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1、<p> 畢業(yè)論文外文資料翻譯</p><p> 題 目 熱處理對三種不同途徑生產(chǎn)的 </p><p> 納米粉氧化鋯晶體結(jié)構(gòu)和形態(tài)的影響</p><p> 學(xué) 院 材料科學(xué)與工程 </p><p> 專 業(yè) 材料科學(xué)與工程 &l
2、t;/p><p> 班 級 </p><p> 學(xué) 生 </p><p> 學(xué) 號 </p><p> 指導(dǎo)教師
3、 </p><p> 二〇一三年三月二一日</p><p> j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 178–185</p><p> journal homepage: ww
4、w.elsevier.com/locate/jmatprotec</p><p> Effect of thermal treatment on the crystal</p><p> structure and morphology of zirconia</p><p> nanopowders produced by</p><p&
5、gt; three different routes</p><p> M.M. Rashad ? , H.M. Baioumy</p><p> Central Metallurgical Research and Development Institute, P.O. Box 87, Helwan, Cairo, Egypt</p><p><b&g
6、t; article</b></p><p> Article history:</p><p><b> info</b></p><p><b> abstract</b></p><p> Zirconia ZrO2 nanopowders have been succe
7、ssfully prepared via three processing routes,</p><p> namely, conventional precipitation (CP), citrate gel combustion (CGC) and microemulsion</p><p> re?ned precipitation (MRP). The formed zir
8、conia particles were characterized using X-ray</p><p> diffraction analysis (XRD), scanning electron microscope (SEM), Fourier transformer infrared</p><p> (FT-IR) spectroscopy and UV–visible
9、absorption spectrum. The results showed that the CP</p><p> route led to the formation of tetragonal ZrO2 phase with low crystallinity at 700 ? C and the</p><p> formed tetragonal phase was tr
10、ansformed to monoclinic ZrO2 phase at temperatures ranged</p><p> Received 24 May 2006</p><p> Received in revised form</p><p> 22 April 2007</p><p> Accepted 23 Ap
11、ril 2007</p><p><b> Keywords:</b></p><p><b> Zirconia</b></p><p><b> Synthesis</b></p><p> Crystal structure</p><p>
12、; Nanoparticles</p><p> Characterization</p><p> from 1000 to 1200 ? C. The CGC route led to formation of monoclinic phase without presence</p><p> tetragonal phase species in t
13、he temperatures range from 1000 to 1200 ? C. In contrast, MRP</p><p> technique led to the formation of tetragonal phase with high crystallinity compared with</p><p> the other processing at 7
14、00 ? C and the produced tetragonal phase was inverted to cubic</p><p> phase by increasing the calcination temperatures from 1000 to 1200 ? C. SEM showed that the</p><p> morphology of the pro
15、duced zirconia nanopowders changed according to synthesis routes</p><p> and thermally treated temperatures.</p><p> © 2007 Elsevier B.V. All rights reserved.</p><p><b>
16、; 1.</b></p><p> Introduction</p><p> Advanced ceramics known as ?ne ceramics are a diverse</p><p> group of inorganic oxides such as zirconia, alumina, tita-</p>&
17、lt;p> nia and non-oxides like silicon carbide, boron carbide and</p><p> silicon nitride. These materials are drawing attention as</p><p> high technology materials because of their superi
18、or mechan-</p><p> ical, thermal, electrical, chemical and optical properties.</p><p> Zirconia ?ne ceramics have an impressive combination</p><p> of properties such as high str
19、ength, hardness, toughness,</p><p> corrosion resistance, low co-ef?cient of friction and biocom-</p><p> patibility. Nearly 80% of produced zirconia in the world is</p><p> used
20、 in conventional applications such as refractories, pig-</p><p> ments, glazers, opaci?ers, abrasives, etc. The ever-increasing</p><p> numbers of ceramics applications have resulted in devel-
21、</p><p> oping of advanced technologies to process nanopowders</p><p> zirconia (Galgali et al., 1995). The advanced applications</p><p> of zirconia nanopowders are including tr
22、ansparent opti-</p><p> cal devices, electrochemical capacitor electrodes, oxygen</p><p> sensors, fuel cells and catalysts including photocatalysts</p><p> (Srdic and Omorjan, 2
23、001; Kongwudthiti et al., 2003). Zir-</p><p> conia catalyzes the hydrogenation of ole?ns, isomerization</p><p> of ole?ns and epoxides and the dehydrations of alco-</p><p> hols
24、. When zirconia is used as support, various reactions</p><p> Corresponding author. Tel.: +20 2 5010642/213; fax: +20 2 5010639.</p><p> E-mail address: rashad133@yahoo.com (M.M. Rashad).</
25、p><p> 0924-0136/$ – see front matter © 2007 Elsevier B.V. All rights reserved.</p><p> doi:10.1016/j.jmatprotec.2007.04.135</p><p><b> ?</b></p><p>
26、j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 178–185</p><p><b> 179</b></p><p> such as Fischer-Tropsch synthesis, methanol synthes
27、is and</p><p> hydrodesulfurization have been reported to proceed with</p><p> higher activity and selectivity than with conventional sup-</p><p> ports (Jung and Bell, 2000). It
28、 is well known that zirconia</p><p> is a low absorption materials usable for coating in the</p><p> near-UV (300 nm) or IR (~8 m) regions. Typical applica-</p><p> tions include
29、 near-UV laser and dielectric mirror designs.</p><p> In addition, about 95% of ferrule, the most important part</p><p> of the optical ?ber connector is now made from zirconia</p><
30、p> ?ne ceramics. It is known that high quality of the ceramic</p><p> is based on the excellent performance of zirconia powder</p><p><b> (5).</b></p><p> Prepari
31、ng a ?ne and an agglomerate free zirconia powder</p><p> is the ?rst and perhaps the most important step in obtaining</p><p> a sintered zirconia ceramic of desirable microstructure and</p&
32、gt;<p> therefore mechanical properties. Various chemistry-based</p><p> novel approaches have been taken for the preparation of zirco-</p><p> nia powders including co-precipitation,
33、hydrothermal, sol gel,</p><p> sonochemical method, microemulsion and thermal decom-</p><p> position processing (Ma et al., 2004; Wu et al., 2003; Lee et al.,</p><p> 1999; Tai
34、et al., 2001; Djuricic et al., 1995; Bourell and Kaysser,</p><p> 1993; Ward and Ko, 1993; Huang and Guo, 1992; Fang et al.,</p><p> 1997; Li et al., 1989; Juarez et al., 2000; Yashima et al.,
35、 1996;</p><p> Yashima et al., 1994; Caruso et al., 1997; Chatterjee et al., 1992;</p><p> Dodd and McCormick, 2002; Roy and Ghose, 2000; Kolen’ko et</p><p> al., 2003; Noh et al
36、., 2003; Somiya and Akiba, 1999; Piticescu et</p><p> al., 2001). The chemical precipitation (CP) method is a suitable</p><p> low cost technique for the mass production compared with</p>
37、;<p> the other mentioned technique. The main drawback is that</p><p> the particle size is not small and has in wide size distribution.</p><p> Microemulsion re?ned precipitation (MRP
38、) gives better chem-</p><p> ical homogeneity with controlling the particle size and size</p><p> distribution. Citrate gel combustion (CGC) technique is used</p><p> to obtain h
39、ighly uniform size and shape controlled nanopar-</p><p><b> ticles.</b></p><p> ZrO2 has three polymorphic phases; monoclinic (m), tetrag-</p><p> onal (t) and cubic
40、(c). Because of its phase transformation</p><p> from tetragonal to monoclinic around the temperatures range</p><p> from 1100 to 2370 ? C, it is a challenging study with potentially</p>
41、<p> practical applications to prepare stabilized tetragonal ZrO2</p><p> powders at low temperatures. Stabilization of t-ZrO2 phase</p><p> is usually achieved by adding oxides of ytt
42、rium, magnesium,</p><p> calcium, thorium, titanium, cerium and ytterbium (Piticescu</p><p> et al., 2001; Jiang et al., 2001; Lascalea et al., 2004; Teterycz et</p><p> al., 200
43、3; Panda et al., 2003; Zhang et al., 2004; Ai and Kang,</p><p> 2004; Bhattacharjee et al., 1991). According to the change in</p><p> thermal treatment, c-ZrO2 phase is stable at all temperatu
44、re</p><p> up to the melting point at 2680 ? C. m-ZrO2 phase is stable</p><p> below 1170 ? C and inverted to t-ZrO2 phase by increasing tem-</p><p> perature over 1200 ? C. t-Zr
45、O2 phase is stable between 1170</p><p> and 2370 ? C by adding stabilized oxides (Stefanc et al., 1999).</p><p> From our knowledge, little information in literature is found</p><p&
46、gt; about the change in the phase transformation and the mor-</p><p> phology of the formed ZrO2 nanopowders that are produced</p><p> by CP, CGC and MRP techniques. The present work aims at&
47、lt;/p><p> comparing the change in crystal structure, morphology, FT-IR</p><p> spectra and UV–visible absorption spectrum of the produced</p><p> ZrO2 nanopowders which are obtaine
48、d by these three process-</p><p> ing routes at different calcination temperatures from 120 to</p><p><b> 1200 ? C.</b></p><p><b> 2.</b></p><p
49、><b> 2.1.</b></p><p> Experimental</p><p> Materials and processing</p><p> The materials used in the present work were, zirconyl chlo-</p><p> ride
50、 ZrOCl2 ·8H2 O purchased from BDH Chemicals Ltd., Poole,</p><p> England, sodium hydroxide and citric acid purchased from El-</p><p> Nasr Pharmaceutical Chemical ADWIC, Egypt, n-pentanol
51、 and</p><p> Triton X-100 (Serva Electrophoresis GmbH, Germany).</p><p> To process ZrO2 powders by CP route, 10 g zirconium</p><p> oxychloride octahydrate was dissolved in 100
52、ml bidistilled</p><p> water using hot plate magnetic stirrer. The desired vol-</p><p> ume of 2 M NaOH was added into the solution until pH</p><p> 10. After 15 min, the produce
53、d precipitate was ?ltered off,</p><p> washed and dried at 120 ? C overnight. The dried ZrO2 ·nH2 O</p><p> calcined at different temperatures from 500 to 1200 ? C at a</p><p&g
54、t; rate of 10 ? C/min and kept at the respective temperature for</p><p><b> 1 h.</b></p><p> To process ZrO2 powders by CGC method, 10 g of zir-</p><p> conium oxych
55、loride octahydrate was dissolved in water. A</p><p> stoichiometric amount of citric acid was added to the aque-</p><p> ous solution. The mixture was evaporated to dryness at 60 ? C.</p>
56、;<p> Then, the produced precursor was dried to 120 ? C overnight.</p><p> The formed precursor was heated again to 500, 700, 1000 and</p><p> 1200 ? C at a rate of 10 ? C/min and kept
57、 at the respective tem-</p><p> perature for 1 h.</p><p> For the MRP method, the authors employed n-pentanol as</p><p> the oil phase and triton X-100 as the surfactant. One mol
58、ar of</p><p> Triton X-100 (non-anionic surfactant) was prepared by dissolv-</p><p> ing in n-pentanol and the processed solution was divided into</p><p> two parts, one part was
59、 added to 10 g zirconyl chloride octahy-</p><p> drate dissolved in small amount of water and the other part</p><p> was used for preparation of 2 M sodium hydroxide. Both two</p><p
60、> solutions were mixed together to precipitate zirconia hydrate</p><p> at pH 10. The precipitated solution was ?ltered, washed, dried</p><p> at 120 ? C, then calcined at different temper
61、atures from 500 to</p><p><b> 1200 ? C.</b></p><p><b> 2.2.</b></p><p> Characterization</p><p> The phase identi?cation and the crystallite
62、 size of the pro-</p><p> cessed ZrO2 nanopowders were characterized by Philips X-Ray</p><p> Diffractometer PW 1730 with nickel ?ltered Cu K radiation</p><p> ?( = 1.5406 A) at
63、40 kV and 30 mA. The crystallite sizes of ZrO2</p><p> nanopowders were determined for the most intense peak</p><p> (1 1 1) plane of ZrO2 crystals from the X-ray diffraction data</p>&
64、lt;p> using the Debye-Scherrer formula:</p><p><b> dRX =</b></p><p><b> k</b></p><p><b> cos Â</b></p><p><b> ˇ&l
65、t;/b></p><p><b> (1)</b></p><p> where dRX is the crystallite size, k = 0.9 is a correction factor</p><p> to account for particle shapes, ˇ the full width at half
66、 max-</p><p> imum (FWHM) of the most intense diffraction plane, the</p><p> ?wavelength of Cu target = 1.5406 A, and  is the Bragg angle.</p><p> The change in crystal mor
67、phologies of the ZrO2 particles</p><p> produced at heated temperature 700 and 1000 ? C for differ-</p><p> ent processing routes were examined by scanning electron</p><p> micro
68、scopy (JEOL-JSM 5410 SEM). Speci?c surface area (SBET ) of</p><p><b> 180</b></p><p> j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 )
69、178–185</p><p> samples was determined by BET surface area analyzer (Nova</p><p> 2000 series, Quantachrome Instruments, UK).</p><p> UV–visible absorption spectrums of the proce
70、ssed ZrO2</p><p> powders using three processing routes at calcination temper-</p><p> ature 1000 ? C were measured using CECIL CE 7200 UV double</p><p> beam spectrophotometer.&
71、lt;/p><p> Vibration spectrum of the crystalline ZrO2 powders at</p><p> calcination temperature 1000 ? C for the different processing</p><p> techniques in KBr were recorded on Fou
72、rier Transformer and</p><p> Pye-Unicam SP 300 instrument.</p><p><b> 3.</b></p><p> Results and discussion</p><p> The XRD patterns of the ZrO2 nanopow
73、ders products syn-</p><p> thesized by precipitation (CP), citrate gel combustion (CGC)</p><p> and microemulsion re?ned precipitation (MRP) techniques at</p><p> different therm
74、al treatment from 120 to 1200 ? C were shown</p><p> in Figs. 1–3. It is clear that the processed samples synthe-</p><p> sized at temperature 120 ? C were amorphous in the three</p>&l
75、t;p> processing techniques and it was also nearly amorphous for</p><p> the produced ZrO2 powders of the precursor sample pow-</p><p> der which treated at the temperature 500 ? C in case
76、of CP</p><p> method. XRD studies also showed that the transformation of</p><p> ZrO2 precursors to the crystalline tetragonal phase (JCPDS #49-</p><p> 1642) occurred as the cal
77、cination temperatures were increased</p><p> Fig. 2 – XRD patterns of the produced ZrO2 powders by CGC</p><p> method at 120, 500, 700, 1000 and at 1200 ? C for 1 and 3 h.</p><p>
78、 between 500 and 700 ? C for heating time 1 h. The crystallite</p><p> sizes of formed single-phase t-ZrO2 nanopowders as calcu-</p><p> lated from XRD analyses using Debye-Scherrer formula o
79、f</p><p> the most intense peaks (1 1 1) plane were in the range of</p><p> 32.90, 10.18 and 20.97 nm at 700 ? C for CP, CGC and MRP</p><p> methods, respectively. The presence o
80、f tetragonal phase in as-</p><p> prepared ZrO2 and the powder formed at low temperature is</p><p> attributed to the fact that the speci?c surface free enthalpy</p><p> of tetra
81、gonal ( = 0.77 J/m2 ) is smaller than that of mono-</p><p> clinic ( = 1.13 J/m2 ). The large surface area of as-synthesized</p><p> nanopowders becomes a thermodynamic barrier for t-ZrO2</
82、p><p> to m-ZrO2 phase transformation. Consequently, tetragonal</p><p> phase is remained. Liang et al. (Liang et al., 2003) explained the</p><p> formation of tetragonal phase at l
83、ow temperature is attributed</p><p> to that the structure of zirconia precursor is regarded as</p><p> hydrous zirconia (ZrO2 ·nH2 O) and the schematic structure unit</p><p>
84、; has 16 zirconium atoms, 20 non-bridging hydroxogroups, 22</p><p> bridging oxide bond and 20 coordinated water and based on</p><p> this model, the following equations is obtained by increa
85、sed</p><p> the temperature up to 700 ? C:</p><p> [Zr16 O22 (OH)20 (H2 O)20 ] · xH2 O</p><p> Naturally dried</p><p><b> ?→</b></p><p&g
86、t; [Zr16 O22 (OH)20 (H2 O)20 ] + xH2 O</p><p><b> (2)</b></p><p> Fig. 1 – XRD patterns of the produced ZrO2 powders by CP</p><p> method at 120, 500, 700, 1000 and
87、at 1200 ? C for 1 and 3 h.</p><p> [Zr16 O22 (OH)20 (H2 O)20 ]?→16ZrO2 + 30H2 O</p><p><b> heat</b></p><p><b> (3)</b></p><p> j o u r n a l
88、 o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 1 9 5 ( 2 0 0 8 ) 178–185</p><p><b> 181</b></p><p> Fig. 3 – XRD patterns of the produced ZrO2 powders by MRP</p&
89、gt;<p> method at 120, 500, 700, 1000 and at 1200 ? C for 1 and 3 h.</p><p> When ZrO2 ·nH2 O is heated up to about 300 ? C, the</p><p> metastable tetragonal zirconia is observed
90、 compared to its</p><p> stable temperature around 1100–2370 ? C. The amorphous to</p><p> tetragonal phase transformation is attributed to the loss of</p><p> water from the amo
91、rphous hydrous zirconia resulting from</p><p> the release of water of hydration and the production of water</p><p> via oblation. Both processes lead to a reduction in the BET sur-</p>
92、<p> face area of the calcined solid and a consequent increase in</p><p> the average particle size (Jung and Bell, 2000). Table 1 showed</p><p> that the relation between the crystalli
93、te size and the surface</p><p> area of the obtained ZrO2 nanopowders produced by differ-</p><p> ent techniques. For CP method, when the crystallite sizes of</p><p> the produce
94、d powders increased from 7 nm for the precursor</p><p> thermally treated at 500 ? C to 32.90 nm at 700 ? C. The surface</p><p> area of amorphous zirconia produced at 120 ? C was 250 m2 /g<
95、;/p><p> which was decreased to 230 m2 /g for the precursor thermally</p><p> treated at 500 ? C and decreased again to 180 and 20 m2 /g for the</p><p> precursor thermally treated
96、at 700 and 1000 ? C, respectively.</p><p> For CGC method, the BET speci?c surface area of amorphous</p><p> zirconia was 280 m2 /g then decreased to 210 m2 /g (crystallite</p><p>
97、; size was 10.18 nm) for the precursor treated at 700 ? C then to</p><p> 60 m2 /g for the sample treated at 1000 ? C (crystallite size was</p><p> 41.2 nm). Moreover, for MRP method, the BET
98、 speci?c surface</p><p> area was also 280 m2 /g then decreased to 200 m2 /g (crystallite</p><p> size was 21 nm) and 45 m2 /g (crystallite size was 57.8 nm) for</p><p> the prec
99、ursors annealing at 700 and 1000 ? C, respectively.</p><p> The tetragonal phase then inverted to pure monoclinic</p><p> phase (JCPDS #37-1484) by increasing the temperature up to</p>
100、<p> 1000–1200 ? C for 1 h in case of CP and CGC techniques. Trans-</p><p> formation from the tetragonal to monoclinic phase have been</p><p> attributed to the relative stability of th
101、ese two phases depend</p><p> on the sum of the free energies from particle surface, bulk</p><p> and strain contribution (Jung and Bell, 2000). Because of the</p><p> lower bulk
102、 free energy of m-ZrO2 and the lower surface free</p><p> energy of t-ZrO2 , the latter phase is stabilized below a critical</p><p> particle size for a given temperature. This critical size i
103、s esti-</p><p> mated to be 10 nm at 298 K. In the absence of particle strain,</p><p> this thermodynamic description has been found to give the</p><p> correct temperature for t
104、he tetragonal to monoclinic phase</p><p> transformation for the particles ranging from 9 nm to 10 m.</p><p> The phase transformation occurred when the size of zirconia</p><p>
105、particles is equal to or greater than the critical size determined</p><p> from an analysis of the thermodynamic stability of small parti-</p><p> cles of t- and m-ZrO2 . The validity of a pur
106、ely thermodynamic</p><p> explanation has been questioned since several investigations</p><p> have observed t-ZrO2 that is larger than the critical particle</p><p> size by talk
107、ing into account factors such as domain boundary</p><p> stresses, nucleation embryos, anionic vacancies and adsorbed</p><p> cations and anions, all of which contribute to the stabiliza-</
108、p><p> tion of t-ZrO2 . On these factors, the effects of external strain</p><p> and the adsorbed ionic species on the surface free energy of</p><p> zirconia can be accommodated wi
109、thin the thermodynamic</p><p> theory for the tetragonal to monoclinic phase transforma-</p><p> tion. In addition, the phase transformation of zirconia starts</p><p> from its s
110、urface region and then gradually develops into the</p><p> bulk. The tetragonal phase in the surface region is dif?cult</p><p> to stabilize. Treatment at progressively higher temperature</
111、p><p> in absence of strain is accompanied by loss of surface area.</p><p> Moreover, when hydrous zirconia inverted to t-ZrO2 , zirconia</p><p> Table 1 – Crystallite size (Cs) and
112、 the speci?c surface area SBET values of zirconia nanopowders synthesized by CP, CGC</p><p> and MRP methods at different calcination temperatures</p><p> Temperature (? C)</p><p>
113、;<b> Cs (nm)</b></p><p><b> 120</b></p><p><b> 500</b></p><p><b> 700</b></p><p><b> 1000</b></p>
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