CN113149014B - Method for preparing boron carbide powder by adopting organic carbon source - Google Patents
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Abstract
The invention provides a method for preparing boron carbide powder by adopting an organic carbon source, which comprises the steps of respectively dissolving zinc nitrate hexahydrate and dimethylimidazole in a solvent methanol; respectively heating the solution, and continuously stirring by magnetic force; pouring the solution of zinc nitrate hexahydrate into the solution of dimethyl imidazole,mixing and standing; carrying out centrifugal separation to obtain ZIF-8 white precipitate, cleaning the white precipitate with methanol, drying the cleaned ZIF-8 powder, and grinding; pyrolyzing the mixture in argon atmosphere to obtain nano porous carbon; taking boric acid H 3 BO 3 And nano porous carbon, dissolving in deionized water, performing ultrasonic dispersion, performing rotary evaporation, drying in an oven, grinding, and sieving with a 100-mesh sieve; calcining to obtain the boron carbide. According to the invention, the NPC which does not contain Zn element impurities and can keep uniform particle size and ordered nanopore structure can be obtained by optimizing the pyrolysis process of the ZIF-8 powder, such as pyrolysis temperature and heat preservation time.
Description
Technical Field
The invention belongs to the technical field of boron carbide, and particularly relates to a method for preparing boron carbide powder by adopting an organic carbon source.
Background
Boron carbide (B) 4 C) Ceramics are the highest hardness (-29.1 GPa) materials, except for diamond and cubic boron nitride, and have low densities (2.52 g/cm) 3 ) The high-elasticity-modulus and high-neutron-absorptivity composite material has the advantages of high elastic modulus, good neutron absorptivity, excellent chemical stability and thermal stability and the like, and is widely applied to the fields of light bulletproof armors, jet plane blade materials, refractory materials, wear-resistant materials, radiation-proof materials and the like.
Although B is 4 The C ceramic has incomparable performance advantages in many engineering fields, but the application of the C ceramic in China can not make a substantial breakthrough all the time. This is mainly due to two points:
(1) Sintering densification is costly.
(2) Low mechanical properties, in particular low fracture toughness (K) IC ～2.2MPa·m 1/2 )。
Therefore, in order to enable B 4 The C ceramic plays a role in national defense and industrial fields in China, and two restriction factors of difficult sintering densification and poor mechanical property must be simultaneously solved.
The micro-morphology analysis of the initial powder and the sintered product in the literature data can show that: initial B used in the research work 4 The particle size of the C powder is very uneven. Except for B in literature reports 4 In addition to the uneven morphology of the C powder, the C powder is suitable for B produced by German H.C.Starck company adopted by most of domestic and foreign researchers 4 C powder is subjected to microscopic morphology analysis, B 4 The C has poor uniformity of particle size and wide particle size distribution of 30-700nm.
In the prior art, graphene is used as a carbon source, and a traditional powder mixing process and a traditional gas-solid reaction process are utilized to prepare superfine boron carbide powder in a hot-pressing sintering furnace. The process used in traditional compounding results in an insufficiently uniform mixing of the two raw materials. Reaction by gas-solid method, with instability, e.g. in vacuum, B 4 C yield was very low. Graphene is a sheet structure with limited specific surface area, for B 2 O 3 Has a small adsorption capacity. Due to B 2 O 3 When reacting with graphene, the reaction is firstly carried out at the edge of the graphene and then extends into the interior of the graphene structure. Graphene edge and interior and B 2 O 3 The carbothermic reduction reaction is asynchronous in time, so that the prepared boron carbide powder has unsatisfactory monodispersity and low uniformity of particle size. In addition, the heating and cooling speed of the hot-pressing furnace is not as fast as that of an SPS furnace, so that the grain size of the synthesized powder is larger.
In addition, the composite powder of the carbon source and the boron source is calcined in vacuum or inert atmosphere, wherein the composite powder is prepared by mixing raw materials by adopting a stirring, ball milling or wet ball milling method, the carbon source is phenolic resin at the temperature of 1350-2200 ℃ in a hot pressing furnace, and the boron source comprises boron oxide or boric acid. However, when the phenolic resin is calcined at a high temperature, carbon having a sheet structure is generated, and the reaction is not synchronized in terms of time. The adsorption capacity of the carbon source with the sheet structure on the boron source is insufficient, the adsorption of the organic porous carbon source on the boron source is obvious in advantage compared with the carbon source with the sheet structure, and in addition, the SPS furnace has high heating and cooling speed on the hot-pressing furnace, so that abnormal growth of crystal grains of the powder is difficult to cause.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for preparing boron carbide powder by adopting an organic carbon source, aiming at obtaining nano B with high purity and monodisperse particle size 4 C powder and B reduction 4 The sintering densification cost of C ceramics is increased, and B is increased 4 The mechanical property of C ceramics, especially the fracture toughness.
The specific technical scheme is as follows:
the method for preparing the boron carbide powder by adopting the organic carbon source comprises the following steps:
the method for preparing the boron carbide powder by adopting the organic carbon source comprises the following steps:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethyl imidazole in a solvent methanol in two containers; respectively adding magnetons into the containers, respectively heating the solution to 25-60 ℃ by using a magnetic stirrer with a heating function, and continuously stirring for 1-1.5 h by magnetic force;
(2) Pouring the solution of zinc nitrate hexahydrate into the dimethyl imidazole solution, mixing and standing for 3-96 h;
(3) Removing the supernatant of the reactant, performing centrifugal separation to obtain ZIF-8 white precipitate, cleaning the white precipitate with methanol, drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8;
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon;
(5) According to the molar ratio of 1-10: 7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in the specific H at 65 ℃ 3 BO 3 Mass ten timesUltrasonically dispersing for 2 hours in deionized water, then performing rotary evaporation, drying in an oven, grinding, and sieving with a 100-mesh sieve;
(6) Calcining in an SPS furnace or a carbon tube furnace to obtain the boron carbide.
In the step (1), the molar ratio of zinc nitrate hexahydrate, dimethyl imidazole and methanol is 1:2 to 8:290 to 727.
In the step (3), the centrifugal separation parameters are 10000rpm and 5min;
methanol was washed three times, each time with the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, centrifuging again to obtain white precipitate again;
the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min.
The drying treatment is drying treatment in an oven, the temperature parameter of the oven is set to be 80-100 ℃, and the drying time is 8-15 h.
The pyrolysis condition in the step (4) is that the temperature of the box-type furnace is 600-1200 ℃, and the heat is preserved for 4-6h.
Rotary evaporation is carried out in the step (5), and the parameters are 70rpm, 70 ℃ and 3h; the parameters of the oven are 100 ℃ and 1h; grinding in a mortar for 5-10 min.
And (6) calcining the SPS furnace at 1600-1900 ℃ for 30 min-2 h.
The invention synthesizes B by taking nano porous carbon obtained after MOFs carbonization as a carbon source 4 And C, powder. ZIF-8 which is widely applied in MOFs materials is selected as a carbon source precursor. And 4, cracking the ZIF-8 at a proper temperature to obtain the NPC powder with an ordered nano-pore structure and regular and uniform appearance. The NPC used can keep the original network structure of the ZIF-8 before cracking, the particle size of the NPC is changed along with the particle size of the ZIF-8, and because of the porous structure of the NPC, the contact area of reactants is increased compared with the traditional solid carbon source, so that the reaction of raw materials at high temperature is more sufficient, the addition amount of a boron source in the reaction can be further reduced, and the B with smaller particle size can be obtained 4 And C, powder.
The method for preparing the boron carbide powder by adopting the organic carbon source can prepare NPC powder with higher yield and high performance, namely, the NPC powder with monodisperse particle size and ordered nanopore structure can be prepared into ZIF-8 powder with uniform particle size and adjustable particle size, and NPC which does not contain Zn element impurities and can keep uniform particle size and ordered nanopore structure can be obtained by optimizing the pyrolysis process of the ZIF-8 powder, such as pyrolysis temperature and heat preservation time.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is an SEM photograph of the product of example 1;
FIG. 3 is an SEM photograph of the product of example 2;
FIG. 4 is an SEM photograph of the product of example 3;
FIG. 5 is an SEM photograph of the product of example 4;
FIG. 6 is an SEM photograph of the product of example 5.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiment.
Example 1
According to the flow shown in fig. 1, the method for preparing boron carbide powder by adopting an organic carbon source comprises the following steps:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethylimidazole in methanol serving as a solvent in two containers; respectively adding magnetons into the containers, respectively heating the solution to 25 ℃ by using a magnetic stirrer with a heating function, and continuously stirring for 1 hour by magnetic force;
the molar ratio of zinc nitrate hexahydrate, dimethyl imidazole and methanol is 1:2.36:727.
(2) Pouring the solution of zinc nitrate hexahydrate into the solution of dimethyl imidazole, mixing and standing for 3 hours;
(3) Removing the supernatant of the reactant, and performing centrifugal separation to obtain ZIF-8 white precipitate, wherein the centrifugal separation parameters are 10000rpm and 5min; the white precipitate was washed with methanol three times, each time in the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, centrifuging again to obtain white precipitate again; the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min.
Drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8; the drying treatment is drying treatment in an oven, the temperature parameter of the oven is set to be 100 ℃, and the heat preservation time is 8 hours.
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon; the pyrolysis condition is that the temperature of the box-type furnace is set to be 800 ℃, and the temperature is kept for 4 hours.
(5) According to a molar ratio of 2:7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in the specific H at 65 ℃ 3 BO 3 Ultrasonically dispersing in deionized water with the mass ten times that of the deionized water for 2 hours, then performing rotary evaporation, drying in an oven, grinding and sieving by a 100-mesh sieve; rotary evaporation at 70rpm, 70 deg.C and 3 hr; the parameters of the oven are 100 ℃ and 1h; grinding in mortar for 5min.
(6) Calcining in an SPS furnace to obtain boron carbide. The calcination condition of the SPS furnace is 1900 ℃, and the temperature is kept for 2h.
The powder SEM photograph of the obtained product is shown in FIG. 2.
Example 2
According to the flow shown in fig. 1, the method for preparing boron carbide powder by adopting an organic carbon source comprises the following steps:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethylimidazole in methanol serving as a solvent in two containers; adding magnetons into the containers respectively, heating the solution to 40 ℃ by using a magnetic stirrer with a heating function, and continuously stirring for 1 hour by magnetic force;
the molar ratio of zinc nitrate hexahydrate, dimethyl imidazole and methanol is 1:3.36:727.
(2) Pouring the solution of zinc nitrate hexahydrate into the dimethyl imidazole solution, mixing and standing for 10 hours;
(3) Removing the supernatant of the reactant, and performing centrifugal separation to obtain ZIF-8 white precipitate, wherein the centrifugal separation parameters are 10000rpm and 5min; the white precipitate was washed with methanol three times, each time in the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, centrifuging again to obtain white precipitate again; the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min.
Drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8; the drying treatment is oven drying treatment, the temperature parameter of the oven is set to be 100 ℃, and the drying time is 8 hours.
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon; the pyrolysis condition is that the temperature of the box-type furnace is set to 850 ℃, and the temperature is kept for 6h.
(5) According to a molar ratio of 2.5:7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in specific H at 65 ℃ 3 BO 3 Ultrasonically dispersing in deionized water with the mass ten times that of the deionized water for 2 hours, then performing rotary evaporation, drying in an oven, grinding and sieving by a 100-mesh sieve; rotary evaporation at 70rpm, 70 deg.C and 3 hr; the parameters of the oven are 100 ℃ and 1h; grinding in mortar for 7min.
(6) Calcining in an SPS furnace to obtain boron carbide. The calcination condition of the SPS furnace is 1850 ℃, and the temperature is kept for 30min.
The SEM photograph of the powder of the obtained product is shown in FIG. 3.
Example 3
According to the flow shown in fig. 1, the method for preparing boron carbide powder by adopting an organic carbon source comprises the following steps:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethyl imidazole in a solvent methanol in two containers; adding magnetons into the containers respectively, heating the solution to 50 ℃ by using a magnetic stirrer with a heating function, and continuously stirring for 1.3h by magnetic force;
the molar ratio of zinc nitrate hexahydrate, dimethyl imidazole and methanol is 1:4.48:727.
(2) Pouring the solution of zinc nitrate hexahydrate into the solution of dimethyl imidazole, mixing and standing for 15 hours;
(3) Removing the supernatant of the reactant, and performing centrifugal separation to obtain ZIF-8 white precipitate, wherein the centrifugal separation parameters are 10000rpm and 5min; the white precipitate was washed with methanol three times, each time in the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, centrifuging again to obtain white precipitate again; the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min.
Drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8; the drying treatment is oven drying treatment, the temperature parameter of the oven is set to be 90 ℃, and the drying time is 10h.
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon; the pyrolysis conditions are that the temperature of the box type furnace is set to be 850 ℃, and the temperature is kept for 5 hours.
(5) According to a molar ratio of 10:7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in the specific H at 65 ℃ 3 BO 3 Ultrasonically dispersing in deionized water ten times the weight of the mixture for 2 hours, then performing rotary evaporation, drying in an oven, grinding, and sieving with a 100-mesh sieve; rotary evaporation at 70rpm, 70 deg.C and 3 hr; the parameters of the oven are 100 ℃ and 1h; grinding with mortar for 8min.
(6) Calcining in an SPS furnace to obtain boron carbide. The calcination condition of the SPS furnace is 1600 ℃, and the temperature is kept for 1h.
The SEM photograph of the powder of the obtained product is shown in FIG. 4.
Example 4
According to the flow shown in fig. 1, the method for preparing boron carbide powder by adopting an organic carbon source comprises the following steps:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethylimidazole in methanol serving as a solvent in two containers; adding magnetons into the containers respectively, heating the solution to 60 ℃ respectively by using a magnetic stirrer with a heating function, and continuously stirring for 1.5 hours by magnetic force;
the molar ratio of zinc nitrate hexahydrate, dimethyl imidazole and methanol is 1:8:290.
(2) Pouring the solution of zinc nitrate hexahydrate into the solution of dimethyl imidazole, mixing and standing for 23 hours;
(3) Removing the supernatant of the reactant, and performing centrifugal separation to obtain ZIF-8 white precipitate, wherein the centrifugal separation parameters are 10000rpm and 5min; the white precipitate was washed with methanol three times, each time in the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, and centrifuging again to obtain the white precipitate again; the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min.
Drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8; the drying treatment is oven drying treatment, the temperature parameter of the oven is set to be 100 ℃, and the drying time is 15h.
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon; the pyrolysis condition is that the temperature of the box-type furnace is set to 900 ℃, and the temperature is kept for 6h.
(5) According to a molar ratio of 5:7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in the specific H at 65 ℃ 3 BO 3 Ultrasonically dispersing in deionized water with the mass ten times that of the deionized water for 2 hours, then performing rotary evaporation, drying in an oven, grinding and sieving by a 100-mesh sieve; rotary evaporation at 70rpm, 70 deg.C for 3 hr; the parameters of the oven are 100 ℃ and 1h; grinding with mortar for 10min.
(6) Calcining in an SPS furnace to obtain boron carbide. The calcination condition of the SPS furnace is 1750 ℃, and the heat preservation is carried out for 1.5h.
The powder SEM photograph of the obtained product is shown in FIG. 5.
Example 5
According to the flow shown in fig. 1, the method for preparing boron carbide powder by adopting an organic carbon source comprises the following steps:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethylimidazole in methanol serving as a solvent in two containers; adding magnetons into the containers respectively, heating the solution to 60 ℃ by using a magnetic stirrer with a heating function, and continuously stirring for 1.5 hours by magnetic force;
the molar ratio of zinc nitrate hexahydrate, dimethyl imidazole and methanol is 1:2:290.
(2) Pouring the solution of zinc nitrate hexahydrate into the solution of dimethyl imidazole, mixing and standing for 96 hours;
(3) Removing the supernatant of the reactant, and performing centrifugal separation to obtain ZIF-8 white precipitate, wherein the centrifugal separation parameters are 10000rpm and 5min; the white precipitate was washed with methanol three times, each time in the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, centrifuging again to obtain white precipitate again; the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min.
Drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8; the drying treatment is oven drying treatment, the temperature parameter of the oven is set to be 100 ℃, and the drying time is 15h.
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon; the pyrolysis condition is that the temperature of the box-type furnace is 1200 ℃, and the temperature is kept for 6h.
(5) According to a molar ratio of 1:7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in the specific H at 65 ℃ 3 BO 3 Ultrasonically dispersing in deionized water with the mass ten times that of the deionized water for 2 hours, then performing rotary evaporation, drying in an oven, grinding and sieving by a 100-mesh sieve; rotary evaporation at 70rpm, 70 deg.C for 3 hr; the parameters of the oven are 100 ℃ and 1h; grinding with mortar for 10min.
(6) And calcining in a carbon tube furnace with high temperature rise and fall speed to obtain the boron carbide. The calcining condition of the carbon tube furnace is 1900 ℃, and the temperature is kept for 2h.
The SEM photograph of the powder of the obtained product is shown in FIG. 6.
Claims (4)
1. The method for preparing the boron carbide powder by adopting the organic carbon source is characterized by comprising the following steps of:
(1) Respectively dissolving zinc nitrate hexahydrate and dimethyl imidazole in a solvent methanol in two containers; respectively adding magnetons into the containers, respectively heating the solution to 25-60 ℃ by using a magnetic stirrer with a heating function, and continuously stirring for 1-1.5 h by magnetic force;
(2) Pouring the solution of zinc nitrate hexahydrate into the solution of dimethyl imidazole, mixing and standing for 3-96 h;
(3) Removing the supernatant of the reactant, performing centrifugal separation to obtain ZIF-8 white precipitate, cleaning the white precipitate with methanol, drying the cleaned ZIF-8 powder, and grinding the dried ZIF-8;
(4) Pyrolyzing ZIF-8 powder in argon atmosphere to obtain nanoporous carbon; the pyrolysis condition is that the temperature of the box-type furnace is 600-1200 ℃, and the temperature is kept for 4-6h;
(5) According to the molar ratio of 1-10: 7 taking boric acid H 3 BO 3 And nanoporous carbon, soluble in specific H at 65 ℃ 3 BO 3 Ultrasonic treatment in deionized water with mass ten timesDispersing for 2h, then performing rotary evaporation, drying in an oven, grinding, and sieving with a 100-mesh sieve;
(6) Calcining in an SPS furnace or a carbon tube furnace to obtain boron carbide, wherein the calcining condition of the SPS furnace is 1600-1900 ℃, and keeping the temperature for 30 min-2 h.
2. The method for preparing boron carbide powder by using an organic carbon source according to claim 1, wherein the molar ratio of zinc nitrate hexahydrate, dimethylimidazole and methanol in step (1) is 1:2 to 8:290 to 727.
3. The method for preparing boron carbide powder by using an organic carbon source according to claim 1, wherein in the step (3), the centrifugal separation parameter is 10000rpm and 5min;
methanol was washed three times, each time with the following procedure: adding methanol into the white precipitate, ultrasonically dispersing to dissolve the white precipitate in the methanol, and centrifuging again to obtain the white precipitate again;
the parameters of the centrifuge for the third cleaning are 10000rpm and 10min in sequence; 10000rpm, 12min;10000rpm, 15min;
the drying treatment is drying treatment in an oven, the temperature parameter of the oven is set to be 80-100 ℃, and the drying time is 8-15 h.
4. The method for preparing boron carbide powder by adopting the organic carbon source according to claim 1, wherein the rotary evaporation in the step (5) is carried out at 70rpm, 70 ℃ and 3h; the parameters of the oven are 100 ℃ and 1h; grinding in a mortar for 5-10 min.
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