The deposition rate and film quality of In,O,-SnO, (ITO) transparent electrodes processed by sputtering are improved when using dense sputtering targets. Unfortunately, IT0 ceramics do not sinter easily. It is shown that addition of TiO, (<1 wt%) to IT0 greatly increases densification without degrading electrical properties of sputtered films. The influence of ZrO, and SiO, was also investigated.
We have developed a wedge-loaded double-cantilever beam adhesion measurement set-up for thin films deposited on glass by sputtering. The test is described in details.Results on the Glass/sublayer/Ag/ZnO multilayer provide evidence that SnO 2 or TiO 2 perform better than ZnO as a sublayer. Then however, rupture within the multilayer shifts to the upper Ag/ZnO interface. The latter is shown to be tougher than the lower ZnO/Ag interface, an asymmetry due to non-equilibrium interfacial structures.
The influence of TiO 2 additives on the sintering behavior therefore, the purpose of the present study is to investigate the role of TiO 2 as sintering additive in In 2 O 3 ceramics. of In 2 O 3 ceramics has been investigated. TiO 2 increases the densification rate, decreases the grain growth during the intermediate stage of sintering, and hinders the pore/ II. Experimental Procedure boundary breakaway that can affect the final stage of Starting powders were fine-grained (0.2 m mean particle sintering. For a given grain size, TiO 2 shifts the grain size and 1-3 m mean agglomerate size), high-purity (99.99 size/density trajectory toward higher densities. TiO 2 mainly wt%) In 2 O 3 (Metaleurop Recherche, Trappes, France). The acts by a second-phase mechanism, but it also may decrease powders were ultrasonically dispersed in ethanol mixed with the decomposition rate of In 2 O 3 . 0.8 wt% of a deflocculating agent. TiO 2 was added as a solution of titanium butoxide (Ti(O(CH 2 ) 3 CH 3 ) 4 , 99 wt% pure) pre-
I. Introductionviously dissolved in absolute ethanol. Hydrolytic polycondensation of the titanium butoxide was obtained by adding T RANSPARENT and conductive thin films made of indium tin deionized water. In the remainder of the text, the materials oxide (ITO) are used in electronic and optoelectronic applidoped with titanium are named TiO 2 -In 2 O 3 and the titanium cations. 1 Direct-current magnetron sputtering of sintered ITO content is expressed as equivalent TiO 2 . After they were stirred targets is a common route for making ITO films. The quality of ultrasonically, the TiO 2 -In 2 O 3 powders were mixed with a the film is better when the target is dense, 2 and, moreover, dense binder (3 wt% of poly(vinyl butyral) dissolved in hot ethanol) targets better resist sputtering erosion. In particular, the surand a plasticizer (0.5 wt% of dibutyl phtalate), vacuum dried, faces of ion-eroded targets are degraded by conical protrusions and pressed to pellets (8 mm in diameter and 3-8 mm in height) ("black spots" or "nodules"), 3 whose number decreases when under a pressure of 150 MPa. The green density of the pellets the target porosity decreases. Unfortunately, ITO ceramics do not was ϳ56% of TD. densify easily. 4 We have previously 5 established the following.Sintering was conducted at temperatures ranging from 1300Њ (i) The typical density of ITO ceramics sintered at 1400ЊC to 1550ЊC, in air, using an electric oven with MoSi 2 heating for 3 h is only 90%. The microstructure is affected by small elements. Isothermal experiments were conducted by rapidly pores and large voids.introducing a preheated (600ЊC for 10 min) specimen into the (ii) ITO vaporizes during heat treatments when non-oxidizhot zone of the oven and heating it for various soaking times. ing atmospheres are used.Heating rates were very fast in comparison to those used for (iii) TiO 2 is an efficient sintering additive. For instance, constant-heating-rate experiments. Dilatometry experiments 0.5 wt% TiO 2 -ITO ceramics densify to nearly theoretical...
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