CN114134567A - 一种高温高压合成羟基氧化铁FeOOH晶体的方法 - Google Patents
一种高温高压合成羟基氧化铁FeOOH晶体的方法 Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 36
- 229910002588 FeOOH Inorganic materials 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 20
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 title claims abstract description 18
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052742 iron Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910003460 diamond Inorganic materials 0.000 claims description 4
- 239000010432 diamond Substances 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 235000014413 iron hydroxide Nutrition 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 239000007858 starting material Substances 0.000 claims description 4
- 238000005553 drilling Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 8
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 abstract description 4
- 229960004887 ferric hydroxide Drugs 0.000 abstract description 2
- 239000013067 intermediate product Substances 0.000 abstract description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical group [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 238000000547 structure data Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000005469 synchrotron radiation Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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Abstract
本发明公开了提供一种高温高压合成羟基氧化铁FeOOH晶体的方法,使用分析纯的氢氧化铁Fe(OH)3和分析纯的铁粉Fe以摩尔比2:1混合研磨均匀作为起始原料,在密闭的铁样品腔中通过高温高压反应得到羟基氧化铁FeOOH晶体样品。参照铁锈生成原理,构建中间产物氢氧化亚铁Fe(OH)2,并设计相对应的组装,在高温高压极端条件下完成羟基氧化铁FeOOH的合成反应。利用羟基氧化铁的高压稳定性,通过高温高压重结晶过程获得了大尺寸的晶体,解决了目前存在的技术难题。
Description
技术领域
本发明涉及地球科学矿物学研究领域,涉及一种高温高压合成羟基氧化铁FeOOH晶体的方法。
背景技术
羟基氧化铁FeOOH的矿物学名为针铁矿,是一种自然界广泛分布的、由赤铁矿风化形成的重要的含水铁矿,也是生活中常见的铁锈的主要成分。最近实验研究表明,羟基氧化铁具有极高的高压稳定性,能够在下地幔底部的极高压力、温度以及氧逸度条件下形成更稳定的、具有黄铁矿结构的过氧化亚铁FeO2。这意味着羟基氧化铁可以通过洋壳俯冲进入地球内部甚至进入下地幔,在地球下地幔乃至核幔边界可能富集结构特殊的过氧化物,它将对地幔模型的建立和地球演化的研究提供新的实验证据。然而,目前的实验基本都采用粉晶同步辐射的结果以及理论计算晶体结构相结合的方法,缺少精确的晶体结构数据来支撑计算结果。因此,需要人工合成羟基氧化铁FeOOH晶体来进一步验证。目前合成羟基氧化铁大多采用化学湿法沉淀,所得产物为颗粒度细小的纳米晶,缺少大尺寸晶体定量其晶体结构。
发明内容
本发明要解决的技术问题是:提供一种高温高压合成羟基氧化铁FeOOH晶体的方法,以填补目前羟基氧化铁晶体生长研究的空白。
本发明的技术方案是:一种高温高压合成羟基氧化铁FeOOH晶体的方法,包括以下步骤:
步骤1、使用分析纯的氢氧化铁Fe(OH)3和分析纯的铁粉Fe以摩尔比2:1混合研磨均匀作为起始原料;
步骤2、使用粉末压片机,将混合物粉末置于Φ5磨具中压成Φ5×4mm圆柱形,将圆柱形样品塞入内腔为Φ5×4mm,外径7mm、厚1mm的铁子母扣中密封;将铁子母扣包裹样品的圆柱形置于h-BN管中,以h-BN为传压介质;
步骤3、将步骤2中装有样品的h-BN管组装在高压合成组装块中并放置在六面顶大压机进行高温高压反应;
步骤4,高温高压反应完成后,将铁子母扣包裹的圆柱形取出,然后使用金刚石切刀剥离表面铁样品腔,将样品取出,在超声中使用酒精清洗后,自然风干样品,即得羟基氧化铁FeOOH晶体。
步骤2所述h-BN管具体操作为:在车床上将大小为Φ10mm的h-BN棒中心钻Φ7mm的孔作成h-BN管,将样品塞入管中,两端拿Φ7mm厚度为2mm的h-BN片密封。
步骤3所述的将h-BN管组装在高压合成组装块中的方法,具体操作包括:选取一块叶腊石块,在叶腊石块中心打一个Φ12mm圆形通孔;在圆形通孔内套一个外径12mm、内径Φ10mm的圆形石墨加热炉;在石墨加热炉中间放置10mm的h-BN管密封的样品;将圆形石墨加热炉上下两端用叶腊石堵头密封。
步骤3所述高温高压反应条件为,升压至3GPa,然后升温到700-750℃,保压保温48h后淬火。
步骤4所述得到的羟基氧化铁为晶体,晶体尺寸为50-100μm,其形态为针状,呈赤黄色。
本发明的创新点和有益效果:
实验研究表明,羟基氧化铁FeOOH晶体合成的难点在于氧逸度的控制。由于FeOOH超高的高压稳定性,容易想到,Fe2O3在H2O溶液中通过长时间的高温高压作用会形成更稳定的FeOOH:
Fe2O3+H2O→2FeOOH+O2
通过在密封含水环境中尝试这个反应,高温高压实验结果发现产物为Fe3O4,无法生成FeOOH。这是因为高压环境本身具有较强的还原性,Fe2O3无法稳定存在而被部分还原为Fe3O4。为了解决这一问题,通过在含水密封样品腔中加入KClO4作为氧源,高温高压实验结果发现产物为Fe2O3,也无法生成FeOOH。这是因为尽管超高氧压条件保护了Fe3+不被部分还原,但是也迫使FeOOH生成反应无法朝着释放氧气的正反应进行。为了解决上述难题,本发明参考铁锈生成的原理,即析氢-吸氧腐蚀中间过程必须生成过度产物氢氧化亚铁Fe(OH)2,然后Fe(OH)2再被氧化生成FeOOH,根据此原理重新设计反应过程和样品组装:
第一步:2Fe(OH)3+Fe→3Fe(OH)2
第二步:4Fe(OH)2+O2→4FeOOH+2H2O
考虑到氢氧化亚铁Fe(OH)2非常不稳定、极易氧化,本发明采用密闭的铁样品腔将外部的氧阻隔,确保在样品腔内Fe(OH)3被Fe还原生成Fe(OH)2,此过程反应极快。由于在长时间的高温高压条件下,铁样品腔会逐渐被氢氧化物碱性腐蚀后失去延展性、进而被破坏后使得外界氧气进入样品腔。事实上,实验也观察到反应完成后,铁样品腔发生龟壳一般的龟裂,可以轻松从样品剥落。在缺少铁样品腔密闭保护作用下,腔体中Fe(OH)2被氧化而生成FeOOH;在更长时间的高温高压条件下,含水矿物FeOOH会进一步通过重结晶快速长大,形成针状的FeOOH的晶体。综上所述,本发明的创新点在于针对铁锈生成原理,构建中间产物氢氧化亚铁Fe(OH)2,设计相对应的组装,在高温高压极端条件下完成羟基氧化铁FeOOH的合成反应。由于羟基氧化铁的高压稳定性,高温高压条件有利于其晶体生长,获得了大尺寸的晶体,解决了目前存在的技术难题。
具体实施方式
实施例1:
一种高温高压合成羟基氧化铁FeOOH晶体的方法,包括以下步骤:
步骤1、使用分析纯的氢氧化铁Fe(OH)3和分析纯的铁粉Fe以摩尔比2:1混合研磨均匀作为起始原料;
步骤2、使用粉末压片机,将混合物粉末置于Φ5磨具中压成Φ5×4mm圆柱形,将圆柱形样品塞入内腔为Φ5×4mm,外径7mm、厚1mm的铁子母扣中密封;将铁子母扣包裹样品的圆柱形置于h-BN管中,以h-BN为传压介质;
步骤3、将步骤2中装有样品的h-BN管组装在高压合成组装块中并放置在六面顶大压机进行高温高压反应,所述高温高压反应条件为,升压至3GPa,然后升温到700℃,保压保温48h后淬火;
步骤4,高温高压反应完成后,将铁子母扣包裹的圆柱形取出,然后使用金刚石切刀剥离表面铁样品腔,将样品取出,在超声中使用酒精清洗后,自然风干样品,即得羟基氧化铁FeOOH晶体,晶体尺寸为50-100μm,其形态为针状,呈赤黄色。
实施例2:
一种高温高压合成羟基氧化铁FeOOH晶体的方法,包括以下步骤:
步骤1、使用分析纯的氢氧化铁Fe(OH)3和分析纯的铁粉Fe以摩尔比2:1混合研磨均匀作为起始原料;
步骤2、使用粉末压片机,将混合物粉末置于Φ5磨具中压成Φ5×4mm圆柱形,将圆柱形样品塞入内腔为Φ5×4mm,外径7mm、厚1mm的铁子母扣中密封;将铁子母扣包裹样品的圆柱形置于h-BN管中,以h-BN为传压介质;
步骤3、将步骤2中装有样品的h-BN管组装在高压合成组装块中并放置在六面顶大压机进行高温高压反应,所述高温高压反应条件为,升压至3GPa,然后升温到750℃,保压保温48h后淬火;
步骤4,高温高压反应完成后,将铁子母扣包裹的圆柱形取出,然后使用金刚石切刀剥离表面铁样品腔,将样品取出,在超声中使用酒精清洗后,自然风干样品,即得羟基氧化铁FeOOH晶体,晶体尺寸为50-100μm,其形态为针状,呈赤黄色。
实施例1-2中,步骤2所述h-BN管具体操作为:在车床上将大小为Φ10mm的h-BN棒中心钻Φ7mm的孔作成h-BN管,将样品塞入管中,两端拿Φ7mm厚度为2mm的h-BN片密封。步骤3所述的将h-BN管组装在高压合成组装块中的方法,具体操作包括:选取一块叶腊石块,在叶腊石块中心打一个Φ12mm圆形通孔;在圆形通孔内套一个外径12mm、内径Φ10mm的圆形石墨加热炉;在石墨加热炉中间放置10mm的h-BN管密封的样品;将圆形石墨加热炉上下两端用叶腊石堵头密封。
以上显示和描述了本发明的基本原理、主要特征和优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种高温高压合成羟基氧化铁FeOOH晶体的方法,其特征在于,包括以下步骤:
步骤1、使用分析纯的氢氧化铁Fe(OH)3和分析纯的铁粉Fe以摩尔比2:1混合研磨均匀作为起始原料;
步骤2、使用粉末压片机,将混合物粉末置于Φ5磨具中压成Φ5×4mm圆柱形,将圆柱形样品塞入内腔为Φ5×4mm,外径7mm、厚1mm的铁子母扣中密封;将铁子母扣包裹样品的圆柱形置于h-BN管中,以h-BN为传压介质;
步骤3、将步骤2中装有样品的h-BN管组装在高压合成组装块中并放置在六面顶大压机进行高温高压反应;
步骤4,高温高压反应完成后,将铁子母扣包裹的圆柱形取出,然后使用金刚石切刀剥离表面铁样品腔,将样品取出,在超声中使用酒精清洗后,自然风干样品,即得羟基氧化铁FeOOH晶体。
2.按照权利要求1所述方法,其特征在于,步骤2所述h-BN管具体操作为:在车床上将大小为Φ10mm的h-BN棒中心钻Φ7mm的孔作成h-BN管,将样品塞入管中,两端拿Φ7mm厚度为2mm的h-BN片密封。
3.按照权利要求1所述方法,其特征在于,步骤3所述的将h-BN管组装在高压合成组装块中的方法,具体操作包括:选取一块叶腊石块,在叶腊石块中心打一个Φ12mm圆形通孔;在圆形通孔内套一个外径12mm、内径Φ10mm的圆形石墨加热炉;在石墨加热炉中间放置10mm的h-BN管密封的样品;将圆形石墨加热炉上下两端用叶腊石堵头密封。
4.按照权利要求1所述方法,其特征在于,步骤3中所述高温高压反应条件为,升压至3GPa,然后升温到700-750℃,保压保温48h后淬火。
5.按照权利要求1所述方法,其特征在于,步骤4中得到的所述羟基氧化铁为晶体,晶体尺寸为50-100μm,其形态为针状,呈赤黄色。
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