CN101663240A - 衍生自用氮掺杂的氧化铈具有通式CeO2-x-yNx的Ce-N-O系统 - Google Patents
衍生自用氮掺杂的氧化铈具有通式CeO2-x-yNx的Ce-N-O系统 Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 19
- 229910000420 cerium oxide Inorganic materials 0.000 title abstract description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title abstract description 3
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 9
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 5
- 239000010436 fluorite Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000002555 ionophore Substances 0.000 claims description 3
- 230000000236 ionophoric effect Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
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- 150000001875 compounds Chemical class 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 5
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- 239000000126 substance Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001785 cerium compounds Chemical class 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000002468 redox effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910003071 TaON Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005404 magnetometry Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
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Abstract
本发明公开了一种衍生自用氮掺杂的氧化铈具有通式CeO2－x－yNx的Ce－N－O系统，其中CeO2－x－yNx具有与未掺杂CeO2相同的结构，并且该Ce－N－O系统在重大的技术和策略相关方面，即作为固体电解质和作为催化剂相关方面能够具有五种类似的用途。Ce3+的存在意味着也可以存在发光性能。该化合物借助于固－气反应利用二氧化铈与氨反应而制备作为起始产物。将二氧化铈置于管式炉中并在氨气氛中加热至温度超过400℃。
Description
技术领域
本发明的对象是一种含有铈、氧和氮的产品，其具有与二氧化铈(铈土)类似的结构和应用(作为催化剂或固体电解质)，或者涉及它的光学性能，以及它的制备。它的生产属于化学分支(chemical sector)，具体而言属于无机材料的制备，而它的应用属于能源(固体电解质)领域、传递(或输运)(催化剂)领域和电子与光学(光学性能)领域。
背景技术
氮掺杂是一种重要的用于改变氧化物性能的方法，例如，降低在光催化剂TiO2中的紫外与可见光之间的带隙能量(Asahi，R.；Morikawa，T；Ohwaki，T；Aoki，K；Taga，Y.Science 2001，293，269)。其他的具有重要应用的氧氮化物是光催化剂TaON(Hitoki，G.；Takata，T.；Kondo，J.N.；Hara，M.；Kobayashi，H.；Domen，K.Chem.Comm.2002，1698)以及CaTaO2N-LaTaON2类型的黄-红颜料(Jansen，M.；Letschert，H.P.Nature，2000，404，980)。二氧化铈(CeO2)作为在燃料电池中的固体电解质或作为在机动车中使用的三效催化剂(或三元催化剂)中的氧贮藏成份而具有重要的技术应用(参见，例如Yao，H.C.；Yu Yao，Y.F.Jour.Catálisis，86，1984，254，and Inaba，H.，Tagawa，H.Solid State Ionics，83，1996，1)。
二氧化铈的氮掺杂之前没有被公布或专利保护。仅有的已知二元氮化的(亚硝化，nitrurado)铈化合物是CeN，而仅有的已知在Ce-N-O系统(体系)中的三相(三元相，ternary phases)铈化合物是CeN1-xOx和Ce2N2O。在CeN中的固体氧溶液(或固体氧溶解)是已知的，其具有氯化钠结构及结构式CeN1-xOx，其中x≤0.5(Brown，R.C.；Clark，N.J.J.Inorg.Nucl.Chem.36，1974，1777)。这些固体溶液是通过CeN与CeO2混合物在真空下在1,500℃下的反应来制备的。同样地，具有化学式Ce2N2O并与Ce2O3具有类似结构的化合物的制备已经被公布(Barker，M.G.；Alexander，I.C.J.Chem.Soc.Dalton1974，2166)。氧氮化物Ce2N2O的合成是由Li2CeN2和Li2O或者CeN与CeO2在真空下在1,000℃下的反应而实施(完成)的。
二氧化铈的氧传导性能或催化性能是与它的萤石(型)结构以及它对于氧的吸收和解吸容量(或能力)相关的，而这是与由Ce4+到Ce3+的部分可逆还原以及氧空穴的产生相联系的。在二氧化铈中用氮部分取代氧必然产生阴离子空穴以维持铈的4+氧化态，另外，如果存在由Ce4+到Ce3+的部分还原，则另外的氧空穴将会产生，这样使得氮化二氧化铈必须使结构式成为CeO2-x-yNx。在二氧化铈的萤石(型)结构中的氮引入必然改变它的氧化还原性能以及氧空穴的体系，这会影响它在其两个最重要的应用，作为催化剂或作为离子导体中的行为。另一方面，Ce3+的存在会导致新化合物作为发光材料的应用。
发明内容
本发明的简要描述
本发明的目的是(提供)一种新产品的制备方法，该产品含有铈、氧和氮。它是第一已知产品，具有这样的组成，该组成表现出二氧化铈(CeO2)的结构并具有化学式CeO2-x-yNx，在结构式中x和y是这样的值：0＜x＜0.5而0＜y＜0.5。这种产品是通过二氧化铈在氨气氛中的热处理而获得的，氨气是氮化、还原性气体，并且氮掺杂和三价铈的比例可以借助于在该方法的过程中所使用的最高温度来控制。本发明的优点在于这样的事实：它是一种仅用氮掺杂的产品，而它在以前是不存在的，与未掺杂的二氧化铈CeO2具有相同的结构，并且该产品可以具有类似的高度相关的技术上和战略上的应用，即，作为固体电解质或作为催化剂。由于铈3+(Ce3+)的存在，它也可以具有发光性能。
本发明的详细描述
本发明的对象是一种新产品，其具有组成CeO2-x-yNx，其中x和y是这样的数值：0＜x＜0.5而0＜y＜0.5。所述化合物另外的特征在于，依据其制备方法，它具有萤石型晶体结构(CaF2)，在该结构中铈占据Ca型晶格位置，而氮和氧占据F型晶格位置。新化合物相对于未掺杂的二氧化铈(CeO2)是晶体同构的。根据本发明，该化合物借助于固-气反应，利用二氧化铈与气态氨反应来制备，作为起始产品。二氧化铈被引入管式炉中，并在氨气氛中加热至温度超过400℃。该反应持续至少两小时。本发明的化合物的益处在于在二氧化铈的萤石(型)结构中的氮引入必然改变它的氧化还原性能以及氧空穴的体系，这会影响它在其两个最重要的应用，作为催化剂和作为离子导体中的行为。另一方面，Ce3+的存在会导致新化合物作为发光材料的应用。
附图说明
图1代表本发明的产品的晶体结构。
图2代表本发明的产品的X-射线衍射图谱。
具体实施方式
产品的制备
将2g的二氧化铈(CeO2)引入反应炉中。该反应炉与氨气进口相连，这使得在整个反应过程中在该气体流下实施完成反应成为可能。反应器以每小时200℃的速率加热至700℃的温度，维持该温度7小时；随后，将反应器冷却至环境温度(室温)。在打开反应炉之后，将经氮化的粉末移出，其已经含有纯的CeO2-x-yNx产品，并表现出如在图2中示出的X-射线衍射图谱。
该组成可以借助于不同的技术进行确定，如元素分析以确定氮含量x，以及作为温度函数的磁化率测量以便确定铈3+(Ce3+)的百分比，并间接确定化学计量系数y。由元素分析，通过一小部分样品的燃烧，得到以重量计的氮的百分比为0.36％(x＝0.04)。将样品的第二部分引入磁强计以获得作为温度函数的磁化率曲线，以便确定铈3+(Ce3+)的百分比。该产品是顺磁性的，并含有摩尔比为2％的铈3+(Ce3+)，其使得可以将化合物结构式确定成为CeO1.93N0.04。
Claims (7)
1.由二氧化铈的氮掺杂产生的具有通式CeO2-x-yNx的Ce-N-O系统，其特征在于x和y是这样的值：0＜x＜0.5而0＜y＜0.5。
2.根据权利要求1所述的由二氧化铈的氮掺杂产生的具有通式CeO2-x-yNx的Ce-N-O系统，其特征在于它具有萤石型晶体结构，在该结构中铈位于Ca型晶格位置，而氮和氧位于F型晶格位置。
3.根据权利要求1所述的由二氧化铈的氮掺杂产生的具有通式CeO2-x-yNx的Ce-N-O系统，其特征在于它具有顺磁特性。
4.获得根据权利要求1～3所述的具有通式CeO2-x-yNx的产品的方法，其特征在于它由在氨气氛中在超过400℃的温度下的二氧化铈而获得。
5.具有通式CeO2-x-yNx的产品用作催化剂的用途。
6.具有通式CeO2-x-yNx的产品用作离子导体的用途。
7.具有通式CeO2-x-yNx的产品用作发光材料的用途。
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| ESP200700482 | 2007-02-23 | ||
| ES200700482A ES2304105B1 (es) | 2007-02-23 | 2007-02-23 | Sistema ce-n-o procedente del dopaje de ceria con nitrogeno de formula general ceo2-x-ynx. |
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| KR102372139B1 (ko) * | 2019-05-09 | 2022-03-08 | 단국대학교 천안캠퍼스 산학협력단 | 산화물 나노입자의 전자밴드 엔지니어링을 통한 광학적 물성 제어 |
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| CN115520893B (zh) * | 2022-08-31 | 2023-08-18 | 贵州大学 | 一种高N掺量纳米CeO2的制备方法 |
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| US7164206B2 (en) * | 2001-03-28 | 2007-01-16 | Intel Corporation | Structure in a microelectronic device including a bi-layer for a diffusion barrier and an etch-stop layer |
| CN1902550B (zh) * | 2003-12-26 | 2012-07-18 | 日产化学工业株式会社 | 形成硬掩模用涂布型氮化膜的组合物 |
| US7368388B2 (en) * | 2005-04-15 | 2008-05-06 | Small Robert J | Cerium oxide abrasives for chemical mechanical polishing |
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| CN108203184A (zh) * | 2018-02-01 | 2018-06-26 | 王建伟 | 一种臭氧催化降解印染废水的处理工艺 |
| CN108217905A (zh) * | 2018-02-01 | 2018-06-29 | 王建伟 | 一种非均相臭氧催化降解印染废水的工艺 |
| CN108218040A (zh) * | 2018-02-01 | 2018-06-29 | 彭玉忠 | 一种催化臭氧降解印染废水的处理工艺 |
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| CN108275767B (zh) * | 2018-02-26 | 2020-09-11 | 宿州滋原科技咨询有限公司 | 一种臭氧催化降解印染废水的处理工艺 |
| CN112313008A (zh) * | 2018-04-24 | 2021-02-02 | 华威大学 | 包含阴离子空位晶格的哈伯-博施催化剂 |
| CN110327958A (zh) * | 2019-06-21 | 2019-10-15 | 齐利华(武汉)资源环境科技有限公司 | 一种co2加氢合成甲醇的催化剂及其制备方法、应用 |
Also Published As
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|---|---|
| JP2010519160A (ja) | 2010-06-03 |
| KR20090115754A (ko) | 2009-11-05 |
| ES2304105B1 (es) | 2009-08-13 |
| WO2008102045A1 (es) | 2008-08-28 |
| US20100148111A1 (en) | 2010-06-17 |
| EP2119673A1 (en) | 2009-11-18 |
| ES2304105A1 (es) | 2008-09-01 |
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