Elektroschmelzwerk Kempten Gmbh

Klaus Reinmuth

Alfred Lipp

Klaus Hunold

Peter Arnold

Jochen Kriegesmann

Karl A Schwetz

Johannes Napholcz

Detlef Von Struensee

Franz Isemann

The invention is an improved theroelement which comprises a graphite/boron carbide thermocouple, the arms of which are constructed as a tube and a rod, arranged concentrically inside the tube, which are electrically connected at one end. One of the arms of the thermocouple consists essentially of boron carbide formed from self bonding boron carbide by pressureless sintering. Prefabricated sleeves of high-purity, boron-oxide-free hexagonal boron nitride are used between the arms of the thermocouple as spacers. Only the end of the arm of the thermocouple constructed as a rod is secured in an electrically conductive connecting piece and the arm is freely mobile in the direction towards the cold junction. As the material for the arm of the thermocouple constructed as a rod, there can be used, for example, boron carbide having a coarse-grained structure and a density of from 60 to 80% TD, which has been manufactured from boron carbide powder having bimodal particle size distribution by means of extrusion, followed by pressureless sintering at from 2000.degree. to 2250.degree. C. The thermoelement can also be manufactured in one operation by means of pressureless sintering of the boron carbide powder in situ. Such a thermoelement comprises, for example, a flexible graphite cord for the arm of the thermocouple constructed as a rod, a boron-nitride envelope and a boron-carbide casing, the envelope and casing having been formed from powders sintered in situ without pressure.

Thermoelement comprising a graphite/boron carbide thermocouple

The invention is a process for the manufacture of shaped articles of reaction-bonded silicon nitride in which pre-shaped articles of silicon powder are heated in a first stage under a nitrogen gas pressure of at least 6 MPa at a heating rate of not more than 50.degree. C. per hour to a reaction temperature below the melting point of silicon, the article is maintained at the reaction temperature for at least 0.5 hours and subsequently, in a second stage, heating the article at a heating rate of at least 500.degree. C. per hour to a temperature above the melting point of silicon and maintaining the article at that temperature for from 1 to 7 hours. The process can nitridate both pre-shaped articles consisting of silicon powder and, optionally, up to 15% by weight Si.sub.3 N.sub.4 powder and those containing up to 10% by weight of a sintering aid such as Y.sub.2 O.sub.3. In the former case, porous shaped articles having a density of from 87 to 91% TD and, in the latter case, dense shaped articles having a density of more than 98% TD, are obtained. In all cases, in a total nitridation time of less than 15 hours, a conversion of at least 95% of the silicon originally present into silicon nitride is achieved, which, in the finished shaped article, is substantially in the .beta.-modification.

Process for the manufacture of shaped articles from reaction-bonded

The invention is a ceramically-bonded large-area neutron absorber articles of low density having a space filling of

Ceramic bonded neutron absorber plates of boron carbide and free carbon

The invention is a shaped article of boron nitride having a density of at least 95% of the theoretical density which consists of polycrystalline hexagonal boron nitride in the form of a homogeneous isotropic microstructure and which has been manufactured from pure boron nitride powder without the concomitant use of sintering aids by isostatic hot-pressing in a vacuum-tight casing at temperatures of from about 1200.degree. to 1500.degree. C. under a pressure of from about 50 to 300 MPa. Boron nitride powders having a free boric oxide content of not more than 1.0% by weight and having a specific surface area of from 5 to 30 m.sup.2 /g are used as starting material. The powders either are filled into prefabricated casings consisting of steel or glass and densified by vibration or are preshaped to form green bodies having pores open to the surface and then placed in prefabricated casings or coated with a material which forms a vacuum-tight casing. The powders or the preshaped green bodies in the vacuum-tight casings are then subjected to an isostatic hot-pressing process in a high-pressure zone using an inert gas such as argon or nitrogen, as the pressure-transfer medium.

Dense shaped articles consisting of polycrystalline hexagonal boron

The invention is substantially pore-free shaped articles which consist essentially of polycrystalline .alpha.- or .beta.-silicon carbide in the form of a single-phase homogeneous microstructure having grain sizes not exceeding 8 .mu.m, and which are manufactured from SiC powder, without the concomitant use of sintering aides, by isostatic hot-pressing in a vacuum-tight casing at temperatures of from about 1900.degree. C. to 2300.degree. C. and at pressures of from about 100 to 400 MPa. The SiC starting materials have .alpha.- and/or .beta.-SiC powders having a total content of metallic impurities not exceeding 0.1% by weight and a particle size of 4 .mu.m and finer.

Shaped polycrystalline silicon carbide articles and isostatic

The invention is substantially pore-free shaped articles consisting essentially of polycrystalline silicon nitride and polycrystalline silicon carbide in the form of a homogeneous microstructure having grain sizes of not more than 10 .mu.m manufactured from mixtures of Si.sub.3 N.sub.4 powder and SiC powder in a weight ratio of from 5:95 to 95:5 without the concomitant use of sintering aids by isostatic hot pressing in a vacuum-sealed casing at temperatures of from 1800.degree. to 2200.degree. C. and a pressure of from 100 to 400 MPa.

Substantially pore-free shaped articles of polycrystalline silicon

The invention is refractory, electrically conductive, mixed materials based on hexagonal boron nitride and at least one electrically conductive component such as titanium boride and zirconium boride, and having a density of at least about 95% of the theoretical density and nondirection-dependent properties, which have been manufactured from powder mixtures that are practically free of oxygen and metal and comprise

Refractory, electrically conductive, mixed materials containing boron

The invention provides substantially pore-free sintered polycrystalline articles comprising .alpha.-silicon carbide, boron carbide and free carbon, the quantitative proportions of which, in percent by weight, are defined by the trapezoidal area having, in the ternary system B/Si/C of FIG. 1 the corner points

Substantially pore-free sintered polycrystalline articles of

The invention relates to dense shaped articles of polycrystalline .alpha.-silicon carbide containing from 0.1 to 0.4%, by weight, of aluminum and optionally, a small amount of nitrogen and/or phosphorus, having a homogeneous virtually single-phase microstructure. The additional constituents are substantially in the form of a solid solution in the .alpha.-SiC lattice. The shaped articles are distinguished by flexural strength of at least 600 N/mm.sup.2 up to 1450.degree. C. and low subcritical crack propagation under mechanical stress. The fracture mechanism is trans granular up to at least 1450.degree. C. The shaped articles are manufactured by simultaneously shaping and hot pressing pulverulent .alpha.-silicon carbide containing a small amount of an aluminum-containing additive, such as aluminum powder, aluminum nitride and/or aluminum phosphide, at temperatures between 1850.degree. C. and 2300.degree. C. under a pressure of at least 100 bar (10 MPa).

Dense shaped articles of polycrystalline .alpha.-silicon carbide and

The invention relates to a process for the manufacture of substantially pore-free shaped articles of polycrystalline material such as aluminium oxide, titanium boride, silicon nitride or silicon carbide, in which pulverulent materials or preformed articles having pores open towards the surface, in a vacuum-tight sealed glass casing that has a viscosity of less than 10.sup.6 Pas at the pressing temperature employed, are isostatically hot-pressed in a high-pressure autoclave using an inert gas as pressure-transfer medium. By being embedded in a flowable pile or by having a layer applied to them in the form of a suspension, the glass-encased powders or articles are brought into contact with a heat-resistant pulverulent material that, upon softening of the glass casing, penetrates into the surface of the glass of reacts with it, with the result that the glass casing is reinforced from the outside at the pressing temperature. As pulverulent materials, there may be used titanium boride, graphite, SiC or boron nitride, which do not react with the glass casing, or glass powder or silica, which react with the glass casing to form a glass melt of at least the same viscosity as, or of a higher viscosity than, the glass casing.

Process for the manufacture of substantially pore-free shaped

The invention is a process for the manufacture of substantially pore-free shaped articles from polycrystalline material, such as tungsten carbide, silicon nitride, titanium boride or silicon carbide, in which encased articles preformed from pulverulent materials and having open pores are isostatically hot-pressed in a vacuum-sealed casing of vitreous or ceramic-like material in a high-pressure autoclave using an inert gas as pressure-transfer medium. Before the application of the casing material, a first layer comprising material that can be decomposed or melted, such as an organic wax or a resin-like product, or of a compressible heat-resistant material such as inorganic fibers or felts, is applied to the preformed articles. Then, the encased articles are thermally treated until the glass or ceramic layer is fused or sintered gas-tight. The articles pretreated in this manner are then isostatically hot-pressed.

The invention relates to dense shaped articles of polycrystalline .beta.-silicon carbide containing small amounts of aluminum and optionally, nitrogen and/or phosphorus, having a virtually single-phase microstructure since the additional constituents are substantially in the form of a solid solution in the .beta.-SiC lattice. The shaped articles are characterized by high temperature flexural strengths of at least 600 N/mm.sup.2 at temperatures up to 1450.degree. C. The fracture mechanism is transgranular up to at least 1450.degree. C. The shaped articles are manufactured by hot-pressing and simultaneously shaping pulverulent .beta.-silicon carbide with small amounts of an aluminum-containing additive, such as aluminum powder or aluminum nitride and/or aluminum phosphide, at temperatures between 1750.degree. C. and 2200.degree. C. under a pressure of at least 100 bar (10 MPa).

Dense shaped articles of polycrystalline .beta.-silicon carbide and

The subject of the invention is thin large-area neutron-absorber plates having a volume composition of from 40 to 60% and preferably from 45 to 60% by volume of boron carbide, from 25 to 5% by volume and preferably 15 to 5% by volume of free carbon, the remainder being pores, a density of from 1.4 to 1.8 g/cm.sup.3, a flexural strength at room temperature of from 15 to 45 N/mm.sup.2, a compressive strength at room temperature of from 25 to 60 N/mm.sup.2, a modulus of elasticity at room temperature of from 10,000 to 20,000 N/mm.sup.2, and a resistance to ionizing radiation of at least 10.sup.11 rad, which plates may be produced by mixing boron carbide powder, containing at least 75% by weight of boron and a proportion of boron oxide of less than 0.5% by weight, and having a particle size distribution of at least 95% finer than 50 .mu.m and, optionally, graphite powder with a pulverulent organic resin binder and a wetting agent, shaping the mixture under pressure at room temperature, curing the resin binder at temperatures of up to 180.degree. C., and then coking the shaped plates with the exclusion of air at temperatures of up to approximately 1000.degree. C. with a controlled temperature increase.

Growing community of inventors

Durach, Germany

Klaus Reinmuth