CN103910345A - Preparation method of boron nitride composite material - Google Patents
Preparation method of boron nitride composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a boron nitride composite material, which comprises the following steps of: uniformly mixing a boron source, a nitrogen source and a coating base material, and drying to obtain a precursor, wherein the mass ratio of the coating base material to the boron source to the nitrogen source is 1:(1-20):(1-40); and carrying out heat treatment on the precursor in the atmosphere of protective gas at 500-2000 DEG C for 6-18h to obtain the boron nitride composite material. The boron nitride composite material comprises the coating base material and boron nitride which is coated on the surface of the coating base material. Compared with preparation method of traditional boron nitride composite material, the preparation method of the boron nitride composite material does not need to import a crystallization additive, so that impurities are not imported and then the product purity is higher.
Description
Technical field
The present invention relates to field of new material preparation, particularly relate to a kind of preparation method of boron nitride composite.
Background technology
Hexagonal boron nitride is a kind of inorganic materials of graphite-like structure, it is high temperature resistant owing to having, high thermal conductivity, radiation hardness, corrosion-resistant, high temperature lubricating and excellent low dielectric and insulating property, therefore at each key areas, as Electronic Packaging industry, aerospace, national defence and nuclear industry have good application.
Matrix material is owing to having the excellent properties of two or more materials concurrently, the remarkable lifting of the over-all properties of material can be widely used in to each industrial circle, boron nitride composite has the excellent high temperature resistance of boron nitride, high thermal conductance, radiation hardness, corrosion-resistant, high temperature lubricating, low dielectric or insulating property, is with a wide range of applications.The preparation method of traditional boron nitride composite, by nitrogenous source and the reaction of boron source, with auxiliary agent crystallizations such as sodium-chlor, calcium sulfate, calcium carbonate.
The preparation method of traditional boron nitride composite, because impurity is introduced in meeting, causes product purity not high, has seriously limited the application of boron nitride composite.
Summary of the invention
Based on this, be necessary to provide the preparation method of the boron nitride composite that a kind of product purity is higher.
A preparation method for boron nitride composite, comprises the steps:
Boron source, nitrogenous source and coated base material are mixed, after being dried, obtain presoma, wherein, the mass ratio of described coated base material, described boron source and described nitrogenous source is 1:1～20:1～40;
Under shielding gas atmosphere; described presoma is heat-treated; described heat treated temperature is 500 DEG C～2000 DEG C; described heat treated time 6h～18h; obtain described boron nitride composite, described boron nitride composite comprises described coated base material and is coated on the boron nitride of described coated substrate surface.
In one embodiment, described boron source is boric acid, metaboric acid or boron oxide, and described nitrogenous source is trimeric cyanamide, ammonium chloride, brometo de amonio or urea.
In one embodiment, described coated base material is SiO
2, TiO
2, Al
2o
3, AlN, BaTiO
3, CCTO, ferrite, Graphene, silica fiber, carbon fiber or carbon nanotube.
In one embodiment, described being operating as after described boron source, described nitrogenous source and described coated base material are added to a little wetting agent that boron source, nitrogenous source and coated base material are mixed mixed and is ground, and described wetting agent is ethanol or water.
In one embodiment, after described being dried, obtain in the operation of presoma, dry temperature is 60 DEG C～100 DEG C.
In one embodiment, described shielding gas atmosphere is nitrogen atmosphere or atmosphere of inert gases.
In one embodiment, obtain in the operation of described boron nitride composite, described heat treated temperature is 600 DEG C～1200 DEG C, described heat treated time 8h～15h.
In one embodiment, described described presoma is heat-treated as being that 5 DEG C/min～20 DEG C/min heat-treats described presoma according to temperature rise rate.
In one embodiment, the crystalline phase that is coated on the boron nitride of described coated substrate surface described in is six side's phases.
In one embodiment, be also included in after the operation that obtains described boron nitride composite the operation that the described boron nitride composite obtaining is ground.
The preparation method of this boron nitride composite, compared with the preparation method of traditional boron nitride composite, does not need to introduce crystallization auxiliary, thereby can not introduce impurity, thereby product purity is higher.
Brief description of the drawings
Fig. 1 is the preparation method's of the boron nitride composite of an embodiment schema;
Fig. 2 a is silicon-dioxide using particle diameter as 400nm as the scanning electron microscope (SEM) photograph of coated base material, the boron nitride composite that makes according to the method for embodiment 1;
Fig. 2 b is silicon-dioxide using particle diameter as 400nm as the scanning electron microscope (SEM) photograph of coated base material, the boron nitride composite that makes according to the method for embodiment 1;
Fig. 2 c is silicon-dioxide using particle diameter as 800nm as the scanning electron microscope (SEM) photograph of coated base material, the boron nitride composite that makes according to the method for embodiment 1;
Fig. 2 d is silicon-dioxide using particle diameter as 800nm as the scanning electron microscope (SEM) photograph of coated base material, the boron nitride composite that makes according to the method for embodiment 1;
Fig. 3 is the FT-IR contrast spectrogram of boron nitride composite, standard silica and the hexagonal boron nitride of two kinds of particle diameters making of embodiment 1;
Fig. 4 a is the XRD spectra of the boron nitride that makes of embodiment 7;
Fig. 4 b is the XRD spectra of standard hexagonal boron nitride.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details are set forth in the following description so that fully understand the present invention.But the present invention can implement to be much different from alternate manner described here, and those skilled in the art can do similar improvement without prejudice to intension of the present invention in the situation that, and therefore the present invention is not subject to the restriction of following public concrete enforcement.
The preparation method of the boron nitride composite of an embodiment as shown in Figure 1, comprises the steps:
S10, boron source, nitrogenous source and coated base material are mixed, obtain presoma after dry.
The mass ratio of boron source and nitrogenous source is 1:2～10.
The mass ratio of coated base material, boron source and nitrogenous source is 1:1～20:1～40.
Boron source is boric acid, metaboric acid or boron oxide, and nitrogenous source is trimeric cyanamide, ammonium chloride, brometo de amonio or urea.
Under boron source and described nitrogenous source high temperature, decompose, thereby avoided the introducing of impurity.
Coated base material can be inorganic materials, can be also organic polymer material, can be the even more material of large size or various different-shapes of nanometer, micron, only needs to ensure the coated minimum thermal treatment temp that can bear 500 DEG C of base material.Concrete, coated base material is SiO
2, TiO
2, Al
2o
3, AlN, BaTiO
3, CCTO, ferrite, Graphene, silica fiber, carbon fiber or carbon nanotube.
After boron source, nitrogenous source and coated base material are added a little wetting agent by being operating as that boron source, nitrogenous source and coated base material are mixed, mix and be ground.Wetting agent can be ethanol or water.
After dry, obtain in the operation of presoma, dry temperature is 60 DEG C～100 DEG C.
S20, under shielding gas atmosphere, S10 is obtained to presoma and heat-treats, obtain boron nitride composite.
The boron nitride composite making comprises coated base material and is coated on the boron nitride of coated substrate surface.
Heat treated temperature is 500 DEG C～2000 DEG C, heat treated time 6h～18h.
In S20, can be coated by control the mass ratio of base material, boron source and nitrogenous source, the thickness of the boron nitride that is coated on coated substrate surface in the boron nitride composite that regulation and control make.
In a preferred embodiment, heat treated temperature is 600 DEG C～1200 DEG C, heat treated time 8h～15h.
Shielding gas atmosphere can be nitrogen atmosphere or atmosphere of inert gases.Rare gas element is specially helium, neon, argon gas, Krypton or xenon.
To presoma heat-treat for: be that 5 DEG C/min～20 DEG C/min heat-treats presoma according to temperature rise rate.
The crystalline phase of the boron nitride that is coated on coated substrate surface making is six side's phases.
In S20, be also included in after the operation that obtains boron nitride composite the operation that the boron nitride composite obtaining is ground.
The preparation method of this boron nitride composite, compared with the preparation method of traditional boron nitride composite, does not need to introduce crystallization auxiliary, thereby can not introduce impurity, thereby product purity is higher.
The preparation method of this boron nitride composite also tool has the following advantages:
1) use cheap raw material can obtain the boron nitride composite of excellent performance, be conducive to reduce costs;
2) using can high temperature labile boron source and nitrogenous source, has reduced the introducing of impurity, and the boron nitride composite making need not pass through loaded down with trivial details pickling, washing process, just can directly drop into industrial application;
3) special nucleus shell structure, be conducive on the material property basis of coated base material, give excellent heat conductivility, thermomechanical property, dielectric properties, heat or chemical stability etc. that boron nitride composite boron nitride has, and can regulate and control by controlling boron nitride shell thickness the performance of boron nitride composite.
Be specific embodiment below.
Embodiment 1
The preparation method of the boron nitride composite of the present embodiment comprises the steps:
Batching: utilize electronic balance to take respectively boric acid 5g, trimeric cyanamide 10g and silicon-dioxide 3g, dried for standby.
Mix: use the mode of grinding, together with boric acid is first fully mixed with trimeric cyanamide, then add silicon-dioxide fully to mix, add afterwards in crucible.
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under argon gas atmosphere, be warming up to 1000 DEG C with the temperature rise rate of 8 DEG C/min, and being incubated 9h, the boron nitride shell that coated one deck is evenly on silica sphere, purity is higher, obtains boron nitride composite after grinding.
Use respectively silicon-dioxide that particle diameter is 400nm and 800nm as coated base material, method according to embodiment 1 prepares boron nitride composite, the boron nitride composite of two kinds of particle diameters that embodiment 1 is made is observed respectively under scanning electronic microscope, obtains Fig. 2 a～Fig. 2 d.
Can be found out by Fig. 2 a～Fig. 2 d, it is coated that the method for embodiment 1 can form boron nitride at silica sphere, and the boron nitride composite obtaining entirety pattern homogeneous, there will not be impurity.The method of embodiment 1 all has good adaptability to the material of various patterns and size, can realize the evenly coated of boron nitride at the material surface of different-grain diameter.
Boron nitride composite, standard silica and the hexagonal boron nitride of two kinds of particle diameters that embodiment 1 is made carry out FT-IR analysis, obtain Fig. 3.
As seen from Figure 3, the characteristic peak occurring in the FT-IR spectrum of the boron nitride composite of two kinds of particle diameters that embodiment 1 makes and the FT-IR spectrum signature peak of standard silica and hexagonal boron nitride are basic identical, thereby have illustrated that the crystalline phase of the boron nitride in the boron nitride composite that embodiment 1 makes is six side's phases.
Analysis chart 3 can find, silicon-dioxide is at 1115cm
-1strong and the wide absorption peak that place is reflected by Si-O-Si antisymmetric stretching vibration, 808cm
-1, 478cm
-1si-O key symmetrical stretching vibration and the flexural vibration at place, and at 947cm
-1the Si-OH flexural vibration absorption peak at place has demonstration on product, and in addition, in boron nitride, B-N bond bending vibrates the 1391cm causing
-1and 820cm
-1the absorption peak at place also appears on the boron nitride composite of product nucleocapsid structure, then in conjunction with Fig. 2 a～Fig. 2 d, can confirm that in boron nitride composite that embodiment 1 makes, silica sphere is evenly being coated hexagonal boron nitride shell.
Embodiment 2
The preparation method of the boron nitride composite of the present embodiment comprises the steps:
Batching: utilize electronic balance to take respectively metaboric acid 3g, urea 8g and Graphene 3g, dried for standby.
Mix: metaboric acid and urea are dissolved in respectively in 20mL water, then add the aqueous solution or other dispersion liquids of Graphene, fully stir 2h after mixing, product stirring and drying afterwards, then adds in crucible.
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under argon gas atmosphere, be warming up to 800 DEG C with the temperature rise rate of 8 DEG C/min, and being incubated 9h, the boron nitride shell that coated one deck is evenly on grapheme material surface, purity is higher, obtains boron nitride composite after grinding.
Embodiment 3
The preparation method of the boron nitride composite of the present embodiment comprises the steps:
Batching: utilize electronic balance to take respectively boron oxide 4g, ammonium chloride 9g and carbon fiber 1g, dried for standby.
Mix: boron oxide and ammonium chloride are dissolved in respectively in 20mL water, fully stir 2h, afterwards carbon fiber is repeatedly soaked-dries in precursor solution, final step adds in crucible after drying.
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under nitrogen atmosphere, be warming up to 700 DEG C with the temperature rise rate of 8 DEG C/min, and being incubated 11h, the boron nitride shell that coated one deck is evenly on carbon fiber surface, purity is higher, obtains boron nitride composite after grinding.
Embodiment 4
The preparation method of the boron nitride composite of the present embodiment comprises the steps:
Batching: utilize electronic balance to take respectively boric acid 6g, brometo de amonio 13g and aluminium nitride 2g, dried for standby.
Mix: boric acid and brometo de amonio are mixed by mechanical ball milling, and sample is dried, then adds aluminum nitride particle, is ground, and adds afterwards in crucible.
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under argon gas atmosphere, be warming up to 500 DEG C with the temperature rise rate of 8 DEG C/min, and being incubated 14h, the boron nitride shell that coated one deck is evenly on aln surface, purity is higher, obtains boron nitride composite after grinding.
Embodiment 5
The preparation method of the boron nitride composite of the present embodiment comprises the steps:
Batching: utilize electronic balance to take respectively metaboric acid 4g, brometo de amonio 13g and carbon nanotube 2g, dried for standby.
Mix: metaboric acid, brometo de amonio powder dissolution, in water or ethanol, are then added to carbon nanotube, soak after 2h, suction filtration obtains filter cake, dries filter cake, adds afterwards in crucible.
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under nitrogen atmosphere, be warming up to 650 DEG C with the temperature rise rate of 8 DEG C/min, and being incubated 9h, the boron nitride shell that coated one deck is evenly in carbon nano tube surface, purity is higher, obtains boron nitride composite after grinding.
Embodiment 6
The preparation method of the boron nitride composite of the present embodiment comprises the steps:
Batching: utilize electronic balance to take respectively boric acid 4g, brometo de amonio 19g and aluminum oxide 3g, dried for standby.
Mix: boric acid and brometo de amonio are dissolved in 50mL water, then add aluminum oxide, stir 2h, after centrifugal oven dry, transfer in crucible;
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under nitrogen atmosphere, be warming up to 1100 DEG C with the temperature rise rate of 18 DEG C/min, and being incubated 7h, the boron nitride shell that coated one deck is evenly on alumina surface, purity is higher, obtains boron nitride composite after grinding.
Embodiment 7
Batching: utilize electronic balance to take respectively boric acid 5g, trimeric cyanamide 10g, dried for standby.
Mix: use the mode of grinding, together with boric acid is fully mixed with trimeric cyanamide, add afterwards in crucible.
Reaction: crucible is placed in to tube furnace, and sets tube furnace parameter, under argon gas atmosphere, be warming up to 1000 DEG C with the temperature rise rate of 8 DEG C/min, and be incubated 9h, obtain boron nitride material after grinding.
The boron nitride material that embodiment 7 is made carries out XRD analysis, obtains Fig. 4 a.Fig. 4 b is the XRD spectra of standard hexagonal boron nitride.
Can be found out by Fig. 4 a and Fig. 4 b, the boron nitride material that embodiment 7 makes is compared with standard hexagonal boron nitride, all there is the h-BN(002 that is positioned at 26.7 °) crystal face and be positioned at the h-BN(100 of 41.5 °) crystal face, therefore can prove that the boron nitride material that embodiment 7 makes is hexagonal boron nitride.
It should be noted that, in Fig. 4 a and Fig. 4 b, shape and the strength difference at peak are larger, are mainly that (002) face of exposure is more because standard hexagonal boron nitride is micron sheet.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for boron nitride composite, is characterized in that, comprises the steps:
Boron source, nitrogenous source and coated base material are mixed, after being dried, obtain presoma, wherein, the mass ratio of described coated base material, described boron source and described nitrogenous source is 1:1～20:1～40;
Under shielding gas atmosphere; described presoma is heat-treated; described heat treated temperature is 500 DEG C～2000 DEG C; described heat treated time 6h～18h; obtain described boron nitride composite, described boron nitride composite comprises described coated base material and is coated on the boron nitride of described coated substrate surface.
2. the preparation method of boron nitride composite according to claim 1, is characterized in that, described boron source is boric acid, metaboric acid or boron oxide, and described nitrogenous source is trimeric cyanamide, ammonium chloride, brometo de amonio or urea.
3. the preparation method of boron nitride composite according to claim 1, is characterized in that, described coated base material is SiO
2, TiO
2, Al
2o
3, AlN, BaTiO
3, CCTO, ferrite, Graphene, silica fiber, carbon fiber or carbon nanotube.
4. the preparation method of boron nitride composite according to claim 1, it is characterized in that, described being operating as after described boron source, described nitrogenous source and described coated base material are added to a little wetting agent that boron source, nitrogenous source and coated base material are mixed mixed and is ground, and described wetting agent is ethanol or water.
5. the preparation method of boron nitride composite according to claim 1, is characterized in that, after described being dried, obtains in the operation of presoma, and dry temperature is 60 DEG C～100 DEG C.
6. the preparation method of boron nitride composite according to claim 1, is characterized in that, described shielding gas atmosphere is nitrogen atmosphere or atmosphere of inert gases.
7. the preparation method of boron nitride composite according to claim 1, is characterized in that, obtains in the operation of described boron nitride composite, and described heat treated temperature is 600 DEG C～1200 DEG C, described heat treated time 8h～15h.
8. the preparation method of boron nitride composite according to claim 1, is characterized in that, described described presoma is heat-treated as being that 5 DEG C/min～20 DEG C/min heat-treats described presoma according to temperature rise rate.
9. the preparation method of boron nitride composite according to claim 1, is characterized in that, described in be coated on the boron nitride of described coated substrate surface crystalline phase be six side's phases.
10. the preparation method of boron nitride composite according to claim 1, is characterized in that, is also included in after the operation that obtains described boron nitride composite the operation that the described boron nitride composite obtaining is ground.
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