Leuchtmann et al. 2014 Nomenclatural realignment of Neotphodium species with genus Epichloe

1909年,Boulenger [1]发现棕黑腹链蛇(Am-phiesma sauteri )。

1962年,Malnate [2]厘定了棕黑腹DOI:10.16605/ki.1007-7847.2023.07.0177湖南省爬行动物新纪录———华西腹链蛇及其系统发育分析收稿日期:2023-07-21;修回日期:2023-10-01;网络首发日期:2024-01-22基金项目:湖南高望界国家级自然保护区陆生脊椎动物调查与小灵猫种群监测与研究(GWJ202301);湖南省古丈县域生物多样性调查与研究(GZ202201)作者简介:黄杰(2001—),男,湖南邵阳人,学生,E-mail:*****************;*通信作者:吴涛(1992—),男,苗族,湖南湘西土家族苗族自治州人,讲师,主要从事动物分类及行为生态研究,E-mail:****************;张佑祥(1966—),男,苗族,湖南湘西土家族苗族自治州人,副教授,主要从事动物学研究,E-mail:*****************。

黄杰1,张自亮2,李辉3,杨鑫宇1,胡小龙1,唐依萍1,刘昕1,刘慧1,张佑祥1*,吴涛1*(1.吉首大学生物资源与环境科学学院,中国湖南吉首416000;2.湖南高望界国家级自然保护区管理局,中国湖南湘西自治州416308;3.湖南师范大学生命科学学院脊椎动物学实验室,中国湖南长沙410081)摘要:2023年5月24日于湖南省高望界国家级自然保护区(28°41′36″N,110°09′30″E;212m)采集到东亚腹链蛇属(Hebius )一雌性物种标本,经形态特征比较,符合华西腹链蛇(Hebius maximus )形态描述;基于线粒体cytb 基因构建的东亚腹链蛇属部分物种的贝叶斯系统发育树显示,该标本与华西腹链蛇(H.maximus )聚为一支,其遗传距离为1.7%~2.2%。

ClarificationofthenomenclatureforMSCPOSITION PAPERClari?cation of the nomenclature for MSC:The International Society for Cellular Therapy positionstatementEM Horwitz 1,K Le Blanc 2,M Dominici 3,I Mueller 4,I Slaper-Cortenbach 5,FC Marini 6,RJ Deans 7,DS Krause 8and A Keating 91Divisions of Stem Cell Transplantation and Experimental Hematology,St Jude Children’s ResearchHospital,Memphis,Tennessee,USA,2Center for Allogeneic Stem Cell Transplantation,Department of Laboratory Medicine,Karolinska UniversityHospital,Karolinska Institute,Stockholm,Sweden,3Laboratory of Cell Biology and Advanced Cancer Therapy,Oncology-Hematology Department,University of Modena and Reggio Emilia,Modena,Italy,4University Children’s Hospital,Department of Hematology and Oncology,Tuebingen,Germany,5Department of Medical Immunology,UMC Utrecht,Utrecht,the Netherlands,6Department of Blood and Marrow Transplant,UT-MD Anderson Cancer Center,Houston,Texas,USA,7Athersys Inc.,Cleveland,Ohio,USA,8Department of Laboratory Medicine,Yale University School of Medicine,NewHaven,Connecticut,USA and 9Department of Medical Oncology and Hematology Princess Margaret Hospital/Ontario Cancer InstituteToronto,Ontario,CanadaThe plastic-adherent cells isolated from BM and other sources have come to be widely known as mesenchymal stem cells (MSC).However,the recognized biologic properties of the unfractionated population of cells do not seem to meet generally accepted criteria for stem cell activity,rendering the name scientifically inaccurate and potentially misleading to the lay public.Nonetheless,a bona fide MSC most certainly exists.To address this inconsistency between nomenclature and biologic properties,and to clarify the terminology,we suggest that the fibroblast-like plastic-adherent cells,regardless of the tissue from which they are isolated,be termed multipotent mesenchymalstromal cells,while the term mesenchymal stem cells is used only for cells that meet specified stem cell criteria.The widely recognized acronym,MSC,may be used for both cell populations,as is the current practice;thus,investigators must clearly define the more scientifically correct designation in their reports.The International Society for Cellular Therapy(ISCT)encourages the scientific community to adopt this uniform nomenclature in all written and oral communications.KeywordsMesenchymal stem cell,MSC,stromal cell.Mesenchymal stem cell (MSC)is the designation com-monly applied to the plastic-adherent cells isolated from BM,adipose and other tissues,with multipotent differ-entiation capacity in vitro .The notion of a stromal stem cell was proposed by Maureen Owen [1,2]based in large part on the work of Friedenstein et al.[3,4].Caplan popularized the term mesenchymal stem cell in the early 1990s [5];however,in the latter half of the decade some investigators opted to omit any reference to a stem cell identity when publishing pre-clinical [6,7]or clinical [8á10]studies of MSC.In 2000,a workshop at the Annual Meeting of the International Society for Cellular Therapy (ISCT),attended by many of the leading investigators in mesenchymal cell therapy,concluded that convincing data to support the ‘stemness’of the unfractionated plastic-adherent cells was lacking [11].Nonetheless,the terminol-ogy has persisted and the acronym MSC is firmly engrained in the vernacular of stem cell biologists and clinical cell therapists.As the ‘stem cell’label has scientific implications that may or may not be strictly correct,the Mesenchymal and Tissue Stem Cell Committee of the ISCT recommends a clarification of the nomenclature for these important cells.The broader aim of this position statement is to foster the use of scientifically accurate, Correspondence to:Edwin M.Horwitz ,MD,PhD,Divisions of Stem Cell Transplantation and Experimental Hematology,St Jude Children’s Research Hospital,Mail Stop 321,/doc/775fd72b3169a4517723a304.html uderdale,Memphis,TN 38105,USA.Cytotherapy (2005)Vol.7,No.5,393á395–2005ISCTDOI:10.1080/14653240500319234standardized terminology to facilitate exchange of knowl-edge among biomedical investigators and dissemination of knowledge,without fueling unrealistic expectations,to the general public.W e propose that the plastic-adherent cells currently described as mesenchymal stem cells be termed multi-potent mesenchymal stromal cells,while the term me-senchymal stem cell should be reserved for a subset of these(or other)cells that demonstrate stem cell activity by clearly stated criteria.For both cell populations,the acronym MSC may be used;thus it is imperative that investigators unequivocally define the acronym in pre-sentations of their work.Rather than renaming the cells or redefining the acronym,which would probably further the confusion in our field,this position statement is a call for clarity of terminology to reduce the existing confusion and avoid misrepresentation.W e arrived at this similar but importantly distinct terminology based on several considerations.First,we believe maintaining the acronym MSC is vital.This term indicates a general cell type to biomedical investigators and has been used extensively in the literature for at least two decades.Thus,we wish to maintain the continuity of the scientific discourse,the electronic literature databases, and again,minimize confusion.Second,we sought to indicate the special biologic properties of the population of plastic-adherent cells,but eliminate the term stem from the nomenclature,as this word,currently,has a specific functional connotation,i.e.a long-term self-renewing cell that is capable of differentia-tion into specific,multiple cell types in vivo.There now seems to be a near universal consensus that the cells isolated by adherence to plastic during ex vivo culture of BM cells have broad biologic properties not shared by‘garden variety’fibroblasts isolated from other sources,e.g. dermal fibroblasts;however,these plastic-adherent marrow cells are not a uniform population of stem cells.In fact,the population of isolated cells is actually quite heterogeneous, which is most easily demonstrated by the relatively small fraction of adherent cells that can generate fibroblast colonies(CFU-F)in vitro.While we do not doubt the multipotentiality of these cells nor their capacity to regenerate tissues,and clearly recognize that the general definition of a stem cell is evolving,we suggest that current data are insufficient to characterize unfractionated plastic-adherent marrow cells as stem cells,and,therefore,suggest using the term multipotent mesenchymal stromal cell to indicate these unique properties without ascribing homo-geneity or stem cell activity.Third,we completely support the notion that a rare, bona fide mesenchymal stem cell exists and must acknowl-edge this fact.However,just as hematologists do not consider human marrow cells selected for CD34expres-sion as a uniform population of stem cells,although this subset clearly contains human hematopoietic stem cells, we should not consider the human marrow cells selected for plastic adherence as a uniform population of stem cells, although that subset may contain mesenchymal stem cells. By further analogy to hematology,biomedical studies of the plastic-adherent cells may be designed to address mesenchymal stem cell activity,just as CD34'cells are used for long-term hematopoietic repopulating activity. Indeed,the in vitro CFU-F may well be an index of a mesenchymal stem cell;however,in vivo demonstrations of long-term survival with self-renewal capacity and tissue repopulation with multi-lineage differentiation are prov-ing to be far more challenging than for hematopoietic stem cells.Fourth,while the entire differentiation potential re-mains to be elucidated and MSC may differentiate to tissues originating in more than one embryonic germ layer, current studies suggest that these cells are of mesenchymal origin.Thus,we wished to maintain this designation to imply the origin,but not the differentiation potential,of the cells.Finally,the cells seem to be found in situ within the supportive stromal compartment of resident tissues.Thus, regardless of the tissue source from which the cells are isolated,e.g.BM,adipose tissue,umbilical cord blood and (mobilized)peripheral blood,the unfractionated popula-tion may be aptly termed stromal cells,avoiding any reference to their biologic or therapeutic potential.Once a mesenchymal stem cell or stem cell activity has been clearly demonstrated,the moniker of stem cell may be accurately applied.Using the term multipotent mesenchymal stromal cells for the plastic-adherent population seems to be the most scientifically accurate descriptor without implying unpro-ven biologic or therapeutic potential.The term mesench-ymal stem cells should be reserved for cells that meet such criteria.W e suggest all investigators in the field adopt this uniform terminology in scientific communications with the expectation that the lay press will follow.Future statements from the ISCT will seek to propose a uniform,394EM Horwitz et al.minimal definition for multipotent mesenchymal stromal cells,and unambiguous criteria to define a putative,bona fide mesenchymal stem cell.W e hope these statements will clarify confusing nomenclature and serve as a foundation for scientific studies and dialog to characterize the biologic properties and therapeutic potential of these important cells.References1Owen M.Lineage of osteogenic cells and their relationship to the stromal system.In:Peck W,ed.Bone and Mineral Research. Elsevier,New York,1985:1á25.2Owen M.Marrow stromal stem cells.J Cell Sci1988;10 (Suppl):63á76.3Friedenstein AJ,Petrakova KV,Kurolesova AI et al.Heterotopic of bone marrow.Analysis of precursor cells for osteogenic and hematopoietic tissues.Transplantation1968;6:230á47.4Friedenstein AJ,Chailakhyan RK,Latsinik NV et al.Stromal cells responsible for transferring the microenvironment of the hemopoietic tissues.Cloning in vitro and retransplantation in vivo.Transplantation1974;17:331á40.5Caplan AI.Mesenchymal stem cells.J Orthop Res1991;9:641á50. 6Pereira RF,Halford KW,O’Hara MD et al.Cultured adherent cells from marrow can serve as long-lasting precursor cells for bone,cartilage,and lung in irradiated mice.Proc Natl Acad Sci USA1995;92:4857á61.7Pereira RF,O’Hara MD,Laptev A et al.Marrow stromal cells asa source of progenitor cells for nonhematopoietic tissues intransgenic mice with a phenotype of osteogenesis imperfecta.Proc Natl Acad Sci USA1998;95:1142á7.8Keating A,Berkahn L,Filshie R.A phase I study of the transplantation of genetically marked autologous bone marrow stromal cells.Hum Gene Ther1998;9:591á600.9Horwitz EM,Prockop DJ,Fitzpatrick LA et al.Transplantability and therapeutic effects of bone marrow-derived mesenchymal cells in children with osteogenesis imperfecta.Nat Med 1999;5:309á13.10Horwitz EM,Gordon PL,Koo WKK et al.Isolated allogeneic bone marrow-derived mesenchymal cells engraft and stimulate growth in children with osteogenesis imperfecta:implications for cell therapy of bone.Proc Natl Acad SciUSA2002;99:8932á7. 11Horwitz EM,Keating A.Nonhematopoietic mesenchymal stem cells:what are they?Cytotherapy2000;2:387á8.Nomenclature for MSC395。

第 63 卷第 2 期2024 年 3 月Vol.63 No.2Mar.2024中山大学学报（自然科学版）（中英文）ACTA SCIENTIARUM NATURALIUM UNIVERSITATIS SUNYATSENI红树植物桐花树内生真菌Talaromyces amestolkiae 30的次生代谢产物*刘洪亮1，赵飞1，唐凤婷1，李锦俊1，张轩1，杜志云1，黄华容1，佘志刚21. 广东工业大学生物医药学院，广东广州 5100062. 中山大学化学学院，广东广州 510006摘要：对红树植物桐花树内生真菌Talaromyces amestolkiae 30的次级代谢产物进行了研究。

采用大米固体发酵培养，色谱分离技术纯化单体，ESIMS和NMR等波谱数据分析，鉴定了12个异香豆素单体化合物：aspergillumarin A（1）、aspergillumarin B（2）、 5，6-dihydroxy-3-（4-hydroxypentyl）-isochroman-1-one（3）、 mucoriso‐coumarin A（4）、 peniisocoumarin H（5）、 peniisocoumarin E（6）、 dichlorodiaportin（7）、 mucorisocoumarin C（8）、 peniiso‐coumarin G（9）、 talumarin A（10）、 5，6，8-trihydroxy-4-（1'-hydroxyethyl）-isocoumarin（11）和sescandelin（12），其中化合物4、6、7首次从篮状属真菌中分离得到。

二倍稀释法抑菌活性测试显示，化合物4、6、7有抑制金黄色葡萄球菌作用；MTT法测试细胞毒活性，表明化合物7对前列腺癌PC-3细胞和VCaP细胞有细胞毒活性。

关键词：红树林真菌；篮状菌；次级代谢产物；异香豆素类中图分类号：O629.9 文献标志码：A 文章编号：2097 - 0137（2024）02 - 0160 - 08The metabolites from mangrove endophytic fungus Talaromyces amestolkiae30LIU Hongliang1， ZHAO Fei1， TANG Fengting1， LI Jinjun1，ZHANG Xuan1， DU Zhiyun1， HUANG Huarong1， SHE Zhigang21. School of Biomedicine， Guangdong University of Technology， Guangzhou 510006， China2. School of Chemistry， Sun Yat-sen University， Guangzhou 510006， ChinaAbstract：The metabolites of the endophytic fungus Talaromyces amestolkiae30 from the mangrove plant Aegiceras corniculatum (L.) Blanco were investigated. The fungus was cultured in rice medium, the monomeric compounds were isolated and purified by the chromatographic technique, and the structures of the compounds were identified by analysis of spectroscopy such as ESIMS and NMR.Twelve known analogues of isocoumarins (1-12) were isolated and identified as aspergillumarin A (1), aspergillumarin B (2), 5,6-dihydroxy-3-(4-hydroxypentyl)-isochroman-1-one (3), mucorisocoumarin A(4), peniisocoumarin H (5), peniisocoumarin E (6), dichlorodiaportin (7), mucorisocoumarin C (8), peni‐isocoumarin G (9), talumarin A (10), 5,6,8-trihydroxy-4-(1'-hydroxyethyl)-isocoumarin (11) and sescan‐delin (12). Among them, compounds 4, 6 and 7 were obtained from the genus Talaromyces for the first time. The antibacterial activities of these compounds were tested in vitro using the twofold dilution method. Compounds 4, 6, and 7 showed inhibitory activity against Staphylococcus aureus. The cytotoxic activity was tested by the MTT assay. Compound 7 showed cytotoxicity against prostate cancer PC-3DOI：10.13471/ki.acta.snus.2023E048*收稿日期：2023 − 10 − 14 录用日期：2023 − 11 − 30 网络首发日期：2024 − 01 − 08基金项目：广东省海洋经济发展（海洋六大产业）专项资金（粤自然资合［2021］48号）作者简介：刘洪亮（1996年生），男；研究方向：制药工程；E-mail：*********************通信作者：黄华容（1978年生），女；研究方向：天然药物化学；E-mail：****************.cn第 2 期刘洪亮，等：红树植物桐花树内生真菌Talaromyces amestolkiae 30的次生代谢产物cells and VCaP cells.Key words ： mangrove fungus ； Talaromyces amestolkiae ； secondary metabolites ； isocoumarin 异香豆素是一类重要的天然产物，广泛存在于自然界中，其种类繁多（Saddiqa et al.，2017； Reveglia et al.，2020；Shabir et al.，2021；Aierken et al.，2023）。

俯冲带变质过程中的含碳流体刘景波【摘要】俯冲带含碳岩石通过俯冲过程的变质反应生成了含碳水流体、富硅酸盐的超临界流体和含碳熔体.不同类型流体的形成与岩石成分和岩石经历的温压条件相关.岩石中碳酸盐矿物脱碳反应的温压条件取决于岩石起初的流体成分:有水存在时,反应发生在低温条件下.在高压条件下,碳酸盐矿物在水或含盐水流体的溶解是生成含碳流体重要的机制,其导致的碳迁移作用可能超过脱碳变质反应的作用.高温条件下,含碳岩石的部分熔融可以生成含碳的熔体,这在热俯冲环境和俯冲带岩石底辟到上覆地幔的情况下是碳迁移重要载体.富硅酸盐的超临界流体可能是在第二临界端点上形成的超临界流体,目前在超高压岩石中观察到的非花岗质成分的多相固体包裹体被认为是这种流体结晶的产物,然而对其理解尚存在很多问题,需要进一步的实验研究.地表含碳岩石在俯冲带被带到深部,俯冲带地温特征的不同导致了不同类型含碳流体的形成,这些流体运移至上覆地幔引起岩石部分熔融产生含碳的岛弧岩浆,岩浆喷出到地表释放了其中的碳,这构成了俯冲带-岛弧系统的碳循环.【期刊名称】《岩石学报》【年(卷),期】2019(035)001【总页数】10页(P89-98)【关键词】俯冲带;碳循环;含碳流体;多相包裹体;熔体包裹体【作者】刘景波【作者单位】中国科学院地质与地球物理研究所,岩石圈演化国家重点实验室,北京100029;中国科学院大学地球与行星科学学院,北京100049【正文语种】中文【中图分类】P542.5;P588.3俯冲带-岛弧系统的碳循环模式可以概括这样一种图景：含碳岩石通过俯冲过程的变质作用形成含碳流体，含碳流体运移至上覆地幔楔交代其中的岩石导致部分熔融产生含碳的岛弧岩浆，岩浆上升到地表将碳以CO2形式释放到地表的物质圈层中去。

岛弧火山作用释放的CO2在碳同位素组成上证明了这种过程的存在。

岛弧岩浆的δ13 C在-0.1‰～-11.6‰之间，这种成分的碳是俯冲带的碳酸盐（δ13 C＝0‰）、蚀变大洋玄武岩及其下覆地慢岩的碳（δ13 C＝-5‰）和俯冲岩石中的有机碳（δ13 C＝-30‰）混合的结果（Sano and Marty，1995；Shaw et al.，2003；De Leeuw et al.，2007）。

微小残留病灶(MRD)监测在慢性淋巴细胞白血病(CLL)中的应用进展任雨虹【摘要】慢性淋巴细胞白血病(chronic lymphocytic leukemia,CLL)是西方国家最常见的成人白血病,在我国的发病率也日益增加.近年来针对CLL的新药层出不穷,微小残留病灶(minimal residual disease,MRD)监测逐渐成为评估疗效的重要手段.本文总结了目前常用的MRD检测方法,包括流式细胞学和基于PCR法的分子学检测,并介绍了其在初治CLL疗效评价、预后评估和在移植后CLL复发预警方面的应用进展.【期刊名称】《复旦学报（医学版）》【年(卷),期】2019(046)003【总页数】5页(P404-407,419)【关键词】慢性淋巴细胞白血病(CLL);微小残留病灶(MRD);监测【作者】任雨虹【作者单位】复旦大学附属中山医院血液科上海 200032【正文语种】中文【中图分类】R733.72慢性淋巴细胞白血病(chronic lymphocytic leukemia,CLL)是一种成熟B淋巴细胞克隆增殖性肿瘤,以淋巴细胞在外周血、骨髓、脾脏和淋巴结聚集为特征,在西方国家的年发病率为4.2/10万,80岁以上人群年发病率甚至超过30/10万[1]。

CLL的治疗方案经历了从传统化疗到化学免疫治疗的转变,但CLL的首要治疗目标仍是获得更深程度的缓解和更持久的无进展生存(progression free survival,PFS)。

能达到更深检测程度的微小残留病灶(minimal residual disease,MRD)监测逐渐成为了疗效评估的重要指标。

不同于其他白血病,CLL预后的高度异质性和累及多部位的特点使得针对其MRD的监测比其他白血病更复杂。

本文将对目前MRD监测在CLL中的应用进展进行介绍。

MRD在CLL中的检测方法作为一项评估疗效深度的监测指标,理想的MRD检测方法需满足可定量、标准化、便捷性的要求。

SPS DISKS- For in vitro use only - Catalogue No. DS65Our SPS Disks can be used for the presumptive identification of Peptostreptococcus anaerobius based on its sensitivity to sodium polyanetholsulphonate (SPS).Studies performed by Wideman et al. and Graves et al. showed that all strains of Peptostreptococcus anaerobius are inhibited by SPS, while other Gram-positive cocci are resistant to SPS. The identification of P. anaerobius is significant since Wideman et al. found that Peptostreptococcus anaerobius may account for one-fifth to one-third of all Gram-positive cocci encountered in clinical specimens. Our SPS Disks contain 1-mg of sodium polyanetholsulphonate and when used as recommended all strains of Peptostreptococcus anaerobius give zones of inhibition ranging from 12 to 30-mm. Recommended Procedure1.Obtain a pure, overnight culture of the testorganism and make an inoculum suspension equivalent to a 0.5 McFarland standard.2.Swab or streak a sample of the suspension onto anon-selective anaerobic blood agar plate or Wilkins-Chalgren Anaerobic Plate in three directions to give a heavy confluent growth.3.Aseptically place a SPS Disk on the agar surface.4.Incubate anaerobically at 35°C for 48 hours.5.Measure the zone of inhibition around the disk tothe nearest millimeter.Interpretation of ResultsA zone of inhibition ≥12-mm indicates SPS sensitivity (S), while a zone of inhibition <12-mm indicates resistance (R) to SPS.Additional biochemical and/or serological tests should be performed on isolated colonies from pure culture in order to complete identification. •Some strains of P. micros are sensitive to SPS. Microscopic differentiation is possiblesince P. micros appear as tiny cocci whereascells of P. anaerobius appear as largecoccobacilli•To ensure the accuracy of the observed results, always run positive and negativecontrols along with the test organismQuality ControlOrganism Expected Results Peptostreptococcus anaerobiusATCC 27337SSPS-sensitivePeptostreptococcus asaccharolyticusATCC 29743RSPS-resistant Storage and Shelf LifeOur SPS Disks should be stored at 4°C to 8°C, and protected from light. Under these conditions they have a shelf life of 26 weeks from the date of manufacture.References1.Balows A, Hausler WJ Herman KL et al.Manual of clinical microbiology. 5th ed.Washington, DC: ASM, 1991.2.Wideman PA, Vargo VL, Citronbaum D andFinegold SM. J. Clin. Micro. 4 (1976).3.Graves MH, Morello JA and Knocka FE.Appl. Microbiol. 27 (1974).Original: September 2000Revised / Reviewed: October 2014。

第53卷第9期表面技术2024年5月SURFACE TECHNOLOGY·43·添加Al(NO3)3对镁合金表面水滑石蒸汽涂层耐蚀性能的影响马言耀，潘仕琪，张芬*，崔蓝月，李硕琦，刘成宝，曾荣昌*（山东科技大学 材料科学与工程学院，山东 青岛 266590）摘要：目的研究原位蒸汽法制备层状双金属氢氧化物（LDH）的反应机理，以及添加Al(NO3)3对AZ91D 镁合金表面水滑石蒸汽涂层耐蚀性的影响和耐蚀机理。

方法在蒸汽源中添加不同浓度的Al(NO3)3，以提供Al3+，采用原位蒸汽法在150 ℃下进行5 h水热反应，在AZ91D镁合金表面制备水滑石蒸汽涂层。

使用XRD、FT-IR、SEM、EDS 等测试手段对水滑石蒸汽涂层进行表征，通过动电位极化、电化学阻抗和盐雾试验，研究水滑石蒸汽涂层的生长机理及腐蚀机理。

结果基于不同浓度梯度的Al(NO3)3，在AZ91D镁合金表面成功制备了水滑石蒸汽涂层，涂层的主要组成物相为Mg(OH)2、Mg-Al-NO3−LDH、Mg-Al-CO32−LDH。

Al(NO3)3/LDH相较于未添加Al(NO3)3得到的LDH，其生长均匀、结构致密，耐腐蚀性能由大到小的顺序为LDH-100、LDH-200、LDH-50、LDH-20、LDH、AZ91D镁合金。

水滑石蒸汽涂层的腐蚀产物主要为Mg(OH)2、MgCO3。

结论在添加100 mmol/L的Al(NO3)3作为蒸汽源时，充足的Al3+保证了合成结构致密水滑石的需要，副产物最少，且耐蚀性最好。

最后，讨论了水滑石蒸汽涂层的生长机理和腐蚀机理。

关键词：镁合金；水滑石；原位蒸汽法；耐蚀性能；成膜机理中图分类号：TG174 文献标志码：A 文章编号：1001-3660(2024)09-0043-13DOI：10.16490/ki.issn.1001-3660.2024.09.005Effect of Al(NO3)3 on the Corrosion Resistance of LDH SteamCoatings on Magnesium Alloy SurfaceMA Yanyao, PAN Shiqi, ZHANG Fen*, CUI Lanyue, LI Shuoqi,LIU Chengbao, ZENG Rongchang*(School of Materials Science and Engineering, Shandong University of Science andTechnology, Shandong Qingdao 266590, China)ABSTRACT: Magnesium and its alloys, due to their remarkable biodegradability and mechanical properties, particularly their specific strength, have gained widespread attention and are being increasingly utilized as a green engineering material. However, their reactive chemical nature makes them susceptible to corrosion, limiting their widespread application. Surface modification techniques now serve as an effective means of enhancing the corrosion resistance of magnesium alloys. Layered double hydroxide (LDH), a layered structural material, has the ability to adsorb corrosive ions, thus protecting the magnesium alloy收稿日期：2023-11-15；修订日期：2024-03-04Received：2023-11-15；Revised：2024-03-04基金项目：国家自然科学基金（51601108，52071191）Fund：National Natural Science Foundation of China (51601108, 52071191)引文格式：马言耀, 潘仕琪, 张芬, 等. 添加Al(NO3)3对镁合金表面水滑石蒸汽涂层耐蚀性能的影响[J]. 表面技术, 2024, 53(9): 43-55.MA Yanyao, PAN Shiqi, ZHANG Fen, et al. Effect of Al(NO3)3 on the Corrosion Resistance of LDH Steam Coatings on Magnesium Alloy Surface[J]. Surface Technology, 2024, 53(9): 43-55.*通信作者（Corresponding author）·44·表面技术 2024年5月substrate. Reports indicate that the Al content in magnesium alloys can affect the LDH content in steam coatings, which in turn affects the corrosion resistance of these coatings. However, the impact of introducing Al outside the magnesium alloy substrate on corrosion resistance remains unclear.The work aims to investigate the in-situ steam synthesis mechanism of LDH and assess how the Al(NO3)3 affects the corrosion resistance and mechanism of LDH steam coatings on AZ91D magnesium alloy surfaces. An in-situ steam method was used to deposit LDH steam coatings on AZ91D magnesium alloy surfaces.This process involved a steam reaction at 150 ℃for 5 hours, during which different concentrations of Al(NO3)3 were added to the steam source solution to generate Al3+. The LDH steam coatings were characterized by XRD, FT-IR, SEM and EDS. Potentiodynamic polarization, electrochemical impedance spectroscopy, and salt spray tests were utilized to evaluate their growth mechanism, corrosion resistance, and corrosion mechanism. The results indicated that LDH steam coatings were successfully deposited on the surface of AZ91D magnesium alloy with different concentration gradients of Al(NO3)3. The main constituent phases of the coatings were Mg(OH)2, Mg-Al-NO3− LDH, and Mg-Al-CO32− LDH. When compared to LDH obtained without Al(NO3)3, the growth of Al(NO3)3/LDH was uniform and the structure was dense.The order of corrosion resistance of LDH-100, LDH-200, LDH-50, LDH-20, LDH, AZ91D magnesium alloy was determined through potentiodynamic polarization, electrochemical impedance, and salt spray tests. The corrosion products of the LDH steam coatings primarily consisted of Mg(OH)2 and MgCO3. When a 100 mmol/L concentration of Al(NO3)3 was used as the steam source, sufficient Al3+ participated in the nucleation and growth of LDH, leading to the synthesis of LDH with the best corrosion resistance. This improvement was attributed to the appropriate concentration of Al3+ promoting the formation of LDH steam coatings with fewer by-products and a dense structure.A discussion on the growth mechanism and corrosion mechanism of LDH steam coatings was also provided. The LDHsteam coatings prepared with Al(NO3)3 as a steam source demonstrates great potential for application on the surface of magnesium alloys as green engineering materials.KEY WORDS: magnesium alloy; layered double hydroxide; in-situ steam method; corrosion resistance; film-forming mechanism近年来，镁及其合金因其比强度高、阻尼性优良等特性而具有巨大的应用潜力[1-5]。

A correlative approach to segmenting phases and ferrite morphologiesin transformation-induced plasticity steel using electron back-scattering diffraction and energy dispersive X-ray spectroscopyAzdiar A.Gazder a,n,Fayez Al-Harbi b,Hendrik Th.Spanke b,David R.G.Mitchell a,Elena V.Pereloma a,ba Electron Microscopy Centre,University of Wollongong,New South Wales2500,Australiab School of Mechanical,Materials and Mechatronic Engineering,University of Wollongong,New South Wales2522,Australiaa r t i c l e i n f oArticle history:Received18April2014Received in revised form18June2014Accepted6July2014Available online19July2014Keywords:Transformation-induced plasticity(TRIP)SteelElectron back-scattering diffraction(EBSD)Energy dispersive X-ray spectroscopy(EDS)Transmission electron microscopy(TEM)Carbon partitioningBainitea b s t r a c tUsing a combination of electron back-scattering diffraction and energy dispersive X-ray spectroscopydata,a segmentation procedure was developed to comprehensively distinguish austenite,martensite,polygonal ferrite,ferrite in granular bainite and bainitic ferrite laths in a thermo-mechanically processedlow-Si,high-Al transformation-induced plasticity steel.The efficacy of the ferrite morphologiessegmentation procedure was verified by transmission electron microscopy.The variation in carboncontent between the ferrite in granular bainite and bainitic ferrite laths was explained on the basis ofcarbon partitioning during their growth.&2014Elsevier B.V.All rights reserved.1.IntroductionAdvanced high strength transformation-induced plasticity(TRIP)steels were mainly developed for automotive applicationsas they possess high strength–ductility ratios,formability andenergy absorption properties[1,2].They are characterised by acomplex multiphase microstructure comprising retained auste-nite,martensite,polygonal ferrite and carbide-free bainites[3–5].Although there are different terminologies in use[6–11],it isgenerally accepted that during the continuous cooling or isother-mal holding of low carbon steels,the formation of intermediateaustenite decomposition products(between diffusional ferrite/pearlite and diffusionless martensite)occurs.In TRIP steels,theyare usually termed as granular bainite and bainitic ferrite.Heregranular bainite is defined as carbide-free bainite with irregular-shaped ferrite or ferrite plates and dispersed blocky martensite/retained austenite constituent.On the other hand,bainitic ferrite isthe arrangement of ferrite laths separated by layers of retainedaustenite and/or martensite[7,10–12].Both ferrites in these twocarbide-free bainitic morphologies exhibit a much higher disloca-tion density than polygonal ferrite as well as a supersaturation incarbon[13–17].Under conventional electron back-scattering diffraction(EBSD)acquisition conditions,TRIP steel microstructures are typicallyindexed as iron fcc(austenite)and bcc(ferrite).Depending onthe TRIP steel alloy composition and thermo-mechanical processinghistory,the various bcc phases(martensite and polygonal ferrite)and ferrite morphologies(ferrite in granular bainite and bainiticferrite laths)then need to be further segmented during the post-processing of the EBSD map.However,to-date the lack of acomprehensive method that consistently distinguishes betweenthe above phases/ferrite morphologies poses a significant hurdle tofurthering our understanding of the complex interplay betweenthem during loading.Over the past15years,the methods to segment phases/ferritemorphologies have relied on various analytical tools that either:(i)quantify the conditions under which the electron back-scattering pattern(EBSP)was acquired,or(ii)make use of thequality metrics of the acquired EBSP after Hough transformation(Table1).The parameters that describe the conditions underwhich the EBSP was acquired are the least used and include theconfidence index(CI)and the pattern misfit angle(PM).The CIContents lists available at ScienceDirectjournal homepage:/locate/ultramicUltramicroscopy/10.1016/j.ultramic.2014.07.0050304-3991/&2014Elsevier B.V.All rightsreserved.n Corresponding author.Tel.:þ61242215904;fax:þ61242213114.E-mail address:azdiar@.au(A.A.Gazder).Ultramicroscopy147(2014)114–132involves a Kikuchi band triplet voting scheme such that within a given inter-planar angular tolerance,the ratio between the candidate orientation with the highest number of votes and the total number of votes is regarded as the most likely solution[18]. Once a solution is selected,the PM is used to calculate the mean angular deviation between the positions of the simulated and experimental EBSPs.On the other hand,the quality metrics of the acquired EBSP that are derived from Hough transformation include the image quality(IQ,also known as the pattern quality(PQ)or band contrast (BC))and the band slope(BS).The IQ/PQ/BC defines the average intensity of the Hough peaks[19]whereas the BS denotes the average slope of the intensity change between the Hough peaks and their surrounding background[20].In practice,the IQ/PQ/BC and BS are greyscaled and binned to a byte range between0 (black)to255(white).Structures with elastically distorted lattices, higher density of crystalline defects or residual stresses(causatives that can be linked to the transformation of austenite to bainite or martensite)present with blurred Kikuchi band edges,diffuse Hough peaks and appear darker with lower IQ/PQ/BC and BS values[21].Conversely,polygonal ferrite presents with sharper Kikuchi band edges,more intense Hough peaks and has higher IQ/ PQ/BC and BS values.The IQ/PQ/BC are the most commonly used parameters to distinguish between features with varying dislocation density by thresholding the distribution between areas of low and high contrast.In order to accomplish this semi-quantitatively,the thresholding procedure relies on the presence of a clear and specific inversion point between individual peaks of the IQ/PQ/ BC distribution.For example,in the case of a bimodal distribution, the threshold is conventionally defined as the lowest value between the two distinct peaks.Taking advantage of this statistical peculiarity,one of thefirst EBSD studies on Fe–1.57Mn–1.46Si–0.91C and Fe–1.57Mn–1.23Al–0.34Si–0.31C(wt%1)TRIP steels by De Meyer et al.[22]used the IQ/PQ/BC to distinguish the ferrite in bainite from polygonal ferrite.The same technique was used to observe/quantify the volume(or area)fractions of:(i)polygonal ferrite and martensite in Fe–3.28Ni–0.12C[23,24],Fe–0.09C dual phase[25],and Fe–1.8Mn–1.51Si–0.2C quench and partitioned TRIP steels[26],(ii)polygonal ferrite and the ferrite in bainite in Fe–1.5Mn–1.5Si–0.2C[27],Fe–1.48Mn–1.08Al–0.28Si–0.27C[28] and Fe–1.6Mn–1.28Si–0.12C[29]TRIP steels,and(iii)the ferrite in bainite and martensite in Fe–1.5Mn–1.5Si–0.6C[30]and Fe–1.43Si–0.58Mn–0.56C–0.47Cr SAE9254steels[31].The BS parameter has been applied less often.Kwon et al.[32] used the BS to distinguish the ferrite in bainite from polygonal ferrite in austempered Fe–1.5Mn–1.5Si–0.2C TRIP steel.The low BS of the ferrite in bainite was ascribed to its formation during theTable1The types of EBSD-based segmentation procedures undertaken to-date on multi-phase steels.Segmentation method SteeltypeSteel composition(wt%)Phases/constituents Ref.Thresholding the distribution of one parameterIQ/PQ/BC TRIP Fe–1.57Mn–1.46Si–0.91C and Fe–1.57Mn–1.23Al–0.34Si–0.31CPolygonal ferrite,ferrite in bainite[22]Fe–1.8Mn–1.51Si–0.2C Polygonal ferrite,martensite[26]Fe–1.5Mn–1.5Si–0.2C Polygonal ferrite,ferrite in bainite[27]Fe–1.48Mn–1.08Al–0.28Si–0.27C Polygonal ferrite,ferrite in bainite[28]Fe–1.6Mn–1.28Si–0.12C Polygonal ferrite,ferrite in bainite[29]Fe–1.5Mn–1.5Si–0.6C Ferrite in bainite,martensite[30]Fe–1.9Si–1.43Mn–0.21C Ferrite in bainite,martensite[43]DP Fe–3.28Ni–0.12C Polygonal ferrite,martensite[23,24]Fe–0.09C Polygonal ferrite,martensite[25]SAE9254Fe–1.43Si–0.58Mn–0.56C–0.47Cr Ferrite in bainite,martensite[31] BS LC bainite–Polygonal ferrite,ferrite in bainite,martensite[20]TRIP Fe–1.5Mn–1.5Si–0.2C Polygonal ferrite,ferrite in bainite[32] (Sub)grain ECD DP–Polygonal ferrite,martensite[20]3rd near neighbour KAM TRIP Fe–1.5Al–1.5Mn–0.2C Polygonal ferrite,ferrite in bainite[41]2nd near neighbour KAM TRIP Fe–1.9Si–1.43Mn–0.21C Ferrite in bainite,martensite[43] Normalised EDS carbon counts TRIP Fe–1.5Al–1.5Mn–0.2C Polygonal ferrite,ferrite in bainite[44] Multi-peak modelling of the distribution of one parameterIQ/PQ/BC IF Fe–0.15Mn–0.002C Polygonal,non-polygonal,acicular and bainitic ferrite,martensite,carbon-rich micro-constituents [34–36]DP Fe–1.55Mn–1.09Al–0.15CHSLA Fe–1.3Mn–0.078CTRIP Fe–1.5Mn–1.5Si–0.2C–0.2Ni Proeutectoid ferrite,ferrite in bainite[37]Fe–23.94Mn–0.86Cr–0.51C–0.28Si–0.14NiPolygonal ferrite,ferrite in bainite,martensite[38]Thresholding the distributions of two parametersCI and IQ/PQ/BC or IQ/PQ/BC and(sub)grain sizeor BS and(sub)grain sizeDP–Polygonal ferrite,martensite[20]CI and IQ/PQ/BC–Fe–1.39Mn–0.69Cr–0.1Si–0.08C Polygonal ferrite,ferrite in bainite,martensite[33] Average(sub)grain IQ/PQ/BC and BS–Fe–2.2Mn–1.0Si–0.06C Polygonal ferrite,martensite[40] Multi-peak modelling of average(sub)grain IQ/PQ/BC and GAMTRIP Fe–1.8Mn–0.5Si–0.2C Polygonal ferrite,ferrite in bainite,martensite[40] Thresholding the distributions of multiple parametersAverage(sub)grain BS,GOS,(sub)grain aspect ratio and area –Fe–1.9Mn–0.2Si–0.2Cr–0.15C andFe–0.93Mn–0.7Cr–0.2Si–0.07CPolygonal ferrite,ferrite in bainite,martensite[45]–Boundary misorientation profiles,(sub)grain size, aspect ratio and average internal misorientation CASTRIP Nb-free,0.04Nb,and0.08Nb Polygonal,non-polygonal and acicular ferrite,ferrite inbainite[46]1Throughout the text,chemical compositions are in weight per cent unlessspecified otherwise.With the exception of C,elements o0.1wt%are not stated.A.A.Gazder et al./Ultramicroscopy147(2014)114–132115austempering process.The ferrite in bainite contained a higher density of geometrically necessary dislocations as a result of the local shear stress concentration induced by the volume expansion during transformation.In the same study,the martensite formed during tensile loading up to3%engineering strain was manually identified using the BC maps.However,the polygonal ferrite,the ferrite in bainite and the martensite fractions were not individu-ally segmented.It is more often the case that the IQ/PQ/BC or BS return asymmetric distributions with a single peak;following which the phase/ferrite morphology segmentation becomes significantly more difficult.In this situation,Waterschoot et al.[33]used a combination of CI and IQ/PQ/BC to qualitatively distinguish between polygonal ferrite,the ferrite in bainite and martensite in Fe–1.39Mn–0.69Cr–0.1Si–0.08C steel.Here structures with the highest CI and IQ/PQ/BC values were considered polygonal ferrite whereas structures with intermediate CI and IQ/PQ/BC values were ferrite in bainite and the ones with the lowest CI and IQ/ PQ/BC values were denoted as martensite.The classification was based on the polygonal ferrite grains having the lowest dislocation density,the ferrite in the bainite containing a higher dislocation density as a result of their isothermal transformation from austenite and the martensite grains possessing the highest defect density due to the strain associated with their transformation.The martensite grains also recorded the lowest CI(or largest PM)as the nominal bct crystal2deviates slightly from a perfect bcc crystal [33].In order to overcome issues related to segmentation in asym-metric distributions with a single peak,Wu et al.[34–36]sug-gested a mathematical multi-peak model.Here the IQ/PQ/BC values werefirst normalised following which the distribution was deconvoluted into multiple,symmetric Gaussian sub-distributions.The number of sub-distributions was the same as the number of phases/ferrite morphologies present such that the sum of their peaks was equal to that of the original single asymmetric peak.The model successfully distinguished between polygonal,non-polygonal,acicular and bainitic ferrite,martensite and carbon-rich micro-constituents in IF,dual phase and high-strength-low-alloy steels;with the separate phases/ferrite morphologies verified by micro and nano-hardness measurements [34,35].Thereafter,Petrov et al.[37]used the multi-peak model to distinguish ferrite in bainite from proeutectoid ferrite in Fe–1.5Mn–1.5Si–0.2C–0.2Ni TRIP steel.This study confirmed that the volume fractions from multi-peak modelling were similar to those obtained from the image processing of the optical micro-graphs after tint etching,conventional thresholding of the IQ/PQ/BC distribution and from magnetic saturation experiments.Mujica et al.[38]made use of the multi-peak model assumption that the IQ/PQ/BC distribution was a superposition of sub-distributions belonging to the various constituent phases/ferrite morphologies to manually threshold and segment the polygonal ferrite,the ferrite in bainite and martensite in Fe–23.94Mn–0.86Cr–0.51C–0.28Si–0.14Ni TRIP steel.Verification of the segmentation was undertaken semi-quantitatively by comparing the boundary misorientation distributions of the individual phases/constituents.Ryde[20]reviewed the segmentation procedures used by various research laboratories via a blind round-robin test on a standard set of low carbon bainitic and dual phase steels.Poly-gonal ferrite,the ferrite in bainite and martensite were segmented in the low carbon bainitic steel by thresholding their BS values; with polygonal ferrite having the largest average values whereas the ferrite in bainite and the martensite had intermediate and the lowest BS values,respectively.On the other hand,martensite was distinguished from polygonal ferrite in a dual phase steel[20]on the basis of:(i)its grain size,such that martensitic substructures had o2m m equivalent circle diameter(ECD)and a majority of o151or4501boundary misorientation angles due to their fast transformation rate,or(ii)a combination of IQ/PQ/BC and(sub) grain size thresholding for critical(sub)grain boundary misorien-tations of1.51and51,respectively,or(iii)a combination of IQ/PQ/ BC and CI thresholding as per Ref.[33],or(iv)a combination of BS and(sub)grain size.In that study,it was noted that method (i)would only work when a clear(sub)grain size difference exists between martensite and polygonal ferrite and that method(iv) was disadvantaged by the need to have successfully indexed pixels;which is not always the case for poorly indexing phases like martensite.Another issue with the IQ/PQ/BC and BS parameters is that the pixels at grain boundary interfaces nominally present with smaller values as a result of the combined EBSP from a diffracting volume that contains contributions from neighbouring but differently oriented substructures[39].In order to reduce grain boundary effects,the IQ/PQ/BC and BS values of(sub)grains can be averaged such that variations within individual(sub)grains are lost but the ability to compare between(sub)grains is enhanced[34,39].Kang et al.[40]successfully used this strategy to segment martensite from polygonal ferrite in Fe–2.2Mn–1.0Si–0.06C dual phase steel. After imposing a51critical boundary misorientation criterion and averaging the pattern quality within each(sub)grain,an IQ/PQ/BC distribution containing two distinct peaks with minimal overlap was generated;following which the two phases were easily segmented.In order to overcome the above limitations associated with the IQ/PQ/BC or BS parameters,Zaefferer et al.[41]suggested using the third nearest neighbour kernel average misorientation(KAM3) and distinguished ferrite in bainite from polygonal ferrite in an intercritically annealed Fe–1.5Al–1.5Mn–0.2C TRIP steel.The KAM captures short range,in-grain orientation gradients and is calcu-lated as the average of the misorientation between the pixel at the centre of the kernel and the individual pixels at the perimeter of the kernel;all of which must belong to the same(sub)grain[42].In Ref.[41],the KAM threshold was determined mathematically as that value where the boundary interface between the polygonal ferrite and the ferrite in bainite was smooth and no scattered pixels belonging to either ferrite morphology appeared within the individual fractions/subsets.Substructures with KAM values less than the threshold were designated as polygonal ferrite whereas those with KAM values greater than or equal to the threshold were quantified as ferrite in bainite.Man et al.[43]tracked the deformation in Fe–1.9Si–1.43Mn–0.21C TRIP steel subjected to ex-situ uniaxial tensile loading up to $23%engineering strain.In order to segment the martensite islands from the“grainy”polygonal ferrite and the ferrite in bainite,the efficacies of the IQ/PQ/BC thresholding[34,35,37] and the second-nearest neighbour KAM schemes were evaluated. With increasing strain,IQ/PQ/BC thresholding resulted in errors caused by surface relief effects whereas the initially bimodal-like KAM distribution of the bcc phases/ferrite morphologies evolved into a broad single peak distribution.As a consequence,the authors concluded that the second-nearest neighbour KAM scheme was only applicable to undeformed or slightly deformed TRIP steel microstructures.2In bcc crystals,the lattice parameters are equal such that a¼b¼c.For bct crystals,the lattice parameters are a¼b a c.In modern EBSD acquisition systems, accurate distinction between bcc ferrite and bct martensite is only possible when there is a Z10%difference in the“c”lattice parameter value.3In order to calculate KAM,the misorientation between the centre pixel and its surrounding neighbours has to be lower than the user-defined critical(sub)grain boundary angle.Note here that the size of a kernel is defined by its n th nearest neighbour.A.A.Gazder et al./Ultramicroscopy147(2014)114–132 116Zaefferer et al.[44]also took advantage of the developments in detector hardware/software integration to obtain EBSD and energy dispersive X-ray spectroscopy(EDS)information simultaneously during the mapping of Fe–1.5Al–1.5Mn–0.2C TRIP steel.Since the EDS information was obtained concurrently as the electron beam rastered over the sample area during EBSD mapping,the variation in the relative elemental counts between pixels was attributed to differences in chemistry.Consequently,the relative carbon counts at every pixel were normalised to the total(nominal)carbon content of the TRIP steel in order to enhance the differences in the carbon distribution between austenite,polygonal ferrite and the ferrite in bainite.The experience gained from single or two step segmentation methodologies over the past decade has led to the realisation that accurate and reliable phase/ferrite morphology segmentation in TRIP steels is only possible when multi-condition schemes are applied.In this regard,one of thefirst such studies was by Kang et al.[40]on Fe–1.8Mn–0.5Si–0.2C TRIP steel.Since the raw IQ/PQ/ BC distribution was asymmetric and comprised a single peak, (sub)grain pattern quality averaging was unable to segment the various phases/ferrite morphologies.Consequently,a combination of(sub)grain pattern quality averaging,Multi-peak modelling and grain average misorientation(GAM4)was used to distinguish martensite and the ferrite in bainite from polygonal ferrite.Here the GAM denotes short range in-(sub)grain orientation variations and is defined as the mean misorientation between adjacent in-grain pixel pairs.More recently,Zhu et al.[45]developed a multi-condition segmentation procedure for intercritically annealed Fe–1.9Mn–0.2Si–0.2Cr–0.15C and thermo-mechanically processed Fe–0.93Mn–0.7Cr–0.2Si–0.07C steels.After imposing a21critical boundary misorientation criterion,a combination of EBSP quality metrics, internal misorientation and morphological criteria were used to segment the equiaxed polygonal ferrite,the ferrite in bainite and martensite in the two steels.First,the(sub)grain band slope average was applied to roughly segment the martensite from the ferrite in bainite and the polygonal ferrite.Thereafter,the ferrite in bainite was segmented from the polygonal ferrite using the grain orienta-tion spread(GOS5)parameter by thresholding such that substruc-tures with GOS o1.51were classified as polygonal ferrite whereas those with GOS Z1.51were ferrite in bainite.From the polygonal ferrite fraction(i)the residual ferrite in bainite was removed using a(sub)grain aspect ratio(42.5)threshold,and(ii)the residual tempered martensite was removed using a(sub)grain area (o0.5m m2)threshold.The latest development in automated identification used a combination of EBSD and Matlab to quantify the area fractions of polygonal ferrite,ferrite in bainite and acicular ferrite in CASTRIP s steel[46].The study made use of boundary misorientation profiles and(sub)grain size,aspect ratio and average internal misorienta-tion to return an area fraction of the various ferrite morphologies. While this technique provides distinct advantages over earlier manual point counting methods,the results cannot be correlated back to substructures in the EBSD map as it does not inherently identify a(sub)grain(or pixel grouping)as belonging to any particular phase/ferrite morphology.With the above outlook in mind,the present study is thefirst to develop a multi-condition segmentation methodology that distin-guishes austenite,martensite,polygonal ferrite and the ferrite in bainite in a reproducible manner for a thermo-mechanically processed low-Si,high-Al TRIP steel.As opposed to short-range in-grain orientation variations like KAM and GAM which return localised misorientation gradients within single(sub)grains and are sensitive to the map step size,this study implements the long-range GOS criterion to perform the initial segmentation.It will be shown that this criterion provides for more effective segmentation between various substructure types as it assigns a single value to all pixels within a particular(sub)grain.This is also one of thefirst studies to utilise the concurrently acquired EBSD and EDS infor-mation to successfully distinguish the ferrite in granular bainite from the bainitic ferrite laths.While the method described in the following paragraphs should not be automated(as due care and attention to phase/ferrite morphology detail needs to be taken for each map),the novel procedures/tools developed here can be readily applied to study the microstructural variations in a wide variety of engineering alloys.2.Experimental and analytical procedureAn Fe–0.15C–2.00Mn–0.30Si–1.00Al–0.05P wt%TRIP steel was received as a6mm thick hot rolled plate from GIFT-POSTECH.The plate was electro-discharge machined into an8(RD)Â20(TD)Â6 (ND)mm3sample and processed on a Gleeble3500thermo-mechanical simulator operating in hydra-wedge mode as follows [47].The sample was heated at2K sÀ1to1523K,held for120s followed by cooling at1K sÀ1to1373K where a25%roughing reduction was applied.The sample was then held for120s in order to condition the recrystallised austenite and then cooled down to thefinish rolling temperature in the non-recrystallised austenite region of1123K.Following a second47%finishing reduction,the sample was slow cooled at1K sÀ1to the accelerated cooling start temperature of953K to form$50%polygonal ferrite.At953K, the cooling rate was increased to20K sÀ1to avoid pearlite formation.Finally,coiling was simulated by holding the sample at743K for1200s to form bainite and then water quenched.The sample was again electro-discharge machined from the centre of its width along the normal direction–rolling direction (ND–RD)and mechanicallyfine ground using15and6m m dia-mond stages.Thereafter,a0.5cm2area of the sample was electropolished on a Struers Lectropol-5using an electrolyte of 330ml methanolþ330ml butoxyethanolþ40ml perchloric acid at50V,$0.95–1.2mA,171C for90s.EBSD and EDS information was obtained simultaneously from a 96.425Â47.5m m2area located at the centre of the ND–RD cross-section using a JEOL JSM-7001Ffield emission gun–scanning electron microscope operating at15kV accelerating voltage and $5.1nA probe current.The microscope wasfitted with a Nordlys-II EBSD detector and an80mm2X-Max EDS detector which interface with the Oxford Instruments AZtec software suite.The EBSD mapping conditions were optimised beforehand with43and 32reflectors employed for the bcc and fcc phases,respectively, 4Â4binning,3background frames,a Hough resolution of60and concurrently indexing individual Kikuchi patterns up to8bands with an Advanced Fit Index(AFI)value of3.The raw EBSD map returned an overall indexing rate of87.16%such that most of the zero solutions were concentrated at boundary interfaces.The employed map step size of0.095μm was equivalent to an EDS map resolution of$1024Â1024pixels.Other EDS–based settings included a20keV energy range,auto-selecting the num-ber of channels,a process time of3and a detector dead time of $45–50%.The carbon K output counts over the full‘TruMap’area without binning returned a single peak Gaussian distribution (relative frequency versus cps)with the highest and maximum4The GAM is calculated for contiguous structures bounded by misorientationsthat are lower than the user-defined critical(sub)grain boundary angle.5The GOS is defined as the mean misorientation deviation between theaverage(sub)grain orientation and each pixel within the(sub)grain.It is calculatedfor contiguous structures bounded by misorientations that are lower than the user-defined critical(sub)grain boundary angle.A.A.Gazder et al./Ultramicroscopy147(2014)114–132117count rates of $1350cps and $3400cps,respectively.When these values were multiplied with the mean dwell time of 0.074s per pixel,$100and $250counts were returned,respectively.While segmentation using EBSD-based parameters was under-taken within the Oxford Instruments (OI)Channel-5software suite,the EDS data was exported to Gatan DigitalMicrograph for thresholding via its associated freeware scripts for X-ray map analysis [48]and then imported back into OI Channel-5for further analysis.Since this paper focuses on the development of an EBSD-EDS-based segmentation procedure,transmission electron microscopy (TEM)was employed in a very limited capacity to con firm the site-speci fic segmentation shown in Section 3.In order to provide supporting correlative evidence for the variation in the ferrite morphologies,a focused ion beam (FIB)section was cut along the red line shown in Fig.1a and Fig.1a(inset)using an xT Nova NanoLab 200Dualbeam located at the University of New South Wales.The FIB section was examined on a JEOL ARM-200F (scanning)transmission electron microscope operating at 200kV.The TEM work was restricted to bright-field imaging.Other techniques such as X-ray microanalysis (EDS)and electron energy loss (EELS)were unsuccess-ful in measuring composition differences between the various ferrite morphologies;the former due to its low sensitivity and latter due to the excessive thickness (i.e.–greater than 2mean free paths)of the FIB section.It is emphasised that no attempt was made to obtain any TEM-based statistical information;as the latter is beyond the scope of the present study.3.EBSD and EDS-based phase and ferrite morphology segmentationAs shown in the secondary electron image,band contrast,band slope and phase maps (Fig.1a –d),the microstructure of thermo-mechanically processed TRIP steel consists of bands oflarge ferrite grains interspersed between layers comprising bainite and austenite/martensite constituent.The banded appearance is the result of the final deformation in the non-recrystallisation region (47%finishing reduction at 1123K)which lead to the pancaking of the austenite grains.The EBSD map was initially post-processed as per Refs.[49–53]by eliminating any potential wild orientation spikes and filling in zero solutions via cyclic extrapolation from 8to 6neighbours.Throughout the text,low-angle boundaries (LAGBs)are de fined as misorientations between 21r θo 151whereas high-angle bound-aries (HAGBs)extend from θZ 151.Subgrain/grain reconstruction was undertaken using 21as the minimum misorientation in order to fix the angular resolution limit and retain orientation contrast information.A minimum spatial resolution of 3times the nominal step size was also maintained constant.The first step consisted of separating out the fcc austenite and isolating all pixels belonging to bcc ferrite (blue pixels in Fig.1d).Consequently,the following segmentation steps were undertaken only on the subset that was originally discriminated as bcc ferrite.It should be noted that irrespective of the type of morpholo-gical ((sub)grain size or aspect ratio)or internal misorientation criteria used in the following paragraphs,the segmentation of the bcc ferrite fraction was accomplished by thresholding the normalised cumulative distribution of that criterion via an opti-mised cut-off value.Unlike other studies that use a fixed cut-off value,we applied a constant rule that computed the optimal cut-off value in order to guarantee reproducibility across different maps.Consequently,our threshold/cut-off value was de fined as that number at which the slope (m ,cf.Figs.2a and 3a insets)of the normalised cumulative distribution with respect to the origin tends to 1([50]and the references therein).In doing so,the variations in the morphological or internal misorientation criteria caused by alloy chemistry and/or thermo-mechanical processing history can be inherently accounted for when dealing with multi-plesamples.Fig.1.(a)Secondary electron image with a 501tilted inset demarcating the location of the FIB slice and EBSD maps of the (b)band contrast,(c)band slope,and (d)phase distribution (red ¼fcc austenite,blue ¼bcc ferrite).In (d)white ¼LAGBs and black ¼HAGBs.(For interpretation of the references to colour in this figure legend,the reader is referred to the web version of this article.)A.A.Gazder et al./Ultramicroscopy 147(2014)114–132118。

专利名称：Elemental concentration determinationusing neutron-induced activation gammaradiation发明人：Feyzi Inanc,Rafay Zahid Ansari,W. AllenGilchrist,David M. Chace申请号：US13223522申请日：20110901公开号：US09261622B2公开日：20160216专利内容由知识产权出版社提供专利附图：摘要：The present disclosure relates to borehole logging methods and apparatusesfor estimating formation properties using nuclear radiation, particularly an apparatus and method for estimating amounts of silicon and/or oxygen in the formation using exposure time information. The method may include using nuclear radiation information from at least one nuclear radiation detector to estimate at least one parameter of interest. The method may also include reducing an error in the estimated formation properties due to speed variations of a nuclear radiation source that activates the silicon and oxygen in the formation. The apparatus may include at least one nuclear radiation detector. The apparatuses may include an information processing device to perform the methods.申请人：Feyzi Inanc,Rafay Zahid Ansari,W. Allen Gilchrist,David M. Chace地址：Spring TX US,Spring TX US,Fort Davis TX US,Houston TX US国籍：US,US,US,US代理机构：Mossman Kumar & Tyler PC更多信息请下载全文后查看。

专利名称：FASTENING MEANS AND METHOD FOR FASTENING AN INSULATING-MATERIALPANEL, AND CORRESPONDINGARRANGEMENT发明人：KRALER, HANS-CHRISTIAN,KRALER, Hans-Christian,HORSMANN, KARL-HEINZ,HORSMANN, Karl-Heinz申请号：EP2014/059479申请日：20140508公开号：WO2014/184092A1公开日：20141120专利内容由知识产权出版社提供专利附图：摘要：The invention relates to a fastening means for fastening an insulating-material panel (26) on a substructure (22), wherein the fastening means (10) has a pressure-exerting disc (12) and an elongate fastening element (16) projecting transversely therefrom. A heat-insulating material (14) is arranged in the manner of a heat-insulating disc on an upper side of the pressure-exerting disc, and is advantageously fastened in a non-releasable manner thereon or produced in one piece therewith. The invention also relates to an arrangement having a substructure and an insulating-material panel, and to a method for fastening an insulating-material panel on a substructure.申请人：E.G.O. ELEKTRO-GERÄTEBAU GMBH,E.G.O. ELEKTRO-GERÄTEBAU GMBH地址：Rote-Tor-Straße 14 75038 Oberderdingen DE国籍：DE代理人：PATENTANWÄLTE RUFF, WILHELM, BEIER, DAUSTER & PARTNER更多信息请下载全文后查看。