陈胜利，赵相东，孙 伟，陈 胜，朱秀芹

（中国石油大学(北京) 化学工程与环境学院，北京 102249；北京纳微标物科技有限公司，北京 102200）

DOI:10.13732/j.issn.1008-5548.2022.02.008

收稿日期： 2021-08-24，修回日期：2021-10-04，在线出版时间：2022-02-08。

基金项目：国家自然科学基金项目，编号：91534120。

第一作者简介：陈胜利(1962—)，男，博士，教授，博士生导师，研究方向为新材料、催化剂及催化反应工程、烃加工、标准化等。E-mail:shenglichen62@163.com;slchen@cup.edu.cn。

摘要： 利用种子聚合法和种子生长法分别合成4种单分散聚苯乙烯微球和1种二氧化硅微球;利用密排阵列-光学显微镜法和扫描电子显微镜法对5种微球的粒径进行定值测量;光学显微镜和扫描电子显微镜的放大倍数分别利用溯源到He-Ne激光波长的测微尺和扫描电子显微镜校准光栅校准。结果表明：4种聚苯乙烯微球粒度标准物质的平均粒径分别为(15.37±0.07)、(28.95±0.12)、(66.49±0.15)、(116.4±0.3)μm，二氧化硅微球的粒径为(9.97±0.05)μm；样品均匀、稳定，定值结果可靠。

关键词： 粒度；标准物质；聚苯乙烯微球；二氧化硅微球；阵列测量

Abstract:Four kinds of samples of monodisperse polystyrene (PS)microspheres and one kind of sample of monodisphere silica microspheres used for microsize standards were synthesized through seeded growth method.Particle sizes of the five kinds of microspheres were determined by using arraysizing-optical microscopy method and SEM method.The magnification of the optical microscopy and SEM were calibrated with the NIST stage micrometer of SRM2800 and a SEM pitch calibration standard，respectively.The certified values of these calibration standards were traced to He-Ne laser wavelength.The results show that the average particle sizes of the four kinds of PS microspheres are (15.37±0.07),(28.95±0.12),(66.49±0.15),(116.4±0.3)μm，respectively.The average size of silica microspheres is (9.97±0.05)μm.The samples are uniform and stable,and the detemination results are reliable.

Keywords:particle size;reference material;polystyrene microsphere;silica microsphere;array sizing

参考文献（References）：

[1]HARTMANA W,DOIRONT D,FU J.Certificate of NIST SRM 1962:3 μm diameter polystyrene spheres[J].Journal of Research of the National Institute of Atandards and Technology,1992,97(2):253-265.

[2]LETTIERITR,HARTMAN A W,HEMBREEGC，et al.Certification of SRM 1960:nominal 10 μm diameter polystyrene spheres (‘space beads’)[J].Journal of Research of the National Institute of Atandards and Technology,1991,96(6):669-691.

[3]RASBERRYS D.Certificate of standard reference material：1961[EB/OL].[2021-08-01].Office of Standard Reference Materials,National Institute of Standard and Technology.USA.https://www-s.nist.gov/srmors/certificates/1961.pdf.

[4]THOM R，MARCHANDISE H,COLINET E.The certification of monodisperse latex spheres in aqueous suspensions with nominal diameter 2.0 μm，4.8 μm and 9.6 μm1[EB/OL].[2021-08-01].BCR information,Commission of the European Communities (Bureau of Community Reference)Report EUR-9662-EN，Brussels，Belgiμm，1985.https://crm.jrc.ec.europa.eu/p/q/166/BCR-166-LATEX-SPHERES-particle-diameter-4-8-microns/BCR-166.

[5]国家市场监督管理总局.关于批准“炭钢成份分析标准物质”等214种国家一级和二级标准物质的通知：国质检量函〔2007〕478号[A/OL].(2007-06-22)[2021-08-01].http://www.samr.gov.cn/jls/djcx/200707/t20070719_302819.html.

[6]国家质量监督检验检疫总局.关于批准“二氧化硅粒度标准物质”等五种国家一级标准物质的通知:国质检量函〔2008〕570号[A].2008-08-06.

[7]国家市场监督管理总局.关于批准“纳米级氧化铝比表面”等121种国家标准物质的通知：国质检量函〔2009〕259号[A/ON].(2009-5-13).http://www.samr.gov.cn/jls/djcx/201003/t20100317_302823.html.

[8]陈胜利,董鹏,袁桂梅，等.亚微米/纳米级聚苯乙烯微球粒度标准物质的研制[J].武汉理工大学学报,2007,29(10):96-100.

[9]KIM J W,SUH K D.Monodisperse polymer particles synthesized by seeded polymerization techniques[J].Journal of Industrial and Engineering Chemistry,2008,14:1-9.

[10]UGELSTADJ,MORK P C.Swelling of oligomer-polymer particles:new methods of preparation of emulsion and polymer dispersions[J].Advances in Colloid and Interface Science,1980,13:101-140.

[11]董鹏.由硅溶胶生长单分散颗粒的研究[J].物理化学学报,1998,14(2):109-114.

[12]CHEN S L,DONG P,YANG G,et al.The size dependence of growth rate of monodisperse silica particles from tetraalkoxy-silane[J].Journal of Colloid Interface Science,1997,189:268-272.

[13]CHEN S L,DONG P,YANG G,et al.Characteristic aspects of formation of new particles during the growth of monosize silica seeds[J].Journal of Colloid Interface Science,1996,180:237-241.

[14]CHEN S L,DONG P,YANG G,et al.Kinetics of formation of monodisperse colloidal silica particles through the hydrolysis and condensation of tetraethylorthosilicate[J].Industrial &Engineering Chemistry ResearchInd,1996,35:4487-4493.

[15]HARTMAN A W.Investigations in array sizing:part I:accuracy of the sizing process[J].Powder Technology,1984，39(1)：49-59.

[16]全浩，韩永志.标准物质及其应用技术[M].2版.北京：中国标准出版社，2003:69.

[17]全国标准物质管理委员会.中华人民共和国标准物质目录：上册[M].北京：中国质检出版社，2017：300-321.

[18]KUBITSCHEK H E.Optical calibration of some monodisperse polystyrene latexes in arrays[J].Nature,1961,192:1148-1150.