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3.3 XPS results
To discuss the oxidation state of Co species, the XPS spectra of Co 2p3/2 and Co 2p1/2 levels for Ag-containing catalysts are shown in Fig. 3a. It is known that the negative shifts of Co 2p3/2 peaks were due to the existence of higher oxidation state of Co4+ [9, 18]. The binding energy of Co 2p3/2 is only 779.3 eV even after the presence of some Co4+ ions in La1-xKxCoO3 perovskites. The binding energy of Co 2p3/2 is about 780.0 eV in present work, which is close to the binding energy of Co in LaCoO3 (779.7) and Co3+ in Co2O3 (779.6 eV)[13][ 20140619-44], Thus, Co species should exist as the low valence (Co2+ and Co3+) instead of Co4+. This result is in accordance to XRD and TPR results.
Fig. 3b shows the XPS spectra of Ag species. For all samples, there are two main binding energy peaks corresponding to Ag 3d5/2 and Ag 3d3/2 levels at 368.2 eV and 374.2 eV with spin orbit separation of 6.0 eV. It has been reported that [14][ 20141011-15, [21] M. Kumar, G.B. Reddy, Phys Status Solidi B 246 (2009) 2232–2237.], Ag 3d5/2 peak at 368.2 eV indicates that Ag species exist as metallic Ag (Ag0) and Ag 3d5/2 peak , at 367.8 eV in the range 367.3–368.6 eV suggest Ag species exist as Ag+ and Ag2+, respectively. Therefore, Ag species in the surface of Ag/LaCoO3 is speculated to be mainly metallic state. The high symmetry of Ag 3d5/2 peak suggests the relatively homogeneous environment of Ag0.
XPS spectra of O1s are demonstrated in Fig. 3c. For La1-XM1XCo1-YM2YO3 perovskites, it was suggested that the binding energy attributed to adsorbed oxygen in oxygen vacancy is 530.8 eV [9], that of chemisorbed oxygen and lattice oxygen are 532.7 eV [17], and 529.8 eV, respectively. [Co0.93La0.07 samples.] Ag/LaCoO3 displayed two peaks. The peak with a lower binding energy (528.6 eV) was assigned to lattice oxygen (Olat). The peak with higher binding energy (531.3-531.6 eV) was attributed to absorbed oxygen (Oads). The content of Oads species is as high as 67.7% on the surface of Ag/LaCoO3-400, which is much higher than that on the surface of Ag/LaCoO3-800 ( 56.6% ) and the data reported in previous works [ ]. This should be caused by the presence of more Ag0.
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3.3 XPS測(cè)定結(jié)果

為了探討鈷物種的氧化態(tài),用于含銀催化劑水平的鈷2p3／2和鈷2p1／2的XPS光譜詳見(jiàn)圖3a。眾所周知，鈷2p3/2峰的負(fù)位移是由于Co4+[9,18]的高氧化態(tài)的存在。鈷2p3/2的鍵能即使是在La1-xKxCoO3鈣鈦礦中出現(xiàn)一些Co4+離子之后也僅為779.3 eV。在本研究中鈷2p3/2的鍵能約為780.0 eV,這接近于鈷在LaCoO3 (779.7)中和Co3+在Co2O3 ( 779.6 eV)中的鍵能[13] [20140619 - 44]，因此,鈷物種應(yīng)該以低價(jià)(Co2+和Co3+)而不是Co4+的形態(tài)存在。這一結(jié)論是依據(jù)XRD和TPR測(cè)定結(jié)果得出的。
圖3b列出銀物種的XPS光譜。對(duì)于全部樣品,對(duì)應(yīng)于銀3d5/2和銀3d3/2在368.2 eV和374.2 eV處有兩個(gè)自旋軌道分離為6.0 eV的鍵能主峰。It h已有報(bào)道[14][20141011-15,[21] M.Kumar,G.B.Reddy, Phys Status Solidi B 246 (2009)2232-2237]說(shuō)在368.2 eV處的銀3d5/2峰表明以金屬銀(Ag0)形態(tài)存在的銀物種和在367.8 eV處的銀3d5/2（測(cè)程為367.3-368.6 eV）峰分別表示以Ag+和Ag2+形態(tài)存在的銀物種。所以,據(jù)推測(cè)在銀/LaCoO3表面的銀物種為主要金屬狀態(tài)。銀3d5/2峰的高對(duì)稱性顯示了Ag0的相對(duì)均勻環(huán)境。
O1s的XPS光譜顯示于圖3c。對(duì)于La1-XM1XCo1-YM2YO3鈣鈦礦,椐認(rèn)為歸因于氧缺位中吸附氧的鍵能為530.8 eV [9],化學(xué)吸附的氧和晶格氧的鍵能分別為532.7 eV [17]和529.8 eV。[ Co0.93La0.07樣品]銀/LaCoO3顯示出兩個(gè)峰。具有較低鍵能(528.6 eV)的峰歸屬于晶格氧(Olat)。具有較高鍵能(531.3-531.6 eV)可歸屬于吸附氧(Oads)。銀/ LaCoO3 - 400表面上Oads物種的含量高達(dá)67.7%，這要比銀/LaCoO3 - 800表面上的含量(56.6%)和以往的研究中的試驗(yàn)數(shù)據(jù)報(bào)告高很多。這是由更多Ag0的存在所引起。

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