CN111807841A - Preparation method of boron carbide ceramic - Google Patents

Preparation method of boron carbide ceramic Download PDF

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Publication number
CN111807841A
CN111807841A CN202010627023.0A CN202010627023A CN111807841A CN 111807841 A CN111807841 A CN 111807841A CN 202010627023 A CN202010627023 A CN 202010627023A CN 111807841 A CN111807841 A CN 111807841A
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boron carbide
carbide ceramic
reaction
raw material
bcl
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刘汝强
王殿春
李晓明
吴思华
周清波
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Shandong Guojing New Material Co ltd
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Shandong Guojing New Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention relates to a preparation method of boron carbide ceramic. The method comprises adopting chemical vapor deposition, using nitrogen as protective diluent gas, and using methane and gaseous BCl3The reaction temperature is controlled to be 1500-2000 ℃, the pressure is controlled to be 200-1000 Pa, and the boron carbide ceramic product is formed on the matrix mould. According to the invention, the boron carbide material with corresponding density is obtained by controlling the reaction temperature, so that the controllability of the material property is improved. The density of boron carbide obtained at higher temperature can reach 2.5g/cm3. The purity of the boron carbide material is 99.95-99.99%.

Description

Preparation method of boron carbide ceramic
Technical Field
The invention relates to a preparation method of boron carbide ceramic, belonging to the technical field of hard ceramic materials.
Background
Boron carbide (B)4C) Is an important superhard material with hardness second to that of diamond and cubic boron nitride in nature. It has the features of high melting point, high modulus, small specific weight, good self-lubricating property, wear resistance, acid and alkali corrosion resistance, radiation resistance, neutron absorption, etc. it is a comprehensive oneThe novel high-performance engineering ceramic material with outstanding performance has important application in the aspects of high-end liquid-gas sealing materials, aerospace engine nozzles, high-end ceramic bearings, high-end bulletproof armor materials, polishing of hard materials, fine abrasives and the like. In addition, the boron carbide ceramic has irreplaceable functions in the aspects of neutron absorption and shielding components of nuclear power reactors and the like.
The boron carbide ceramic has extremely strong covalent bond and large grain boundary resistance, is a ceramic material which is extremely difficult to sinter, the conventional normal pressure sintering method can only achieve about 80 percent of compactness, and the obtained boron carbide ceramic has poor performance. In order to improve the sintering density and performance of boron carbide ceramics, hot-pressing sintering method and liquid-phase sintering method are generally adopted. The hot pressing sintering method is to apply pressure of tens of megapascals in the sintering process to promote boron carbide sintering densification, for example, chinese patent documents CN1803714A, CN1541981A, and the like. The hot-pressing sintering method has low yield, high cost and simple product structure, and is difficult to produce in large scale.
The liquid phase sintering method is to add proper amount of Y into boron carbide2O3、Al2O3、La2O3And (3) the low-melting-point substances are utilized to generate partial liquid phase to promote sintering in the sintering process. Such as chinese patent documents CN1552667A, CN1438201A, etc. The boron carbide ceramics prepared by the liquid phase sintering method have relatively poor performance, and the performance of the materials is rapidly deteriorated due to liquid phase precipitation when the boron carbide ceramics are used at high temperature.
The normal pressure sintered boron carbide ceramic has the outstanding advantages of low process cost, capability of preparing products with complex structures and suitability for large-scale production, but the density of the traditional normal pressure sintered boron carbide is generally 2.0-2.1g/cm3The density is about 80%, the purity is about 90%, and how to improve the density and the purity of the boron carbide ceramic becomes a key difficult problem to be broken through urgently.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of boron carbide ceramic based on a chemical vapor deposition method, which can obviously improve the purity and density of boron carbide and has controllable density.
The technical scheme of the invention is as follows:
a process for preparing boron carbide ceramic includes chemical vapor deposition, nitrogen as protecting diluent gas, methane and gaseous BCl3The reaction temperature is controlled to be 1500-2000 ℃, the pressure is controlled to be 200-1000 Pa, and the boron carbide ceramic product is formed on the matrix mould.
According to the invention, the reaction temperature is controlled at 1500-3Boron carbide of (2); the reaction temperature is controlled at 1900-2000 ℃ to obtain the density of 2.45-2.50g/cm3The high-density boron carbide.
In more detail, the preparation method of the boron carbide ceramic comprises the following steps:
(1) after the substrate is arranged on a rotating device, the substrate is placed in a chemical vapor deposition reaction chamber, a furnace cover is closed, the temperature is increased and the vacuum is pumped, and when the temperature reaches 800-950 ℃, the temperature is kept for 30-60 min under the condition that the vacuum degree is 200-500 Pa;
(2) continuously introducing nitrogen as protective diluent gas according to BCl3∶CH4Mixing raw material methane and gaseous BCl in a volume ratio of (0.01-1): (0.5-50)3Introducing the mixture into a reaction chamber, heating to 1500-2000 ℃, controlling the vacuum degree to be 200-1000 Pa, introducing raw material gas for reaction for 15-40h, and depositing on a matrix mold to form a boron carbide ceramic product; after the reaction is finished, closing a raw material gas source;
(3) and after cooling, taking down the boron carbide ceramic on the matrix mold to obtain the boron carbide ceramic product.
According to the invention, in the step (1), the temperature is 900 ℃, and the vacuum degree is 300-400 Pa.
Preferably, in step (2), the boron carbide is prepared from methane and gaseous BCl3Volume ratio of BCl3∶CH4＝(0.02-0.05):(30-40)。
According to the present invention, in the step (2), it is preferable that the raw material gas CH4And BCl3The purity of the product is more than or equal to 99.99 percent;
preferably, in step (2), the degree of vacuum is 500-700Pa when preparing boron carbide.
According to the invention, in the step (2), the raw material gas is preferably introduced for a reaction time of 20 to 30 hours. The time for introducing the raw material gas is selected according to the thickness of the boron carbide to be grown.
Preferably, according to the present invention, in step (2), when the reaction temperature is 1500-3Boron carbide of (2); when the reaction temperature is 1900-2000 ℃, the density of 2.45-2.50g/cm can be obtained3The high-density boron carbide.
According to the invention, the material of the matrix is preferably graphite material, and the shape of the matrix can be processed according to the use requirement.
The method is suitable for manufacturing nozzles for sand blasting machines, nozzles for high-pressure water cutting machines, sealing rings, ceramic tools and dies and the like.
The invention has the technical characteristics and beneficial effects that:
1. the invention can obtain the boron carbide material with corresponding density by controlling the reaction temperature, and improves the controllability of the material property compared with the traditional sintering preparation method.
2. The invention can obtain the boron carbide material with high density and high density at higher reaction temperature, and compared with the traditional sintering preparation method, the boron carbide material with higher performance can be obtained. The density can reach 2.5g/cm3。
3. The invention uses high-purity raw material CH4And BCl3Compared with the traditional sintering preparation method, the method for preparing the high-purity boron carbide does not need substances such as a catalyst and the like, reduces the introduction of impurities, improves the purity of the boron carbide material, and realizes the preparation of the high-purity boron carbide material with the purity of 99.95-99.99%.
4. The invention can obtain products with corresponding shapes by controlling the shapes of the molds, thereby improving the plasticity of the products.
Drawings
FIG. 1 is a photograph of a real object of boron carbide prepared in example 1.
FIG. 2 is a scanning electron micrograph of the product prepared in example 2.
FIG. 3 is a graph of the density of boron carbide produced at different reaction temperatures, with the abscissa being temperature (. degree. C.) and the ordinate being density (%).
Detailed Description
The present invention will be further described by way of examples, but not limited thereto, with reference to the accompanying drawings.
Example 1
Installing a substrate in a rotating device, placing the substrate in a chemical vapor deposition reaction chamber, closing a furnace cover, heating and vacuumizing, preserving heat for 60min under the condition that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, then taking nitrogen as protective diluent gas, heating the reaction chamber to 1550 ℃ and taking nitrogen as protective diluent gas under the condition that the vacuum degree is 500Pa, introducing raw material gas, CH4∶BCl3The volume ratio of 30: 0.02, the reaction time of the raw material gas is 30h, the boron carbide is formed on the matrix by reaction and deposition, the boron carbide ceramic is taken down after the boron carbide ceramic is taken out of the furnace, and the density of the product is 2.30g/cm3。
Example 2
Installing the substrate in a rotating device, placing in a chemical vapor deposition reaction chamber, closing a furnace cover, heating and vacuumizing, keeping the temperature for 60min under the conditions that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, then taking nitrogen as protective diluent gas, heating the reaction chamber to 1500 ℃, taking nitrogen as protective diluent gas under the conditions that the vacuum degree is 500Pa, introducing raw material gas, CH4∶BCl3And (3) introducing raw material gas according to the volume ratio of 40:0.05, reacting for 25h, and reacting and depositing on the substrate to form boron carbide.
Example 3
Installing a substrate in a rotating device, placing the substrate in a chemical vapor deposition reaction chamber, closing a furnace cover, heating and vacuumizing, preserving heat for 60min under the condition that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, then taking nitrogen as protective diluent gas, heating the reaction chamber to 1550 ℃ and taking nitrogen as protective diluent gas under the condition that the vacuum degree is 700Pa, introducing raw material gas, CH4∶BCl3The volume ratio of 30: 0.02, the raw material gas is introduced for reaction for 30h, and the reaction is deposited on the substrateForming boron carbide.
Example 4
Mounting the substrate on a rotating device, placing in a chemical vapor deposition reaction chamber, closing a furnace cover, heating and vacuumizing, keeping the temperature for 60min under the conditions that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, then taking nitrogen as protective diluent gas, heating the reaction chamber to 1950 ℃, taking nitrogen as protective diluent gas under the conditions that the vacuum degree is 500Pa, introducing raw material gas, CH4∶BCl3The volume ratio of 30: 0.02, the raw material gas is introduced for reaction for 35h, and boron carbide is formed on the substrate through reaction and deposition. The density of the obtained boron carbide ceramic product is 2.50g/cm3。
Example 5
Mounting the substrate on a rotating device, placing in a chemical vapor deposition reaction chamber, closing a furnace cover, heating and vacuumizing, keeping the temperature for 60min under the conditions that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, then taking nitrogen as protective diluent gas, heating the reaction chamber to 1950 ℃, taking nitrogen as protective diluent gas under the conditions that the vacuum degree is 700Pa, introducing raw material gas, CH4∶BCl3And (3) introducing raw material gas according to the volume ratio of 40:0.05, reacting for 20h, and reacting and depositing on the substrate to form boron carbide.
Comparative example 1
Installing the substrate in a rotating device, placing the substrate in a chemical vapor deposition reaction chamber, closing a furnace cover, heating and vacuumizing, keeping the temperature for 60min under the conditions that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, then taking nitrogen as protective diluent gas, heating the reaction chamber to 1400 ℃, taking nitrogen as protective diluent gas under the condition that the vacuum degree is 500Pa, introducing raw material gas, CH 4: BCl3The volume ratio of 30: 0.02, the raw material gas is introduced for reaction for 30h, and boron carbide is formed on the substrate through reaction and deposition.
Comparative example 2
Installing the substrate in a rotating device, placing in a chemical vapor deposition reaction chamber, closing a furnace cover, heating, vacuumizing, keeping the temperature for 60min under the conditions that the temperature reaches 900 ℃ and the vacuum degree is 300Pa, and then taking nitrogen as protective diluent gasHeating the reaction chamber to 1550 deg.C, introducing raw material gas CH 4: BCl under the condition of 1500Pa vacuum degree and nitrogen as protective diluent gas3The volume ratio of 30: 0.02, the raw material gas is introduced for reaction for 30h, and boron carbide is formed on the substrate through reaction and deposition.
The first experimental example: experimental tests were carried out on the boron carbide materials prepared in the examples and comparative examples.
The density and the compactness of the ceramic are measured by using an Archimedes drainage method in GB/T25995-2010, the bending strength of the ceramic is measured according to GB/T6569-1996, and the Vickers hardness of the ceramic is measured according to GB/T16534-1996 by using a micro Vickers hardness tester. The product performance test results are shown in table 1.
TABLE 1 product Performance test results
Figure BDA0002566896380000051
As can be seen from Table 1, the product of example 4 of the present invention has the highest density and mechanical properties, and the ceramic density can reach 2.50/cm3The compactness can reach 99.8 percent, the bending strength of the ceramic is more than 550MPa, and the Vickers hardness of the ceramic can reach 3600HV 1. By using the method of the invention, boron carbide ceramics with different densities and strengths can be prepared according to actual needs. The density of the product of comparative example 2 was lower than that of the product of example 1, and it can be seen that too high a vacuum resulted in an increase in the gas deposition rate, resulting in a decrease in density and a decrease in density.
Experiment example two: compactness curve of boron carbide prepared at different reaction temperatures
According to the preparation method of example 1, the density curves of boron carbide prepared at different reaction temperatures were measured at 1500 ℃, 1550 ℃, 1600 ℃, 1650 ℃, 1700 ℃, 1750 ℃, 1800 ℃, 1850 ℃, 1900 ℃, 1950 ℃, 2100 ℃, 2150 ℃, 2200 ℃ and 2250 ℃ respectively, as shown in FIG. 3. And calculating the density of the product at different temperatures to obtain the density of the product at different temperatures, and then drawing a curve.

Claims (9)

1. Of boron carbide ceramicsThe preparation method comprises adopting chemical vapor deposition, taking nitrogen as protective diluent gas, and taking methane and gaseous BCl3The reaction temperature is controlled to be 1500-2000 ℃, the pressure is controlled to be 200-1000 Pa, and the boron carbide ceramic product is formed on the matrix mould.
2. The method of preparing a boron carbide ceramic according to claim 1, comprising the steps of:
(1) after the substrate is arranged on a rotating device, the substrate is placed in a chemical vapor deposition reaction chamber, a furnace cover is closed, the temperature is increased and the vacuum is pumped, and when the temperature reaches 800-950 ℃, the temperature is kept for 30-60 min under the condition that the vacuum degree is 200-500 Pa;
(2) continuously introducing nitrogen as protective diluent gas according to BCl3∶CH4Mixing raw material methane and gaseous BCl in a volume ratio of (0.01-1): (0.5-50)3Introducing the mixture into a reaction chamber, heating to 1500-2000 ℃, controlling the vacuum degree to be 200-1000 Pa, introducing raw material gas for reaction for 15-40h, and depositing on a matrix mold to form a boron carbide ceramic product; after the reaction is finished, closing a raw material gas source;
(3) and after cooling, taking down the boron carbide ceramic on the matrix mold to obtain the boron carbide ceramic product.
3. The method for preparing boron carbide ceramic according to claim 2, wherein in the step (1), the temperature is 900 ℃ and the vacuum degree is 300 to 400 Pa.
4. The method of producing a boron carbide ceramic according to claim 2, wherein in the step (2), when producing boron carbide, methane and gaseous BCl are used3Volume ratio of BCl3∶CH4＝(0.02-0.05):(30-40)。
5. The method of producing a boron carbide ceramic according to claim 2, wherein in the step (2), the raw material gas CH4And BCl3The purity of the product is more than or equal to 99.99 percent.
6. The method according to claim 2, wherein the degree of vacuum in step (2) is 500-700 Pa.
7. The method according to claim 2, wherein in the step (2), the raw material gas is introduced for a reaction time of 20 to 30 hours.
8. The method for preparing boron carbide ceramic as claimed in claim 1 or 2, wherein the reaction temperature is controlled at 1500-3Boron carbide.
9. The method for preparing boron carbide ceramic as claimed in claim 1 or 2, wherein the reaction temperature is controlled at 1900-2000 ℃ to obtain a density of 2.45-2.50g/cm3The high-density boron carbide.
CN202010627023.0A 2020-07-02 2020-07-02 Preparation method of boron carbide ceramic Pending CN111807841A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005056872A1 (en) * 2003-12-08 2005-06-23 Trex Enterprises Corp. Method of making chemical vapor composites
CN101830703A (en) * 2010-04-06 2010-09-15 中南大学 Carbon fiber reinforced boron carbide composite material and preparation method thereof
CN102503429A (en) * 2011-10-17 2012-06-20 宁波伏尔肯机械密封件制造有限公司 Preparation method for sintering boron carbide ceramic under constant pressure
CN105622144A (en) * 2016-01-11 2016-06-01 山东理工大学 Method for preparing resin-dispersed zirconium boride, boron carbide-carbon fiber friction material
US20160272548A1 (en) * 2013-10-16 2016-09-22 Schunk Ingenieurkeramik Gmbh Method for the Production of Shaped Articles from Reaction-bonded, Silicon-infiltrated Silicon Carbide and/or Boron Carbide and Thus Produced Shaped Body
CN106006644A (en) * 2016-05-19 2016-10-12 深圳市鑫成炭素科技有限公司 Preparation method of nano boron carbide powder
CN106631112A (en) * 2016-12-29 2017-05-10 中国科学院上海应用物理研究所 Preparation method of hollow ceramic microsphere

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005056872A1 (en) * 2003-12-08 2005-06-23 Trex Enterprises Corp. Method of making chemical vapor composites
CN101830703A (en) * 2010-04-06 2010-09-15 中南大学 Carbon fiber reinforced boron carbide composite material and preparation method thereof
CN102503429A (en) * 2011-10-17 2012-06-20 宁波伏尔肯机械密封件制造有限公司 Preparation method for sintering boron carbide ceramic under constant pressure
US20160272548A1 (en) * 2013-10-16 2016-09-22 Schunk Ingenieurkeramik Gmbh Method for the Production of Shaped Articles from Reaction-bonded, Silicon-infiltrated Silicon Carbide and/or Boron Carbide and Thus Produced Shaped Body
CN105622144A (en) * 2016-01-11 2016-06-01 山东理工大学 Method for preparing resin-dispersed zirconium boride, boron carbide-carbon fiber friction material
CN106006644A (en) * 2016-05-19 2016-10-12 深圳市鑫成炭素科技有限公司 Preparation method of nano boron carbide powder
CN106631112A (en) * 2016-12-29 2017-05-10 中国科学院上海应用物理研究所 Preparation method of hollow ceramic microsphere

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