Tube furnace

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Tube furnace being used during synthesis of aluminium chloride using HCl and aluminium Horno tubular.jpg
Tube furnace being used during synthesis of aluminium chloride using HCl and aluminium

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]

Illustrative applications

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.

Related Research Articles

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.

<span class="mw-page-title-main">Sintering</span> Process of forming and bonding material by heat or pressure

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.

<span class="mw-page-title-main">Crucible</span> Container in which substances are heated

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.

<span class="mw-page-title-main">Molybdenum disulfide</span> Chemical compound

Molybdenum disulfide is an inorganic compound composed of molybdenum and sulfur. Its chemical formula is MoS
2
.

<span class="mw-page-title-main">Fused quartz</span> Glass consisting of pure silica

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 in which other ingredients are added which change the glasses' optical and physical properties, such as lowering the melt temperature. Fused quartz, therefore, has high working and melting temperatures, making it less desirable for most common applications.

<span class="mw-page-title-main">Vacuum distillation</span> Low-pressure and low-temperature distillation method

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.

<span class="mw-page-title-main">Refractory</span> Materials resistant to decomposition under high temperatures

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.

<span class="mw-page-title-main">Metal-halide lamp</span> Type of 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.

<span class="mw-page-title-main">Heating element</span> Device that converts electricity into heat

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.

<span class="mw-page-title-main">Borosilicate glass</span> Glass made of silica and boron trioxide

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.

Molybdenum trioxide describes a family of inorganic compounds with the formula MoO3(H2O)n where n = 0, 1, 2. The anhydrous compound is produced on the largest scale of any molybdenum compound since it is the main intermediate produced when molybdenum ores are purified. The anhydrous oxide is a precursor to molybdenum metal, an important alloying agent. It is also an important industrial catalyst. It is a yellow solid, although impure samples can appear blue or green.

<span class="mw-page-title-main">Total organic carbon</span> Concentration of organic carbon in a sample

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.

<span class="mw-page-title-main">Ceramic metal-halide lamp</span>

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.

<span class="mw-page-title-main">Hot cathode</span> Type of electrode

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.

<span class="mw-page-title-main">Hydrothermal synthesis</span> Techniques for crystallizing substances

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.

<span class="mw-page-title-main">Infrared heater</span> Device designed to create radiative heat

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.

<span class="mw-page-title-main">Chemical transport reaction</span> Process for purification and crystallization of non-volatile solids

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.

<span class="mw-page-title-main">Carbon diselenide</span> Chemical compound

Carbon diselenide is an inorganic compound with the chemical formula CSe2. It is a yellow-orange oily liquid with pungent odor. It is the selenium analogue of carbon disulfide and carbon dioxide. This light-sensitive compound is insoluble in water and soluble in organic solvents.

<span class="mw-page-title-main">Materials for use in vacuum</span>

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.

Hafnium compounds are compounds containing the element hafnium (Hf). Due to the lanthanide contraction, the ionic radius of hafnium(IV) (0.78 ångström) is almost the same as that of zirconium(IV) (0.79 angstroms). Consequently, compounds of hafnium(IV) and zirconium(IV) have very similar chemical and physical properties. Hafnium and zirconium tend to occur together in nature and the similarity of their ionic radii makes their chemical separation rather difficult. Hafnium tends to form inorganic compounds in the oxidation state of +4. Halogens react with it to form hafnium tetrahalides. At higher temperatures, hafnium reacts with oxygen, nitrogen, carbon, boron, sulfur, and silicon. Some compounds of hafnium in lower oxidation states are known.

References

  1. J. D. Corbett "Synthesis of Solid-State Materials" in Solid State Chemistry: Techniques, A. K. Cheetham and P. Day, Eds. Clarendon, Oxford, 1987. ISBN   0-19-855165-7.
  2. Harker, J. A. (December 1905). "On a New Type of Electric Furnace, with a Redetermination of the Melting-Point of Platinum". Proceedings of the Royal Society A. 76 (507): 235–249. Bibcode:1905RSPSA..76..235H. doi: 10.1098/rspa.1905.0023 .
  3. J. F. Revelli, "Tantalum Disulfide (TaS2) and Its Intercalation Compounds" Inorganic Syntheses 1995, volume 30, pp. 155. doi : 10.1002/9780470132616.ch32