CN103333343A - Preparation method of poly-zirconium-boron-silazane precursor - Google Patents
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Abstract
A preparation method of a poly-zirconium-boron-silazane precursor comprises the following steps: 1, weighing an organic zirconium compound, boron haloalkane, halogenosilane and micromolecular disilazane at the molar ratio of 1:(0.1-10):(0.1-10):(3-30); 2, respectively dissolving the boron haloalkane and the halogenosilane in organic solvents; 3, adding the organic zirconium compound to a reaction vessel, vacuumizing, filling dry nitrogen gas and precooling the reaction vessel; 4, adding the organic solvent of the boron haloalkane adn the organic solvent of the halogenosilane to the reaction vessel, and dripping the micromolecular disilazane in the reaction vessel; 5, after the dripping is finished, heating the reaction vessel to 150-500 DEG C, and preserving heat for 2-30 hours; 6, cooling the reaction vessel to 120-350 DEG C, distilling under reduced pressure and cooling to the room temperature. The poly-zirconium-boron-silazane precursor prepared according to the method is especially suitable for preparing ultra-high temperature ceramic materials.
Description
Technical field
The present invention relates to a kind of preparation method of poly-zirconium borosilicate azane precursor, especially relate to the preparation method of the polynary ceramic precursor of elements such as a kind of Si of containing, B, N, C, Zr.
Background technology
The polynary pottery that contains elements such as Si, B, N, C, Zr has excellent hot strength, high-modulus and excellent high-temperature oxidation and high-temperature creep resistance, therefore, Si-B-N-C-Zr system pottery has important application prospects in Aeronautics and Astronautics, weapons, naval vessels etc. need the field of high strength, high-modulus, high temperature resistant, anti-oxidant, heat-shock resistance, high temperature and creep resistance material.
The ultrahigh-temperature pottery (Ultra-High-Temperature Ceramics, UHTC) (
Adv. Mater. Process,
2010168 (6): 26-28), refer generally to the stupalith that can be for a long time uses in temperature more than 1800 ℃, can adapt to hypersonic long-time flight, atmospheric layer reenters, strides extreme environments such as aerial flight, rocket propulsion system and hot metal melting, can be used as key positions such as aircraft nose cone, the leading edge of a wing, numbers of hot-side engine, industrial high temperature furnace wall and heat-resistant tube, be the ultrahigh-temperature material that has potentiality (
Am. Ceram. Soc. Bull,
2012, 91 (1): 22-28).Along with ZrB
2-SiC-ZrC, ZrB
2-SiC-C, ZrB
2-SiC-AlN, ZrB
2The exploitation of pottery such as-SiC-BN, multicomponent system show more comprehensively performance advantage.Studies show that ZrB
2-SiC-BN based material has better fracture toughness property, has certain length-to-diameter ratio mainly due to BN, with other weak interface that forms mutually, has formed the stress relaxation of crack propagation and crack tip, thus absorbed crack propagation process energy (
Mater.Des,
2011, 32:401-405).In polynary superhigh temperature ceramic material, by ZrB
2, the Si-B-N-C-Zr multicomponent material system performance that constitutes such as SiC and nitride is the most excellent, has important application prospects.
The precursor conversion method is the effective ways of preparation superhigh temperature ceramic material.The preceramic polymer method mainly is by zirconates or contains the synthetic Zr polymkeric substance that contains of chemical reaction of zirconium molecule and organic monomer that pyrolysis transforms preparation Zr based ultra-high temperature pottery.As simple mixing of tetrabutyl zirconate and Vinylstyrene can be obtained uniform and stable liquid precursor, be specially adapted to infiltration pyrolysis (PIP) prepared ZrC pottery (
J. Mater.Sci,
2010(45): 6401 – 6405); By boron azane and Zr (NEt
2)
4The polymkeric substance pyrolysis that obtains of reaction prepare the many units of Zr-B-N pottery (
J.Inorg.Organomet.Polym.Mater,
2007, 17 (2): 423-437); By silazane and ZrCl
4Or Zr (NEt
2)
4Reaction obtain poly-zirconium silazane (
Chin.Chem. Lett, 2002, 13 (12): 1225-1226;
Chin. J. Polym. Sci,
2003, 21 (1): 99-101); Utilize liquid poly-silicon-carbon silane PSCS and Zr (acac)
4Prepared in reaction Si-Zr-C ceramic precursor (
J. Eur. Ceram. Soc,
2002(22): 2577-2585), by PSCS and Cp
2ZrCl
2, ZrCl
4, Zr (NEt
2)
4Mix the back 380 ℃ of scission reactions also can obtain the Si-Zr-C ceramic precursor (the polymer journal,
2008(6): 621-625), adopt electrochemical method for synthesizing also can synthesize the Si-Zr-C ceramic precursor (the polymer journal,
2011(6): 596-601).
But, still do not have the report about Si-B-N-C-Zr ceramic precursor or poly-zirconium borosilicate azane precursor Preparation Method at present.
Summary of the invention
Technical problem to be solved by this invention is that a kind of preparation method of poly-zirconium borosilicate azane precursor is provided.
The present invention solve that its technical problem adopts technical scheme be: a kind of preparation method of poly-zirconium borosilicate azane precursor may further comprise the steps:
(1) in organic zirconate: boron alkyl halide: halosilanes: the mol ratio of small molecules disilazane is the preferred 1-8 of 1:0.1-10(): the preferred 1-8 of 0.1-10(): the ratio preferred 4-15 of 3-30() takes by weighing organic zirconate, boron alkyl halide, halosilanes, small molecules disilazane;
Described small molecules disilazane is the alkyl silyl disilazane, and its general molecular formula is: (R
5 3Si)
2NR
6Wherein, R
5=H, methyl, ethyl, propyl group, butyl or phenyl, R
6=methyl, ethyl, propyl group, butyl or phenyl;
(2) be dissolved in boron alkyl halide, halosilanes in the organic solvent respectively;
(3) organic zirconate that takes by weighing is joined in the reactor of belt stirrer, constant pressure funnel, water distilling apparatus, vacuumize, fill drying nitrogen at least three times repeatedly, and reactor is chilled to subzero 2-35 ℃ in advance;
(4) will be dissolved with the organic solvent of boron alkyl halide, the organic solvent that is dissolved with halosilanes joins in the reactor, again the small molecules disilazane is placed constant pressure funnel, on one side stir, on one side the small molecules disilazane is joined in the reactor in the mode that drips;
Perhaps, earlier the small molecules disilazane is joined in the reactor, then step (2) gained is dissolved with the organic solvent of boron alkyl halide, the organic solvent that is dissolved with halosilanes mixes the back and adds in the constant pressure funnel, stir on one side, on one side the mixed solution of the organic solvent that will be dissolved with the boron alkyl halide and the organic solvent that is dissolved with halosilanes join in the reactor in the mode that drips;
(5) dropwise after, with the preferred 0.3-0.5 of 0.2-1.0 ℃/min(℃/min) heat-up rate reactor is heated to 150-500 ℃ (preferred 250-350 ℃), and insulation 2-30 hour (preferred 8-16 hour) under this temperature;
(6) temperature of reactor is down to 120-350 ℃ (preferred 150-300 ℃), underpressure distillation 0.5-5 hour (preferred 1-3 hour) is cooled to room temperature under this temperature.
Further, in the step (1), the molecular formula of described boron alkyl halide is as follows: BX
aR
1 3-aWherein, halogen X=Cl or Br; R
1=H, methyl, ethyl, propyl group, butyl or phenyl; A=1,2 or 3; The boron alkyl halide of described different substituents can use or mix use separately.
Further, in the step (1), described halosilanes is alkyl halogen silanes, and its general molecular formula is: R
2 mR
3 nSiR
4 (4-m-n)Wherein, alkyl R
2, R
3=H, methyl, ethyl, propyl group, butyl or phenyl; Halogen R
4=Cl or Br; M and n=0,1,2 or 3, m+n＜4; The halosilanes of described different substituents can use or mix use separately.
Further, in the step (2), described organic zirconate can be compounds such as zirconium tetrachloride, bis cyclopentadienyl zirconium dichloride, four (dimethylamino) zirconium or basic zirconium chloride.
Further, in the step (2), described organic solvent can be normal hexane, pentamethylene or toluene etc.
Further, in the step (6), the vacuum tightness of described underpressure distillation is 1-50kPa.
The poly-zirconium borosilicate azane precursor that the present invention makes is elementary composition by Si, B, N, C, Zr, H etc., can be for the preparation of ceramic fiber, coating, ceramic bulk material and ceramic matric composite.
The raw material that the present invention selects for use is easy to get, and is cheap, and cost is low, and reaction process is simple, and prepared precursor good processability can satisfy the needs of different environments for use.
Description of drawings
Fig. 1 is the typical infrared spectrogram of the poly-zirconium borosilicate azane precursor of the embodiment of the invention 1 gained;
Fig. 2 is the full spectrogram of XPS of the poly-zirconium borosilicate azane precursor of the embodiment of the invention 1 gained;
Fig. 3 is the thermogravimetric curve figure of the poly-zirconium borosilicate azane precursor of the embodiment of the invention 1 gained.
Embodiment
The invention will be further described below in conjunction with embodiment.
Present embodiment may further comprise the steps:
(1) takes by weighing zirconium tetrachloride 0.15mol, boron trichloride 0.15mol, trichlorosilane 0.15mol, heptamethyldisilazane 0.9mol;
(2) boron trichloride and trichlorosilane are dissolved in the normal hexane;
(3) the zirconium tetrachloride adding that takes by weighing is had in the 250ml there-necked flask of agitator, constant pressure funnel, water distilling apparatus, vacuumize, fill drying nitrogen three times repeatedly, and with extremely subzero 15 ℃ of reactor cooling;
(4) hexane solution of boron trichloride, the hexane solution of trichlorosilane are injected in the there-necked flask of drying nitrogen protection, again heptamethyldisilazane is injected in the constant pressure funnel, stir on one side, on one side heptamethyldisilazane is added in the there-necked flask in the mode that drips;
(5) dropwise after, heating up with the speed of 0.5 ℃/min is heated to 270 ℃ with reactor, and insulation 10 hours under this temperature;
(6) temperature of reactor is down to 150 ℃, underpressure distillation 0.5 hour (vacuum tightness 1kPa) is cooled to room temperature under this temperature, namely obtains solid-state poly-zirconium borosilicate azane precursor 15.8g.
The present embodiment gained gathers zirconium borosilicate azane precursor, and its infrared spectrogram, the full spectrogram of XPS and thermogravimetric curve are respectively as Fig. 1, Fig. 2 and shown in Figure 3.
As shown in Figure 1, contain Si-N, B-N, Si-CH in the precursor structure
3, N-CH
3Deng chemical bond.
As shown in Figure 2, the target precursor mainly is made up of Si, B, N, C, Zr and O.
As shown in Figure 3, the ceramic yield of target precursor is about 69%.
Embodiment 2
Present embodiment may further comprise the steps:
(1) takes by weighing bis cyclopentadienyl zirconium dichloride 1.5mol, methyl dichloro boron 0.3mol, silicon tetrachloride 0.15mol, N-ethyl hexamethyldisilazane 4.5mol;
(2) methyl dichloro boron and silicon tetrachloride are dissolved in the pentamethylene;
(3) the bis cyclopentadienyl zirconium dichloride adding that takes by weighing is had in the 500ml there-necked flask of agitator, constant pressure funnel, water distilling apparatus, vacuumize, fill the drying nitrogen quadruplication, and with extremely subzero 10 ℃ of reactor cooling;
(4) will be dissolved with the pentamethylene of methyl dichloro boron, the pentamethylene that is dissolved with silicon tetrachloride is injected in the there-necked flask of drying nitrogen protection, again N-ethyl hexamethyldisilazane is injected in the constant pressure funnel, stir on one side, on one side N-ethyl hexamethyldisilazane is added in the there-necked flask in the mode that drips;
(5) dropwise after, with the temperature rise rate of 0.5 ℃/min reactor is heated to 300 ℃, and insulation 12 hours under this temperature;
(6) temperature of reactor is down to 165 ℃, underpressure distillation 0.5 hour (vacuum tightness 10kPa) is cooled to room temperature under this temperature, namely obtains solid-state poly-zirconium borosilicate azane precursor 27.5g.
The solid-state poly-zirconium borosilicate azane precursor of present embodiment gained detects through infrared spectra, XPS and thermal weight loss, contains Si-N, B-N, Si-CH in the precursor structure
3, N-CH
3Deng chemical bond, the target precursor mainly is made up of Si, B, N, C, Zr and O, and the ceramic yield of target precursor is about 63%.
Embodiment 3
Present embodiment may further comprise the steps:
(1) takes by weighing bis cyclopentadienyl zirconium dichloride 0.015mol, phenyl boron dichloride 0.15mol, butyl trichlorosilane 0.15mol, N-methyl hexaethyl disilazine 0.1mol;
(2) phenyl boron dichloride and butyl trichlorosilane are dissolved in the toluene;
(3) the bis cyclopentadienyl zirconium dichloride adding that takes by weighing is had in the 250ml there-necked flask of agitator, constant pressure funnel, water distilling apparatus, vacuumize, fill the drying nitrogen quadruplication, and with extremely subzero 10 ℃ of reactor cooling;
(4) will be dissolved with the toluene of phenyl boron dichloride, the toluene that is dissolved with butyl trichlorosilane is injected in the there-necked flask of drying nitrogen protection, again the N-methyl hexaethyl disilazine of getting is injected in the constant pressure funnel, stir on one side, on one side N-methyl hexaethyl disilazine is added in the there-necked flask in the mode that drips;
(5) dropwise after, with the temperature rise rate of 0.3 ℃/min reactor is heated to 320 ℃, and insulation 12 hours under this temperature;
(6) temperature of reactor is down to 182 ℃, underpressure distillation 1 hour (vacuum tightness 25kPa) is cooled to room temperature under this temperature, namely obtains solid-state poly-zirconium borosilicate azane precursor 12.3g.
The solid-state poly-zirconium borosilicate azane precursor of present embodiment gained detects through infrared spectra, XPS and thermal weight loss, contains Si-N, B-N, Si-CH in the precursor structure
3, N-CH
3Deng chemical bond, the target precursor mainly is made up of Si, B, N, C, Zr and O, and the ceramic yield of target precursor is about 68%.
Embodiment 4
Present embodiment may further comprise the steps:
(1) takes by weighing four (dimethylin) zirconium 0.5mol, ethyl two chloroborane 0.15mol, dichloro hydrogen silicon 0.6mol, N-phenyl hexamethyldisilazane 2mol;
(2) ethyl two chloroboranes and dichloro hydrogen silicon are dissolved in the normal hexane;
(3) four (dimethylin) zirconium adding that takes by weighing is had in the 500ml there-necked flask of agitator, constant pressure funnel, water distilling apparatus, vacuumize, fill drying nitrogen three times repeatedly, and with extremely subzero 20 ℃ of reactor cooling;
(4) will be dissolved with the normal hexane of ethyl two chloroboranes, the normal hexane that is dissolved with dichloro hydrogen silicon is injected in the there-necked flask of drying nitrogen protection, again N-phenyl hexamethyldisilazane is injected in the constant pressure funnel, stir on one side, on one side N-phenyl hexamethyldisilazane is added in the there-necked flask in the mode that drips;
(5) dropwise after, with the temperature rise rate of 0.5 ℃/min reactor is heated to 280 ℃, and insulation 8 hours under this temperature;
(6) temperature of reactor is down to 140 ℃, underpressure distillation 0.5 hour (vacuum tightness 40kPa) is cooled to room temperature under this temperature, namely obtains solid-state poly-zirconium borosilicate azane precursor 38.3g.
The solid-state poly-zirconium borosilicate azane precursor of present embodiment gained detects through infrared spectra, XPS and thermal weight loss, contains Si-N, B-N, Si-CH in the precursor structure
3, N-CH
3Deng chemical bond, the target precursor mainly is made up of Si, B, N, C, Zr and O, and the ceramic yield of target precursor is about 59%.
Embodiment 5
Present embodiment may further comprise the steps:
(1) takes by weighing basic zirconium chloride 0.25mol, boron trichloride 0.15mol, dichloro propyl silane 0.45mol, N-phenyl hexamethyldisilazane 1.5mol;
(2) boron trichloride and dichloro propyl silane are dissolved in the normal hexane;
(3) the basic zirconium chloride adding that takes by weighing is had in the 250ml there-necked flask of agitator, constant pressure funnel, water distilling apparatus, vacuumize, fill drying nitrogen three times repeatedly, and with extremely subzero 15 ℃ of reactor cooling;
(4) will be dissolved with the normal hexane of boron trichloride, the normal hexane that is dissolved with the dichloro propyl silane is injected in the there-necked flask of drying nitrogen protection, again N-phenyl hexamethyldisilazane is injected in the constant pressure funnel, stir on one side, on one side N-phenyl hexamethyldisilazane is added in the there-necked flask in the mode that drips;
(5) dropwise after, with the temperature rise rate of 0.5 ℃/min reactor is heated to 250 ℃, and insulation 8 hours under this temperature;
(6) temperature of reactor is down to 120 ℃, underpressure distillation 0.5 hour (vacuum tightness 50kPa) is cooled to room temperature under this temperature, namely obtains solid-state poly-zirconium borosilicate azane precursor 26.9g.
The solid-state poly-zirconium borosilicate azane precursor of present embodiment gained detects through infrared spectra, XPS and thermal weight loss, contains Si-N, B-N, Si-CH in the precursor structure
3, N-CH
3Deng chemical bond, the target precursor mainly is made up of Si, B, N, C, Zr and O, and the ceramic yield of target precursor is about 55%.
Embodiment 6
Present embodiment may further comprise the steps:
(1) takes by weighing four (diethylamino) zirconium 0.5mol, propyl group dichloride boron 0.3mol, diphenyl dichlorosilane 0.15mol, heptamethyldisilazane 0.9mol;
(2) propyl group dichloride boron and diphenyl dichlorosilane are dissolved in the normal hexane;
(3) four (diethylamino) zirconium adding that takes by weighing is had in the 250ml there-necked flask of agitator, constant pressure funnel, water distilling apparatus, vacuumize, fill drying nitrogen three times repeatedly, and with extremely subzero 15 ℃ of reactor cooling;
(4) earlier heptamethyldisilazane is joined in the there-necked flask, to be dissolved with the normal hexane of propyl group dichloride boron again, the normal hexane that is dissolved with diphenyl dichlorosilane is injected in the constant pressure funnel after mixing, stir on one side, on one side will be dissolved with the normal hexane of diphenyl dichlorosilane, the mixed solution that is dissolved with the normal hexane of propyl group dichloride boron joins in the there-necked flask in the mode that drips;
(5) dropwise after, with the temperature rise rate of 0.5 ℃/min reactor is heated to 330 ℃, and insulation 15 hours under this temperature;
(6) temperature of reactor is down to 195 ℃, underpressure distillation 1 hour (vacuum tightness 6kPa) is cooled to room temperature under this temperature, namely obtains solid-state poly-zirconium borosilicate azane precursor 29.5g.
The solid-state poly-zirconium borosilicate azane precursor of present embodiment gained detects through infrared spectra, XPS and thermal weight loss, contains Si-N, B-N, Si-CH in the precursor structure
3, N-CH
3Deng chemical bond, the target precursor mainly is made up of Si, B, N, C, Zr and O, and the ceramic yield of target precursor is about 67%.
Claims (6)
1. the preparation method of a poly-zirconium borosilicate azane precursor is characterized in that, may further comprise the steps:
(1) in organic zirconate: boron alkyl halide: halosilanes: the mol ratio of small molecules disilazane is that the ratio of 1:0.1-10:0.1-10:3-30 takes by weighing organic zirconate, boron alkyl halide, halosilanes, small molecules disilazane;
Described small molecules disilazane is the alkyl silyl disilazane, and its general molecular formula is: (R
5 3Si)
2NR
6Wherein, R
5=H, methyl, ethyl, propyl group, butyl or phenyl, R
6=methyl, ethyl, propyl group, butyl or phenyl;
(2) be dissolved in boron alkyl halide, halosilanes in the organic solvent respectively;
(3) organic zirconate that takes by weighing is joined in the reactor of belt stirrer, constant pressure funnel, water distilling apparatus, vacuumize, fill drying nitrogen at least three times repeatedly, and reactor is chilled to subzero 2-35 ℃ in advance;
(4) will be dissolved with the organic solvent of boron alkyl halide, the organic solvent that is dissolved with halosilanes joins in the reactor, again the small molecules disilazane is placed constant pressure funnel, on one side stir, on one side the small molecules disilazane is joined in the reactor in the mode that drips;
Perhaps, earlier the small molecules disilazane is joined in the reactor, then step (2) gained is dissolved with the organic solvent of boron alkyl halide, the organic solvent that is dissolved with halosilanes mixes the back and adds in the constant pressure funnel, stir on one side, on one side the mixed solution of the organic solvent that will be dissolved with the boron alkyl halide and the organic solvent that is dissolved with halosilanes join in the reactor in the mode that drips;
(5) dropwise after, with the heat-up rate of 0.2-1.0 ℃/min reactor is heated to 150-500 ℃, and insulation 2-30 hour under this temperature;
(6) temperature of reactor is down to 120-350 ℃, under this temperature underpressure distillation 0.5-5 hour, be cooled to room temperature.
2. the preparation method of poly-zirconium borosilicate azane precursor according to claim 1, it is characterized in that: in the step (1), the molecular formula of described boron alkyl halide is as follows: BX
aR
1 3-aWherein, halogen X=Cl or Br; R
1=H, methyl, ethyl, propyl group, butyl or phenyl; A=1,2 or 3; The boron alkyl halide of described different substituents uses separately or mixes and use.
3. the preparation method of poly-zirconium borosilicate azane precursor according to claim 1 and 2, it is characterized in that: in the step (1), described halosilanes is alkyl halogen silanes, and its general molecular formula is: R
2 mR
3 nSiR
4 (4-m-n)Wherein, alkyl R
2, R
3=H, methyl, ethyl, propyl group, butyl or phenyl; Halogen R
4=Cl or Br; M and n=0,1,2 or 3, m+n＜4; The halosilanes of described different substituents uses separately or mixes and use.
4. the preparation method of poly-zirconium borosilicate azane precursor according to claim 1 and 2, it is characterized in that: in the step (2), described organic zirconate is zirconium tetrachloride, bis cyclopentadienyl zirconium dichloride, four zirconiums or basic zirconium chloride.
5. the preparation method of poly-zirconium borosilicate azane precursor according to claim 1 and 2, it is characterized in that: in the step (2), described organic solvent is normal hexane, pentamethylene or toluene.
6. the preparation method of poly-zirconium borosilicate azane precursor according to claim 1 and 2, it is characterized in that: in the step (6), the vacuum tightness of described underpressure distillation is 1-50kPa.
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| CN105801866A (en) * | 2016-03-01 | 2016-07-27 | 江苏赛菲新材料有限公司 | Method for preparing aluminum-containing polyborosilazane ceramic precursor |
| CN114213664A (en) * | 2021-12-22 | 2022-03-22 | 哈尔滨工业大学 | Synthesis method of five-component SiBCNZr ceramic precursor |
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