TW202229207A - Neutron moderator material and method for producing the same - Google Patents

Neutron moderator material and method for producing the same Download PDF

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TW202229207A
TW202229207A TW110101999A TW110101999A TW202229207A TW 202229207 A TW202229207 A TW 202229207A TW 110101999 A TW110101999 A TW 110101999A TW 110101999 A TW110101999 A TW 110101999A TW 202229207 A TW202229207 A TW 202229207A
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powder
fluoride
metal
aluminum
neutron
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TWI804800B (en
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陳榮志
劉正同
管琪芸
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中國鋼鐵股份有限公司
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The present invention relates to a neutron moderator material and a method for producing the same. Metal fluoride powders, lithium fluoride powders and aluminum metal powders are utilized to fabricate the neutron moderator material, and a composite powder is formed by multiple stages of dry mixing processes. Next, the composite powder is subjected to a hot pressing process to form the neutron moderator material. The neutron moderator material has fine and uniform structures and high relative density, therefore being applied in a boron neutron capture therapy device.

Description

中子減速材料及其製作方法Neutron deceleration material and method of making the same

本發明係有關一種複合材料,特別是提供一種中子減速材料及其製作方法。The present invention relates to a composite material, and in particular provides a neutron deceleration material and a manufacturing method thereof.

標靶放射線治療係常用之癌症治療手段,其中標靶放射線治療主要係利用硼中子捕獲治療(Boron Neutron Capture Therapy;BNCT)的機制來進行。BNCT之原理主要係先將親癌細胞的含硼藥物注入癌症患者之身體內,以藉由血液循環與癌細胞結合。當癌細胞位置聚集濃度足夠高的含硼藥物時,從原子爐或加速器型的中子束源產生器射出能量適當的熱中子束,並照射在腫瘤部位。由於熱中子會與含硼藥物產生核反應,而***為具有高生物破壞能力之輻射性粒子,因此可破壞癌細胞的DNA結構。由於此些輻射性粒子的射程不超過單一癌細胞的直徑範圍,故在破壞癌細胞之DNA結構時,輻射性粒子對正常細胞的傷害可被降到最低。據此,癌細胞附近的正常細胞組織可被保護。Targeted radiation therapy is a commonly used cancer treatment method, wherein the targeted radiation therapy is mainly performed by the mechanism of Boron Neutron Capture Therapy (BNCT). The principle of BNCT is mainly to inject cancer-friendly boron-containing drugs into the body of cancer patients to combine with cancer cells through blood circulation. When a sufficiently high concentration of boron-containing drugs is accumulated at the cancer cell site, a thermal neutron beam with appropriate energy is emitted from a nuclear furnace or accelerator-type neutron beam source generator and irradiated at the tumor site. Because thermal neutrons will have a nuclear reaction with boron-containing drugs and split into radioactive particles with high biological destructive ability, they can damage the DNA structure of cancer cells. Since the range of these radioactive particles does not exceed the diameter range of a single cancer cell, the damage of the radioactive particles to normal cells can be minimized when destroying the DNA structure of cancer cells. According to this, normal cell tissues near cancer cells can be protected.

適合BNCT的中子能量為1 eV至10 keV,故中子束源產生器所產生的高能中子射線可透過減速材料(moderator materials)進行減速,並降低其能量。一般係採用金屬氟化物-鋁-氟化鋰複合材料作為熱中子減速材料,其中金屬鋁的含量為20體積百分比至50體積百分比,氟化鋰含量小於2體積百分比,而其他則為金屬氟化物。一個先前技術提出一種BNCT熱中子減速材料,其組成為氟化鋁-鋁-氟化鋰,且氟化鋰的含量為1體積百分比。此先前技術係採用熱均壓製程(Hot Isostatic Pressing;HIP)來製作此複合材料。然而,此先前技術並未明確揭示如何將含量極少的氟化鋰陶瓷粉體均勻地分散在複合材料中,且其並未明確揭示如何利用熱均壓製程來製作中子減速材料。另外,熱均壓製程一般須先將粉體填充至金屬容器中,並進行真空封罐(canning)。然後,將封罐的金屬容器放入熱均壓設備中,利用氣體作為壓力介質,以對金屬容器進行等向加壓,藉此完成複合材料的成型及緻密化。由於熱均壓製程受到金屬容器拘束力的影響,其得料率一般僅65%至80%,故具有較高之製造成本。The neutron energy suitable for BNCT is 1 eV to 10 keV, so the high-energy neutron rays generated by the neutron beam source generator can be decelerated by moderator materials and reduce their energy. Generally, metal fluoride-aluminum-lithium fluoride composite materials are used as thermal neutron deceleration materials, in which the content of metal aluminum is 20 volume percent to 50 volume percent, the lithium fluoride content is less than 2 volume percent, and the others are metal fluorides. . A prior art proposes a BNCT thermal neutron deceleration material whose composition is aluminum fluoride-aluminum-lithium fluoride, and the content of lithium fluoride is 1 volume percent. The prior art uses a Hot Isostatic Pressing (HIP) process to fabricate the composite. However, this prior art does not clearly disclose how to uniformly disperse the lithium fluoride ceramic powder with a very small content in the composite material, and it does not clearly disclose how to use the hot isopressing process to fabricate the neutron moderator material. In addition, in the hot isopressing process, the powder is generally filled into a metal container and vacuum sealed. Then, the sealed metal container is put into a hot equalizing equipment, and the metal container is isotropically pressurized by using gas as a pressure medium, thereby completing the molding and densification of the composite material. Because the hot isolating process is affected by the binding force of the metal container, the yield is generally only 65% to 80%, so it has a high manufacturing cost.

有鑑於此,亟須提供一種中子減速材料及其製作方法,以改進習知中子減速材料之製作方法具有低得料率的缺陷。In view of this, there is an urgent need to provide a neutron moderator material and a manufacturing method thereof, so as to improve the conventional manufacturing method of the neutron moderator material, which has the disadvantage of low yield.

因此,本發明之一態樣是在提供一種中子減速材料的製作方法,其藉由多階段之乾式混粉製程來混合粉體材料,並以熱壓製程緻密化複合粉體,而可製得組織均勻且緻密的中子減速材料。Therefore, one aspect of the present invention is to provide a method for manufacturing a neutron deceleration material, which can mix powder materials by a multi-stage dry powder mixing process, and densify the composite powder by a hot pressing process. A uniform and dense neutron deceleration material is obtained.

本發明之另一態樣是在提供一種中子減速材料,其係利用前述之製作方法所製得。Another aspect of the present invention is to provide a neutron deceleration material, which is produced by the aforementioned production method.

根據本發明之一態樣,提出一種中子減速材料的製作方法。此製作方法係先提供金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體。其中,金屬氟化物粉體不包含氟化鋰。基於中子減速材料為100體積百分比,金屬鋁粉體之用量為20體積百分比至50體積百分比,氟化鋰粉體之用量為0.5體積百分比至2體積百分比,且餘量為金屬氟化物粉體。然後,對氟化鋰粉體與一部分之金屬鋁粉體進行第一乾式混粉製程,以形成金屬鋁-氟化鋁複合粉體。接著,對金屬氟化物粉體、剩餘之金屬鋁粉體與前述之金屬鋁-氟化鋁複合粉體進行第二乾式混粉製程,以形成金屬氟化物-金屬鋁-氟化鋁複合粉體。之後,對金屬氟化物-金屬鋁-氟化鋁複合粉體進行熱壓製程,即可形成中子減速材料。According to an aspect of the present invention, a method for manufacturing a neutron decelerating material is provided. In this manufacturing method, metal fluoride powder, lithium fluoride powder and metal aluminum powder are firstly provided. However, the metal fluoride powder does not contain lithium fluoride. Based on 100 volume percent of the neutron moderator material, the amount of metal aluminum powder is 20 to 50 volume percent, the amount of lithium fluoride powder is 0.5 to 2 volume percent, and the balance is metal fluoride powder . Then, a first dry powder mixing process is performed on the lithium fluoride powder and a part of the metal aluminum powder to form a metal aluminum-aluminum fluoride composite powder. Next, a second dry mixing process is performed on the metal fluoride powder, the remaining metal aluminum powder and the aforementioned metal aluminum-aluminum fluoride composite powder to form a metal fluoride-metal aluminum-aluminum fluoride composite powder . After that, the metal fluoride-metal aluminum-aluminum fluoride composite powder is subjected to a hot pressing process to form a neutron deceleration material.

依據本發明之一些實施例,前述之金屬氟化物粉體包含氟化鎂、氟化鋁及/或氟化鈣。According to some embodiments of the present invention, the aforementioned metal fluoride powder includes magnesium fluoride, aluminum fluoride and/or calcium fluoride.

依據本發明之一些實施例,前述氟化鋰粉體之平均粒徑為1 μm至3 μm。According to some embodiments of the present invention, the average particle size of the lithium fluoride powder is 1 μm to 3 μm.

依據本發明之一些實施例,前述金屬鋁粉體之平均粒徑為5 μm至15 μm。According to some embodiments of the present invention, the average particle size of the aforementioned metal aluminum powder is 5 μm to 15 μm.

依據本發明之一些實施例,前述金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體之純度均大於99%。According to some embodiments of the present invention, the purity of the aforementioned metal fluoride powder, lithium fluoride powder and metal aluminum powder are all greater than 99%.

依據本發明之一些實施例,於進行前述之第一乾式混粉製程時,氟化鋰粉體與部分之金屬鋁粉體的體積比值為0.05至0.1。According to some embodiments of the present invention, when the aforementioned first dry powder mixing process is performed, the volume ratio of the lithium fluoride powder to a part of the metal aluminum powder is 0.05 to 0.1.

依據本發明之一些實施例,前述第一乾式混粉製程之混合時間為0.5小時至1小時,而第二乾式混粉製程之混合時間為0.5小時至1小時。According to some embodiments of the present invention, the mixing time of the first dry powder mixing process is 0.5 hour to 1 hour, and the mixing time of the second dry powder mixing process is 0.5 hour to 1 hour.

依據本發明之一些實施例,前述熱壓製程之溫度為550℃至620℃,而熱壓製程之壓力為5 MPa至55 MPa。According to some embodiments of the present invention, the temperature of the aforementioned hot pressing process is 550° C. to 620° C., and the pressure of the hot pressing process is 5 MPa to 55 MPa.

依據本發明之一些實施例,前述熱壓製程之時間為1小時至6小時。According to some embodiments of the present invention, the time of the aforementioned hot pressing process is 1 hour to 6 hours.

根據本發明之另一態樣,提出一種中子減速材料,其係藉由前述之製作方法所製得。其中,中子減速材料之相對密度不小於99.5%,且中子減速材料中最大顆粒的粒徑係不大於500 μm。According to another aspect of the present invention, a neutron deceleration material is provided, which is prepared by the aforementioned manufacturing method. Among them, the relative density of the neutron deceleration material is not less than 99.5%, and the particle size of the largest particle in the neutron deceleration material is not greater than 500 μm.

應用本發明中子減速材料及其製作方法,其係多階段地混合金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體,而使氟化鋰粉體均勻地嵌埋於金屬鋁粉體之表面,進而可製得具有均勻組織之複合粉體。其次,藉由熱壓製程之緻密化,所成型之中子減速材料可具有緻密之組織結構,而可滿足中子捕獲設備的應用需求。另外,本發明係藉由乾式混粉製程來混合粉體材料,故不須使用有機溶劑等混合載體,故可降低材料之製作成本,並達到環保減廢之要求。By applying the neutron deceleration material and the manufacturing method thereof of the present invention, the metal fluoride powder, the lithium fluoride powder and the metal aluminum powder are mixed in multiple stages, so that the lithium fluoride powder is evenly embedded in the metal aluminum powder The surface of the body can be obtained, and then a composite powder with a uniform structure can be obtained. Secondly, through the densification of the hot pressing process, the formed neutron deceleration material can have a dense structure, which can meet the application requirements of neutron capture equipment. In addition, the present invention mixes powder materials through a dry powder mixing process, so it is not necessary to use a mixing carrier such as an organic solvent, thereby reducing the material production cost and meeting the requirements of environmental protection and waste reduction.

以下仔細討論本發明實施例之製造和使用。然而,可以理解的是,實施例提供許多可應用的發明概念,其可實施於各式各樣的特定內容中。所討論之特定實施例僅供說明,並非用以限定本發明之範圍。The manufacture and use of embodiments of the present invention are discussed in detail below. It should be appreciated, however, that the embodiments provide many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific embodiments discussed are provided for illustration only, and are not intended to limit the scope of the invention.

請參照圖1,其係繪示依照本發明之一些實施例之中子減速材料的製作方法之流程示意圖。於方法100中,先提供金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體,並對氟化鋰粉體與部分之金屬鋁粉體進行第一乾式混粉製程,以製得金屬鋁-氟化鋰複合粉體,如操作110與操作120所示。金屬氟化物粉體不包含氟化鋰。在一些實施例中,金屬氟化物粉體可包含氟化鎂、氟化鋁、氟化鈣、其他適當之金屬氟化物,或者前述材料之任意混合。在其他實施例中,為了提升所製得中子減速材料之性質,金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體之純度均大於99%。Please refer to FIG. 1 , which is a schematic flowchart of a method for manufacturing a neutron deceleration material according to some embodiments of the present invention. In the method 100, metal fluoride powder, lithium fluoride powder and metal aluminum powder are firstly provided, and a first dry powder mixing process is performed on the lithium fluoride powder and part of the metal aluminum powder to obtain the metal powder. The aluminum-lithium fluoride composite powder is shown in operation 110 and operation 120 . The metal fluoride powder does not contain lithium fluoride. In some embodiments, the metal fluoride powder may comprise magnesium fluoride, aluminum fluoride, calcium fluoride, other suitable metal fluorides, or any combination of the foregoing materials. In other embodiments, in order to improve the properties of the prepared neutron moderator material, the purity of the metal fluoride powder, the lithium fluoride powder and the metal aluminum powder are all greater than 99%.

基於後續所製得之中子減速材料為100體積百分比,金屬鋁粉體之用量可為20體積百分比至50體積百分比,氟化鋰粉體之用量為0.5體積百分比至2體積百分比,且其餘量為金屬氟化物粉體。當金屬鋁粉體、氟化鋰粉體與金屬氟化物粉體之用量不為前述之範圍時,後續所製得之複合材料無法滿足中子減速材料之應用需求。Based on 100 volume percent of the neutron deceleration material prepared subsequently, the amount of metal aluminum powder can be 20 to 50 volume percent, the amount of lithium fluoride powder is 0.5 to 2 volume percent, and the rest It is metal fluoride powder. When the amounts of metal aluminum powder, lithium fluoride powder and metal fluoride powder are not within the aforementioned ranges, the composite material obtained subsequently cannot meet the application requirements of neutron deceleration materials.

於進行第一乾式混粉製程時,氟化鋰粉體與部分之金屬鋁粉體可採用本發明所屬技術領域常用之技術手段或設備來混合,故在此不另贅述。其中,由於氟化鋰粉體之硬度係高於金屬鋁粉體的硬度,故於第一乾式混粉製程所形成之金屬鋁-氟化鋰複合粉體中,氟化鋰之陶瓷粉體係嵌埋於金屬鋁粉體之表面。在一些實施例中,為了提升第一乾式混粉製程之混合嵌埋效果,金屬鋁粉體之平均粒徑較佳係大於氟化鋰粉體的平均粒徑。在一些具體例中,氟化鋰粉體之平均粒徑可為1 μm至3 μm,而金屬鋁粉體之平均粒徑為5 μm至15 μm。當氟化鋰與/或金屬鋁粉體之平均粒徑為前述之範圍時,氟化鋰粉體可更均勻地嵌埋於金屬鋁粉體之表面,而有助於提升所製得中子減速材料的性質。During the first dry powder mixing process, the lithium fluoride powder and part of the metal aluminum powder can be mixed by using technical means or equipment commonly used in the technical field of the present invention, so it is not repeated here. Among them, since the hardness of lithium fluoride powder is higher than that of metal aluminum powder, in the metal aluminum-lithium fluoride composite powder formed by the first dry powder mixing process, the ceramic powder system of lithium fluoride is embedded in the ceramic powder system. Buried on the surface of metal aluminum powder. In some embodiments, in order to improve the mixing and embedding effect of the first dry powder mixing process, the average particle size of the metal aluminum powder is preferably larger than the average particle size of the lithium fluoride powder. In some specific examples, the average particle size of the lithium fluoride powder may be 1 μm to 3 μm, and the average particle size of the metal aluminum powder may be 5 μm to 15 μm. When the average particle size of the lithium fluoride and/or the metal aluminum powder is within the aforementioned range, the lithium fluoride powder can be more uniformly embedded on the surface of the metal aluminum powder, which helps to increase the neutrons produced. Properties of the deceleration material.

於進行第一乾式混粉製程時,氟化鋰粉體與部分之金屬鋁粉體的體積比值可為0.05至0.1。當氟化鋰粉體與金屬鋁粉體之體積比值為前述之範圍時,氟化鋰粉體可更均勻地嵌埋於金屬鋁粉體之表面,而有助於提升所製得中子減速材料的性質。其次,為了提升氟化鋰粉體與金屬鋁粉體之混合均勻性,第一乾式混粉製程混合時間可為0.5小時至1小時。During the first dry powder mixing process, the volume ratio of the lithium fluoride powder to a part of the metal aluminum powder may be 0.05 to 0.1. When the volume ratio of the lithium fluoride powder to the metal aluminum powder is within the aforementioned range, the lithium fluoride powder can be more uniformly embedded on the surface of the metal aluminum powder, which is helpful to improve the neutron deceleration obtained. properties of the material. Secondly, in order to improve the mixing uniformity of the lithium fluoride powder and the metal aluminum powder, the mixing time of the first dry powder mixing process may be 0.5 hour to 1 hour.

於進行操作120後,將所形成之金屬鋁-氟化鋰複合粉體,以及金屬氟化物粉體與剩餘之金屬鋁粉體添加至混粉設備中,以進行第二乾式混粉製程,而可形成金屬氟化物-金屬鋁-氟化鋁複合粉體,如操作130所示。在一些實施例中,操作120與操作130可於相同之混粉設備中進行,故於進行操作120後,金屬氟化物粉體與剩餘之金屬鋁粉體可直接添加至混粉設備中。惟本發明並不以此為限,在其他實施例中,操作120與操作130亦可於不同之混粉設備中進行。相同地,第二乾式混粉製程可採用本發明所屬技術領域常用之技術手段或設備來混合,故在此不另贅述。在一些實施例中,第二乾式混粉製程之混合時間可為0.5小時至1小時。After the operation 120 is performed, the formed metal aluminum-lithium fluoride composite powder, the metal fluoride powder and the remaining metal aluminum powder are added to the powder mixing equipment to perform the second dry powder mixing process, and A metal fluoride-metal aluminum-aluminum fluoride composite powder may be formed, as shown in operation 130 . In some embodiments, operations 120 and 130 may be performed in the same powder mixing equipment, so after operation 120 is performed, the metal fluoride powder and the remaining metal aluminum powder may be directly added to the powder mixing equipment. However, the present invention is not limited to this, and in other embodiments, the operation 120 and the operation 130 may also be performed in different powder mixing equipment. Similarly, the second dry powder mixing process can be mixed using technical means or equipment commonly used in the technical field to which the present invention pertains, so it will not be repeated here. In some embodiments, the mixing time of the second dry powder mixing process may be 0.5 hour to 1 hour.

前述之第一乾式混粉製程與第二乾式混粉製程的進行均不額外添加有機溶劑或其他具有相似功效之載體,故本發明之第一乾式混粉製程與第二乾式混粉製程可減少溶劑之使用,而達到環保減廢之要求。The aforementioned first dry powder mixing process and the second dry powder mixing process are carried out without additional addition of organic solvents or other carriers with similar effects, so the first dry powder mixing process and the second dry powder mixing process of the present invention can be reduced. The use of solvents can meet the requirements of environmental protection and waste reduction.

於進行操作130後,對所形成之金屬氟化物-金屬鋁-氟化鋁複合粉體進行熱壓製程,以製得本發明之中子減速材料,如操作140與操作150所示。於進行熱壓製程時,金屬氟化物-金屬鋁-氟化鋁複合粉體可於高溫高壓下被成型並緻密化,而使所製得之中子減速材料具有不小於99.5%的相對密度,且於中子減速材料中,最大顆粒之粒徑係不大於500 μm。故,本案所製得之中子減速材料具有細緻且均勻之組織,而可滿足應用之需求。After operation 130 is performed, a hot pressing process is performed on the formed metal fluoride-metal aluminum-aluminum fluoride composite powder to obtain the neutron deceleration material of the present invention, as shown in operation 140 and operation 150 . During the hot pressing process, the metal fluoride-metal aluminum-aluminum fluoride composite powder can be formed and densified under high temperature and high pressure, so that the obtained neutron deceleration material has a relative density of not less than 99.5%, And in the neutron deceleration material, the particle size of the largest particle is not more than 500 μm. Therefore, the neutron deceleration material prepared in this case has a fine and uniform structure, which can meet the application requirements.

在一些實施例中,熱壓製程之溫度可為550℃至620℃,而壓力可為5 MPa至55 MPa。當熱壓製程之溫度與壓力為前述之範圍時,金屬氟化物-金屬鋁-氟化鋁複合粉體可較有效地被緻密化,而形成可滿足應用需求之中子減速材料。在此些實施例中,熱壓製程之時間可為1小時至6小時。當熱壓製程之時間為此範圍時,熱壓製程對於金屬氟化物-金屬鋁-氟化鋁複合粉體可具有更佳之緻密化效果,而有助於提升所製得中子減速材料之性質。In some embodiments, the temperature of the hot pressing process may be 550°C to 620°C, and the pressure may be 5 MPa to 55 MPa. When the temperature and pressure of the hot pressing process are within the aforementioned ranges, the metal fluoride-metal aluminum-aluminum fluoride composite powder can be densified more effectively to form a neutron deceleration material that can meet the application requirements. In such embodiments, the time of the hot pressing process may be 1 hour to 6 hours. When the time of the hot pressing process is within this range, the hot pressing process can have a better densification effect on the metal fluoride-metal aluminum-aluminum fluoride composite powder, and help to improve the properties of the prepared neutron moderator material. .

其次,經熱壓製程後,本發明所製得之中子減速材料的得料率不小於95%,故本發明之製作方法可有效地製得中子減速材料,而可降低其製作成本。Secondly, after the hot pressing process, the yield of the neutron deceleration material prepared by the present invention is not less than 95%, so the production method of the present invention can effectively prepare the neutron deceleration material, and can reduce its production cost.

在一些應用例中,本發明經熱壓製程所製得之中子減速材料具有特定之組成,且具有緻密均勻的組織,故可作為硼中子捕獲治療設備之中子減速材料。In some application examples, the neutron deceleration material prepared by the hot pressing process of the present invention has a specific composition and has a dense and uniform structure, so it can be used as a neutron deceleration material for boron neutron capture therapy equipment.

以下利用實施例以說明本發明之應用,然其並非用以限定本發明,任何熟習此技藝者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾。The following examples are used to illustrate the application of the present invention, but it is not intended to limit the present invention. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention.

實施例1Example 1

首先,提供58.5體積百分比之氟化鎂、40體積百分比之金屬鋁與1.5體積百分比之氟化鋰,且氟化鎂、金屬鋁與氟化鋰之純度均大於99.5%,其中金屬鋁之平均粒徑為5 μm,而氟化鋰之平均粒徑為1 μm。然後,將1.5體積百分比之氟化鋰與15體積百分比之金屬鋁放入高效混合設備中,以進行第一乾式混粉製程,以形成金屬鋁-氟化鋰複合粉體。其中,第一乾式混粉製程之時間為30分鐘。First, provide 58.5 volume percent of magnesium fluoride, 40 volume percent of metal aluminum and 1.5 volume percent of lithium fluoride, and the purity of magnesium fluoride, metal aluminum and lithium fluoride are all greater than 99.5%, and the average particle size of metal aluminum is greater than 99.5%. The particle diameter is 5 μm, and the average particle diameter of lithium fluoride is 1 μm. Then, 1.5 volume percent of lithium fluoride and 15 volume percent of metal aluminum are put into high-efficiency mixing equipment to perform the first dry powder mixing process to form metal aluminum-lithium fluoride composite powder. Wherein, the time of the first dry powder mixing process is 30 minutes.

於進行第一乾式混粉製程後,將25體積百分比之金屬鋁與58.5體積百分比之氟化鎂添加至高效混合設備中,以與金屬鋁-氟化鋰複合粉體進行第二乾式混粉製程,而形成氟化鎂-金屬鋁-氟化鋰複合粉體。其中,第一乾式混粉製程之時間為60分鐘。After the first dry powder mixing process, 25 volume percent of metal aluminum and 58.5 volume percent of magnesium fluoride were added to the high-efficiency mixing equipment to perform the second dry powder mixing process with the metal aluminum-lithium fluoride composite powder , and form magnesium fluoride-metal aluminum-lithium fluoride composite powder. Wherein, the time of the first dry powder mixing process is 60 minutes.

接著,將所形成之氟化鎂-金屬鋁-氟化鋰複合粉體倒入石墨熱壓模具中,並於550℃下,以50 MPa之壓力進行熱壓製程。經熱壓成型與緻密化6小時後,即可製得實施例1之氟化鎂-金屬鋁-氟化鋰複合材料(即中子減速材料),其組成為58.5%氟化鎂-40%金屬鋁-1.5氟化鋰%,並以電子顯微鏡觀察實施例1之中子減速材料的顯微組織(如圖2A所示)。實施例1之中子減速材料的得料率為96%。Next, the formed magnesium fluoride-metal aluminum-lithium fluoride composite powder was poured into a graphite hot pressing mold, and a hot pressing process was performed at 550° C. with a pressure of 50 MPa. After 6 hours of hot pressing and densification, the magnesium fluoride-metal aluminum-lithium fluoride composite material (ie, neutron deceleration material) of Example 1 can be obtained, and its composition is 58.5% magnesium fluoride-40% Metal aluminum-1.5% lithium fluoride, and the microstructure of the neutron deceleration material in Example 1 was observed with an electron microscope (as shown in FIG. 2A ). The yield of the neutron deceleration material in Example 1 was 96%.

實施例2Example 2

首先,提供69體積百分比之氟化鋁、30體積百分比之金屬鋁與1體積百分比之氟化鋰,且氟化鋁、金屬鋁與氟化鋰之純度均大於99.5%,其中金屬鋁之平均粒徑為10 μm,而氟化鋰之平均粒徑為2 μm。然後,將1體積百分比之氟化鋰與20體積百分比之金屬鋁放入高效混合設備中,以進行第一乾式混粉製程,以形成金屬鋁-氟化鋰複合粉體。其中,第一乾式混粉製程之時間為45分鐘。First, provide 69 volume percent of aluminum fluoride, 30 volume percent of metal aluminum and 1 volume percent of lithium fluoride, and the purity of aluminum fluoride, metal aluminum and lithium fluoride are all greater than 99.5%, and the average particle size of metal aluminum is greater than 99.5%. The particle diameter is 10 μm, and the average particle diameter of lithium fluoride is 2 μm. Then, 1 volume percent of lithium fluoride and 20 volume percent of metal aluminum are put into high-efficiency mixing equipment to perform the first dry powder mixing process to form metal aluminum-lithium fluoride composite powder. Wherein, the time of the first dry powder mixing process is 45 minutes.

於進行第一乾式混粉製程後,將10體積百分比之金屬鋁與69體積百分比之氟化鋁添加至高效混合設備中,以與金屬鋁-氟化鋰複合粉體進行第二乾式混粉製程,而形成氟化鋁-金屬鋁-氟化鋰複合粉體。其中,第一乾式混粉製程之時間為45分鐘。After the first dry powder mixing process, 10 volume percent of metal aluminum and 69 volume percent of aluminum fluoride are added to the high-efficiency mixing equipment to perform the second dry powder mixing process with the metal aluminum-lithium fluoride composite powder , and form aluminum fluoride-metal aluminum-lithium fluoride composite powder. Wherein, the time of the first dry powder mixing process is 45 minutes.

接著,將所形成之氟化鋁-金屬鋁-氟化鋰複合粉體倒入石墨熱壓模具中,並於620℃下,以5 MPa之壓力進行熱壓製程。經熱壓成型與緻密化3小時後,即可製得實施例2之氟化鋁-金屬鋁-氟化鋰複合材料(即中子減速材料),其組成為69%氟化鋁-30%金屬鋁-1氟化鋰%,並以電子顯微鏡觀察實施例2之中子減速材料的顯微組織(如圖2B所示)。實施例2之中子減速材料的得料率為99.9%。Next, the formed aluminum fluoride-metal aluminum-lithium fluoride composite powder was poured into a graphite hot pressing mold, and a hot pressing process was performed at 620° C. with a pressure of 5 MPa. After 3 hours of hot pressing and densification, the aluminum fluoride-metal aluminum-lithium fluoride composite material (ie, the neutron deceleration material) of Example 2 can be obtained, and its composition is 69% aluminum fluoride-30% Metal aluminum-1 lithium fluoride %, and the microstructure of the neutron deceleration material in Example 2 was observed with an electron microscope (as shown in FIG. 2B ). The yield of the neutron deceleration material in Example 2 was 99.9%.

請參照圖2A與圖2B。實施例1與實施例2所製得之中子減速材料均具有緻密且均勻之組織,故可應用於中子捕獲設備。其中,實施例1之中子減速材料的相對密度為99.6%,且其中最大顆粒組織的粒徑係小於250 μm,而實施例2之中子減速材料的相對密度為99.9%,且其最大顆粒組織的粒徑係小於150 μm。Please refer to FIG. 2A and FIG. 2B . The neutron deceleration materials prepared in Example 1 and Example 2 have dense and uniform structures, so they can be used in neutron capture equipment. Among them, the relative density of the neutron deceleration material in Example 1 is 99.6%, and the particle size of the largest particle structure is less than 250 μm, while the relative density of the neutron deceleration material in Example 2 is 99.9%, and its largest particle The particle size of the tissue is less than 150 μm.

據此,藉由本發明中子減速材料及其製作方法,其係分階段地混合金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體,而可有效地將氟化鋰粉體嵌埋於金屬鋁粉體之表面,進而可有助於提升所製得中子減速材料的性質。其中,藉由分階段進行的乾式混粉製程,金屬氟化物粉體、氟化鋰粉體與金屬鋁粉體可均勻地混合,而有助於提升中子減速材料的品質,並可提升其得料率。另外,由於本發明之混粉製程不須額外添加有機溶劑或其他液態載體,故可達到環保減廢之要求,並可降低製作成本。Accordingly, according to the present invention, the neutron deceleration material and the method for producing the same can effectively embed the lithium fluoride powder by mixing the metal fluoride powder, the lithium fluoride powder and the metal aluminum powder in stages. On the surface of the metal aluminum powder, it can help to improve the properties of the prepared neutron deceleration material. Among them, through the dry powder mixing process carried out in stages, the metal fluoride powder, lithium fluoride powder and metal aluminum powder can be uniformly mixed, which helps to improve the quality of the neutron deceleration material and its Yield rate. In addition, since the powder mixing process of the present invention does not need to add an additional organic solvent or other liquid carrier, it can meet the requirements of environmental protection and waste reduction, and can reduce the production cost.

雖然本發明已以實施方式揭露如上,然其並非用以限定本發明,在本發明所屬技術領域中任何具有通常知識者,在不脫離本發明之精神和範圍內,當可作各種之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為準。Although the present invention has been disclosed in the above embodiments, it is not intended to limit the present invention. Anyone with ordinary knowledge in the technical field to which the present invention pertains can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the appended patent application.

100:方法 110,120,130,140,150:操作 100: Method 110, 120, 130, 140, 150: Operation

為了對本發明之實施例及其優點有更完整之理解,現請參照以下之說明並配合相應之圖式。必須強調的是,各種特徵並非依比例描繪且僅係為了圖解目的。相關圖式內容說明如下。 圖1係繪示依照本發明之一些實施例之中子減速材料的製作方法之流程示意圖。 圖2A與圖2B分別係顯示本發明之實施例1與實施例2之中子減速材料的電子顯微鏡照片。 In order to have a more complete understanding of the embodiments of the present invention and their advantages, please refer to the following description together with the corresponding drawings. It must be emphasized that the various features are not drawn to scale and are for illustrative purposes only. The contents of the relevant diagrams are described below. FIG. 1 is a schematic flow chart illustrating a method for fabricating a neutron deceleration material according to some embodiments of the present invention. FIG. 2A and FIG. 2B respectively show electron microscope photographs of the neutron deceleration material of Example 1 and Example 2 of the present invention.

國內寄存資訊(請依寄存機構、日期、號碼順序註記) 無 國外寄存資訊(請依寄存國家、機構、日期、號碼順序註記) 無 Domestic storage information (please note in the order of storage institution, date and number) none Foreign deposit information (please note in the order of deposit country, institution, date and number) none

100:方法 100: Method

110,120,130,140,150:操作 110, 120, 130, 140, 150: Operation

Claims (10)

一種中子減速材料的製作方法,包含: 提供一金屬氟化物粉體、氟化鋰粉體與一金屬鋁粉體,其中該金屬氟化物粉體不包含氟化鋰,基於該中子減速材料為100體積百分比,該金屬鋁粉體之一用量為20體積百分比至50體積百分比,該氟化鋰粉體之一用量為0.5體積百分比至2體積百分比,且餘量為該金屬氟化物粉體; 對該氟化鋰粉體與一部分之該金屬鋁粉體進行一第一乾式混粉製程,以形成一金屬鋁-氟化鋁複合粉體; 對該金屬氟化物粉體、剩餘之該金屬鋁粉體與該金屬鋁-氟化鋁複合粉體進行一第二乾式混粉製程,以形成一金屬氟化物-金屬鋁-氟化鋁複合粉體;以及 對該金屬氟化物-金屬鋁-氟化鋁複合粉體進行一熱壓製程,以形成該中子減速材料。 A manufacturing method of a neutron deceleration material, comprising: Provide a metal fluoride powder, lithium fluoride powder and a metal aluminum powder, wherein the metal fluoride powder does not contain lithium fluoride, based on the neutron deceleration material is 100 volume percent, the metal aluminum powder One dosage is 20 volume percent to 50 volume percent, one dosage of the lithium fluoride powder is 0.5 volume percent to 2 volume percent, and the balance is the metal fluoride powder; performing a first dry powder mixing process on the lithium fluoride powder and a part of the metal aluminum powder to form a metal aluminum-aluminum fluoride composite powder; A second dry powder mixing process is performed on the metal fluoride powder, the remaining metal aluminum powder and the metal aluminum-aluminum fluoride composite powder to form a metal fluoride-metal aluminum-aluminum fluoride composite powder body; and A hot pressing process is performed on the metal fluoride-metal aluminum-aluminum fluoride composite powder to form the neutron deceleration material. 如請求項1所述之中子減速材料的製作方法,其中該金屬氟化物粉體包含氟化鎂、氟化鋁及/或氟化鈣。The method for producing a neutron deceleration material according to claim 1, wherein the metal fluoride powder comprises magnesium fluoride, aluminum fluoride and/or calcium fluoride. 如請求項1所述之中子減速材料的製作方法,其中該氟化鋰粉體之一平均粒徑為1 μm至3 μm。The method for producing a neutron deceleration material according to claim 1, wherein an average particle size of the lithium fluoride powder is 1 μm to 3 μm. 如請求項1所述之中子減速材料的製作方法,其中該金屬鋁粉體之一平均粒徑為5 μm至15 μm。The method for producing a neutron deceleration material according to claim 1, wherein an average particle size of the metal aluminum powder is 5 μm to 15 μm. 如請求項1所述之中子減速材料的製作方法,其中該金屬氟化物粉體、該氟化鋰粉體與該金屬鋁粉體之純度均大於99%。The method for producing a neutron deceleration material according to claim 1, wherein the purity of the metal fluoride powder, the lithium fluoride powder and the metal aluminum powder are all greater than 99%. 如請求項1所述之中子減速材料的製作方法,其中於進行該第一乾式混粉製程時,該氟化鋰粉體與該部分之該金屬鋁粉體之體積比值為0.05至0.1。The method for manufacturing a neutron deceleration material according to claim 1, wherein during the first dry powder mixing process, the volume ratio of the lithium fluoride powder to the part of the metal aluminum powder is 0.05 to 0.1. 如請求項1所述之中子減速材料的製作方法,其中該第一乾式混粉製程之一混合時間為0.5小時至1小時,而該第二乾式混粉製程之一混合時間為0.5小時至1小時。The method for producing a neutron deceleration material according to claim 1, wherein a mixing time of the first dry powder mixing process is 0.5 hour to 1 hour, and a mixing time of the second dry powder mixing process is 0.5 hour to 1 hour. 1 hour. 如請求項1所述之中子減速材料的製作方法,其中該熱壓製程之一溫度為550℃至620℃,而該熱壓製程之一壓力為5 MPa至55 MPa。The method for manufacturing a neutron deceleration material according to claim 1, wherein a temperature of the hot pressing process is 550°C to 620°C, and a pressure of the hot pressing process is 5 MPa to 55 MPa. 如請求項8所述之中子減速材料的製作方法,其中該熱壓製程之一時間為1小時至6小時。The method for producing a neutron deceleration material according to claim 8, wherein a time of the hot pressing process ranges from 1 hour to 6 hours. 一種中子減速材料,藉由如請求項1至9中之任一項所述之製作方法所製得,其中該中子減速材料之一相對密度不小於99.5%,且該中子減速材料中之最大顆粒的一粒徑不大於500 μm。A neutron moderating material, obtained by the manufacturing method as described in any one of claims 1 to 9, wherein a relative density of the neutron moderating material is not less than 99.5%, and the neutron moderating material is The particle size of the largest particle is not more than 500 μm.
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TWI691238B (en) * 2019-04-12 2020-04-11 中國鋼鐵股份有限公司 Manufacturing method for neutron moderating material

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