Sintering particle size

Whenever possible the study of the structure of agglomerates should commence with determination of the size distribution (or at least, average size) of the particles of which the agglomerate is made up. In certain cases (e.g., if the solid is supplied to the investigator as an agglomerate that has been well sintered) particle size measurement may be out of the question. The investigator must then pass on directly to the characterization procedures discussed below... 

Synthesis temperature affects the particle size of the boride powder which is extremely important for densification. Powders obtained at lower synthesis temperature have finer size and better sinterability. Particle size of boron carbide also affects the reaction temperature and finally the product quality. As boron carbide grain size increases, the oxide rednction processes and diffusional processes slow... 

The characteristics of a powder that determine its apparent density are rather complex, but some general statements with respect to powder variables and their effect on the density of the loose powder can be made. (/) The smaller the particles, the greater the specific surface area of the powder. This increases the friction between the particles and lowers the apparent density but enhances the rate of sintering. (2) Powders having very irregular-shaped particles are usually characterized by a lower apparent density than more regular or spherical ones. This is shown in Table 4 for three different types of copper powders having identical particle size distribution but different particle shape. These data illustrate the decisive influence of particle shape on apparent density. (J) In any mixture of coarse and fine powder particles, an optimum mixture results in maximum apparent density. This optimum mixture is reached when the fine particles fill the voids between the coarse particles. 

Lubricants protect die and punch surfaces from wear and bum-out of the compact during sintering without objectionable effects or residues. They must have small particle size, and overcome the main share of friction generated between tool surfaces and powder particles during compaction and ejection. They must mix easily with the powder, and must not excessively impede powder flow (see Lubrication and lubricants). 

In the sheet-forming process, stainless steel, bronze, nickel-base alloys, or titanium powders are mixed with a thermosetting plastic and presintered to polymerize the plastic. Sintering takes place in wide, shallow trays. The specified porosity is achieved by selecting the proper particle size of the powder. Sheet is available in a variety of thicknesses between 16 x 30 mm and as much as 60 x 150 cm. A sheet can be sheared, roUed, and welded into different configurations. 

Extra-Fine Precipitated Hydroxide. Very fine (< 1 /im-diameter) particle size hydroxide is produced by precipitation under carefully controlled conditions using specially prepared hydroxide seed. Precipitation is usually carried out at low (30 —40°C) temperatures causing massive nucleation of fine, uniform hydroxide particles (Fig. 5). Tray or tumiel Ape dry ers are used to dry the thorouglily washed filter cake to a granular product wliich is easily pulverized to obtain the fine hydroxide. Alternatively, the washed product is spray dried. Precipitation from an organic-free aluniinate Hquor, such as that obtained from the soda—sinter process, fields a very wliite product. Tlie fine precipitated hydroxide is used by the paper and plastic industries as fillers. 

Barium carbonate of finely controlled particle size reacts in the soHd state when heated with iron oxide to form barium ferrites. Magnetically aligned barium ferrite [11138-11-7] powder can be pressed and sintered into a hard-core permanent magnet which is used in many types of small motors. Alternatively, ground up magnetic powder can be compounded into plastic strips which are used in a variety of appHances as part of the closure mechanism. 

The primary driviag force for material transport comes from the chemical potential difference that exists between surfaces of dissimilar curvature within the system. The greater the curvature, ie, the finer the particle size, the greater the driving force for material transport and sintering. 

The values of m given above conform to Hemng s scaling law (1950) which states that since the driving force for sintering, the transport length, the area over which uansport occurs and the volume of matter to be transported are proportional to a, and respectively, the times for equivalent change in two powder samples of initial particle size ai q and 2,0 are... 

Example. The Pechini method for fuel cell electrode preparation. La, Ba, Mn niU ates - - CgHgO — citrate complex - - C2FI6O2 — gel. Metal nitrates are complexed with citric acid, and then heated with ethylene glycol to form a transparent gel. This is then heated to 600 K to decompose the organic content and then to temperatures between 1000 and 1300K to produce tire oxide powder. The oxide materials prepared from the liquid metal-organic procedures usually have a more uniform particle size, and under the best circumstances, this can be less than one micron. Hence these particles are much more easily sintered at lower temperatures than for the powders produced by tire other methods. 

Here p is the density, a is the particle size, C and n are constants, Q is the activation energy for sintering, R is the gas constant and T is the absolute temperature, n is typically about 3, and Q is usually equal to the activation energy for grain boundary diffusion. 

Diatomaceous media are available in various shapes. Their relatively uniform particle size establishes high efficiency in retaining solid particles of sizes less than 1/tm as well as certain types of bacteria. Media in the form of plates and cartridges are manufactured by sintering a mixture of diatomite with a binder. 

If the phases present can be unambiguously identified, microscopy can be used to determine the geometry of interface initiation and advance, and to provide information about particle sizes of components of mixed reactants in a powder. Problems of interpretation arise where materials are poorly crystallized and where crystallites are small, opaque, porous or form solid solutions. With the hot-stage microscope, the progress of reactions can be followed in some instances and the occurrence of sintering and/or melting detected. 

CVD-derived powders may prove very useful and profitable in the production of bulk ferroelectric materials which are produced by hot-pressing or sintering. These powders offer great uniformity, small particle size, and high reactivity (see Ch. 19). 

Boride Mean particle size (fim) Binder nature and content (wt%) Compacting pressure X 10 (N m ) Sintering T (°C) Holding time (min) Sintering atmosphere or vacuum V (pressure in torr) Relative density (% theoreiicaJ) Remarks Ref. 

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