5.

从上述实施例可以看出,本实用新型提供的用于以硅烷为介质制备高丰度硅-28同位素的气体扩散级联,具有流量大、效率高、成本低的优点,可以用于制备丰度为99%以上的硅-28同位素。同时,气体扩散分离过程为物理分离过程,不引入其它杂质,制备出的高丰度硅-28同位素化学纯度高。将该气体扩散级联用于高丰度硅-28同位素的制备,适于工业应用。It can be seen from the above embodiments that the gas diffusion cascade provided by the utility model for preparing high-abundance silicon-28 isotopes using silane as a medium has the advantages of large flow, high efficiency and low cost, and can be used to prepare silicon-28 isotopes with an abundance of more than 99%. At the same time, the gas diffusion separation process is a physical separation process, and no other impurities are introduced, and the prepared high-abundance silicon-28 isotope has a high chemical purity. The gas diffusion cascade is used for the preparation of high-abundance silicon-28 isotopes, which is suitable for industrial applications.

以上已经描述了本实用新型的各实施例,上述说明是示例性的,并非穷尽性的,并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下,对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。本文中所用术语的选择,旨在最好地解释各实施例的原理、实际应用或对市场中的技术改进,或者使本技术领域的其它普通技术人员能理解本文披露的各实施例。The embodiments of the present invention have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or technical improvements in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims (9)

1.一种用于以硅烷为介质制备丰度为99%以上的硅-28同位素的气体扩散级联,其特征在于,包括:1. A gas diffusion cascade for preparing silicon-28 isotope with an abundance of more than 99% using silane as a medium, characterized in that it comprises: 多个气体扩散分离装置,和a plurality of gas diffusion separation devices, and 在硅烷气体的流动方向上位于每个所述气体扩散分离装置之前的高速磁悬浮气体压缩机;a high-speed magnetically suspended gas compressor located before each of the gas diffusion separation devices in the flow direction of the silane gas; 从所述气体扩散级联的轻馏分端得到以天然丰度的硅烷为介质制备的丰度为99%以上的硅-28同位素。From the light fraction end of the gas diffusion cascade, silicon-28 isotope with an abundance of more than 99% is obtained, which is prepared using natural abundance silane as a medium. 2.根据权利要求1所述的气体扩散级联,其特征在于,所述气体扩散级联由通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数为1.009~1.011的气体扩散分离装置构成:将多个气体扩散分离装置并联以构成分离级,再将多个所述分离级串联。2. The gas diffusion cascade according to claim 1 is characterized in that the gas diffusion cascade is composed of a gas diffusion separation device with a silane basic total separation coefficient of 1.009 to 1.011 obtained by measuring a four-stage full reflux diffusion cascade experiment: a plurality of gas diffusion separation devices are connected in parallel to form a separation stage, and then a plurality of the separation stages are connected in series. 3.根据权利要求2所述的气体扩散级联,其特征在于,通过四级全回流扩散级联实验测量得到的硅烷基本全分离系数不小于1.010。3. The gas diffusion cascade according to claim 2 is characterized in that the silane basic total separation coefficient obtained by measuring the four-stage full reflux diffusion cascade experiment is not less than 1.010. 4.根据权利要求1~3中任一项所述的气体扩散级联,其特征在于,所述气体扩散级联的总级数为200~600级。4 . The gas diffusion cascade according to claim 1 , wherein the total number of stages of the gas diffusion cascade is 200 to 600. 5.根据权利要求4所述的气体扩散级联,其特征在于,所述气体扩散级联的总级数为280~300级。5 . The gas diffusion cascade according to claim 4 , wherein the total number of stages of the gas diffusion cascade is 280 to 300. 6.根据权利要求1~3中任一项所述的气体扩散级联,其特征在于,所述气体扩散级联的供料级位于距离重馏分端3~100级的位置,所述气体扩散级联的轻馏分流量为所述供料级的供料流量的0.01~0.05倍,所述气体扩散级联的总流量为所述供料级的供料流量的1800~3500倍。6. The gas diffusion cascade according to any one of claims 1 to 3, characterized in that the feed stage of the gas diffusion cascade is located 3 to 100 stages away from the heavy fraction end, the light fraction flow rate of the gas diffusion cascade is 0.01 to 0.05 times the feed flow rate of the feed stage, and the total flow rate of the gas diffusion cascade is 1800 to 3500 times the feed flow rate of the feed stage. 7.根据权利要求6所述的气体扩散级联,其特征在于,所述气体扩散级联的供料级位于距离重馏分端5~50级的位置。7. The gas diffusion cascade according to claim 6, characterized in that the feed stage of the gas diffusion cascade is located 5 to 50 stages away from the heavy fraction end. 8.根据权利要求1~3中任一项所述的气体扩散级联,其特征在于,从所述气体扩散级联的重馏分端中得到的重馏分的硅-28同位素丰度小于92.1%,所述重馏分包含硅-30同位素副产品。8. The gas diffusion cascade according to any one of claims 1 to 3, characterized in that the heavy fraction obtained from the heavy fraction end of the gas diffusion cascade has a silicon-28 isotope abundance of less than 92.1%, and the heavy fraction contains a silicon-30 isotope byproduct. 9.根据权利要求1~3中任一项所述的气体扩散级联,其特征在于,所述天然丰度的硅烷气体的纯度为高于99.9%。9. A gas diffusion cascade according to any one of claims 1 to 3, characterised in that the purity of the natural abundance silane gas is higher than 99.9%.
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