GB2218711A - Process for producing powdered refractory inorganic compounds and metal compositions - Google Patents

Process for producing powdered refractory inorganic compounds and metal compositions Download PDF

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GB2218711A
GB2218711A GB8906445A GB8906445A GB2218711A GB 2218711 A GB2218711 A GB 2218711A GB 8906445 A GB8906445 A GB 8906445A GB 8906445 A GB8906445 A GB 8906445A GB 2218711 A GB2218711 A GB 2218711A
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mass
mixture
argon
oxide
charge
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Alexandr Grigorievic Morzhanov
Inna Petrovna Borovinskaya
Sos Sarkisovich Mamian
Vitaly Mikhailovich Maslov
Vladimir Ivanovic Vershinnikov
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Institut Strukturnoi Makrokinetiki Akademii Nauk
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/20—Methods for preparing sulfides or polysulfides, in general
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
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    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/0828—Carbonitrides or oxycarbonitrides of metals, boron or silicon
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    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/08—Other phosphides
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/907—Oxycarbides; Sulfocarbides; Mixture of carbides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/921—Titanium carbide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/935—Carbides of alkali metals, strontium, barium or magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/949—Tungsten or molybdenum carbides
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/06—Metal silicides
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/04—Metal borides
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/0617—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with vanadium, niobium or tantalum
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    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/076—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with titanium or zirconium or hafnium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Silicon Compounds (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Powder Metallurgy (AREA)
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  • Carbon And Carbon Compounds (AREA)
  • Developing Agents For Electrophotography (AREA)

Description

1 2218711 M&C FOLIO: 230P58317 WANGDOC: 0092D PROCESS FOR PRODUCING
POWDERED INORGANIC COMPOUNDS AND METAL COMPOSITIONS The present invention relates to a process for producing powdered refractory inorganic compounds and metal compositions and to a charge for said process.
The present invention is useful in powder metallurgy for the production of hard alloys, refractory materials and materials resistant to corrosive media. and in the manufacture of composite ceramic materials.
The invention provides a process having novel starting components for producing firm, powdery refractory, inorganic compounds and metal compositions of elements of Groups I-VIII of the Periodic Table which are of uniform particle size and phase.
The process comprises preparation of a charge containing an element of Groups IV-VI of the Periodic Table and an element selected from the group consisting of nitrogen. carbon. boron. silicon. sulphur and phosphorus, placing the charge into the reaction zone. wherein a self-propagating high-temperature synthesis of 2 the desired product is conducted, followed by the isolation of the. desired product f rom the reaction zone, the charge additionally comprising:
- at least one element of Groups I-III and VII-VIII of the Periodic Table, - and/or at least one hydride of elements of Groups I-III of the Periodic Table, and/or at least one oxide and/or halide of elements of Groups IVIII of the Periodic Table, - and nitrogen, carbon, boron, silicon, sulphur, and/or phosphorus and/or an oxide, halide, and/or organic compound thereof, - and halides of alkali metals, ammonium halide, polystyrene, polyethylene, and/or urea, and isolating the desired product by treating the product of the synthesis with a solution of a mineral acid.
Through the present invention it has become possible to obtain fine powders (with a particle size from 0.1 to 10.01im) which have a uniform phase and particle size composition. Furthermore. it has also become possible to obtain powdery refractory inorganic compounds and metal compositions of elements of Groups I-VIII of the Periodic Table.
j, p tt 3 I- c In accordance with the present invention it is preferred to use a charge consisting of a mixture of 12.00 to 80.95% by mass of at least one element of Groups I-VIII and/or at least one oxide or halide thereof, 0. 05-31.50% by mass of nitrogen, carbon, boron, silicon, sulphur, phosphorus, and/or oxides, halides and/or organic compounds thereof: 19.0- 56.5% by mass of at least one metal of Groups I-III of the Periodic Table, and/or at least one hydride thereof, and additives in an amount of from 1 to 25% by mass of the mixture, said additives consisting of oxides of Group II metals, halides of alkali metals, ammonium halide, polystyrene, poylethylene and/or urea.
According to the present invention, to obtain a product which has a uniform particle size and to ensure fine particles of the resulting powdery compounds and compositions, it is preferred that the charge contain, as additives, 5 to 25% by mass oxides of metals of Group II of the Periodic Table and/or 1-5% by mass of halides of alkali metals, ammonium halide, polystyrene, polyethylene and/or urea.
In a preferred embodiment. to obtain a refractory inorganic compound with uniform particle size of 2-5 lim, a charge consisting substantially of a mixture of 56.0% by mass of titanium dioxide, 8.3% by mass of 4 carbon. 35.7% by mass of magnesium, and additives 10.0% by mass of the mixture of magnesium oxide and 3.0% by mass of the mixture of polystyrene - is used, and isolation of the product is effected by treating the product of the synthesis with a solution of hydrochloric acid.
In another preferred embodiment. to obtain a metal composition of elemental titanium and elemental nickel with a particle size of 2.0 to 5. 01im, a charge consisting substantially of a mixture of 26.50% by mass of titanium dioxide. 25.50% by mass of nickel oxide. 26.50% by mass of calcium, 21.45% by mass of zinc, 0.05% by mass of carbon black and an additive - 24.0% by mass of the mixture of calcium oxide - is used, and isolation of the product is effected by way of treatment of the synthesised product with a solution of sulphuric acid.
Other objects and advantages of the present invention will now become more fully apparent from the following detailed description and Examples.
Suitable starting components are:
(1) Elements of Groups I-VIII of the Periodic Table taken seperately or in combination, their oxides, their halides, for example a powder of elemental titanium with a powder of elemental tungsten; a powder of elemental 1 11 I- tungsten with tungsten oxide and tungsten chloride; a powder of elemental titanium with elemental tungsten and tungsten chloride; titanium oxide with tungsten oxide. The ratio between the compounds given in the above combinations depends on the requirements (regarding the chemical and phase compositions) imposed on the desired product and is equal. as is known, to a value within the range of from 0 to 1.
(II) Elements of Groups I-III of the Periodic Table taken separately or in combination and their hydrides, for example, a powder of metallic magnesium; a mixture of a powder of metallic calcium with calcium hydride in any ratio: a mixture of metallic powders of lithium, calcium and aluminium in any ratio; a mixture of metallic powders of lithium, aluminium and magnesium hydride in any ratio. depending on the desired product.
(III) Nitrogen, carbon, boron, silicon, sulphur, phosphorus, taken either separately or in combination, their oxides, their halides and their organic compounds. For example. nitrogen; nitrogen and carbon; carbon and boron; carbon and boron oxide; boron chloride and polyethylene; silicon with silicon oxide and silicon chloride. The ratio between the substances mentioned in the above combinations depends on the requirements imposed on the desired product.
6 The starting charge for the synthesis of the desired product is prepared by mixing the three starting components. According to a preferred aspect, use is made of 12.0%-80.95% by mass of component (I), 19.0-56.5% by mass of component (II) and 0.05-31.5% by mass of component (III).
When component (I) is present in the charge in an amount of less than about 12.0% by mass. the ratio between the reactants is not optimal. and this results in an increased temperature of burning (synthesis) and in non-uniformity of the phase composition of the desired product and its particle size.
When component (I) is present in an amount exceeding about 80.95% by mass, the excess enters into the burning process as ballast, thus causing arrest of propagation of the front of combustion through the entire reaction volume and disturbing the phase and particle-size uniformity of the desired product.
An amount of less than about 19.0% by mass of component (II) results in an unreacted excess of component (I) in the product, disturbing the particle-size and phase uniformity of the product.
9 7 L A content of component (II) in excess of about 56.5% by mass, during synthesis. results in intensive evaporation of the excess of this component. which also gives rise to a detrimental effect on the particlesize and phase uniformity of the product.
The content of component (III) in the charge is determined by the content of components (I) and (II).
According to the present invention, into the charge obtained by mixing of components (I), (II) and (III) are introduced additives: about 5 to 25% by mass of the obtained mixture of oxides of Group II metals and/or about 1-5% by mass of the obtained mixture of halides of alkali metal s, ammonium halide, polystyrene, polyethylene and/or urea.
The addition of a mixture of additives in the form of oxides of Group II metals makes it possible to lower the synthesis temperature. since these oxides do not decompose or contaminate the final product, and crystallisation of the desired product occurs under 'mild' conditions. thus enabling the production of a uniform fine powder. To ensure uniformity of particle size and structure, said oxides are selected from the group of oxides of alkali-earth metals. so they are identical with oxides of component (II), these oxides 8 also allowing a rather easy purification of the desired product. When these oxides are used in an amount of -less than about 5% by mass. an essential reduction of temperature for the required conditions of crystallisation during the synthesis may not be attained. The use of the oxides in an amount of more than about 25% by mass tends to decrease the combustion temperature, thus impairing the uniformity of the powdery product obtained.
Additional introduction of halides of alkali metals, ammonium halide, polystyrene, polyethylene and/or urea into the above-mentioned mixture of the components (I), (II) and (III), leads to a lowering of the synthesis temperature due to their decomposition during synthesis; this gives a result similar to the incorporation irr the mixture of Group II oxides. The amount of the additionally introduced halides of alkali metals, ammonium halide, polystyrene, polyethyl ene and/or urea should correspond to the amount of the introduced Group II oxides. The evolution of a great amount of gaseous substances results in a gasostatic disintegration of the final product directly in the front of combustion. Furthermore, the decomposing additive contains the elements necessary for a complete conversion of the final product; these are carbon in the polymer composition for obtaining carbides, nitrogen in urea for i G 9 1 i:
nitrides. The introduction of halides of alkali metals or ammonium halide makes it possible to lower the synthesis temperature without contamination of the final product, since the formed gaseous products are readily volatile.
The use of the decomposing additive in an amount of less than about 1% by mass tends to be insufficient. since it does not result in the formation of a required amount of gas. The use of the decomposing additive in an amount of more than about 5% by mass tends to result in a decreased temperature of synthesis and in non-uniformity of the final product.
The charge. prepared as above. is then placed into a reactor ensuring a self-propagating high-temperature synthesis. for which a reactor of a conventional design can be used.
The ignition of the upper layer of the charge may be initiated by use of, for example. a tungsten coil connected to a source of 50-60V and 5-20A. Thereafter high-temperature synthesis is self-propagating.
The product of the synthesis contains impurities of side combustion products (compounds of component (II)). These impurities may be removed by treating the product in solutions of mineral acids. for example in solutions of hydrochloric or sulphuric acid. After acid treatment. the product is dried at a temperature within the range of from 100 to 1500C for a period of 4 to 5 hours.
The thus-obtained product is a powdery substance of uniform phase and particle size-composition: its particle size varies within the range of from 0.1 to 10.Olim. The resulting product. in its morphology. is readily distinguishable from similar products obtained by other methods.
Control of the obtained product can be effected by chemical. X-ray scanning and diffraction analysis.
The process according to the present invention makes it possible to obtain a powdery product with the above-specified characteristics using as the starting components more readily available and less-expensive raw materials - oxides and halides instead of previously employed expensive and hardly available metal powders.' 11 Moreover, the process according to the present invention makes it possible to obtain compounds of Groups I-VIII of the Periodic Table which, due to a low exothermicity of interaction of the starting elemental. metallic and non-metallic components, could not have been obtained earlier under conditions of a self-propagating high-temperature synthesis, e.g. boron and tungsten carbides.
It will be appreciated that the present invention also provides ignitable charges as defined above.
Example 1
Titanium dioxide powder (56% by mass), magnesium powder (35.7% by. mass) and carbon black (8.3% by mass) are charged into a stainless-steel drum and mixed for 5 hours. Thereafter 10% by mass of a powder of magnesium oxide and 3% by mass of a powder of polystyrene are added and the powders are further mixed and charged into a reactor. Upon handling the powders are rammed. The reactor is then closed. purged 2-3 times with an inert gas, filled with argon. sealed and the charge locally ignited by means of a tungsten coil connected to a 50-60V, 5-20A source.Combustion temperature reaches 12 2,30011C. On completion of combustion, the reactor, together with the final product, is cooled to 1CC. The product is discharged from the reactor and treated in a solution of hydrochloric acid. The isolated powder is titanium carbide (TiC) with uniform particles of a dark-grey colour and size of 2 to 5lim. The product is single-phased with a cubic lattice of NaCl type.
The resulting titanium carbide can be used as the starting powder for the manufacture of hard-alloy materials and abrasive pastes without any preliminary preparation (grinding. screening).
further experiments were performed as described in Example 1, under the conditions shown in the following Table.
_1 Q 7 Table
Method for Preparing Powdered High-,.lelzing Inorganic Compositions and Metal Compositions E x a m p 1 e s 7!-prociuct!Ratio of !obtained!com-oonents 1!in charge 1 !Type and amount lof additive tl;iediuni!Pressure, atm 1 itherma- Idecompo- ily ising istable jadditive j,-it. jwt.% 1 2 3 1 4 5 6 7 -hy- 1 0 I TiC Tio 5599 'M go poyet 2 4 6 I.C 2 #8 argon mg 35968 c 6 #42 i i i -- - - - - - - - - - - - - - - - - - - - - - - - - - 2. Ti C Tio 2 55p9 mgo poly- Oj5 8 25#0 ethyleneargon lig 350 C 8,3 - - - - - - --- - - - - - - - - - - - - - - - - - - 3. TiG T'025610 poly- 10 Mg 35,7 cao styreae argon C 893 16,0 1/0 4. TIC; TiO 55 09 CaO PO!y 2 'j M 35o7 ethylene heli= J00 c 8,4 20,3 - - - - - - - - - - - - - - - - - -- TIC 5692 LILED p oly Mg '02 3595 2#9 ethylenehelium 50 c 8p3 Op5 -- - - - - - - - - - - - 6 TIC TiO 2 5192 1d g 1595 Ca 25P6 c 7 p 7 PO.Ly ia ethylene 2 p 0 argon 200.
- I! I 22187 11 Table (continued) 1 j Process temperature 9400 2000 Formula of Grain size compound range 9 10 Ti C 0,97 0,1 - 2,0 - - - - - - - - - - TIC 011.116 0,i - 2,0 TIC 0,95 0,7 - 2,0 1800 TIC 019 2 2500 22C)0 TIC 0,95 1,0 - 6,0 TiCO, 93 M-3,0 1 1 - ^v 1 C.
4; 2218711 Table (continued) 7. TiC Tio 51,2 Cao Poly- 50 2 ethylene argon Ug 15#5 20f5 Ca 25p6 3PO - - - - - - - - - - - - - - - - - - - - - - - - - - - 8. TiC TiO; 51 ' 1.1 Cao 150 1 ', g 15,5 20 2225 p 6 so nil argon 7J7 5 9. C TiO 46,96 JAgo poly P Ca 4"5 20 ethylene argon t" I ?D j 6 9 Cao io - - - - 7 - - _rl- - - - - - - 10. TiC;iiu; 4696 C---0 !"I Ga 4695 -20 6,9 POI y- 1 1 0 5C0 I000 II. Tic T'02. 54, 0!150 poly- 50 Ca 5 6, 5 20 ethyleneargon C -8.9 2 0 12. Tic TiO 2;54,6 CaO poly- styrene argon Ag 16,6 15 CdH2 2317 0 c 511 - - - - - - I - - - - - - - - - - - - - - - - - -- 13. TiC' T iO 54,6 Mgo 40 Mg I0, 0 5 nil argon CaH2 23 p 7 C_:' 0 - C 511 1510 TiC TiD 2 54 1.1 go poly- 70 C ethylene argon US 16 20,0 CaH 2 22?7 Ito C 6,1 "' 187 11 10.
Table (continued) 2'0 4V 8 9 10 2100 TiCO v 97 ORI - 2#0 TiCO 39 TiC 0 9 tS 0II - 3P0 0397 OF I 2.1 1 0 P 3C31 0 T TiCC) #96 OP.L - ppo TiC 0#92 Opi - 3PO 13. 22200 TZO 1.97 0 p!- 2 PO 2300 TiGO 995 091 - 510 t r) n 2Z. 1 8) 7 11 -I - -"2 - - 157 7i-CN- - 3 U02 59 g 5 us 36j 4P4 59 visa EZ 36pI 15 2,0 494 !c. ' iiN- 7. i j I&G c iggo CH40112 5,0 2#2 Table (continued) nitrogen 90 nitrogen 60 D TiCN TiO 2 595 40 CH 014 amonia 25 M, 1 7,0 2, 4 p 4 a 16 TiCN T 10 5 40 ammon a 30 365 1, 1 5,0 3,C c 4#4 -2 P -Q37 -n!7t30,g8n 7c7 LIS 1610 10,0 4#0 CaH 2 V 6 C 3 p 9 - - - - -- - - - - - - - - - - - - - - - - - -- - 20. TiCK TiO 52,5 -0 ON nitrogen 25 2 M6, CH4 2 bf g 16,0 8,0 410 CaH2 27,6 C 3#9 I. TiCN T'02 52,5 CaO KCZ ammonia 30 M G 16.0 JO,O 4,0 CaH 2 27,6 C 3j9 7j. -T-iC-N- - - -572,35 T '02 M 5 16#0 CaH2' 27 P6 c 3 p 9 - - - - - - - - - - - - - - CaO CH 4 0 N P ammonia 7 0 5,0 4,0 22187-11 Table (continued) 15. 2500 TiC 0,5'VO 945 0 p 1-2 9 0 2 10 0 TiCO u, I - 3 9 0 16. 4'i//0 4 2 TiCO 9 4 91V0 9 4 6 011-290 18. 1 KI 0. TiCO r 4 9 /V 0 #45 0$1-5$0 19. 1-1. 9.0 0 TiCO p 47 A10 147 0 y 1-2 70 20. IBOO T ZO $ 5A/0 #42 0 # 1-3 $0 21. 1900 T iCO AI, 0945 OgI-220 2000 M.00 9 4 9 A10 p 4 5 0 p 1-3,0 2218711 I- -- -j- 23. T'C-"1B2 - - - - - S_ TiO 2 49#7 15gI C,-. 24,8 c 317 2,0210 6r7 j, i - - _ _4_ Use 15,0 CaO B Table (continued) polye thylene argon Y- 4 o _T_iC_-T_iB_ T_iO -4-91-7 _11190 -Poly-- I00 Mg 2 15)1 15,oethy- r4 lene argon %.Ja 2LI 16 C 3t7 3PO 3 617 25. TiC-'.I'iB TO 49#7 CaO Poly- 200 2 2 4.
0,:, suy U g 15#1 1 -1 rene argon Ca 2418 C 317 4 PO e 3 617 - - - - - - - - - _,; -- - - - - - - - - - - - - - 26 TiC-LriB2 T L 2 52,7 g) poly e thy- lene argon 15)1 J, 0 Ca 24,98 3,0 C 307 3 337 27. TiC- S! C T io, 4007 Migo poly- 30 Mg 12p4 1510 e thy Ca 2014 CaO lene argon si 14p3 290 C 1212 'B. TiC-SiC iiO 40,1 mgO poly MG 2 12 P4 1510 ethy Ca 20P4 Cao lene argon si 1403 5,0 C 1212 2218711 Table (continued) -io ----- 2400 TiC-TiB 2 0 P 1-2 0 2500 TiC-TiB OPI-210 r_ P300 Tiv-TiB) OvI-5#0 2400 T IC - TiB 0,1-2#0 2 2i. 1900 TiC -SiC 011-290 28. 1900 TiC- SiC' 0 #1-390 z i 1, -2218711 2 29. T:L3-.iC Table (continued) 3 TJ'_ 4-0 97 m., 12 #4 0 Ca 20#4 14#3 1292 4 5 poly sty rene 210 mgo I0,0 CaO 2P0 argon 7 70 - - - - - - - - - - - - - - - - - - - - - - - - - - - 30. Ti 5 si 3 Tio 2 3915 MSO poly- 90 io 1717 101 0 ethy 2 lene ar.,on :"g 1912 CaO 2 f 0 Ca 213,6 10,0 - - - - - - - - - - - - - - - - - - - - - - - - - - - - 31. TiC-SUC T io 2 4017 M SO nil argon 200 1.16 12,4 2jO C a 20 P4 Cao si 14 3 20,0 C 11-2 2 - - - - - - - - - - - - - - - - - - - - - - - - - - - - _32. Ti5 Si3 iD p 39,5 0 poly- I00 w U0 1707 15,0 s "' Y_ 2 reae argon - -9 I9p2 410 Ca 23j6 - - - - - - - - - - - - - - - - - - - - - - - - - - - - 33. z vc Z102 '.5 5 # 9 Cao Poly- 50 C aH, 3807 18,0 ethy 2 leae argon C 5p4 2#0 J4. zrC Zr02 55)9 CaO poly- 70 CaH 3897 1510 sty- 2 rene argon C 514 410 --- - -- -- - --- - - - - - - - - - -- -- - 35. z xC., Zr02 55,9 mgo poly 3817 16,0 ethy C 2 lene argon C 514 4 00 2218711 Table (continued) 29 2000 TiC-SiC OpI-290 19C.0 Ti sI 0 9 1-2 PO 5- 3 31. 20UGO Tn i c - S i c OpI-2,0 32. 19 G 0 Ti 5-S'3 0 sI-3 PO 33. 1850 zrc 0 r97 0 I-m'2 30 1900 zrc 0996 0,1-2,0 35. 1900 Zr n CO #97 0 p 1-3 10 1 t 2218711 Table (continued) 7 - - - - - - - - - - - - - 36. Z.CO 5 -9- _tW - -Po-ly: 70 Zr02 5 f sty CaH 2 38?7 IOJIO rene argon C 5s4 Cao 2pO I010 17 W 0 37. Z L-ro 2 63, Ub poly- II0 ethy- 12;4 IOPO lene nitrogen CaH, 21f5 CaO 2PO C 3,0 10,0 879 3 -,1 0 PolY - - - - - - 1-50 Zr2 0 ethy Ulo- 12,4 1830 lene nitroopen CaH2 21J5 2PO C 3PO 39. Z ICN Zro 653, I 30 poly- 120 2 S.1-y M n v 19 1214 5;0 - ene ammonia ;'0 CaH, 21,5 CaO C, - 310 5,0 40. Z il-" N zro 63 1 - M90 0.T nitrogerl70 2 1 Gj'4 1' 2 U9 12#4 2090 4 p 0 CaH2 21P5 c 390 41. ZrC N 3 1 1.1 Zr02 6 J 9 go H CO I nitrogen 90 g 1294 590 2,0 CaH2 2195 CaO c 300 1090 2 4-218.7 11 - 24. - Table (continued) 2200 1900 zrc 096 0 p 1-3 90 7n rk.oo 1119 N 0 #46 OPI-210 2100 z _-c 0148 N 0 #45 OvI-2,0 )9. 1900 z reo 949 N 0947 OPI-390 1 2218711 Table (continued) I _ _2_ 42. Zi-CN 43. Zi.G-ZrB2 - - - - - Z102 mg Ca c B dO 3 M so 11 99 18,0 !9,6,9 5 p 3 4 _5_ CaO KCI is Ito.
ammonia poly ethy lene argon 2#0 - 200 44. ZrC-Z.VB2 Z10 60,3 CaO poly300 1j 2 eth,r- U 9 li,9 20,0 lene e-rgon Ca 19j6 295 C 2 p 9 - 3 513 45. Z rC- Z=B z1o to 3 CaO poly- 300 2 2 sty- Lis 1119 20,0 rene argon Cai9p6 310 C 1) -;p B:) p 3 poly- - --------------- --------- 4j. -ZrC-ZrB z ro 6 60 2 2, 003 MgO styrene argon 11 g lit 1 9 I6,o Ca 19#6 C 2 f 9 2,0 B 5#3 47. zre,,-Sic Zro 55,0 160 poly- 700 e thy 14 21,8 IO,o lene argon Si 12p5 CaO 2#0 C 10#7 IOPO A-218711 Table (continued) J 42.
1800 ZrCOY49 N 0,46 OPI-390 43. 2400 zrc-zrB 2 0,1-290 44. 2400 ZrC- ZrB2 OsI-2P0 2400 zr C - ZrB? 0.91-210 46. 2300 ZrCi;- ZrB2 0,1-210 47. 2200 zrc- sic 0,1-2,0 48. 2300 zrc- sic 0,1-2,0 4 2218711 Table (continued) - - --- - - - - - - - - - - - - - - - - - - - - - - - 2 3 4 5 6 7 _ - ilj - - - - 00 z 2 55 p poly- Z8 Z: ',:S G to jo Lis 2, 1 9 8 2090 ethy lene argon sI 12#5 300 c 10 #7 49. ZrG-SIC Zr02.1 1 0 mg 0 PO ly- I000 MS 2198 1810 sty rene argon si 1215 3P0 IJ #7 DO. ZIC-sic Zr02 5, 0 CaO poly- U9 2118 1510 sty rene argon si 12p5 500 C 10 #7 - - - - - - - - - - - - - - - - - 51 -ZxC-Sio Zr02 55 PO CaO poly - - - - - - - 1000 us 2198 101 0 sty rene argon si 12p5 mgo 4#0 c 1097 510 52. ZrB2 Zro 2 52,9 M90 Nacl 200 CaH 2 - 36,9 16,4 2 P 7 argorl B 10,2 - - - - - - - - - - - - - - - - - - - - - - - - - - - 53. ZXB2 Zro 2 52,9 CaO NaC1 180 CaH2 36,9 18,0 2 P 0 argon.
B IOp2 54. ZrB ZZO 52#9 CaO Poly- 200 2 2 ethy CaH 2 36P9 I010 lene argon B 10,2 11go 2,0 IOPO 2218711 Table (continued) 2200 f? -..rC-Sic ORI-3P0 2100 091-5JO 51. 2200 z 4-1,2 - S i c 0,1-3,0 1650 L-B - ---0 2. 3 U J.
isoo Z.rB p 0,1-315 117 54. 1850, rB 2 OsI-3s5 2218711 29 Table (continued.) 55. ZrS'2 Zr02 30p8 CaO Poly- I00 L, I -H 2 3991 817 styrene argon S'02 30'1 4,3 T - 72,rSi2 Zr02 30,8 CaO poly 1.1, n-H 3911 5#0 ethy1, 2 lene arvon -.0 S'02 I I 1jgCY 210 57. ZrS12 Z ro 2 3018 Ugo NaCI 50 Mg:'2 3911 ISO 5,0 arc-on CD S'02 3011 - - - - - - - - - - - - - 58. ZrSi 17 30,8 CaO UaCl 90 2 r02 M iigH 2 39,1 15,0 4,0 argon 02 3011 59. CaB6 CaO 12,0 go Doly- 50 hi 56,5 12,6 ethy lene argon B203 31,5 IP7 CaO 12 0 11 E;O poly- 40 0 Ca36 p styrene argon Mg 56,5 15,0 B 2 0 3 31,5 215 61. CaB 6 CaO IIVO MgO poly- 50 ethy mg 47 P4 5#0 lene argon B203 4jt6 CaO 2 f 0 5PO 62. LaB 6 LaCl 3 65fO MgO poly B 16,0 8,7 styreneargon 50 Ca 1910 4.03 2218711 - 30 Table (continued) 2100 ZI --S i 1 1,0-390 1? 2200 - r73 170C.
2 c:a 3 ' 0 0 P 1-2 PO - - - - - - -- 0 p 1-2,0 0 9 1-2 #0 P50 - CaB 0 0,1-390 D 50 Lad 6 OfflI-2to 1700 L e-B 6 0 p 1-2,0 1 2218711 - 31 1 Table (continued) 4- -6- 63. LaB6 LJ(ICE 65jO Ugo Poly- 40 B 16,0 15 0 e thy lene argon Ca 1910 490 64. La36 La C1 3 65,0 Cj 0 poly- 50 e thy- B 16,0 12,0 leae argon Ca 1900 3;0 65. LaB La.'13 6510 Cao poly- 70 6 B 1610 5 F 0 sty- rexie argon Ca 19,0 0 210 I010 0 7504 mgo poly- 90 Go, TaC Ta 2 5 ethy 1.1 g 20,6 12,0 lene argon C 4 f 0;) PO 67. TaC Ta20 5 -75,4 CaO poly- 70 Mg 20,6 15,0 ethy lene C 410 215 68. TaC Ta205 75,4 CaO PolyI00 , J.
lig 20,6 5,0 S UY rene argon 400 MCIO 1,5 0 10,5 79 & _aC7 - - - Ta5 '(5,4- -C7aO- - _pO_1Y- I00 11 g 20,6 14,0 sty- reneargon C 410 2,5 70. Ta132 Ta20 5 43,0 Ago Ca 43 0 8 7 B203 14: 0 70- 4 #3 argon 2218711 Table (continued) 9 10 64. 1-150 '-'B 6 0 pI-2PO I,aB r, 0 p 1-2 90 656.
2000 TaC ORI-290 07. i900 TaC 0 t 1-2,0 68. 2000 TaC 0 1 1-2 PO 69. 1900 TaC OPI-255 70. 2200 TaB2 0 t 1-2 #0 p 9218711 Table (continued) 3_ -4 - - - 5 71. Taj32 TapO 43JO Iro 111a Cl - 5 Q Ca 43P0 14,0 4,0 B 2 0 3 1490 argon 72. TaC-TaB2 Ta 50 205 9,0 '0 1,017 9 sty B203 P7 IIP5 rene argon C 213 200 i990 - - T - - T - - - T - - - - - - - I - 73. aC_TaB Ta,:,o r-9,0 M 0 poly- 2 5 9p7 5jO sty B203 rene argon C 2?3 Cao 3$0 Mg 1900 10,0 7 - - - - - - - - - - - - - - - - - - - - - - - - - - (4. ',,aC-'a3p poly18205 69,0 90 e thy B203 917 15,0 1 ene argon C 2 p 3 4,0 11 t? 1 w 1900 - - - - - - - - - - - - - - - - - - - - - - 7.5. TaC-TaB Ta205 74,0 CaO poly- 40 2 B 0 ii,e 15,5 e thy-.
P 3 lene argon c 90 395 rp m b.> 12P2 76. Ta-C',11- Ta-0- - 67-5- _CaO_ KCI 70 2 5 '10 nitro- Ca, 7 15,0- 3,0 gen C 1,8 - - - - - - - - - - - - - - - 17. TaCN Ta20 5 67 P5 Cao Ca 3097 5,0 c 1,8 11 go 5#0 CH 0 11 nitro- 50 4 p 300 gen 2218711 Table (continued) 2000 TP-B2 OpI-390 ri - I- 1900 laC-TaB2 0, L 310 m _m I _ 0 a B OpI-2,0 K -1 1 74. 1600 LaC-'LaB2 Piti-lto 5. 1800 Ta0-,TaB2 07 I-2j 0 (6.
17 0 2000 TaCO 46 N 0346 011-290 1900 TaCO 949N 0,46 OPI-230 2278711 78. TaCIT- a'205 Ca Table (continued) 67 #5 mgo C"'40112 3097 15P0 290 1,8 z---7 ammonia 50 0 6 1 5 CaO M1 hyclra- 70 7 9. TaCI.1 Ta2 5 ' 1 zine Ca 3037 14,0 2,5 T 8 M 60. TaCII L a 205 E 7 p 5 1. L_. 0 H01 hydra- 50 Ca 30 #7 1670 1 & 5 zine c 1,6 (p 62,8 Me 90 &P05 go poly C alq 1179 15, 0 ?thy 2 lene argon 1 (-? _;J, l#5 3 p 0 S i 6 YO 0 038 82.TaC-SiC Ta2Q5 621t8 CaO poly CaE 11$9 18,0 ethy- lene argon m:g 10,5 2 p 0 S i 870 c 638 8 3. TaC-Sic Ta20 62,8 CaO poly- 80 C aH 5 1119 1500 sty 2 rene argon U g 1015 310 s i 6,0 C 6,8 2218711 -36, - Table (continued) -io - - - - I.T 78 1800 TaCO 4 9 4 0 P46 0,1-2,5 IT 79. 1900 Ta Co 94 9 ' 0947 0 01-2 #5 rn ' 11 i600 Laki U Y4C 0,47 OvI-2P0 81. 1 G 0 TaC-SiC 0 p I - 2, 5 62. 2050 Ta(w-sic 0j-3P0 20. 5 0 TaC-Si C OPI-390 2218711 Table (continued) 84. TaC-Sic Ta;,O 62 PS M r-,. 0 poly- 70 IT styrene argon CaH2 1,9 15jO U3. 1015 2PO Si 6PO C 608 E35. "'10E"'2!A 00 3 31 3 F 3 Mgo poly- 90 Si 0 27 #7 19 e thy lene argoa 3910 318 8 6..7.-, o s i 1AO0 33,3 "go Poly- 80 2 3 0 - Si 0) 27,7 1810 s lkyrene ax g o n 3910 1,0 67. 'Icsi,, M 0 0 3 333 3 CaO poly- 70 Sio 27 f1l 7 15;0 e thy 2 lene ar Ir 0.11 C, 11 39, 0 510 7 - - - - - - - - - - - - - - - - - - - - - - - 68..1josi)f 3313 CaO poly 2 003 0 styrene arcron S'-02 27 # 7 181 Mg 3910 3)0 - - - - - - - - - - - - - - - - - - - - - - - - - - - - I C 0 44f5 CaO poly- 60 890 "r3 2 Cr2 3 styrene argon Ca 5018 16,3 C 417 294 f-I 0 90. Cr3G2 Cr 203 44 t5 11go Poly- Ca 50,8 15,0 styrene argon C 4#7 295 91. Cr 3 C 2 Cr2 03 44,5 mgC poly- 80 e thy Ca 5018 590 lene argon C 417 Cao 2PO I010 218711 2- Table (continued) 2000 TaC-Si C 0 9 1-2 PO 85..7 OD 110 Ci L$. ' 2 0 p 1-2 PO KOO 1 0si p 0j-2,0 87. - 2000 M03i9 0 P IL-2,5 8-8. 2000 110sip 0,1-2,0 I" 89. 2000 Cr,C 2 0 I-2tO 90. 2000 Cr 3 C 2 OsI-2 0 91. 1900 Cr3 C2 0 p 1-2 #5 D 221; 8711 I 92. Ce 3C2 3 203 44 5 Lto Ca 50 8 15tO c 4P7 Table (continued) 4 6 poly ethy lene -argon 3pO 71n-C-1 - -57-2- -'.(g-o- _Ra-C-1 2 9 ME 27,0 5,0 30 3203 15,8 - - - 7 - - - argon W - - - - - - 57-, J -daO- ja31 - - - - - - M'n CI2 m.7 27,0 15,0 4,0 argon B 2 0 3 15,6 9:). ld2 La2 65,8 CaO 60 03 ethy Ca 2415 1090 leae arson G 997 5,0 6 _I7a 0 65,13 CaD poly (2 18 3 Ca 24p5 15,a styrene argon C 9#7 4#0 7_ '!jC2_ Ta20_3 _65-,87 -h(-go- _Po1y-- 60 Ca 24,5 1500 ethy lene, argon - C 9#7 3,,0 8 72j)- 70 Lac 2 p C& 24 P.5 I0,0 styrene argon C 9,7 CaO 300 5,0 W2C 7#0 3 7I-,o- 7B_aO_ - _PO_1Y --- - - - - 90 VgH 25,0 19.2 ethy- 2 lene argon C 4,0 308 1 I - IOU.- i-C -Vju- - TITO- 711-go' -P31F -- - - - MtH2 25,0 1500 styrene argon C 4#0 3,0 - - - - - - - - - - - za_ - - - - -- - - - - - t i f 2218711 Table (continued) 92. 19001 er 3 C 2 0j-2.0 93. 1900 btnB 0,1-2,0 94. 1600 WB 0,1-2,0 95. ISOO La C2 OpI-290 96. 1750 La C 2 0,1-2,5 97. 1600 L aC2 OsI-2,0 98. 1800 LaC2 ORI-2y5 99. 2000 W2C I 5 100. 1900 ---------------- W 2G I - 3 a I0J. w 2 c wo 3 1. 1 E...d 2 c 4 71,0 CaO 2590 1690 4,0 2 4-218711 Table (continued) polyethylene 4PO argon 102. C WC16 c'B, 9 CaO Poly- 70 2 Z n 2 0 p 9 io to ethy- argon lene Al 910 3FO C 112 - - - - - - - - - - - - - - - - - - - - - - - - - - - - 103. q C wC1 C& 9 ".1 go poly- 60 2 7-11 6 20 P9 1510 ethy lene argon A.e 900 4#0 C 112 - -8 - pc7ly7:
104. _,.",_C C C 19 11.1 go.1. 6 0 2 0 S 6y_ r7n 0 rene argon Z 2099 18 0 -A! 9 0 /9 C I ? 105. "'1 C Vicl 68,9 CaO poly- 50 2 '7 n sty- :j 2019 1610 rene argon A 1 910 2,u C 02 106. 1102 C 1100 53P4 1.1 Cp poly- 5 3 ethy Mg 1811 17,5 lene, a r,--,, o n 17 Li n 2401 210 C 414 - - - - - - - - - - - - - - - - - - - - - - - - - - U00 5314 CaO poly- 5 07 M02C 3 sty Mg 18,1 10,0 rene argon Zn 24#1 U go 115 C.404 5;0 2218711 Table (continued) I0I. IS 50 V1 2 c 0,1-2,0 102. 1950;/ 2 c 0 #1-4 PO 103. 1600 C 011-490 "r..f c 0 P 1-4 &0 104..1800 bg 2 105. 17 50 w 1-4 0 1 2C 0 0 b C6. 2000 110,c 0)1-295 107. 1900 mopc 0 V 1 -2 p 5 2218711 I 108._ 102C 14 003 11g c 53P4 17 ,n 2491 474 Table (continued) CaO poly18)0 ethylene 2 p 5 argon 7_ I0 Poly- 109. IIJOB2 it.003 3012 h1g, 0.1. 10 17 VI 41 2 15,0 sbyrene argon lu 15j3 2 F 5 ZD B203 13,3 - - - - - - - - - - - - - - - - - - - - - - - - - - - 110. MOB MOO 30P2 0 Poly- 15 2 17 3 ethy , n 4 1 f 2 18 YO lene argon Li 15p3 2#0 32 0 3 13,3 - - - - - - - - - - - - - - - - - - - - - - - -- I.1. "VI 0 13 4003 3032 Cao)oly-!5 17 41 2 18 0 styreneargon Zn I f mg 1513 2,0 B2 0 3 1313 - - - - - - - - - - - - - - 112. M032 moo 3 3092 41 92 1513 13P3 4,9 4 1 p 0 491 11g B203 113. Pe4C F. e 203 Ca c CaO PolyI000 e -Iijhy - lene argon Ugo 2,0 I000 ) Ii: - M L? 0 PO 12#5 styrene argon 432 114. Fe C 0 5499 Ugo poly- 15 4 p' 2 3 ethy- Ca 4110 1800 lene argon C 4 p 1 212 2218711 108. 1950 - - -9MOPC Table (continued) 0,1-2,0 109. 2100 1.1 c B 5 0.9 1,3P0 1, LIO. 2100 lloB2 OlI-3,0 111. 2000 111o32 OrI-3,5 112. 1900 110B2 0 # I - 2 p 0 113. 1900 Fe4 c 091-290 114. 1900 Fe4 c 0$1-290 2 2187 11 Z ---45- Table (contiaued) 115. Fe4C 11 e 203 54#9 ugo poly- 20 Ca 41PO 5,0 ethy lene argon c 4,1 CaO 1,5 I010 3,3 M90 A6 Poly- 50 ug 2I$q I-1,0 e thy B 86argon 117. NiB NiO 68,3 go Poly- 30 ethy U g 2119 IOR 0 lene argon B 9,8 2,0 ----------------------------- 116. NiB NO 63;3 CaO poly- 50 sty- Ug 21,9 15#0 rene axgon B 9'a 3#0 119. CoB2 C,00 24#5 Ca 52,5 B203 23P0 mg() polyethy16v3 lene argoix 2#4 120. CoB coo 24,5 ugo - poly- 50 2 sty Ca 52p5 16f5 rene argon %0 23,0 2.5 121. G032 coo ca. B203 ugo polyethy5,0 lene CaO 15#0 U5 -TIO 2 62,9 -Ugo CH40 30 119 3791 808 2,7 Ammonia j2-,9_ -ijO 11 60 2 m g 37,1 15,0 3,0 nitrogen W a 2218711 115. 1950 "4 c 0,1-2,0 0 116. 2200 NIB 0,1-2,5 117. 2100 NiB 0,1-2,0 118. 2200 Nis OpI-3,0 119. 2100 C032 OvI-295 120. 2100 C032 0,1-2,5 121. 2000 -- COB2 0 1-2,0 - - - - - - - - -- - - - - 7 - - - -- - - - - - - - 122. 1650 Tivo,93 0,1-2,0 1 A p 221817 11 1 2 3 124. TiN Table (continued) 2'02 Mg 4 5 6 7 6299 CaO CI - - - - - - 90- 37PI ISPO 390 nitrogen 125. Z ril 0 fIto VC, 29 m - o 12,9 - - - - - - - - - - - - - - - - 126. ZrN -r02 1190 P9 0 - - - - - - - CaO Kcl hydra- 70 zine 1,2 !Igo CH 4 Oil 2 armraonia 1880 2PO - - - 127. Z rlj' r02 0 Mgo KCI nitroven 70 Mg 29#0 1510 1 p 5 Q 128. Nb2ll 1, b;)O 5 46 #0 CaO Na:140 3 nitrogen I000 Ca 5410 10 3PO 129.. 'ITb., ' b 46,0 mgo::a1TO 700 211 20 5 3 Ca 5430 15PO^ 5pO =0 1 0 130. Tal Ta2 5 73 1 0 0 Mgo Kcl 80 i.gH 2 13,0 1030 1 95 ammonia CaH 2 10 to CaO 590 131. TaN Ta2 0 5 7790 m gO Pal'C'3 I00 ': -"H 2 1380 5#0 490 nitrogen CaH 2 10,0 132. TalT Ta20 5 77PO Cao C ' H40."12 Lig H 2 1390 20 DO 2 p 0 nitrogen Ca.H 2 IOPO Z4-6- -daO- Wj - - - o 4 12 I3. A111 Al 3 9 4 hydra 1 zine CaH2 5594 10,0 3,7 2 Table (continued) 1 6 9 10 124. 2100 TiN 0995 0 p 1 -2 p 5 Z? IT 125. 2050 10 996 OpI-2,0 T 126. 1980 - 10 090 OvI-2,5 127. 2000 i 0,95 OpI-2#5 rPB, L - 2000 ',:bg'.-1 0,1-2,0 129. 2100:N b 11 0j-270 2.
MaN 130. 2000 L 0 # 1 -2 p 5 131. 2100 Tall ORI-390 132. 2200 Talz 0,1-2,5 133. 2000 A IN 2.2_ 18 7 11 Table (continued) Y - - - - - - - - T - - - -4- - - - 3 - -6- - - -7- T3.- 115 A1203 4416 Ugo NaN03 nitro- 100- CaH2 5514 15sO 2,0 gen - - - - - - - - - - - - - - - - - - - - - -- 135. AlN A12 0 3 4416 CaO CH40"T2 nitro- Ieo CaH 2 5504 Ioto 2,0 gen.
11go.
5fO 136. UB B203 55#0 Ugo nil nitro- 200 gen mg 45so To,o j.
710 137. L'2C L'2 co 3 C5,0 Ugo nil argon to 590 590 - - - - - - - - - - - - - - - - - - - - - J38 Ti-Ni TJ 0 2 26,5 CaO nil argon 20 no Ca Zn c 139. Pe-Cr Pe 2 0 3 Cr 2 0 3 1Ag CaH2 c 35,5 24 #0 26#5 21j45 0305 35p7 33,6 18,0 2114 992 ori Ugo nil argon 30 n r z.21 87 11 -50 Table (c ontinued) I31f. 2100 ADI 0 P 1-2#5 135. 2200 A ril 0 #1-290 136. 2200 NB 0,1-5,0 137. IC-00 Li 2 c 0 9 1-3 y 0 136. 16000 Ti -ITi - 210-5,0 139. 1500 Pe - Cr 390-590 t 2218711 I - 2 14. Pe-Co 3 Pe2035,79 4 L1g 0 -Coo 68,10 22,0 21 80 C.P 4 922 c 0709 Table (continued) nil 6 7 n-it-ro--- Oen 141. v'f'_R e -,-,o 7205 MTO poly- I n3 ethy 0 25pO 59 lene argon U 31 2204 1 to C ovi 142. Zr-W 0 U g-0 nil a=-on - r? 4 47 p 5 5 "' 'i n.1 0 11 k, 36 p 5 10 9 AI 15tO CaO ,'o 3 Il45 15#0 c 0,05 143. Mlo-Cu Ca20 3590 nil argon 095 !A0C12 4510 2590 mg 19P8 0 0 p 2 221 '87 11 Table (continued) 1 8 9 10 - - - - - - - - - - - - - - - - 140. IaliGO Pe - CO 1,0-3,0 n 141. 1 1.5 8 0 d _Plc 1'0-3,0 142. 1700 110-210 1 143. 1500.'10 Cu 230-590 -11 1 x k 2218711 Table (continued) 144 M9Y6 B203 46,7 1 15 m& 53,3 to its TiC -MoC MO 8 8 Cao 200 T102 U95 121,0 W9 3397 2 146 wC.TaG Ta 2695 CaO 30 Mg 15 9 0 c 4,0 Table (continued) 1 8 9 10 1414 1800 M9B6 01-20 1950 TiC.MoC o,i-290 146 2050 niC-TaG 1,0-2,5 1 54

Claims (14)

  1. 2' 187 11 Z_ 1. A process for producing powdery refractory inorganic compounds'and metal compositions comprising:
    - preparation of a charge consisting of - a mixture of 12.0 to 80.95% by mass of at least one substance selected from the group consisting of elements of Groups I to VIII of the Periodic Table; 0.05 to 31.5% by mass of at least one substance selected from the group consisting of nitrogen, carbon, boron, silicon, sulphur. phosphorus. and oxides, halides and organic compounds thereof: 19.0 to 56.5% by mass of at least one substance selected from the group consisting of metals of Groups I to III of the Periodic Table, and their hydrides; - and additives in an amount of from 1 to 25% by mass of said mixture consisting of at least one compound selected from the group consisting of oxides of metals of Group II of the Periodic Table, halides of alkali metals, ammonium halide, polystyrene, polyethylene and urea., - introduction of the prepared mixture into the reaction zone, - ignition of said mixture in said reaction zone for carrying out, in said reaction zone, a self-propagating high-temperature synthesis of the desired product; - treatment of the desired product resulting from said synthesis with a solution of mineral acid for purification of the desired product.
  2. 2. A process according to Claim 1, wherein the charge contains, as the additives, 5-25% by mass of said mixture of oxides of metals of Group II of the Periodic Table, and/or 1-5% by mass of said mixture compound selected from the group consisting of halides of alkali metals, ammonium halide, polystyrene, polyethylene and urea.
    C i 1 i f 1
  3. 3. A process according to Claim 1 or 2, wherein a charge is used which consists substantially of a mixture of 56.0% by mass of titanium dioxide, 8.3% by mass of carbon. 35.7% by mass of magnesium and additives magnesium oxide in the amount of 10.0% by mass of said mixture and polystyrene in the amount of 3.0% by mass o f said mixture and the treatment of the desired product is effected by means of a solution of hydrochloric acid.
  4. 4. A process according to claim 1 or 2. wherein a charge is used consisting of a mixture of 26.50% by mass of titanium dioxide. 25.50% by mass of nickel oxide. 26.5% by mass of calcium. 21.45% by mass of zinc. 0. 05% by mass of carbon black and additives - calcium oxide in the amount of 24.0% by mass of said mixture and the treatment of the desired product is effected by means of a solution of sulphuric acid.
  5. 5. A process according to any preceding claim. essentially as disclosed in the Specification and set forth in the Examples.
  6. 6. An ingnitable charge comprising:
    a) at least one element, oxide and/or halide of Groups I-VIII of the Periodic Table, and/or b) at least one hydride or element of Groups I-III, and c) nitrogen, carbon, boron, silicon, sulp'hur, and/or phosphorus and/or an oxide, halide, and/or organic compound of any of these elements d)-i) an oxide of a Group II metal, and/or ii) a halide of an alkali metal, ammonium halide, polystyrene, polyethylene, and/or urea.
  7. 7. A charge according to claim 6 wherein component a) comprises: a powder of elemental titanium with a powder of elemental tungsten; a powder of elemental tungsten 56 with tungsten oxide and tungsten chloride; a powder of elemental titanium with elemental tungsten and tungsten chloride; or titanium oxide with tungsten oxide in a _ratio between 0 and 1, component b) comprises: a powder of metallic magnesium; a mixture of a powder of metallic calcium with calcium hydride in any ratio; a mixture of metallic powders of lithium. calcium. and aluminium in any ratio; or a mixture of metallic powders of lithium. aluminium and magnesium hydride in any ratio. and/or component c) comprises: nitrogen; nitrogen and carbon; carbon and boron; carbon and boron oxide; boron chloride and polyethylene; or silicon with silicon oxide and silicon chloride.
  8. 8. A charge according to claim 6 or 7 wherein components a, b and c are present in a ratio of 12.00-80.95: 19.0-56.5: 0.05-31.50 provided that the total is equal to 100, component d being present in a ratio of 1-25% of the mixture of a, b and c.
  9. 9. A charge according to any of claims 6-8 comprising 5-25% of component d i).
  10. 10. A charge according to any of claims 6-9 comprising 1-5% of component d ii).
  11. 11. A charge substantially as described herein with particular reference to the Examples.
  12. 12. A process for producing powdered refractory materials comprising combustion of a charge according to any of claims 6-11.
  13. 13. A process according to claim 12 wherein the product is leached with a mineral acid.
  14. 14. The product of the process of claim 12 or 13.
    Published 1989 at The Patent Office. State House, 66'71 High HOIL-orn. Londor- WC 1R 4TP n--Lher copies maybe obtained from The Patent Oface. Sales Branch, St Mary Cray, Orpington, Kent BR5 3RD. Printed by Multiplex techniciues ltd, St Mary Cray, Kent, Con. 1187 1
GB8906445A 1988-03-22 1989-03-21 Process for producing powdered inorganic compounds and metal compositions. Expired - Lifetime GB2218711B (en)

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Cited By (4)

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US5932505A (en) * 1996-11-04 1999-08-03 Rutgers, The State University Hydrofluoric acid resistant ceramic mortar
RU2525174C1 (en) * 2013-02-18 2014-08-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государстенный университет" Method of producing metal sulphide
EP3181274A4 (en) * 2014-08-13 2018-04-18 Nano Tech Co. Ltd. Method for producing titanium carbonitride powder
RU2697140C1 (en) * 2018-11-29 2019-08-12 Федеральное государственное бюджетное учреждение науки Институт структурной макрокинетики и проблем материаловедения им. А.Г. Мержанова Российской академии наук Method of producing powder based on refractory compounds

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US7794580B2 (en) * 2004-04-21 2010-09-14 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
JP5220353B2 (en) * 2007-04-12 2013-06-26 独立行政法人科学技術振興機構 Self-propagating high-temperature synthesis method
CN109775674A (en) * 2019-04-02 2019-05-21 青岛瓷兴新材料有限公司 A kind of silicon nitride magnesium raw powder's production technology
CN113185300A (en) * 2021-05-24 2021-07-30 兰州理工大学 Macro-particle-size-controllable ZrB2Method for preparing powder

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US3726643A (en) * 1970-04-09 1973-04-10 I Khim Fiz Akademii Nauk Method of producing refractory carbides,borides,silicides,sulfides,and nitrides of metals of groups iv,v,and vi of the periodic system
US4058592A (en) * 1976-06-30 1977-11-15 Union Carbide Corporation Preparation of sub-micron metal oxide powders from chloride-containing compounds
US4431448A (en) * 1980-02-20 1984-02-14 Merzhanov Alexandr G Tungsten-free hard alloy and process for producing same
WO1988004649A1 (en) * 1986-12-16 1988-06-30 Kennametal Inc. Macrocrystalline tungsten monocarbide powder and process for producing

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SU617485A1 (en) * 1975-06-26 1978-07-30 Отделение Ордена Ленина Институт Химической Физик Ан Ссср Method of obtaining refractory inorganic materials
JPS5226400A (en) * 1975-08-26 1977-02-26 Nippon Shinkinzoku Kk Process for recovering valuable metals from metallic scraps as simple carbide or as solid solution
JPS5627441A (en) * 1979-08-14 1981-03-17 Matsushita Electric Ind Co Ltd Printer unit
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US3726643A (en) * 1970-04-09 1973-04-10 I Khim Fiz Akademii Nauk Method of producing refractory carbides,borides,silicides,sulfides,and nitrides of metals of groups iv,v,and vi of the periodic system
US4058592A (en) * 1976-06-30 1977-11-15 Union Carbide Corporation Preparation of sub-micron metal oxide powders from chloride-containing compounds
US4431448A (en) * 1980-02-20 1984-02-14 Merzhanov Alexandr G Tungsten-free hard alloy and process for producing same
WO1988004649A1 (en) * 1986-12-16 1988-06-30 Kennametal Inc. Macrocrystalline tungsten monocarbide powder and process for producing

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5932505A (en) * 1996-11-04 1999-08-03 Rutgers, The State University Hydrofluoric acid resistant ceramic mortar
RU2525174C1 (en) * 2013-02-18 2014-08-10 Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Алтайский государстенный университет" Method of producing metal sulphide
EP3181274A4 (en) * 2014-08-13 2018-04-18 Nano Tech Co. Ltd. Method for producing titanium carbonitride powder
RU2697140C1 (en) * 2018-11-29 2019-08-12 Федеральное государственное бюджетное учреждение науки Институт структурной макрокинетики и проблем материаловедения им. А.Г. Мержанова Российской академии наук Method of producing powder based on refractory compounds

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IT8941550A0 (en) 1989-03-16
GB2218711B (en) 1992-02-26
HUT53842A (en) 1990-12-28
CS176289A2 (en) 1990-10-12
DD283654A5 (en) 1990-10-17
SE8900918L (en) 1989-09-23
FR2629078A1 (en) 1989-09-29
CH679854A5 (en) 1992-04-30
JPH01278403A (en) 1989-11-08
CS274771B2 (en) 1991-10-15
DE3908715A1 (en) 1989-10-05
YU56289A (en) 1990-12-31
IT1233763B (en) 1992-04-14
NL8900695A (en) 1989-10-16
GB8906445D0 (en) 1989-05-04
ATA62189A (en) 1992-01-15
CN1041554A (en) 1990-04-25
SE8900918D0 (en) 1989-03-15

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