CN108249443A - A kind of method for the boron carbide nano-powder for preparing carbon package - Google Patents
A kind of method for the boron carbide nano-powder for preparing carbon package Download PDFInfo
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- CN108249443A CN108249443A CN201810189072.3A CN201810189072A CN108249443A CN 108249443 A CN108249443 A CN 108249443A CN 201810189072 A CN201810189072 A CN 201810189072A CN 108249443 A CN108249443 A CN 108249443A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
A kind of method for the boron carbide nano-powder for preparing carbon package, mainly by boric acid and sucrose B in molar ratio:C=1:1 mixing, and be added in deionized water and stir the boric acid for being completely dissolved, obtaining water white transparency and sucrose mixed solution；Obtained water white transparency mixed solution in 80 200 DEG C of heating, dryings and is stirred, obtains red brown solid, solid is ground with agate mortar, Red-brown powder is made；Obtained Red-brown powder is heated to 1,550 1600 DEG C under vacuum, the slow cooling after ten minutes of heat preservation 5 obtains the B of carbon package4C boron carbide nano-powders.The raw materials used in the present invention is cheap and easy to get, and preparation process is simple, available for mass producing；Excessive carbon is controlled in Nano grade, B4The grain size of C powders is small and uniform, generally in 100nm hereinafter, B4The carbon wrapping layer of C nano particle is uniform, and thickness is less than 5nm.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of preparation method of boron carbide nano-powder.
Background technology
Boron carbide (B4C) have that density is low, intensity and hardness are high, excellent high-temperature stability and chemical stability etc. are special
Point in fields such as national defence, nuclear energy, aerospace, machinery, wear-proof techniques, is just increasingly showing its wide development and application prospect.
Particularly in ceramic armour, B4Hardness highest, the density of C ceramics are minimum, although its higher price, in the item for ensureing performance
Under part, to mitigate in armor system of the weight as primary premise, B4C is still preferentially selected.B4C bulletproof ceramics are widely used in anti-
Play clothing, infantry fighting vehicles and the armor facing of light armored vehicle and armed helicopter web.
Usual B4The sintering of C ceramics is utilized at very high temperature and uses B4C powders through pressureless sintering or hot pressed sintering and
Into, according to Hall-Petch laws, the hardness of the thinner sintered body of crystal grain can be higher.Therefore, the crystal grain refinement of predecessor becomes
One raising B4The effective way of C ceramic performances.Then, people try B4C is prepared into nano-powder, then by using suitable
When sintering method (such as SPS sintering) as possible inhibit sintering during crystal grain grow up, achieve preferable effect.Such as：
B.M.Moshtaghioun et al. uses high energy ball mill method by B4C powder finings are to submicron order, after annealing with electric discharge etc.
Ion is sintered, and is prepared hardness and is reached~the B of 38GPa4C ceramics.And it is the consistency for improving block, it is sintered B4It is usually required during C
Various sintering aids are added in powder with acceleration of sintering.Recently, by adding the nanoscales carbon materials such as graphene, carbon nanotube
The method of material, the method using high pressure or discharge plasma sintering synthesize B4The fracture toughness of C bulks is significantly improved.
Carbothermic method is as industrially prepared B4The main method of C powders, in order to avoid there is boron oxide remaining during preparation, carbon was usually
Amount.
Invention content
The object of the present invention is to provide it is a kind of it is simple for process, of low cost, do not have that boron oxide is remaining, carbon can be controlled to use
The method of the boron carbide nano-powder for preparing carbon package of amount.The present invention is mainly by vacuum high-temperature reaction method, with cheap
Boric acid (the H being easy to get3BO3) and sucrose (C12H22O11) it is raw material, by different heating temperature, it is obtained by the reaction in high vacuum conditions
The B of carbon package4C nano powder.
Technical scheme is as follows：
(1) by boric acid (H3BO3) and sucrose (C12H22O11) B in molar ratio:C=1:1 mixing, obtains mixed powder, later
It is added in deionized water and stirs the boric acid for being completely dissolved, obtaining water white transparency and sucrose mixed solution.For ensure boric acid with
Sucrose fully dissolves, and the mixed powder of 5g boric acid and sucrose is added in every 100ml deionized waters；
(2) the water white transparency mixed solution that step (1) obtains in 80-200 DEG C of heating, drying and is stirred, obtains bronzing
Solid grinds solid with agate mortar, and Red-brown powder is made；
(3) Red-brown powder that step (2) obtains is attached in graphite crucible, crucible is put into tube furnace, in tubular type
Furnace interior vacuum is less than 10-3It is begun to warm up after Pa, is warming up to 1550-1600 DEG C, slow cooling after heat preservation 5-10 minutes obtains carbon
The B of package4C boron carbide nano-powders.
Compared with the prior art, the present invention has the following advantages：
1st, raw materials used cheap and easy to get, preparation process is simple, available for mass producing.
2nd, B is being prepared4Excessive carbon is controlled in Nano grade in C nano powder process, makes effective sintering
Additive, while control B4The grain size of C powders is small and uniform, generally in below 100nm.
3、B4The carbon wrapping layer of C nano particle is uniform, and thickness is less than 5nm.
Description of the drawings
Fig. 1 is the B of carbon package that the embodiment of the present invention 1 obtains4C boron carbide nano-powder X-ray diffractograms and B4C is managed
By the X-ray diffractogram of model；
Fig. 2 is the B of carbon package that the embodiment of the present invention 1 obtains4C boron carbide nano-powder Raman figures；
Fig. 3 is the B of carbon package that the embodiment of the present invention 1,2,3,4 obtains4C boron carbide nano-powder scanning electron microscope (SEM) photographs；Figure
In：A is embodiment 1, b is embodiment 2, c is embodiment 3, d is embodiment 4；
Fig. 4 is the B of carbon package that the embodiment of the present invention 1 obtains4C boron carbide nano-powder transmission electron microscope pictures.
Specific embodiment
Embodiment 1
Boric acid (the H that AlfaAesar Chemical Co., Ltd. is produced3BO3) and sucrose (C12H22O11) B in molar ratio:C=1:1
Mixing is added in deionized water and is stirred to being completely dissolved, adds in 5g mixed powders per 100ml deionized waters, obtain water white transparency
Boric acid and sucrose mixed solution；Obtained water white transparency mixed solution with 80 DEG C of heating, dryings and is stirred on constant temperature heating plate
It mixes, obtains red brown solid, solid is ground with agate mortar, Red-brown powder is made；Obtained Red-brown powder is attached to
In graphite crucible, crucible is put into vacuum tube furnace, is less than 10 in tube furnace inner vacuum-3Begun to warm up after Pa, with 8 DEG C/
The heating rate of min is at the uniform velocity warming up to 1550 DEG C, keeps the temperature slow cooling after five minutes, obtains the B of carbon package4C boron carbide nano powders
Body.
Analyzed using X-ray diffractometer (Bruker D8, Germany) obtaining powder, as shown in Figure 1, by with
The X ray diffracting spectrum of B4C theoretical models simulation compares, and powder is mainly by B4C phases are formed, it can also be seen that amorphous carbon wideization
Peak；Obtained powder is analyzed using Raman spectrometer (HORIBA Jobin Yvon), as shown in Fig. 2, its main component
By B4C and C is formed.It is (as shown in Figure 4) as can be seen that B with reference to transmission electron microscope (Titan ETEM G2) analysis result4C
Nano grain surface wrapping layer is amorphous carbon layer, and thickness is less than 5nm.As shown in Fig. 3 (a), obtained from scanning electron microscope
Shape appearance figure (SEM, Hitachi S-4800) as can be seen that powder grain size it is small and uniform.
Embodiment 2
Boric acid (the H that AlfaAesar Chemical Co., Ltd. is produced3BO3) and sucrose (C12H22O11) B in molar ratio:C=1:1
Mixing is added in deionized water and is stirred to being completely dissolved, adds in 5g mixed powders per 100ml deionized waters, obtain water white transparency
Boric acid and sucrose mixed solution；Obtained water white transparency mixed solution with 90 DEG C of heating, dryings and is stirred on constant temperature heating plate
It mixes, obtains red brown solid, solid is ground with agate mortar, Red-brown powder is made；Obtained Red-brown powder is attached to
In graphite crucible, crucible is put into vacuum tube furnace, is less than 10 in tube furnace inner vacuum-3It is begun to warm up after Pa, with 200
DEG C/heating rate of 3min is at the uniform velocity warming up to 1550 DEG C, slow cooling after heat preservation 6 minutes obtains the B of carbon package4C boron carbides are received
Rice flour body.
Analyzed using X-ray diffractometer (Bruker D8) obtaining powder, by with B4The X of C theoretical models simulation
X ray diffraction collection of illustrative plates compares, and powder is mainly by B4C phases are formed；Using Raman spectrometer (HORIBAJobin Yvon) to what is obtained
Powder is analyzed, and main component is by B4C and C is formed.As shown in Fig. 3 (b), it can be seen that the grain size of powder is small and uniform.
Embodiment 3
Boric acid (the H that AlfaAesar Chemical Co., Ltd. is produced3BO3) and sucrose (C12H22O11) B in molar ratio:C=1:1
Mixing is added in deionized water and is stirred to being completely dissolved, adds in 5g mixed powders per 100ml deionized waters, obtain water white transparency
Boric acid and sucrose mixed solution；By obtained water white transparency mixed solution on constant temperature heating plate with 200 DEG C of heating, dryings simultaneously
Stirring, obtains red brown solid, solid is ground with agate mortar, and Red-brown powder is made；Obtained Red-brown powder is filled
Into graphite crucible, crucible is put into vacuum tube furnace, is less than 10 in tube furnace inner vacuum-3It is begun to warm up after Pa, with 8
DEG C/heating rate of min is at the uniform velocity warming up to 1600 DEG C, slow cooling after heat preservation 8 minutes obtains the B of carbon package4C boron carbides are received
Rice flour body.
Analyzed using X-ray diffractometer (Bruker D8) obtaining powder, by with B4The X of C theoretical models simulation
X ray diffraction collection of illustrative plates compares, and powder is mainly by B4C phases are formed；Using Raman spectrometer (HORIBA Jobin Yvon) to obtaining
Powder analyzed, main component is by B4C and C is formed.As shown in Fig. 3 (c), it can be seen that the grain size of powder is small and equal
It is even.
Embodiment 4
Boric acid (the H that AlfaAesar Chemical Co., Ltd. is produced3BO3) and sucrose (C12H22O11) B in molar ratio:C=1:1
Mixing is added in deionized water and is stirred to being completely dissolved, adds in 5g mixed powders per 100ml deionized waters, obtain water white transparency
Boric acid and sucrose mixed solution；Will) obtained water white transparency mixed solution on constant temperature heating plate with 100 DEG C of heating, dryings simultaneously
Stirring, obtains red brown solid, solid is ground with agate mortar, and Red-brown powder is made；Obtained Red-brown powder is filled
Into graphite crucible, crucible is put into vacuum tube furnace, is less than 10 in tube furnace inner vacuum-3It is begun to warm up after Pa, with 200
DEG C/heating rate of 3min is at the uniform velocity warming up to 1600 DEG C, heat preservation slow cooling after ten minutes obtains the B of carbon package4C boron carbides
Nano-powder.
Analyzed using X-ray diffractometer (Bruker D8, Germany) obtaining powder, by with B4C theory moulds
The X ray diffracting spectrum that pattern is intended compares, and powder is mainly by B4C phases are formed；Utilize Raman spectrometer (HORIBA Jobin
Yvon) obtained powder is analyzed, main component is by B4C and C is formed.As shown in Fig. 3 (d), it can be seen that powder
Grain size is small and uniform.
Claims (1)
1. prepare the method for the boron carbide nano-powder of carbon package, it is characterised in that：It includes the following steps：
(1) by boric acid (H3BO3) and sucrose (C12H22O11) B in molar ratio:C=1:1 mixing, obtains mixed powder, by every 100ml
The ratio of the mixed powder of 5g boric acid and sucrose is added in deionized water, mixed powder is added in deionized water and is stirred to complete
Fully dissolved obtains the boric acid of water white transparency and sucrose mixed solution；
(2) the water white transparency mixed solution that step (1) obtains in 80-120 DEG C of heating, drying and is stirred, obtains bronzing and consolidate
Body grinds solid with agate mortar, and Red-brown powder is made；
(3) Red-brown powder that step (2) obtains is attached in graphite crucible, crucible is put into tube furnace, in tube furnace
Portion's vacuum is less than 10-3It is begun to warm up after Pa, is warming up to 1550-1600 DEG C, slow cooling after heat preservation 5-10 minutes obtains carbon package
B4C boron carbide nano-powders.
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| CN201810189072.3A CN108249443A (en) | 2018-03-08 | 2018-03-08 | A kind of method for the boron carbide nano-powder for preparing carbon package |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019624A (en) * | 2018-09-27 | 2018-12-18 | 西安科技大学 | A kind of low temperature synthesizing flaky ZrB2The method of superfine powder |
| CN112194491A (en) * | 2020-10-15 | 2021-01-08 | 山东亚赛陶瓷科技有限公司 | Pressureless sintering boron carbide ceramic powder and preparation method and application thereof |
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| CN104261408A (en) * | 2014-09-18 | 2015-01-07 | 山东大学 | Method for synthesizing boron carbide nano-powder by utilizing sol-gel method |
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2018
- 2018-03-08 CN CN201810189072.3A patent/CN108249443A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261408A (en) * | 2014-09-18 | 2015-01-07 | 山东大学 | Method for synthesizing boron carbide nano-powder by utilizing sol-gel method |
Non-Patent Citations (1)
| Title |
|---|
| 林爽: "低温前驱体裂解法合成碳化硼粉体的研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019624A (en) * | 2018-09-27 | 2018-12-18 | 西安科技大学 | A kind of low temperature synthesizing flaky ZrB2The method of superfine powder |
| CN109019624B (en) * | 2018-09-27 | 2021-12-03 | 西安科技大学 | Low-temperature synthesized flaky ZrB2Method for preparing superfine powder |
| CN112194491A (en) * | 2020-10-15 | 2021-01-08 | 山东亚赛陶瓷科技有限公司 | Pressureless sintering boron carbide ceramic powder and preparation method and application thereof |
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Application publication date: 20180706 |