CN115626859B - Metal composite boron powder and preparation method thereof - Google Patents
Metal composite boron powder and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of composite boron powder, and particularly relates to metal composite boron powder and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Carrying out ball milling and mixing on boron powder and metal oxide powder to obtain mixed powder; (2) And carrying the mixed powder by carrier gas after optional vacuum drying, and conveying the mixed powder to a position 10-30cm below the bottommost part of the plasma flame, and controlling the plasma power to be 20-30kw so that the metal oxide is gasified and reacts with hydrogen to generate metal particles, and the metal particles are distributed on the surface of the boron particles to obtain the metal composite boron powder. The method can enable the metal oxide and the hydrogen to generate gas phase reaction to generate extremely fine nano-scale metal particles which are dispersed and distributed in a simple substance form and adsorbed on the surfaces of the boron powder particles, and the prepared metal composite boron powder has good dispersibility, uniform compounding and good combustion performance, and the compounding process can be continuously carried out, thereby being suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of composite boron powder, and particularly relates to metal composite boron powder and a preparation method thereof.
Background
The amorphous boron powder has the characteristic of high energy, but the surface of the amorphous boron powder has a compact low-melting-point oxide layer, the oxide layer forms a liquid state in the combustion process, the further diffusion of oxygen can be hindered, when the amorphous boron powder is applied to the fields of high-energy solid fuels, explosives and the like, the amorphous boron powder has the problems that the continuous combustion is difficult after being ignited, the combustion performance is poor, and the high-energy characteristic cannot be fully exerted. Many possible solutions have been proposed by the public for eliminating or suppressing the oxide layer. Experiments of students prove that the combustion performance of the boron composite powder subjected to metal surface coating treatment is obviously improved compared with the original sample, including but not limited to shortening of ignition time, improvement of combustion speed, increase of combustion time, reduction of residual total boron in residues and the like, and the compatibility of the treated metal composite boron powder and a propellant system is improved to a certain degree.
In the prior art, partial work is carried out on the preparation of the metal composite boron powder, and the preparation of the metal composite boron powder can be realized by a multi-arc ion Plating (PVD) method, a ball milling method and the like. When the metal-coated boron powder is prepared by the PVD method, the problem that the metal is difficult to uniformly coat the surface of the boron powder can occur, and the method is limited by the target material, has high preparation cost and low efficiency and is difficult to realize batch preparation. The ball milling method realizes the micro-metallurgical bonding of boron powder and metal by grinding the boron powder and the metal powder for a long time, the composite uniformity and the micro-dispersion degree are not ideal, and a large amount of material deposition can occur in the ball milling process to cause uniform composite failure aiming at the composite of tungsten, molybdenum and other refractory metals.
Disclosure of Invention
The invention aims to overcome the defects of poor combustion performance and the like of metal composite boron powder caused by poor uniformity of boron powder and metal composite in the prior art, and provides the metal composite boron powder and the preparation method thereof.
In order to achieve the above object, in a first aspect, the present invention provides a method for producing a metal composite boron powder, comprising the steps of:
(1) Carrying out ball milling and mixing on boron powder and metal oxide powder to obtain mixed powder;
(2) And carrying the mixed powder by carrier gas after optional vacuum drying to be sent to a position 10-30cm below the bottommost part of the plasma flame, and controlling the plasma power to be 20-30kw so that the metal oxide is gasified and reacts with hydrogen to generate metal particles, and the metal particles are distributed on the surface of the boron particles to obtain the metal composite boron powder.
Preferably, in the step (1), the mixed powder is carried by the carrier gas and is sent to a position 10-25cm below the bottommost part of the plasma flame.
In some preferred embodiments, in step (2), the mixed powder is fed at a rate of 10 to 30g/min.
More preferably, the feeding rate of the mixed powder is 10 to 20g/min.
In some preferred embodiments, in step (2), the gas source of the plasma comprises argon and hydrogen, and the flow rate of the introduced hydrogen is not more than 100L/min, wherein the flow rate ratio of the argon to the hydrogen is 1-3:1.
in some preferred embodiments, the particle size of the boron powder in the mixed powder is in the range of 0.3 to 6 μm and the particle size of the metal oxide powder is in the range of 5 to 45 μm.
In some preferred embodiments, in step (1), the metal oxide comprises molybdenum oxide and/or tungsten oxide.
In some preferred embodiments, in the step (1), the mass ratio of the metal oxide to the boron powder is 1:4-45.
In some preferred embodiments, in step (1), the conditions for ball milling and mixing comprise: the ball-material ratio is 5-8, the frequency is 15-25Hz, and the time is 30-240min.
In some preferred embodiments, step (1) further comprises: before ball milling and mixing, the boron powder is subjected to ball milling pre-dispersion treatment.
More preferably, the conditions of the ball milling pre-dispersion treatment include: the ball-material ratio is 10-15, the frequency is 10-30Hz, and the time is 60-300min.
In a second aspect, the present invention provides a metal composite boron powder prepared by the method of the first aspect, the metal composite boron powder comprising micron-sized boron particles and nano-sized metal particles dispersed on the surfaces of the boron particles, the metal composite boron powder being prepared byThe metal mass content is 2-15%, and the laser granularity of the metal composite boron powder meets the following requirements: d 50 ＜1μm，D[4,3]＜1μm。
Preferably, the particle size of boron particles in the metal composite boron powder is 0.2-3 μm, and the particle size of metal particles is below 100 nm.
Has the advantages that:
according to the invention, the metal composite boron powder is prepared by a plasma method, particularly, the mixed powder is conveyed to a proper position below the bottommost part of plasma flame, and proper plasma power is matched, so that metal oxide and hydrogen can generate gas phase reaction to generate extremely fine nano-scale metal particles, and the boron reaction of the boron powder is avoided; the nanoscale metal particles have large specific surface area and high surface energy, are dispersed and distributed in a simple substance form and are adsorbed on the surfaces of the boron powder particles, and the problems of poor compounding uniformity and the like of conventional ball milling and other composite methods are solved. The obtained metal composite boron powder has the structure that a layer of nano metal simple substance particles is adsorbed on the surface of boron particles, namely the surface of the boron particles is coated with a layer of metal simple substance particles, and the coating layer and boron still exist in the original simple substance form without forming a compound. Under the same condition, if the powder feeding position of the mixed powder is too high, the reaction temperature is higher, the boron powder is possibly gasified and reacts with the generated molybdenum or tungsten metal to generate boride, so that the preparation of the metal composite boron powder fails; the powder feeding position is too low, the reaction temperature is low, the analyzed product is a mixture of boron composite boron powder and molybdenum oxide, mainly because the temperature of the position is low, part of molybdenum oxide does not react with hydrogen, molybdenum oxide powder is formed after cooling, and the molybdenum oxide powder is mixed into the generated molybdenum composite boron powder.
The metal composite boron powder has good dispersibility, uniform compounding and excellent combustion performance, and the compounding process can be continuously carried out, so the metal composite boron powder is particularly suitable for preparing refractory metal composite boron powder such as tungsten, molybdenum and the like. The metal coated on the surface of the boron particle can play a role in promoting combustion when boron powder is combusted, and is particularly suitable for the field of boron-containing fuels.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is an electron microscope image of the molybdenum composite boron powder of example 1 of the present invention at magnification 20000 times.
Fig. 2 is an SEM surface scanning overall view of the molybdenum composite boron powder of example 1 of the present invention at a magnification of 1000 times.
Fig. 3 is a scanning Mo distribution diagram of an SEM surface of the molybdenum composite boron powder of example 1 of the present invention at 1000 times magnification, and a gray portion is Mo.
FIG. 4 is a SEM surface scanning B distribution diagram at 1000 times magnification of the molybdenum composite boron powder of example 1 of the invention, and the gray part is B.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
In the invention, the ball-to-feed ratio is measured by mass. The position which is 10-30cm below the bottommost part of the plasma flame refers to the position which is 10-30cm below the bottommost part of the plasma flame and counted by the lowest point of the plasma flame.
In a first aspect, the present invention provides a method for preparing a metal composite boron powder, comprising the steps of:
(1) Carrying out ball milling and mixing on boron powder and metal oxide powder to obtain mixed powder;
(2) And carrying the mixed powder by carrier gas after optional vacuum drying, and conveying the mixed powder to a position 10-30cm below the bottommost part of the plasma flame, and controlling the plasma power to be 20-30kw so that the metal oxide is gasified and reacts with hydrogen to generate metal particles, and the metal particles are distributed on the surface of the boron particles to obtain the metal composite boron powder.
The mixed powder is sent to a position 10-30cm below the bottommost part of the plasma flame, so that the metal oxide in the mixed powder and the hydrogen in the plasma flame gas source only have reduction reaction to generate extremely fine nano-scale metal particles in a low-temperature region with the temperature of 1200-2000 ℃, and do not react with boron powder to generate boride; meanwhile, before the reaction, the metal oxide is gasified, under the influence of plasma thermal disturbance gas, the metal oxide and reaction gas hydrogen are uniformly dispersed on the surface of the boron particles after being mixed, and after the reduction reaction temperature is reached, the gas-gas reaction is instantly carried out, so that the generated metal nano particles can be uniformly dispersed on the surface of the boron particles, and the metal composite boron powder is obtained. In the combustion process of boron particles, the nano metal particles coated on the surface can play a role in efficiently promoting the combustion of boron powder, promote the boron powder to complete the combustion and release enough energy.
The mixed powder is fed to a position 10-30cm below the bottommost part of the plasma flame, and specifically, the mixed powder can be 10, 11, 12, 13, 15, 18, 20, 23, 25, 28, 30cm and the like.
Preferably, the mixed powder is carried by a carrier gas to be sent to a position 10-25cm below the bottommost part of the plasma flame after optional vacuum drying. Under this preferred scheme, more do benefit to and promote the combustion behavior of gained metal composite boron powder.
The feeding rate of the mixed powder is 10 to 30g/min, and specifically, it may be 10, 11, 12, 13, 15, 18, 20, 23, 25, 28, 30g/min, or the like.
In some preferred embodiments, in the step (2), the feeding rate of the mixed powder is 10 to 20g/min. Under the preferred scheme, the feeding amount of the mixed powder is appropriate, so that the mixed powder is more beneficial to timely and rapid gasification of the metal oxide and participates in the reaction with hydrogen, thereby further promoting uniform and rapid generation of nano particles, and the nano particles are dispersed and distributed more uniformly on the surfaces of the boron particles; thereby further improving the combustion performance of the metal composite boron powder.
It is to be understood that the flow rate of the carrier gas is only required to satisfy the above-mentioned feeding rate of the mixed powder. The carrier gas is preferably argon.
In some preferred embodiments, the gas source of the plasma comprises argon and hydrogen, the flow rate of the introduced hydrogen is not more than 100L/min, wherein the flow rate ratio of the argon to the hydrogen is 1-3:1.
in some preferred embodiments, the particle size of the mixed powder is in the range of 0.3 to 45 μm. More preferably, the particle size of the boron powder in the mixed powder is in the range of 0.3 to 6 μm and the particle size of the metal oxide powder is in the range of 5 to 45 μm. Under the preferable scheme, the metal particles with the particle size mainly concentrated between 30 nm and 80nm are generated in the step (2), the metal particles are adsorbed on the surfaces of the boron particles in a large amount in the form of simple substances, the specific surface area is large, the surface energy is high, and the rapid combustion of boron powder is promoted.
In some preferred embodiments, in the step (2), the vacuum drying conditions include: the vacuum degree is less than or equal to-0.09 MPa, the drying temperature is more than or equal to 90 ℃, and the drying time is more than or equal to 10 hours. Under the preferable scheme, the influence of residual moisture in the powder on the reaction can be reduced, and the reduction reaction is promoted more favorably.
The type of the metal oxide is only required to be capable of gasifying in the plasma flame environment and reacting with hydrogen to generate metal particles, and further coating the boron particles, and can be selected by a person skilled in the art according to requirements. In some preferred embodiments, in step (1), the metal oxide comprises molybdenum oxide and/or tungsten oxide.
The proportion of the raw materials can be selected by those skilled in the art according to requirements. In some preferred embodiments, in the step (1), the mass ratio of the metal oxide to the boron powder is 1:4-45.
In some preferred embodiments, in step (1), the conditions for ball milling and mixing comprise: the ball-material ratio is 5-8, the frequency is 15-25Hz, and the time is 30-240min. Under the preferred scheme, the raw materials can be mixed more uniformly, and the subsequent generated metal nano particles can be more favorably and uniformly dispersed on the surface of the boron particles.
The ball milling and mixing mode can be roller ball milling and other modes, and can be selected by the skilled in the art according to requirements.
In some preferred embodiments, step (1) further comprises: before ball-milling and mixing, the boron powder is subjected to ball-milling pre-dispersion treatment. Under the preferred scheme, the boron powder is firstly subjected to ball milling pre-dispersion treatment, so that even the boron powder with smaller particle size can be uniformly coated subsequently.
More preferably, the conditions of the ball milling pre-dispersion treatment include: the ball-material ratio is 10-15, the frequency is 10-30Hz, and the time is 60-300min.
The ball milling pre-dispersion treatment mode can be roller ball milling or planetary ball milling, and can be selected by a person skilled in the art according to requirements.
In a second aspect, the present invention provides a metal composite boron powder prepared by the method of the first aspect, wherein the metal composite boron powder comprises micron-sized boron particles and nano-sized metal particles dispersed on the surfaces of the boron particles, the metal content in the metal composite boron powder is 2-15% by mass, and the laser particle size of the metal composite boron powder satisfies: d 50 ＜1μm，D[4,3]＜1μm。
Preferably, the particle size of boron particles in the metal composite boron powder is 0.2-3 μm, and the particle size of metal particles is below 100 nm.
The present invention is further illustrated in detail below with reference to specific examples. Wherein, the gas source of plasma in the example is argon and hydrogen, the flow of introducing the hydrogen is 90L/min, wherein the flow ratio of the argon to the hydrogen is 2:1.
example 1
A method for preparing metal composite boron powder comprises the following steps:
(1) Firstly, carrying out ball-milling pre-dispersion treatment on boron powder, wherein the conditions of the ball-milling pre-dispersion treatment comprise: the ball-material ratio is 12;
and then, mixing molybdenum oxide and the obtained boron powder according to the mass ratio of 1:15, ball milling and mixing to obtain mixed powder with the granularity of 0.3-45 mu m, wherein the granularity of boron powder in the mixed powder is 0.3-6 mu m, and the granularity of metal oxide powder is 5-45 mu m; wherein the ball milling mixing conditions comprise: the ball material ratio is 6;
(2) Then, drying the mixed powder in vacuum, controlling the vacuum degree to be less than or equal to-0.09 MPa, controlling the drying temperature to be more than or equal to 100 ℃, and controlling the drying time to be more than or equal to 15h;
then, mixing the molybdenum oxide powder with argon carrier gas, conveying the mixture to a position 10cm below the bottommost part of the plasma flame, wherein the conveying speed of the mixed powder is 10g/min, and the plasma power is controlled to be 30kw, so that the molybdenum oxide is gasified and reacts with hydrogen to generate nano molybdenum particles, and the molybdenum particles are dispersedly distributed on the surfaces of the boron particles to obtain the molybdenum composite boron powder. Wherein the particle size of the boron particles is 0.2-3 μm, and the particle size of the molybdenum particles is below 100 nm.
The mass content of metals in the obtained molybdenum composite boron powder is 5.42%, and the laser granularity meets the following requirements: d 50 =0.587μm，D[4,3]=0.797 μm. An electron microscope image of the molybdenum composite boron powder is shown in fig. 1, SEM surface scanning is shown in fig. 2, fig. 3 and fig. 4, and a lens image of the molybdenum composite boron powder is combined, so that the two sides of an adsorption interface in the obtained composite exist in the form of Mo and B simple substances, and Mo is dispersed on the surface of boron particles uniformly in a dispersing mode through tiny nano particles.
Example 2
The procedure is as in example 1, except that the feed is carried out at a different location, specifically mixed with an argon carrier gas and fed to 30cm below the very bottom of the plasma flame.
The mass content of metal in the obtained molybdenum composite boron powder is 5.15%, and the laser granularity meets the following requirements: d 50 =0.671μm，D[4,3]=0.873 μm. Molybdenum and boron in the molybdenum composite boron powder exist in a simple substance form, and the molybdenum is dispersed on the surface of boron particles uniformly in a dispersing mode by using extremely small nano particles.
Example 3
The procedure is as in example 1, except that the mixed powder is fed at a rate of 30g/min.
The mass content of metals in the obtained molybdenum composite boron powder is 5.29%, and the laser granularity meets the following requirements: d 50 =0.662μm，D[4,3]=0.891 μm. Molybdenum and boron in the molybdenum composite boron powder exist in a simple substance form, and the molybdenum is dispersed on the surface of boron particles uniformly in the form of extremely small nano particles.
Comparative example 1
The procedure of example 1 was followed except that the feeding position was varied, specifically, it was mixed with the argon carrier gas and fed 35cm below the bottommost portion of the plasma flame.
The feeding position temperature is low, the analyzed product is a mixture of boron composite boron powder and molybdenum oxide, mainly because the position temperature is low, part of molybdenum oxide does not react with hydrogen, molybdenum oxide powder is formed after cooling, and the molybdenum oxide powder is mixed into the generated molybdenum composite boron powder.
Comparative example 2
The procedure of example 1 was followed except that the feeding position was varied, specifically, it was mixed with the argon carrier gas and fed to 5cm below the bottommost portion of the plasma flame.
The feeding position is too high, the reaction temperature is high, the boron powder has possibility of gasification and reacts with the generated molybdenum metal to generate boride, so that the preparation of the metal composite boron powder fails.
Comparative example 3
The molybdenum composite boron powder is prepared by a conventional ball milling process (500 g of boron powder and 25g of molybdenum powder, mixing and ball milling are carried out, the ball-material ratio is 5.
Test example
The products obtained in the above examples and comparative examples were subjected to a performance test: the combustion heat value of the boron powder is tested by using an oxygen bomb calorimeter, and the change condition of the combustion performance of the boron powder after molybdenum composite modification is directly reflected by the combustion heat value. The test results are shown in table 1 below.
TABLE 1
| Example numbering | Calorific value of combustion (J/g) |
| Composite boron powder | 18968.94 |
| Example 1 | 34028.19 |
| Example 2 | 30995.48 |
| Example 3 | 31206.04 |
| Comparative example 1 | 26811.06 |
| Comparative example 2 | 20092.34 |
| Comparative example 3 | 19194.83 |
According to the results, the metal composite boron powder with the specific structure can be obtained by adopting the scheme of the embodiment of the invention, wherein the metal simple substance is dispersed and uniformly dispersed on the surface of the boron particles in the form of the extremely small nano particles, so that the combustion performance of the metal composite boron powder is obviously improved. Comparative examples 1-2, which are outside the scope of the present invention, or comparative example 3, which employs a conventional ball milling process, have significantly lower combustion performance than the inventive examples.
Further, according to the embodiment 1 and the embodiment 2 of the present invention, it can be seen that the combustion performance of the obtained metal composite boron powder is better by adopting the preferable scheme of the present invention.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (8)
1. A method for preparing metal composite boron powder is characterized by comprising the following steps:
(1) Carrying out ball milling and mixing on boron powder and metal oxide powder to obtain mixed powder; the granularity of boron powder in the mixed powder is 0.3-6 mu m, and the granularity of metal oxide powder is 5-45 mu m; the metal oxide comprises molybdenum oxide and/or tungsten oxide;
(2) Then drying the mixed powder in vacuum, carrying the dried mixed powder by carrier gas, and conveying the mixed powder to a position 10-30cm below the bottommost part of the plasma flame, and controlling the plasma power to be 20-30kw so that metal oxide is gasified and reacts with hydrogen to generate metal particles, wherein the metal particles are distributed on the surface of the boron particles to obtain metal composite boron powder; wherein the feeding rate of the mixed powder is 10-30g/min, and the vacuum drying conditions comprise: the vacuum degree is less than or equal to-0.09 MPa, the drying temperature is more than or equal to 90 ℃, and the drying time is more than or equal to 10 hours.
2. The method of claim 1, wherein in step (1), the mixed powder is carried by the carrier gas to a position 10-25cm below the bottommost portion of the plasma flame.
3. The method according to claim 1, wherein in the step (2), the mixed powder is fed at a rate of 10 to 20g/min.
4. The method of claim 1, wherein in step (2), the source gas of the plasma comprises argon and hydrogen, the flow rate of the hydrogen is not more than 100L/min, and the flow rate ratio of the argon to the hydrogen is 1-3:1.
5. the method according to claim 1, wherein in the step (1), the mass ratio of the metal oxide to the boron powder is 1:4-45; and/or, in the step (1), the conditions of ball milling and mixing comprise: the ball-material ratio is 5-8, the frequency is 15-25Hz, and the time is 30-240min.
6. The method of claim 1, wherein step (1) further comprises: performing ball-milling pre-dispersion treatment on the boron powder before ball-milling and mixing; the ball milling pre-dispersion treatment conditions comprise: the ball-material ratio is 10-15, the frequency is 10-30Hz, and the time is 60-300min.
7. A metal composite boron powder prepared by the method of any one of claims 1-6, wherein the metal composite boron powder comprises micron-sized boron particles and nanoscale metal particles dispersed on the surfaces of the boron particles, the metal content of the metal composite boron powder is 2-15% by mass, and the laser particle size of the metal composite boron powder satisfies the following conditions: d 50 ＜1μm，D[4,3]＜1μm。
8. The metal composite boron powder according to claim 7, wherein the particle size of the boron particles in the metal composite boron powder is from 0.2 to 3 μm, and the particle size of the metal particles is 100nm or less.
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