Article(id=1320099050083431410, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320099031116792469, articleNumber=null, orderNo=null, doi=10.14062/j.issn.0454-5648.20240292, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1713715200000, receivedDateStr=2024-04-22, revisedDate=1715443200000, revisedDateStr=2024-05-12, acceptedDate=null, acceptedDateStr=null, onlineDate=1792665739793, onlineDateStr=2026-10-22, pubDate=1734624000000, pubDateStr=2024-12-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1792665739793, onlineIssueDateStr=2026-10-22, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1792665739793, creator=13701087609, updateTime=1792665739793, updator=13701087609, issue=Issue{id=1320099031116792469, tenantId=1146029695717560320, journalId=1263187385517883426, year='2024', volume='52', issue='12', pageStart='3663', pageEnd='3904', issueExtLink='null', onlineDate='null', pubDate='1734624000000', pubDateStr='2024-12-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1792665735272, creator='13701087609', updateTime=1792666214857, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1320101042704994698, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320099031116792469, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1320101042704994699, tenantId=1146029695717560320, journalId=1263187385517883426, issueId=1320099031116792469, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=3695, endPage=3702, ext={EN=ArticleExt(id=1320099050699994099, articleId=1320099050083431410, tenantId=1146029695717560320, journalId=1263187385517883426, language=EN, title=Preparation and Properties of Silica Nanotube Aerogels, columnId=1319726165087077079, journalTitle=Journal of the Chinese Ceramic Society, columnName=Research Article, runingTitle=null, highlight=null, articleAbstract=
Introduction Silica aerogels are highly porous materials with interconnected three-dimensional networks of silica particles, which are typically obtained via removing the liquid in gels under supercritical conditions. Silica aerogels are widely applied in the fields of thermal insulation, adsorption, catalysis, and energy storage due to their ultralow density, large surface area, and unique nanoporous structure. However, silica aerogels are fragile at relatively low stresses due to the existence of rigid skeleton consisting of weak linking of silica particles. The inherent brittleness and poor reliability restrict the application of aerogel materials to a certain extent. In this paper, the preparation and properties of SiO2 nanotube aerogels (SiO2-NTA) with a three-dimensional nanotubular network structure were investigated.
Methods For the prepatation of carbon aerogels (CA) as sacrificial templates, 3.24 g of resorcinol and 4.4 mL of formaldehyde solution were dissolved in 95.5 mL of deionized water. The solution was stirred for 1 h, and 3.9 mg of sodium carbonate was added. After further stirring for 30 min, the precursor solution was poured into a container, sealed and cured in an oven at 85 ℃ for 72 h to obtain a resorcinol-formaldehyde wet gel. The gel was washed with ethanol for several times to completely remove the residual solvents. The wet gel was dried using supercritical carbon dioxide to obtain the resorcinol-formaldehyde aerogel, which was subsequently placed in a tubular furnace and carbonized in a nitrogen atmosphere to obtain the CA templates.
SiO2-NTA were prepared via chemical vapor deposition (CVD) with argon as carrier gas, tetraethoxysilane and aqueous ammonia solution as silicon and oxygen sources, respectively. Firstly, tetraethoxysilane source tank was heated to 60 ℃. Then, CA templates were placed in CVD chamber, and was heated to different deposition temperatures (i.e., 100, 150, 200, 250 ℃ and 300 ℃), respectively. C/SiO2 composite aerogels (CA@SiO2) were prepared via introducing tetraethoxysilane (5 mL/min) and aqueous ammonia (15 mL/min) into the chamber, and depositing for 20 h at a target pressure. Finally, CA@SiO2 was calcined in air at 500 ℃, and SiO2-NTA was obtained after removing the templates.
The microstructural features and pore morphology of aerogels were determined by a model SEM4000Pro scanning electron microscope (SEM) and a model TH-F120 transmission electron microscope (TEM). The specific surface area and total pore volume were measured based on Nitrogen adsorption-desorption isotherms in a model V-Sorb X800 N2 adsorption analyzer. The compressive strength and Young's modulus of SiO2-NTA specimens were measured by a model UTM-4103 electronic universal testing machine at a crosshead speed of 0.5 mm/min.
Results and discussion SiO2-NTA prepared by CVD method has a three-dimensional nanotubular network structure. The inner part of the skeleton is hollow, and the average thickness of tube wall ranges from 3 nm to 7 nm. The deposition temperature and pressure have a significant influence on the microstructure as well as density of SiO2-NTA. The deposition rate and weight gain of aerogels increase gradually, and accompany the skeleton coarsening process as the deposition temperature increases from 100 ℃ to 250 ℃, which inhibits the shrinkage of the SiO2-NTA after calcination. Silica preferentially deposits on the outside of the template as the deposition temperature further increases to 300 ℃, resulting in the blocking of SiO2-NTA surface. The density of SiO2-NTA firstly decreases and then increases as the temperature increases, which is strongly dependent on both weight gain and linear shrinkage. Similarly, SiO2-NTA density ranges from 65 mg/cm3 to 51 mg/cm3 with the increase of pressure. The preparation of SiO2-NTA based on CVD method is essentially a reaction transport process of multi-component fluids in a porous template. It is thus necessary to balance the mass transfer rate and reaction rate to obtain SiO2-NTA with a homogeneous microstructure.
Compared with CA, the specific surface area and total pore volume of CA@SiO2 decrease significantly because of the preferential deposition of silica at defects and junctions of framework. After calcination in air, the feature mesopore is formed via removal of the carbon skeleton, and the specific surface area and total pore volume of SiO2-NTA can reach 592.717 m2/g and 1.047 cm3/g, respectively. The high pore volume and nanotubular skeletons lead to the low density of SiO2-NTA. SiO2-NTA shows relatively excellent mechanical properties. The elastic modulus and the stress at 60% strain of nanotube aerogels are 0.70 MPa and 0.83 MPa, respectively, and the specimens have no obvious fatigue damage after 100 cycles of compression, further indicating that SiO2-NTA has an outstanding structural reliability in a certain range of strain. In addition, SiO2-NTA also exhibits an excellent machinability while keeping a low density, compared with conventional silica aerogels, and a thin-walled aerogel specimen with a wall thickness of 200 μm can be obtained via processing.
Conclusions SiO2-NTA with a three-dimensional nanotubular network structure could be prepared via CVD of silica coating on the skeleton of CA sacrificial templates. The deposition temperature and pressure had a significant influence on the microstructure as well as density of SiO2-NTA. Within a certain range, the density of SiO2-NTA reduced as the deposition temperatures and pressure increased because of the decrease of linear shrinkage after calcination. However, as the temperature further increased, silica preferentially deposited on the outside of the template, resulting in the blocking of SiO2-NTA surface. The preparation of SiO2-NTA based on CVD method was essentially a reaction transport process of multi-component fluids in porous template. It is necessary to balance the mass transfer rate and reaction rate to obtain SiO2-NTA with a homogeneous microstructure. The specific surface area and total pore volume of SiO2-NTA could reach 592.717 m2/g and 1.047 cm3/g, respectively. The high pore volume and nanotubular skeletons led to the low density of SiO2-NTA. SiO2-NTA had relatively excellent mechanical properties. The elastic modulus and the stress at 60% strain of nanotube aerogels were 0.70 MPa and 0.83 MPa, respectively, and the specimen could be significantly compressed without obvious brittle fracture. Moreover, SiO2-NTA had a superior machinability due to its outstanding structural reliability, which could be processed by turning, milling and laser.
, authors=Ning LI, Ruiwen NIU, Zhibing HE, Taimin YI, Jing LI, Shuai ZHANG, Mengsheng YANG, Yunjian CHEN, Bo KE, authorsList=Ning LI, Ruiwen NIU, Zhibing HE, Taimin YI, Jing LI, Shuai ZHANG, Mengsheng YANG, Yunjian CHEN, Bo KE, authorCompany=null, correspAuthors=Jing LI, authorNote=
LI Ning (1986-), male, Ph.D., Associate Professor. E-mail: lncaep@163.com
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2纳米管气凝胶的制备工艺及性能, columnId=1263922770220560512, journalTitle=硅酸盐学报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=
SiO2气凝胶在隔热、吸附、催化等领域有着广泛应用，为进一步改善其力学性能、加工性能，本工作以碳气凝胶为模板，正硅酸乙酯为硅源、氨水为氧源，通过化学气相沉积方法制备得到具有三维纳米管多孔结构的SiO2纳米管气凝胶。研究反应温度、压力对材料微结构、密度的影响，制备获得组织均匀的SiO2纳米管气凝胶，需匹配反应物的传质速率和反应速率。制备的SiO2纳米管气凝胶具有优异的力学性能及突出的结构可靠性，材料弹性模量为0.70 MPa，60%应变时对应的材料应力为0.83 MPa，在压缩应变很大时没有发生脆性断裂。此外SiO2纳米管气凝胶可采用车削、铣削、激光加工等多种手段加工成型，表现出了优异的加工性能。
, authors=李宁, 牛瑞文, 何智兵, 易泰民, 李婧, 张帅, 杨蒙生, 陈云建, 柯博, authorsList=李宁, 牛瑞文, 何智兵, 易泰民, 李婧, 张帅, 杨蒙生, 陈云建, 柯博, authorCompany=null, correspAuthors=李婧, authorNote=
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李婧（1984—），女，博士，副研究员。
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李宁（1986—），男，博士，副研究员。
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