CN106932305A - 一种B4C-Al2O3芯块硼10线密度测定方法 - Google Patents
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 2
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- 230000033228 biological regulation Effects 0.000 claims 1
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- 150000002500 ions Chemical class 0.000 description 12
- 229910052580 B4C Inorganic materials 0.000 description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
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- ZOXJGFHDIHLPTG-IGMARMGPSA-N boron-11 atom Chemical compound [11B] ZOXJGFHDIHLPTG-IGMARMGPSA-N 0.000 description 1
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- 238000003837 high-temperature calcination Methods 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
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Abstract
本发明涉及一种硼10线密度测定方法,具体涉及一种B4C-Al2O3芯块硼10线密度测定方法。具体包括以下步骤:步骤一、试样处理;步骤二、点样,制备样品带;步骤三、测定,得到硼10的富集度;步骤四、计算样品的硼-10线密度。本发明成功建立了碳化硼-氧化铝芯块中硼富集度和硼-10线密度的检测方法,利用发明内容中列举的实验条件可以精确测定碳化硼-氧化铝芯块中硼同位素丰度,解决了生产中急需的碳化硼-氧化铝芯块中硼-10线密度测定工作,满足了碳化硼-氧化铝芯块中硼-10线密度检测的需求。
Description
技术领域
本发明涉及一种硼10线密度测定方法,具体涉及一种B4C-Al2O3芯块硼10线密度测定方法。
背景技术
碳化硼氧化铝芯块是用碳化硼粉末和氧化铝粉末按一定比例混合后经高温煅烧而成,碳化硼的硬度仅次于金刚石,不溶于酸、碱。而氧化铝俗称刚玉,质较硬,不溶于水,微溶于碱和酸。因此经高温煅烧后的碳化硼氧化铝化学性质更稳定,更难溶于酸、碱,目前碳化硼和氧化铝粉末中杂质元素的测定公开发表的文献较多,而碳化硼氧化铝芯块溶解方法和杂质的测定目前还未见公开报道。国内外关于碳化硼-氧化铝芯块中硼-10线密度的测定方法的研究成果未见公开报道。
发明内容
本发明要解决的技术问题是提供一种B4C-Al2O3芯块硼10线密度测定方法,依据碳化硼-氧化铝芯块实验需求,建立试样溶解,对硼同位素测定条件选择,完成对碳化硼-氧化铝芯块中硼-10,硼-11同位素质量丰度测定的检测方法,并结合硼总量测定结果计算B4C-Al2O3芯块的硼-10线密度的方法。
为解决上述技术问题,本发明一种B4C-Al2O3芯块硼10线密度测定方法,具体包括以下步骤:
步骤一、试样处理,先用游标卡尺测量芯块样品长度a;采用直接熔融法,将碳化硼-氧化铝研磨过筛,称取约20mg,置于烧杯中,再加入10mLNa2CO3溶液,使用时搅拌摇匀,得到试样溶液;
步骤二、点样,制备样品带;
步骤三、测定,将步骤二的样品带装入热电离质谱仪离子源腔体内,启动真空泵,然后分析样品,即可得到硼10的富集度;
步骤四、硼-10线密度按照计算,根据硼10富集度,计算样品的硼-10线密度。
所述步骤二中,制备样品带,材料选择高纯钽带,涂样前使用质谱专用除气装置在小于5×10-5Pa的真空下对钽带加热除气30min,以除去钽带表面的水和杂质;用微量移液器吸取3μL发射剂,滴加在样品带中央,将样品带电流缓慢升至1.2A,直至石墨浆体蒸干,然后用微量移液器吸取2μL步骤一中的试样溶液,滴加在干的石墨上面,再用微量移液器吸取2μL浓度为8μg/μL的Na2CO3溶液,滴加在滤液液滴上面,维持1.2A的电流将液滴加热蒸干,继续调节样品带电流增大至2.0A至样品带呈暗红色后立即停止升温,将电流降至1.2A;再用微量移液器吸取3μL发射剂覆盖住滴加液滴部位的样品带,维持1.2A的电流加热蒸干,得到样品带。
所述步骤三中的分析样品,以400s的时间将样品带的电流升至2.0A,检测89Na2BO2 +的离子流强度,并增大样品带电流升温使89Na2BO2 +的离子流强度达到0.1V,进行离子流聚焦,使89Na2BO2 +的信号达到最高点;继续增大样品带电流升温使89Na2BO2 +的离子流强度达到0.5V,信号稳定后开始采集数据,即可得到硼10的富集度。
所述步骤四中,按下式计算样品的硼-10线密度;
式中:
ρ—碳化硼-氧化铝芯块中硼-10线密度,单位为克每厘米(g/cm);
—碳化硼-氧化铝芯块中硼-10丰度,单位为百分数(%);
ω(B)—碳化硼-氧化铝芯块中硼总量,单位为克每克(g/g);
a—碳化硼-氧化铝芯块的长度,单位为厘米(cm)。
所述步骤二中,发射剂:石墨浆体:乙醇:水=1:20:80。
所述步骤三中,启动真空泵,使离子源真空小于50μPa,分析室真空小于4μPa。
本发明的有益技术效果在于:成功建立了碳化硼-氧化铝芯块中硼富集度和硼-10线密度的检测方法,利用发明内容中列举的实验条件可以精确测定碳化硼-氧化铝芯块中硼同位素丰度,解决了生产中急需的碳化硼-氧化铝芯块中硼-10线密度测定工作,满足了碳化硼-氧化铝芯块中硼-10线密度检测的需求。
附图说明
图1为本发明一种B4C-Al2O3芯块硼10线密度测定方法流程图。
具体实施方式
下面结合附图和实施例对本发明作进一步详细说明。
本发明一种B4C-Al2O3芯块硼10线密度测定方法,具体包括以下步骤:
步骤一、试样处理,先用游标卡尺测量芯块样品长度a,单位为厘米;采用直接熔融法,将碳化硼-氧化铝研磨过筛,选粒度小于200目的粉末,称取约20mg,置于烧杯中,再加入10mLNa2CO3溶液(8μg/μL),使用时搅拌摇匀,得到试样溶液;
步骤二、点样,制备样品带,材料选择高纯钽带,尺寸为厚0.00098英寸,宽0.0299英寸,涂样前使用质谱专用除气装置在小于5×10-5Pa的真空下对钽带加热除气30min,以除去钽带表面的水和杂质;用微量移液器吸取3μL发射剂(石墨浆体:乙醇:水=1:20:80),滴加在样品带中央,将样品带电流缓慢升至1.2A,直至石墨浆体蒸干,然后用微量移液器吸取2μL步骤一中的试样溶液,滴加在干的石墨上面,再用微量移液器吸取2μL Na2CO3溶液(8μg/μL),滴加在滤液(8.1)液滴上面,维持1.2A的电流将液滴加热蒸干,继续调节样品带电流增大至2.0A至样品带呈暗红色(加热不超过3s)后立即停止升温,将电流降至1.2A;再用微量移液器吸取3μL发射剂(石墨浆体:乙醇:水=1:20:80)覆盖住滴加液滴部位的样品带,维持1.2A的电流加热蒸干,得到样品带;
步骤三、测定,将步骤二的样品带装入热电离质谱仪离子源腔体内,启动真空泵,使离子源真空小于50μPa,分析室真空小于4μPa;然后分析样品;
测定时以400s的时间将样品带的电流升至2.0A,检测89Na2BO2 +的离子流强度,并增大样品带电流升温使89Na2BO2 +的离子流强度达到0.1V,进行离子流聚焦,使89Na2BO2 +的信号达到最高点;继续增大样品带电流升温使89Na2BO2 +的离子流强度达到0.5V,信号稳定后开始采集数据,即可得到硼10的富集度;
步骤四、硼-10线密度按照计算,根据硼10富集度,结合硼总量,按下式计算样品的硼-10线密度;
式中:
ρ—碳化硼-氧化铝芯块中硼-10线密度,单位为克每厘米(g/cm);
—碳化硼-氧化铝芯块中硼-10丰度,单位为百分数(%);
ω(B)—碳化硼-氧化铝芯块中硼总量,单位为克每克(g/g);
a—碳化硼-氧化铝芯块的长度,单位为厘米(cm)。
精密度,检测碳化硼-氧化铝中硼同位素丰度,实验使用的碳化硼-氧化铝为天然硼,天然硼10B的范围为18.93%~20.39%,结果见表1。
表1碳化硼-氧化铝芯块中硼同位素丰度测量结果
由表1可见,采用两种处理方法10B测定结果均符合天然硼的范围,精密度由于0.020%。
Claims (6)
1.一种B4C-Al2O3芯块硼10线密度测定方法,其特征在于:具体包括以下步骤:
步骤一、试样处理,先用游标卡尺测量芯块样品长度a;采用直接熔融法,将碳化硼-氧化铝研磨过筛,称取约20mg,置于烧杯中,再加入10mLNa2CO3溶液,使用时搅拌摇匀,得到试样溶液;
步骤二、点样,制备样品带;
步骤三、测定,将步骤二的样品带装入热电离质谱仪离子源腔体内,启动真空泵,然后分析样品,即可得到硼10的富集度;
步骤四、硼-10线密度按照计算,根据硼10富集度,计算样品的硼-10线密度。
2.根据权利要求1所述的一种B4C-Al2O3芯块硼10线密度测定方法,其特征在于:所述步骤二中,制备样品带,材料选择高纯钽带,涂样前使用质谱专用除气装置在小于5×10-5Pa的真空下对钽带加热除气30min,以除去钽带表面的水和杂质;用微量移液器吸取3μL发射剂,滴加在样品带中央,将样品带电流缓慢升至1.2A,直至石墨浆体蒸干,然后用微量移液器吸取2μL步骤一中的试样溶液,滴加在干的石墨上面,再用微量移液器吸取2μL浓度为8μg/μL的Na2CO3溶液,滴加在滤液液滴上面,维持1.2A的电流将液滴加热蒸干,继续调节样品带电流增大至2.0A至样品带呈暗红色后立即停止升温,将电流降至1.2A;再用微量移液器吸取3μL发射剂覆盖住滴加液滴部位的样品带,维持1.2A的电流加热蒸干,得到样品带。
3.根据权利要求2所述的一种B4C-Al2O3芯块硼10线密度测定方法,其特征在于:所述步骤三中的分析样品,以400s的时间将样品带的电流升至2.0A,检测89Na2BO2 +的离子流强度,并增大样品带电流升温使89Na2BO2 +的离子流强度达到0.1V,进行离子流聚焦,使89Na2BO2 +的信号达到最高点;继续增大样品带电流升温使89Na2BO2 +的离子流强度达到0.5V,信号稳定后开始采集数据,即可得到硼10的富集度。
4.根据权利要求3所述的一种B4C-Al2O3芯块硼10线密度测定方法,其特征在于:所述步骤四中,按下式计算样品的硼-10线密度;
式中:
ρ—碳化硼-氧化铝芯块中硼-10线密度,单位为克每厘米(g/cm);
—碳化硼-氧化铝芯块中硼-10丰度,单位为百分数(%);
ω(B)—碳化硼-氧化铝芯块中硼总量,单位为克每克(g/g);
a—碳化硼-氧化铝芯块的长度,单位为厘米(cm)。
5.根据权利要求4所述的一种B4C-Al2O3芯块硼10线密度测定方法,其特征在于:所述步骤二中,发射剂:石墨浆体:乙醇:水=1:20:80。
6.根据权利要求5所述的一种B4C-Al2O3芯块硼10线密度测定方法,其特征在于:所述步骤三中,启动真空泵,使离子源真空小于50μPa,分析室真空小于4μPa。
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