A tube furnace is an electric heating device used to conduct syntheses and purifications of inorganic compounds and occasionally in organic synthesis. One possible design consists of a cylindrical cavity surrounded by heating coils that are embedded in a thermally insulating matrix. Temperature can be controlled via feedback from a thermocouple. More elaborate tube furnaces have two (or more) heating zones useful for transport experiments. Some digital temperature controllers provide an RS-232 interface, and permit the operator to program segments for uses like ramping, soaking, sintering, and more. Advanced materials in the heating elements, such as molybdenum disilicide (MoSi2) offered in certain models can now produce working temperatures up to 1800 °C. This facilitates more sophisticated applications. [1] Common material for the reaction tubes include alumina, Pyrex, and fused quartz, or in the case of corrosive materials molybdenum or tungsten tubes can be used.
The tube furnace was invented in the first decade of the 20th century and was originally used to manufacture ceramic filaments for Nernst lamps and glowers. [2]
An example of a material prepared using a tube furnace is the superconductor YBa2Cu3O7. A mixture of finely powdered CuO, BaO, and Y2O3, in the appropriate molar ratio, contained in a platinum or alumina "boat," is heated in a tube furnace at several hundred degrees under flowing oxygen. Similarly tantalum disulfide is prepared in a tube furnace followed by purification, also in a tube furnace using the technique of chemical vapor transport. [3] Because of the availability of tube furnaces, chemical vapor transport has become a popular technique not only in industry (see van Arkel–de Boer process) but also in the research laboratory.
Tube furnaces can also be used for thermolysis reactions, involving either organic or inorganic reactants. One such example is the preparation of ketenes which may employ a tube furnace in the 'ketene lamp'. Flash vacuum pyrolysis often utilize a fused quartz tube, usually packed with quartz or ceramic beads, which is heated at high temperatures.
Solid-state chemistry, also sometimes referred as materials chemistry, is the study of the synthesis, structure, and properties of solid phase materials. It therefore has a strong overlap with solid-state physics, mineralogy, crystallography, ceramics, metallurgy, thermodynamics, materials science and electronics with a focus on the synthesis of novel materials and their characterization. A diverse range of synthetic techniques, such as the ceramic method and chemical vapour depostion, make solid-state materials. Solids can be classified as crystalline or amorphous on basis of the nature of order present in the arrangement of their constituent particles. Their elemental compositions, microstructures, and physical properties can be characterized through a variety of analytical methods.
Sintering or frittage is the process of compacting and forming a solid mass of material by pressure or heat without melting it to the point of liquefaction. Sintering happens as part of a manufacturing process used with metals, ceramics, plastics, and other materials. The nanoparticles in the sintered material diffuse across the boundaries of the particles, fusing the particles together and creating a solid piece.
A crucible is a ceramic or metal container in which metals or other substances may be melted or subjected to very high temperatures. Although crucibles have historically tended to be made out of clay, they can be made from any material that withstands temperatures high enough to melt or otherwise alter its contents.
Fused quartz, fused silica or quartz glass is a glass consisting of almost pure silica (silicon dioxide, SiO2) in amorphous (non-crystalline) form. This differs from all other commercial glasses, such as soda-lime glass, lead glass, or borosilicate glass, in which other ingredients are added which change the glasses' optical and physical properties, such as lowering the melt temperature, the spectral transmission range, or the mechanical strength. Fused quartz, therefore, has high working and melting temperatures, making it difficult to form and less desirable for most common applications, but is much stronger, more chemically resistant, and exhibits lower thermal expansion, making it more suitable for many specialized uses such as lighting and scientific applications.
Vacuum distillation or distillation under reduced pressure is a type of distillation performed under reduced pressure, which allows the purification of compounds not readily distilled at ambient pressures or simply to save time or energy. This technique separates compounds based on differences in their boiling points. This technique is used when the boiling point of the desired compound is difficult to achieve or will cause the compound to decompose. Reduced pressures decrease the boiling point of compounds. The reduction in boiling point can be calculated using a temperature-pressure nomograph using the Clausius–Clapeyron relation.
In materials science, a refractory is a material that is resistant to decomposition by heat or chemical attack that retains its strength and rigidity at high temperatures. They are inorganic, non-metallic compounds that may be porous or non-porous, and their crystallinity varies widely: they may be crystalline, polycrystalline, amorphous, or composite. They are typically composed of oxides, carbides or nitrides of the following elements: silicon, aluminium, magnesium, calcium, boron, chromium and zirconium. Many refractories are ceramics, but some such as graphite are not, and some ceramics such as clay pottery are not considered refractory. Refractories are distinguished from the refractory metals, which are elemental metals and their alloys that have high melting temperatures.
High-intensity discharge lamps are a type of electrical gas-discharge lamp which produces light by means of an electric arc between tungsten electrodes housed inside a translucent or transparent fused quartz or fused alumina arc tube. This tube is filled with noble gas and often also contains suitable metal or metal salts. The noble gas enables the arc's initial strike. Once the arc is started, it heats and evaporates the metallic admixture. Its presence in the arc plasma greatly increases the intensity of visible light produced by the arc for a given power input, as the metals have many emission spectral lines in the visible part of the spectrum. High-intensity discharge lamps are a type of arc lamp.
A metal-halide lamp is an electrical lamp that produces light by an electric arc through a gaseous mixture of vaporized mercury and metal halides. It is a type of high-intensity discharge (HID) gas discharge lamp. Developed in the 1960s, they are similar to mercury vapor lamps, but contain additional metal halide compounds in the quartz arc tube, which improve the efficiency and color rendition of the light. The most common metal halide compound used is sodium iodide. Once the arc tube reaches its running temperature, the sodium dissociates from the iodine, adding orange and reds to the lamp's spectrum from the sodium D line as the metal ionizes. As a result, metal-halide lamps have high luminous efficacy of around 75–100 lumens per watt, which is about twice that of mercury vapor lights and 3 to 5 times that of incandescent lights and produce an intense white light. Lamp life is 6,000 to 15,000 hours. As one of the most efficient sources of high CRI white light, metal halides as of 2005 were the fastest growing segment of the lighting industry. They are used for wide area overhead lighting of commercial, industrial, and public places, such as parking lots, sports arenas, factories, and retail stores, as well as residential security lighting, automotive headlamps and indoor cannabis grow operations.
A heating element is a device used for conversion of electric energy into heat, consisting of a heating resistor and accessories. Heat is generated by the passage of electric current through a resistor through a process known as Joule Heating. Heating elements are used in household appliances, industrial equipment, and scientific instruments enabling them to perform tasks such as cooking, warming, or maintaining specific temperatures higher than the ambient.
Borosilicate glass is a type of glass with silica and boron trioxide as the main glass-forming constituents. Borosilicate glasses are known for having very low coefficients of thermal expansion, making them more resistant to thermal shock than any other common glass. Such glass is subjected to less thermal stress and can withstand temperature differentials without fracturing of about 165 °C (300 °F). It is commonly used for the construction of reagent bottles and flasks, as well as lighting, electronics, and cookware.
Total organic carbon (TOC) is an analytical parameter representing the concentration of organic carbon in a sample. TOC determinations are made in a variety of application areas. For example, TOC may be used as a non-specific indicator of water quality, or TOC of source rock may be used as one factor in evaluating a petroleum play. For marine surface sediments average TOC content is 0.5% in the deep ocean, and 2% along the eastern margins.
A ceramic metal-halide lamp (CMH), also generically known as a ceramic discharge metal-halide (CDM) lamp, is a type of metal-halide lamp that is 10–20% more efficient than the traditional quartz metal halide and produces a superior color rendition.
In vacuum tubes and gas-filled tubes, a hot cathode or thermionic cathode is a cathode electrode which is heated to make it emit electrons due to thermionic emission. This is in contrast to a cold cathode, which does not have a heating element. The heating element is usually an electrical filament heated by a separate electric current passing through it. Hot cathodes typically achieve much higher power density than cold cathodes, emitting significantly more electrons from the same surface area. Cold cathodes rely on field electron emission or secondary electron emission from positive ion bombardment, and do not require heating. There are two types of hot cathode. In a directly heated cathode, the filament is the cathode and emits the electrons. In an indirectly heated cathode, the filament or heater heats a separate metal cathode electrode which emits the electrons.
Hydrothermal synthesis includes the various techniques of crystallizing substances from high-temperature aqueous solutions at high vapor pressures; also termed "hydrothermal method". The term "hydrothermal" is of geologic origin. Geochemists and mineralogists have studied hydrothermal phase equilibria since the beginning of the twentieth century. George W. Morey at the Carnegie Institution and later, Percy W. Bridgman at Harvard University did much of the work to lay the foundations necessary to containment of reactive media in the temperature and pressure range where most of the hydrothermal work is conducted.
The flux method is a crystal growth method where starting materials are dissolved in a solvent (flux), and are precipitated out to form crystals of a desired compound. The flux lowers the melting point of the desired compound, analogous to a wet chemistry recrystallization. The flux is molten in a highly stable crucible that does not react with the flux. Metal crucibles, such as platinum, titanium, and niobium are used for the growth of oxide crystals. Ceramic crucibles, such as alumina, zirconia, and boron nitride are used for the growth of metallic crystals. For air-sensitive growths, contents are sealed in ampoules or placed in atmosphere controlled furnaces.
An infrared heater or heat lamp is a heating appliance containing a high-temperature emitter that transfers energy to a cooler object through electromagnetic radiation. Depending on the temperature of the emitter, the wavelength of the peak of the infrared radiation ranges from 750 nm to 1 mm. No contact or medium between the emitter and cool object is needed for the energy transfer. Infrared heaters can be operated in vacuum or atmosphere.
In chemistry, a chemical transport reaction describes a process for purification and crystallization of non-volatile solids. The process is also responsible for certain aspects of mineral growth from the effluent of volcanoes. The technique is distinct from chemical vapor deposition, which usually entails decomposition of molecular precursors (e.g. SiH4 → Si + 2 H2) and which gives conformal coatings. The technique, which was popularized by Harald Schäfer, entails the reversible conversion of nonvolatile elements and chemical compounds into volatile derivatives. The volatile derivative migrates throughout a sealed reactor, typically a sealed and evacuated glass tube heated in a tube furnace. Because the tube is under a temperature gradient, the volatile derivative reverts to the parent solid and the transport agent is released at the end opposite to which it originated (see next section). The transport agent is thus catalytic. The technique requires that the two ends of the tube (which contains the sample to be crystallized) be maintained at different temperatures. So-called two-zone tube furnaces are employed for this purpose. The method derives from the Van Arkel de Boer process which was used for the purification of titanium and vanadium and uses iodine as the transport agent.
Molybdenum tetrachloride is the inorganic compound with the empirical formula MoCl4. The material exists as two polymorphs, both being dark-colored paramagnetic solids. These compounds are mainly of interest as precursors to other molybdenum complexes.
Materials for use in vacuum are materials that show very low rates of outgassing in vacuum and, where applicable, are tolerant to bake-out temperatures. The requirements grow increasingly stringent with the desired degree of vacuum to be achieved in the vacuum chamber. The materials can produce gas by several mechanisms. Molecules of gases and water can be adsorbed on the material surface. Materials may sublimate in vacuum. Or the gases can be released from porous materials or from cracks and crevices. Traces of lubricants, residues from machining, can be present on the surfaces. A specific risk is outgassing of solvents absorbed in plastics after cleaning.
Kiln furniture are devices and implements inside furnaces used during the heating of manufactured individual pieces, such as pottery or other ceramic or metal components. Kiln furniture is made of refractory materials, i.e., materials that withstand high temperatures without deformation. Kiln furniture can account for up to 80% of the mass of a kiln charge.