CN103396125B - Preparation method for boron-carbon-nitrogen porous ceramic - Google Patents

Preparation method for boron-carbon-nitrogen porous ceramic Download PDF

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CN103396125B
CN103396125B CN201310331011.3A CN201310331011A CN103396125B CN 103396125 B CN103396125 B CN 103396125B CN 201310331011 A CN201310331011 A CN 201310331011A CN 103396125 B CN103396125 B CN 103396125B
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carbon nitrogen
boron carbon
organic precursor
bcn
boron
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CN103396125A (en
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温广武
张涛
覃春林
钟博
夏龙
宋亮
王新宇
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Harbin Institute of Technology
Harbin Institute of Technology Weihai
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Abstract

The invention relates to a preparation method for boron-carbon-nitrogen porous ceramic. A boron-carbon-nitrogen (BCN) organic precursor-polyacrylonitrile fiber compound is prepared by using a boron-carbon-nitrogen (BCN) organic precursor as a binder and nano polyacrylonitrile fibers prepared by an electrostatic spinning method as a skeleton. The compound is sintered under a nitrogen (N2) protection atmosphere in a furnace by heating to a temperature of 1,400 DEG C at a speed of 3 DEG C/min and keeping the temperature for 1.5 h. The BCN porous ceramic prepared by the method is uniform in aperture, simple in process and low in cost, has excellent thermal shock resistance, high temperature oxidation resistance and high specific strength, and is suitable for preparing high-temperature resistant components and thermal insulated components of spacecrafts.

Description

A kind of preparation method of boron carbon nitrogen porous ceramics
Technical field
The present invention relates to a kind of composite ceramic material preparation method, specifically the preparation method of a kind of boron carbon nitrogen (BCN) porous ceramics.It is combined and is prepared BCN porous ceramics by the nano polypropylene nitrile fiber that adopts BCN organic precursor method to prepare with method of electrostatic spinning.
Background technology
Along with the development of modern aerospace technology, traditional lagging material shows obvious deficiency.Research and develop high performance matrix material, become at present one of emphasis of Materials science research in the world.In order to prepare, to be applicable to resistance to elevated temperatures good, the novel material of the heat-proof quality that specific tenacity is high and excellent, and researchist has started to pay close attention to the porous ceramic film material of thermotolerance and scale resistance excellence.Boron carbon nitrogen (BCN) ternary ceramics and other ceramic phase ratio, have density little, can processing, self-lubricating, high strength at high temperature, thermostability and the low expansion that anti-oxidant, dielectricity is adjustable, good.Its oxidation resistance temperature is more much higher than carbon fiber, therefore, is having wide application aspect aerospace flight technology field, the protective layer that can be used as anti-ablation cover, radome, anti-NEUTRON PROTECTION cover and reentry.But the preparation of current most of boron carbon nitrogen (BCN) pottery or the vapour deposition process based on traditional, be difficult to prepare large-sized block ceramic, and boron carbon nitrogen (BCN) material of vesicular structure have not been reported.Because boron carbon nitrogen (BCN) pottery itself is difficult to sintering, high to the purity requirement of raw material, this give prepare boron carbon nitrogen (BCN) porous ceramics, particularly shaped piece, foam, fiber has brought very large difficulty.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of method simply, easily operation, production cost is low, ceramic porous nickel, the preparation method of the boron carbon nitrogen porous ceramics that high temperature oxidation resistance is good.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of preparation method of boron carbon nitrogen porous ceramics, is characterized in that: it comprises the following steps:
(1) first preparing boron carbon nitrogen (BCN) organic precursor method 1:0.3 ~ 6 is dissolved in trichlorine boron azine and aniline in toluene in molar ratio; Room temperature lower magnetic force stirs 2～5h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 80～120 ℃ of heating jacket reflux 10～30 minutes, is cooled to room temperature; Under 30～45 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen (BCN) organic precursor method, stand-by;
(2) nano polypropylene nitrile (PAN) fiber of being prepared by method of electrostatic spinning adds in above-mentioned boron carbon nitrogen (BCN) organic precursor method preparing, dipping 10 ~ 15min, then ultrasonic dispersion 15 ~ 35min, obtain boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 40 ~ 55%, and the mass content of boron carbon nitrogen (BCN) organic precursor method is 60 ~ 45%;
(3) by disperse after boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 1 ~ 5mm, weight 1 ~ 6g; Between every upper and lower two-layer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen (BCN) precursor 2 ~ 5g, boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 15 ~ 50 layers again;
(4) the above-mentioned ceramic boat that boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is housed is gone in sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure (Pressure of Ambient Temperature before heating up) is controlled at 1.5 ~ 3.5 MPas (MPa);
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen (BCN) porous ceramics.
The present invention is take boron carbon nitrogen (BCN) organic precursor method as binding agent, and nano polypropylene nitrile fiber prepared by method of electrostatic spinning is that skeleton is prepared into boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body.Boron carbon nitrogen (BCN) organic precursor method Heat stability is good, does not occur being cross-linked at 150 ℃, cracking phenomenon below.Organic and characteristic inorganic materials are connected, prepare black boron carbon nitrogen (BCN) porous ceramics.Against existing technologies, the inventive method simply, easily operation, reproducible, production cost is low, the boron carbon nitrogen porous ceramics porous nickel of preparation, pottery porosity is adjustable, controls the porosity of B-C-N ceramic by controlling the number of plies of polyacrylonitrile fibre and sintering air pressure.Boron carbon nitrogen porous ceramics high temperature oxidation resistance is good.Ceramic yield can reach 78%.The boron carbon nitrogen porous ceramics of preparation has good heat-shock resistance, high temperature oxidation resistance and high specific tenacity.There is huge using value at spacecraft high temperature resistant component, heat insulating member.
Accompanying drawing explanation
Fig. 1 is the SEM microscopic appearance figure of boron carbon nitrogen (BCN) porous ceramics.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
A preparation method for boron carbon nitrogen porous ceramics, it comprises the following steps:
(1) prepare boron carbon nitrogen (BCN) organic precursor method.Trichlorine boron azine and aniline are dissolved in toluene 1:0.3 ~ 6 in molar ratio; Room temperature lower magnetic force stirs 2～5h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 80～120 ℃ of heating jacket reflux 10～30 minutes, is cooled to room temperature; Under 30～45 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen (BCN) organic precursor method, stand-by;
?(2) nano polypropylene nitrile (PAN) fiber of being prepared by method of electrostatic spinning adds in above-mentioned boron carbon nitrogen (BCN) organic precursor method preparing, dipping 10 ~ 15min, then ultrasonic dispersion 15 ~ 35min, make boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 40 ~ 55%, and the mass content of boron carbon nitrogen (BCN) organic precursor method is 60 ~ 45%;
(3) by boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 1 ~ 5mm, weight 1 ~ 6g; Between every upper and lower two-layer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen (BCN) precursor 2 ~ 5g, boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 15 ~ 50 layers;
(4) above-mentioned multilayer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is placed in to ceramic boat and goes to sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure (Pressure of Ambient Temperature before heating up) is controlled at 1.5 ~ 3.5 MPas (MPa);
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen (BCN) porous ceramics.
BCN porous ceramics scanning electron microscope microscopic appearance prepared by the present invention as shown in Figure 1.Porous nickel distributes as can see from Figure 1, and pore dimension is about 5-10 μ m.Carbon nano fiber diameter after the carbonization of polyacrylonitrile fibre fiber is about 100nm, and middle and boron carbon nitrogen (BCN) lamella interconnects.
Boron carbon nitrogen (BCN) porous ceramics productive rate is the test result 1500 ℃ time according to thermogravimetric analysis (TG).Boron carbon nitrogen (BCN) ceramic yield=(quality m after 1500 ℃ of thermal treatments 1)/(spraying BCN precursor quality m 2+ PAN fiber quality m 3).
The molecular-weight average of boron carbon nitrogen (BCN) precursor is affected by the consumption of polymerization time, temperature and aniline.In polymerized at room temperature process, increase successively to 5h molecular-weight average from 2h; Polymerization temperature is higher, the corresponding also increase of precursor molecular-weight average obtaining; At polymerization time 2h, trichlorine boron azine: aniline=1:0.3(mol ratio) time, molecular weight minimum 2261; Polymerization time 5h arrives trichlorine boron azine: when aniline=1:4.5, molecular-weight average has maximum 6782.When trichlorine boron azine: form white solid when aniline=1:6.
Embodiment 1: a kind of preparation method of boron carbon nitrogen porous ceramics, it comprises the following steps:
(1) prepare boron carbon nitrogen (BCN) organic precursor method by trichlorine boron azine and aniline in molar ratio 1:0.3 be dissolved in toluene; Room temperature lower magnetic force stirs 2h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 80 oin C heating jacket, reflux 10 minutes, is cooled to room temperature; Under 35 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen (BCN) organic precursor method, stand-by;
(2) nano polypropylene nitrile (PAN) fiber of being prepared by method of electrostatic spinning adds in above-mentioned boron carbon nitrogen (BCN) organic precursor method preparing, dipping 10min, then ultrasonic dispersion 15min, make boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 40%, and the mass content of boron carbon nitrogen (BCN) organic precursor method is 60%;
(3) by boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 1mm, weight 1g; Between every upper and lower two-layer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen (BCN) precursor 2g, boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 15 layers;
(4) above-mentioned multilayer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is placed in to ceramic boat and goes to sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure (Pressure of Ambient Temperature before heating up) is controlled at 3.5 MPas (MPa);
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen (BCN) porous ceramics.
B-C-N ceramic productive rate is 72.5%, and porosity is 58%.
Embodiment 2: a kind of preparation method of boron carbon nitrogen porous ceramics, it comprises the following steps:
(1) prepare boron carbon nitrogen (BCN) organic precursor method by trichlorine boron azine and aniline in molar ratio 1:1 be dissolved in toluene; Room temperature lower magnetic force stirs 3h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 90 ℃ of heating jacket reflux 18 minutes, is cooled to room temperature; Under 40 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen (BCN) organic precursor method, stand-by;
(2) nano polypropylene nitrile (PAN) fiber of being prepared by method of electrostatic spinning adds in above-mentioned boron carbon nitrogen (BCN) organic precursor method preparing, dipping 15min, then ultrasonic dispersion 20min, make boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 50%, and the mass content of boron carbon nitrogen (BCN) organic precursor method is 50%;
(3) by boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 3mm, weight 3g; Between every upper and lower two-layer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen (BCN) precursor 2g, boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 20 layers;
(4) above-mentioned multilayer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is placed in to ceramic boat and goes to sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure (Pressure of Ambient Temperature before heating up) is controlled at 2.8 MPas (MPa);
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen (BCN) porous ceramics.
B-C-N ceramic productive rate is 77.6%, and porosity is 69.1%.
Embodiment 3: a kind of preparation method of boron carbon nitrogen porous ceramics, it comprises the following steps:
(1) prepare boron carbon nitrogen (BCN) organic precursor method by trichlorine boron azine and aniline in molar ratio 1:3 be dissolved in toluene; Room temperature lower magnetic force stirs 4h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 100 ℃ of heating jacket reflux 25 minutes, is cooled to room temperature; Under 40 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen (BCN) organic precursor method, stand-by;
(2) nano polypropylene nitrile (PAN) fiber of being prepared by method of electrostatic spinning adds in above-mentioned boron carbon nitrogen (BCN) organic precursor method preparing, dipping 15min, then ultrasonic dispersion 30min, make boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 55%, and the mass content of boron carbon nitrogen (BCN) organic precursor method is 45%;
(3) by boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 3.6mm, weight 3.5g; Between every upper and lower two-layer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen (BCN) precursor 3g, boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 35 layers;
(4) above-mentioned multilayer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is placed in to ceramic boat and goes to sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure (Pressure of Ambient Temperature before heating up) is controlled at 2.0 MPas (MPa);
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen (BCN) porous ceramics.
B-C-N ceramic productive rate is 76.9%, and porosity is 70.4%.
Embodiment 4: a kind of preparation method of boron carbon nitrogen porous ceramics, it comprises the following steps:
(1) prepare boron carbon nitrogen (BCN) organic precursor method by trichlorine boron azine and aniline in molar ratio 1:6 be dissolved in toluene; Room temperature lower magnetic force stirs 5h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 120 ℃ of heating jacket reflux 30 minutes, is cooled to room temperature; Under 45 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen (BCN) organic precursor method, stand-by;
(2) nano polypropylene nitrile (PAN) fiber of being prepared by method of electrostatic spinning adds in above-mentioned boron carbon nitrogen (BCN) organic precursor method preparing, dipping 15min, then ultrasonic dispersion 35min, make boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 48%, and the mass content of boron carbon nitrogen (BCN) organic precursor method is 52%;
(3) by boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 5mm, weight 5.8g; Between every upper and lower two-layer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen (BCN) precursor 5g, boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 50 layers;
(4) above-mentioned multilayer boron carbon nitrogen (BCN) organic precursor method-polyacrylonitrile nanofiber complex body is placed in to ceramic boat and goes to sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure (Pressure of Ambient Temperature before heating up) is controlled at 1.5 MPas (MPa);
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen (BCN) porous ceramics.
B-C-N ceramic productive rate is 78.2%, and porosity is 74.5%.

Claims (1)

1. a preparation method for boron carbon nitrogen porous ceramics, is characterized in that: it comprises the following steps:
(1) first preparing boron carbon nitrogen organic precursor method 1:0.3 ~ 6 is dissolved in trichlorine boron azine and aniline in toluene in molar ratio; Room temperature lower magnetic force stirs 2～5h, then removes by filter white precipitate; Then the filtrate of clarification is placed in to 80～120 ℃ of heating jacket reflux 10～30 minutes, is cooled to room temperature; Under 30～45 ℃ of conditions, unnecessary toluene solvant is fallen in underpressure distillation, obtains faint yellow thick boron carbon nitrogen organic precursor method, stand-by;
(2) the nano polypropylene nitrile fiber of being prepared by method of electrostatic spinning adds in the above-mentioned boron carbon nitrogen organic precursor method preparing, dipping 10 ~ 15min, then ultrasonic dispersion 15 ~ 35min, obtain boron carbon nitrogen organic precursor method-polyacrylonitrile nanofiber complex body, wherein polyacrylonitrile nanofiber mass content is 40 ~ 55%, and the mass content of boron carbon nitrogen organic precursor method is 60 ~ 45%;
(3) by disperse after boron carbon nitrogen organic precursor method-polyacrylonitrile nanofiber complex body laying in ceramic boat, every layer of boron carbon nitrogen organic precursor method-polyacrylonitrile nanofiber complex body is of a size of 100 × 100mm, thickness is 1 ~ 5mm, weight 1 ~ 6g; Between every upper and lower two-layer boron carbon nitrogen organic precursor method-polyacrylonitrile nanofiber complex body, spray boron carbon nitrogen organic precursor method 2 ~ 5g, boron carbon nitrogen organic precursor method-polyacrylonitrile nanofiber complex body laying number of plies is 15 ~ 50 layers again;
(4) the above-mentioned ceramic boat that boron carbon nitrogen organic precursor method-polyacrylonitrile nanofiber complex body is housed is gone in sintering oven, and with 3 oc/min rises to 1400 oc is also incubated 1.5h, adopts N in stove 2atmosphere protection; Nitrogen original pressure is controlled at 1.5 ~ 3.5 MPas;
(5) insulation cools to room temperature with the furnace after finishing, and can obtain black boron carbon nitrogen porous ceramics.
CN201310331011.3A 2013-08-01 2013-08-01 Preparation method for boron-carbon-nitrogen porous ceramic Expired - Fee Related CN103396125B (en)

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CN109825900B (en) * 2019-01-23 2021-03-02 中国人民解放军国防科技大学 Preparation method of BCN (BCN-BCN) nano ceramic fiber
CN111454396B (en) * 2020-05-25 2021-10-08 福建华夏蓝新材料科技有限公司 Weather-resistant polyacrylate emulsion and preparation method thereof

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