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    Co-polymeric boro-silazane(s) prodn. useful for prodn. of ceramics - by reacting mixts. of tris-di:chloro silyl-ethyl-borane(s) and di- or tri-chloro silane(s) with ammonia, for coating steel
    2.
    发明专利
    Co-polymeric boro-silazane(s) prodn. useful for prodn. of ceramics - by reacting mixts. of tris-di:chloro silyl-ethyl-borane(s) and di- or tri-chloro silane(s) with ammonia, for coating steel 未知

    公开(公告)号：DE4320784A1

    公开(公告)日：1994-01-05

    申请号：DE4320784

    申请日：1993-06-23

    Applicant: HOECHST AG

    Inventor： RIEDEL RALF DR ,  KIENZLE ANDREAS DIPL CHEM ,  PETZOW GUENTER PROF DR ,  BRUECK MARTIN DIPL ING ,  VAAHS TILO DR

    IPC: C04B35/571 ,  C04B35/589 ,  C08G77/60 ,  C08G77/62 ,  D01F6/78 ,  D01F9/10 ,  C04B35/58

    Abstract: The prodn. of copolymeric boro-silazanes (II) comprises reacting a mixt. of tris-silyl-borane(s) of formula B-(CH2H4-SiCl2X)3 (I) and chlorosilane(s) of formula R1SiCl3 or R2R3SiCl2 with ammonia; -C2H4- = -CH2-CH3- or -CHMe-; X = Cl or 1-4C aliphatic residue; and R1-R3 = H or 1-4C aliphatic residue. Also new are boro-silazane copolymers of formula (II), obtd. by the above prodn. R = 1-4C aliphatic residue; and a + b + c + d = 1. The amt. of ammonia used is pref. sufficient to saturate all the Si-Cl gps. and bind the obtd. HCl as NH4Cl, and cpd. (I) and the chlorosilane are reacted as a soln. in organic solvent. The reactants are mixed at -10 to +10 deg. C and the mixt. is heated to 10-100 deg. C. (I) are prepd., e.g. by reaction of corresp. vinyl silanes of formula CH2=CH-SiCl2X with BH3-THF as described in J. Organomet. Chem. 34 (1972) C0 and 135 (1977) 249, and in Zhur. Obshchei. Khim. 30 (1960) 3615. Pref. solvents are, e.g. cyclohexane, toluene, THF etc. USE/ADVANTAGE - (II) are new B-contg. polyislazanes, useful for the prodn. of B- and Si-contg. ceramics with improved adhesion, hardness and surface quality, which are useful for coating steel etc., esp. for the surface coating of machine components which are mechanically and chemically stressed. (II) may also be shaped before pyrolysis, e.g. to form ceramic fibres which are useful for reinforcement of Al (alloys) and ceramic components. The prodn. of ceramic materials comprises pyrolysis of (II) at 500-2000 deg. C under nitrogen or argon (for materials contg. Si, B, C and N) or in an ammonia-contg. atmos. (for materials contg. Si, B and N). Also new are ceramic materials as above, produced by the prodn.

    Boron-contg. poly:carbo:siloxane(s), useful for prodn. of ceramics - by reacting tris-chloro:silyl:ethyl-borane(s) with diol(s) in presence of organic base
    3.
    发明专利
    Boron-contg. poly:carbo:siloxane(s), useful for prodn. of ceramics - by reacting tris-chloro:silyl:ethyl-borane(s) with diol(s) in presence of organic base 未知

    公开(公告)号：DE4320787A1

    公开(公告)日：1994-01-05

    申请号：DE4320787

    申请日：1993-06-23

    Applicant: HOECHST AG

    Inventor： RIEDEL RALF DR ,  KIENZLE ANDREAS DIPL CHEM ,  PETZOW GUENTER PROF DR ,  BRUECK MARTIN DIPL ING ,  VAAHS TILO DR

    IPC: C04B35/571 ,  C08G77/56 ,  C08G77/60 ,  D01F6/78 ,  D01F9/10 ,  C04B35/58

    Abstract: B-contg. polycarbosiloxanes (II) are produced by reacting tris-silyl-borane(s) of formula B(-C2H4-SiCl2X)3 (I) with diols of formula HO-R'-OH in presence of organic base. In (I), gp. -C2H4 is -CH2-CH2- or -CHMe-; X is Cl or 1-4C aliphatic residue; R' is 2-4C alkphatic residue. In (II), R is 1-4C aliphatic residue; and a + b is 1. At least equimolar amts. of diol are used, and cpd. (I) is reacted as a soln. in organic solvent; the reactants are mixed at -10 to +10 deg. C and the mixt. heated at 10-200 deg. C. Pref. (I) are prepd., e.g. by reaction of corresp. vinylsilanes of formula CH2=CH-SiCl2X with BH3.THF as described in J. Organomet. Chem. 34 (1972) C9 and 135 (1977) 249, and in Zhur. Obshchei. Khim. 30 (1960) 3615. Pref. diol is ethane-1,2-diol, propane-1,3-diol or butane-1,4-diol. Suitable solvents are e.g. hexane, toluene, THF etc., and the base is, e.g. Et3N, pyridine etc. USE/ADVANTAGE - (II) are new B-contg. polycarbosiloxanes, useful for the prodn. of B- and Si-contg. ceramics with good adhesion, hardness and surface quality, which are useful for coating steel, etc. esp. for the surface coating of machine components which are subjected to mechanical and chemical stress. (II) can also be shaped before pyrolysis, e.g. to give ceramic fibres which are useful for reinforcement of Al, Al alloys and ceramic components. In an example, tris-((dichloromethylsilyl)ethyl)-borane (I) are prepd. by reacting 216g dichloomethylvinylsilane in 255 ml toluene with 255 ml 2M soln. of BH3.SMe2 in toluene, followed by evapn. of solvent to give 233g (I). Mixt. of 12.55g (I), 13.7g pyridine and 50 ml THF was treted at 01-0 deg. C with a mixt. of 10 ml THF and 5.5g ethylene glycol, then stirred for 2 hrs. at 30 deg. C and worked up by filtration and evapn. to give 7.8g (II). Soln. of (II) in THF was spun and drawn off at 200 m/min. to give fibres of dia. 20-30 microns. Fibres were dried at 50-60 deg. C in argon and then pyrolysed in argon by heating to 1100 deg. C at 1.5 deg./min. and maintaining this temp. for a further 1 hr. Ceramic yield was 54 wt.%. Prod. had fibre dia., 10-25 microns; tensile strength, 1 GPa; EDX and X-ray diffraction analysis indicated an amorphous material with a homogeneous distribution of Si, C, B and O.

    6.
    发明专利
    未知

    公开(公告)号：DE3909978A1

    公开(公告)日：1990-09-27

    申请号：DE3909978

    申请日：1989-03-25

    Applicant: HOECHST AG

    Inventor： PEUCKERT MARCELLUS DR ,  VAAHS TILO DR ,  BRUECK MARTIN ,  KLEINER HANSS-JERG DR ,  RIEDEL RALF DR ,  SEHER MARTIN ,  PETZOW GUENTHER PROF DR

    IPC: C01B21/068 ,  C04B35/58 ,  C04B35/589 ,  C04B35/626

    Abstract: The invention relates to a novel sinterable ceramic powder, to its preparation and to its further processing to give a silicon nitride ceramic, and to this material itself and its use. The sinterable ceramic powder is produced by melting a polysilazane or dissolving it in an organic solvent, suspending a powdered sinter aid in this melt or solution, then pyrolyzing the melt, or the residue obtained after evaporation of the solvent, at 500 DEG to 1600 DEG C. in a protective gas atmosphere, the polysilazane either A) being obtainable by reacting at least one of the oligosilazanes of the formula (I) +TR in which a, b, c and d are the mole fractions of the respective structural units and where 0 in which R and R* can be identical or different and R and R* are C1-C4-alkyl, vinyl or phenyl and R' is C1-C4-alkyl and x and y are the mole fractions of the two structural units, where x+y=1 and x=0.7-0.95. A molded article can be formed from the ceramic powder thus obtained and a silicon nitride ceramic then produced by sintering. However, a molded article can also be formed from the solidified melt or the still unpyrolyzed residue obtained after evaporating the solvent and this article can then by pyrolyzed and sintered. Components subject to severe mechanical, thermal and corrosive stress can be produced from the ceramic obtained.

    8.
    发明专利
    未知

    公开(公告)号：DE59009828D1

    公开(公告)日：1995-12-07

    申请号：DE59009828

    申请日：1990-03-22

    Applicant: HOECHST AG

    Inventor： PEUCKERT MARCELLUS DR ,  VAAHS TILO DR ,  BRUECK MARTIN ,  KLEINER HANS-JERG DR ,  RIEDEL RALF DR ,  SEHER MARTIN ,  PETZOW GUENTER PROF DR

    IPC: C01B21/068 ,  C04B35/58 ,  C04B35/589 ,  C04B35/626

    Abstract: The invention relates to a novel sinterable ceramic powder, to its preparation and to its further processing to give a silicon nitride ceramic, and to this material itself and its use. The sinterable ceramic powder is produced by melting a polysilazane or dissolving it in an organic solvent, suspending a powdered sinter aid in this melt or solution, then pyrolyzing the melt, or the residue obtained after evaporation of the solvent, at 500 DEG to 1600 DEG C. in a protective gas atmosphere, the polysilazane either A) being obtainable by reacting at least one of the oligosilazanes of the formula (I) +TR in which a, b, c and d are the mole fractions of the respective structural units and where 0 in which R and R* can be identical or different and R and R* are C1-C4-alkyl, vinyl or phenyl and R' is C1-C4-alkyl and x and y are the mole fractions of the two structural units, where x+y=1 and x=0.7-0.95. A molded article can be formed from the ceramic powder thus obtained and a silicon nitride ceramic then produced by sintering. However, a molded article can also be formed from the solidified melt or the still unpyrolyzed residue obtained after evaporating the solvent and this article can then by pyrolyzed and sintered. Components subject to severe mechanical, thermal and corrosive stress can be produced from the ceramic obtained.

    Prodn. of boron-contg. poly:silane(s), useful for prodn. of ceramics - by reacting tris-chloro:silyl:ethyl-borane(s) with alkali metal(s)
    9.
    发明专利
    Prodn. of boron-contg. poly:silane(s), useful for prodn. of ceramics - by reacting tris-chloro:silyl:ethyl-borane(s) with alkali metal(s) 未知

    公开(公告)号：DE4320786A1

    公开(公告)日：1994-01-05

    申请号：DE4320786

    申请日：1993-06-23

    Applicant: HOECHST AG

    Inventor： RIEDEL RALF DR ,  KIENZLE ANDREAS DIPL CHEM ,  PETZOW GUENTER PROF DR ,  BRUECK MARTIN DIPL ING ,  VAAHS TILO DR

    IPC: C04B35/571 ,  C04B35/589 ,  C08G77/60 ,  D01F6/78 ,  D01F9/10 ,  C04B35/58

    Abstract: B-contg. polysilanes (II) are produed by reacting tris-silyl-borane(s) of formula B-(C2H4-SiCl2X)3 (I) with metallic Li, Na and/or K. In (I), -C2H4- is -CH2-CH2- or -CHMe-; and X is Cl or 1-4C aliphatic residue. In (II), R = 1-4C aliphatic residue; and a + b is 1. At least equimolar amts. of alkali metal are useed, and the reaction is carried out in organic solvent, by adding the other reactants at 50-120 deg. C and then heating at 60-200 deg. C, pref. with exposure to ultrasound. Pref. (I) are prepd., e.g. by reaction of corresp. vinylsilanes of formula CH2=CH-SiCl2X with BH3.THF as described in J. Organomet. Chem. 34 (1972) C9 and 135 (1977) 249, and in Zhur. Obshchei. Thim. 30 (1960) 3615. Suitable solvents are, e.g. heptane, toluene, THF etc. USE/ADVANTAGE - (II) are new B-contg. polysilanes, useful for the prodn. of B- and Si- contg. ceramics with good adhesion, hardness and surface quality, which are useful for coating steel etc., esp. for the surface coating of machine components which are subjected to mechanical and chemical stress. (II) can also be shaped before pyrolysis, e.g. to give ceramic fibres which are useful for reinforcement of Al, Al alloys and ceramic components. In an example, tris-((dichloromethylsilyl) ethyl)-borane (I) was prepd. by reacting 216g dichloromethylvinylsilane in 255 ml toluen with 255 ml 2M soln. of BH3.SM32 in toluene, followed by evapn. of solvent to give 233g (I). Refluxing suspension of Na/K alloy (obtd. by melting 2.83g Na with 10.05g K) in THF was treated slowly with 27.5g (I), under the action of ultrasound. Mixt. was then worked up by filtration and evapn. to give polymer (II), contg. (apporx.) 42.8 wt.% C, 8.4 wt.% H, 11.8 wt.% B, 32.1 wt.% Si, below 0.2 wt.% Cl. 2.5g (II) was pressed-moulded to form a cylinder which was pyrolysed by heating under N2 to 1200 deg. C at 1 deg./min. and maintaining this temp. for a further 3 hrs. Black ceramic prod. obtd. showed slight shrinkage but no evidence of melting; X-ray diffraction analysis showed no crystalline phases.

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