Amorphous heat treatment

Ti Precursor Characteristics. The phase of the as-received hydrous Ti gel was both XRD and TEM amorphous. Heat treatment of the as-received gel at 130°C produced a mixture of an amorphous phase with anatase. Increase in the reaction temperature to the 150°C hydrothermal treatment produced anatase crystallites, whereas calcination at 600°C produced a rutile phase. Further investigation proceeded with only the as-received gel and hydrothermally treated precursor, hereafter referred to as the anatase precursor. Observation of the precursor morphology by TEM indicated a fine gel structure and a lOnm granular nature for the as-received hydrous gel and anatase precursor, respectively. 

Good corrosion resistance and partially amorphous heat treatment of alloy increases the catalytic activity and decreases the polarization... 

Sodium Poly(4-styrene sulfonate). The sol—gel processing of TMOS in the presence of sodium poly-4-styrene sulfonate (NaPSS) has been used to synthesize inorganic—organic amorphous complexes (61). These sodium siUcate materials were then isotherm ally crystallized. The processing pH, with respect to the isoelectric point of amorphous siUca, was shown to influence the morphology of the initial gel stmctures. Using x-ray diffraction, the crystallization temperatures were monitored and were found to depend on these initial microstmctures. This was explained in terms of the electrostatic interaction between the evolving siUcate stmctures and the NaPSS prior to heat treatment at elevated temperatures. 

Extrusion Resins. Extmsion of VDC—VC copolymers is the main fabrication technique for filaments, films, rods, and tubing or pipe, and involves the same concerns for thermal degradation, streamlined flow, and noncatalytic materials of constmction as described for injection-molding resins (84,122). The plastic leaves the extmsion die in a completely amorphous condition and is maintained in this state by quenching in a water bath to about 10°C, thereby inhibiting recrystallization. In this state, the plastic is soft, weak, and pHable. If it is allowed to remain at room temperature, it hardens gradually and recrystallizes partially at a slow rate with a random crystal arrangement. Heat treatment can be used to recrystallize at controlled rates. 

After preparing a homogeneous solution of the precursors, powder precipitation is accompHshed through the addition of at least one complexing ion. For PLZT, frequently OH in the form of ammonium hydroxide is added as the complexing anion, which results in the formation of an amorphous, insoluble PLZT-hydroxide. Other complexing species that are commonly used are carbonate and oxalate anions. CO2 gas is used to form carbonates. Irrespective of the complexing anion, the precipitated powders are eventually converted to the desired crystalline oxide phase by low temperature heat treatment. 

Solution Deposition of Thin Films. Chemical methods of preparation may also be used for the fabrication of ceramic thin films (qv). MetaHo-organic precursors, notably metal alkoxides (see Alkoxides, metal) and metal carboxylates, are most frequently used for film preparation by sol-gel or metallo-organic decomposition (MOD) solution deposition processes (see Sol-GEL technology). These methods involve dissolution of the precursors in a mutual solvent control of solution characteristics such as viscosity and concentration, film deposition by spin-casting or dip-coating, and heat treatment to remove volatile organic species and induce crystaHhation of the as-deposited amorphous film into the desired stmcture. 

C), and is much less reactive it is therefore safer and easier to handle, and is essentially non-toxic. The amorphous material can be transformed into various crystalline red modifications by suitable heat treatment, as summarized on the right hand side of Fig. 12.3. It seems likely that all are highly polymeric and contain three-dimensional networks formed by breaking one P-P bond in each P4 tetrahedron and then linking the remaining P4 units into chains or rings of P atoms each of which is pyramidal and 3 coordinate as shown schematically below ... 

The high corrosion resistance of amorphous alloys disappears on heat treatment that produces crystallisation . Figure 3.71 shows an example of the... 

Fig. 3.71 Change in polarisation curve of amorphous Fe-10Cr-l3P-7C alloy in 1 N HCI with the time of heat treatment at 723 K. The time of heat treatment is expressed in the figure in...

Little information exists on low-T precipitation of borides from solution. Chromium, cobalt and platinum borides are the only ones claimed to have been obtained from aqueous solution ". Ni2B and C02B are precipitated from a solution of nickel or cobalt acetates by adding a solution of sodium tetrahydroborate ". The formation of these borides at RT gives amorphous products. Hence, heat treatment at 300-700°C leads to crystalline NijB as the main constituent, although the average composition of the precipitate corresponds to NijB . 

Darkowski and Cocivera [94] investigated trialkyl- or triarylphosphine tellurides, as low-valent tellurium sources, soluble in organic solvents. They reported the cathodic electrodeposition of thin film CdTe on titanium from a propylene carbonate solution of tri-n-butylphosphine telluride and Cd(II) salt, at about 100 °C. Amorphous, smooth gray films were obtained with thicknesses up to 5.4 p,m. The Te/Cd atomic ratio was seen to depend on applied potential and solution composition with values ranging between 0.63 and 1.1. Polycrystalline, cubic CdTe was obtained upon annealing at 400 C. The as-deposited films could be either p- or n-type, and heat treatment converts p to n (type conversion cf. Sect. 3.3.2). 

A colorless gel formed which was isolated by vacuum evaporation of the volatiles. The resulting colorless glassy solid was pyrolyzed in vacuo at 900°C for 24 hours in a quartz tube and the evolved volatiles identified as NH3 and NH4CI. The remaining solid was briefly (2 hours) heated in air at 1200°C in order to remove minor carbon impurities and to improve crystallinity. This solid was then treated at room temperature with 40% aqueous HF to remove boric acid and silica formed in small quantities. The solid obtained at 900°C was identified as boron nitride however, the majority of the material was amorphous. After treatment at 1200°C, white crystalline boron-nitride was obtained in about 55% yield. 

Figure 1 shows the powder X-ray diffraction (XRD) pattern of the as-prepared Li(Nio.4Coo.2Mno.4)02 material. All of the peaks could be indexed based on the a-NaFeC>2 structure (R 3 m). The lattice parameters in hexagonal setting obtained by the least square method were a=2.868A and c=14.25A. Since no second-phase diffraction peaks were observed from the surface-coated materials and it is unlikely that the A1 ions were incorporated into the lattice at the low heat-treatment temperature (300°C), it is considered that the particle surface was coated with amorphous aluminum oxide. 

Partially Crystalline Transition Metal Sulphide Catalysts. Chiannelli and coworkers (6, 7, 8) have shown how, by precipitation of metal thio-molybdates from solution and subsequent mild heat-treatment many selective and active hydrodesulphurization catalysts may be produced. We have shown (18) recently that molybdenum sulphide formed in this way is both structurally and compositionally heterogeneous. XRES, which yields directly the variation in Mo/S ratio shows up the compositional nonuniformity of typical preparations and HREM images coupled to SAED (see Figure 2) exhibit considerable spatial variation, there being amorphous regions at one extreme and highly crystalline (18, 19) MoS at the other. 

General Aspects and Heat Treatment Effects. After him formation, for most of the hlms aimed at electronic applications (other than amorphous oxides, such as Si02), the hlms are subjected to a heat treatment process for removal of residual organic species (entrapped solvent as well as the organic constituents associated with the precursor species), densihcation (elimination of residual porosity and structural free volume in the him), and crystallization. 

The variation in the initial Tg s show the effect on processability of the structures of the diol and the dibromobenzene. Two of the systems, those based on thiodiphenol and dihydroxybiphenyl, gave crystalline products which could not be made amorphous upon heat treatment. The effect on chain flexibility of dibromobenzene structure could be seen with the two hydroquinone systems. In this case, the meta isomer gave an initial Tg of 12°C while the more rigid para system had a Tg of 59°C. Variation of diol structure shows a parallel effect as shown with the resorcinol/j>-dibromobenzene system. This material has a softening temperature of 20°C. 

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