针对国产高端稀土卤化物试剂品种少、纯度低、深度净化除杂难度大等问题，本研究系统研究了无水稀土卤化物的深度净化除杂过程中关键杂质元素的传质机理及深度提纯除杂技术，并形成公斤级规模的制备能力。
\r\n以卤化铵脱水法进行高纯无水稀土卤化物制备工艺开发，制备出无水稀土卤化物YbCl3、ErCl3、YBr3、NdI3。
\r\n基于实验室制备工艺，进一步开展了公斤级规模制备工艺的探索，完成了4种高纯无水稀土卤化物试剂公斤级生产线建设和调试，开发出了4项高纯稀土卤化物及类卤化物试剂公斤级规模工艺，建立了公斤级规模工艺文件，公斤级产品纯度及放射性指标均达到指标要求。
\r\n由于稀土材料的特殊性，本数据集实体不对外公开，仅共享元数据。如需获取数据集实体，请联系数据管理者。", "ds_source": "
本数集中的相关数据均为试验数据。其中数据包含了水合稀土卤化物的热重分析测试数据、水合稀土卤化物的脱水过程表征数据、水合稀土卤化物在卤化铵保护下脱水的中间产物XRD表征数据和氧含量分析测试数据、水合稀土卤化物在卤化铵保护下所得产品的XRD表征数据和氧含量分析测试数据、基于卤化铵脱水法进一步深度除氧纯化所得终产品的XRD表征数据和氧含量分析测试数据。
\r\n本研究中分别采用酸卤化铵脱水法开展了高纯无水稀土卤化物的制备工艺研究。
\r\n采用梅特勒托利多公司生产的TGA/DSC1型同步热分析仪对所制备的水合稀土氯化物进行差示扫描量热分析（DSC）和热重分析（TG），样品粉末在氩气气氛中以10℃/min的速率从30℃加热到600℃，氩气流速为100ml/min。
\r\n采用脉冲加热惰气熔融-红外线吸收法对所制得高纯无水稀土氯化物样品中微量氧含量进行测定。所用设备为钢研纳克NCS ON-3000型氧氮分析仪，整台设备置于惰性气体手套箱内，可有效避免环境水分对测试结果的影响。
\r\n采用日本理学公司生产的Smartlab型X射线衍射仪对合成样品进行物相分析（Co靶，λ=0.178752nm）。测试前，在气体手套箱中将研磨充分的稀土氯化物样品压实于可密封的XRD样品载玻片上，采用聚酰亚胺薄膜将载玻片覆盖、密封，避免测试过程中样品与空气中水分发生反应。
", "ds_process_way": "本数集中的水杂质含量、氧杂质含量以及XRD物相表征的相关数据均为试验原始数据，其中XRD数据为使用origin作图软件进行数据表达。
\r\n本数据集中热重分析数据为使用origin作图软件对数据基线拉平处理后作图进行数据表达。
", "ds_quality": "本数集中相关数据在多次重复实验中数据重复性好。因此，本数据集可作为研究高纯稀土卤化物及类卤化物制备工艺的可靠指标。
", "ds_acq_start_time": "2022-11-01 00:00:00", "ds_acq_end_time": "2025-12-31 00:00:00", "ds_acq_place": "有研稀土新材料股份有限公司试验基地", "ds_acq_lon_east": null, "ds_acq_lat_south": null, "ds_acq_lon_west": null, "ds_acq_lat_north": null, "ds_acq_alt_low": null, "ds_acq_alt_high": null, "ds_share_type": "apply-access", "ds_total_size": 0, "ds_files_count": 0, "ds_format": "*.tif，*.pdf", "ds_space_res": "", "ds_time_res": "", "ds_coordinate": "无", "ds_projection": "", "ds_thumbnail": "cc8faa5e-c096-408b-81c3-52788e548cf8.png", "ds_thumb_from": 0, "ds_ref_way": "", "paper_ref_way": "", "ds_ref_instruction": "无", "ds_from_station": "", "organization_id": "af683ce0-400b-4f2f-9242-f45f0621e11a", "ds_serv_man": "李红星", "ds_serv_phone": "0931-4967592", "ds_serv_mail": "ncdc@lzb.ac.cn", "doi_value": "", "subject_codes": [ "410" ], "quality_level": 0, "publish_time": "2026-05-19 16:01:57", "last_updated": "2026-05-19 17:27:16", "protected": false, "protected_to": null, "lang": "zh", "cstr": "", "i18n": { "en": { "title": "Dataset of Preparation Process for High-purity Anhydrous Rare Earth Halides Compounds", "ds_format": "*.tif、*.pdf", "ds_source": "The relevant data in this dataset are all experimental data. The data includes thermogravimetric analysis test data of hydrated rare earth halides, dehydration process characterization data of hydrated rare earth halides, XRD characterization data and oxygen content analysis test data of intermediate products dehydrated by hydrated rare earth halides under ammonium halide protection, XRD characterization data and oxygen content analysis test data of products obtained by hydrated rare earth halides under ammonium halide protection, XRD characterization data and oxygen content analysis test data of final products obtained by further deep deoxygenation purification based on ammonium halide dehydration method.
", "ds_quality": "The relevant data in this dataset has good repeatability in multiple repeated experiments. Therefore, this dataset can serve as a reliable indicator for studying the preparation process of high-purity rare earth halides and halide like compounds.
", "ds_ref_way": "", "ds_abstract": "In response to the problems of limited variety, low purity, and difficulty in deep purification and impurity removal of domestically produced high-end rare earth halide reagents, this study systematically investigated the mass transfer mechanism and deep purification and impurity removal technology of key impurity elements in the deep purification and impurity removal process of anhydrous rare earth halides, and developed a kilogram scale preparation capability.
\r\nDevelopment of a high-purity anhydrous rare earth halide preparation process using ammonium halide dehydration method, resulting in the production of anhydrous rare earth halides YbCl3, ErCl3, YBr3, and NdI3.
\r\nBased on laboratory preparation processes, further exploration of kilogram scale preparation processes was carried out, and the construction and commissioning of four high-purity anhydrous rare earth halide reagent kilogram scale production lines were completed. Four high-purity rare earth halide and halide like reagent kilogram scale processes were developed, and kilogram scale process documents were established. The purity and radioactive indicators of kilogram scale products met the requirements.
\r\nDue to the special nature of rare earth materials, this dataset is not publicly available and only shares metadata. To obtain the entity of the dataset, please contact the data manager.", "ds_time_res": "", "ds_acq_place": "Youyan Rare Earth New Materials Co., Ltd. Experimental Base", "ds_space_res": "", "ds_projection": "", "ds_process_way": "
The water impurity content, oxygen impurity content, and XRD phase characterization data in this dataset are all experimental raw data, with XRD data expressed using Origin plotting software.
", "ds_ref_instruction": "Nothing" } }, "submit_center_id": "ncdc", "data_level": 0, "recommendation_value": 0, "license_type": "https://creativecommons.org/licenses/by/4.0/", "doi_reg_from": "reg_local", "cstr_reg_from": "reg_local", "doi_not_reg_reason": null, "cstr_not_reg_reason": null, "is_paper_in_submitting": false, "ds_topic_tags": [ "稀土卤化物", "卤化铵脱水法；稀土离子；高效脱水；除氧纯化" ], "ds_subject_tags": [ "工程与技术科学基础学科" ], "ds_class_tags": [], "ds_locus_tags": [], "ds_time_tags": [], "ds_contributors": [ { "true_name": "史雅囡", "email": "shiyanan@grirem.com", "work_for": "有研稀土新材料股份有限公司", "country": "中国" } ], "ds_meta_authors": [ { "true_name": "史雅囡", "email": "shiyanan@grirem.com", "work_for": "有研稀土新材料股份有限公司", "country": "中国" } ], "ds_managers": [ { "true_name": "史雅囡", "email": "shiyanan@grirem.com", "work_for": "有研稀土新材料股份有限公司", "country": "中国" } ], "category": "其他" }