CN108863373A - A kind of preparation method of graphene/carbon boron ceramic composite - Google Patents
A kind of preparation method of graphene/carbon boron ceramic composite Download PDFInfo
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- CN108863373A CN108863373A CN201810820900.9A CN201810820900A CN108863373A CN 108863373 A CN108863373 A CN 108863373A CN 201810820900 A CN201810820900 A CN 201810820900A CN 108863373 A CN108863373 A CN 108863373A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
Abstract
The present invention provides a kind of preparation method of graphene/carbon boron ceramic composite and the product according to prepared by this method, preparation step include：Expanded graphite powder is pre-processed under ultrasound, obtains flake graphite alkene suspension, then with boron carbide powder, binder mixed grinding, mist projection granulating is then carried out, obtains powder；It is sintered under vacuum or ar gas environment using dual temperature heat pressing process, obtains graphene/carbon boron ceramic composite.Heat pressing process proposed by the present invention can reduce the long-time heating temperature of boron carbide ceramics, obtain the tissue that crystal boundary is complete, crystal grain is tiny, and this material has excellent mechanical property, can be used for armour or wear resistant appliance.Present invention process can effectively improve flake graphite alkene dispersing uniformity in boron carbide, and be easy to carry out industrial amplification, be suitable for large-scale production.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, are related to the preparation process of boron carbide ceramics material, especially a kind of
The preparation method of graphene/carbon boron ceramic composite.
Background technique
Boron carbide ceramics material have it is high-strength, high it is hard, High-temperature-resandant andant wear-resistant is good, density is small, fabulous ballistic performance etc. is all
More advantages can reduce the weight of protective device itself while providing shellproof protection, be that bullet-proof vest and aircraft cockpit are contour
Hold the preferred material of protective device.But the sintering of boron carbide ceramics material is extremely difficult, needs in 2300 DEG C or more sintering
Comparatively dense material can be obtained, and it is broken brittleness and is usually only no more than 2.5MPam1/2, preparation cost is high, prevents more
It is poor to send out resilience energy power, limits it and is more widely applied.For this purpose, there has been proposed the method for many toughenings, as long fibre toughening,
Crystal whisker toughened, yttria stabilizator etc., the complex process that these method for toughening have, it is difficult to large-scale production, some toughening effects
It is limited, it cannot fundamentally solve the brittleness problems of boron carbide ceramics material.
Graphene is to be currently known the highest material of intensity, and it is various composite materials that ideal tensile strength, which is 110~130GPa,
Ideal reinforcement.But graphene is easy to reunite, and often will disperse unevenness in ceramic matrix, it is difficult to reach the strong of anticipation
Toughening effect.
Summary of the invention
The present invention provides the methods that high efficiency prepares graphene/carbon boron ceramic composite, to solve graphene original
The densification sintering problem of the problem of expecting higher cost, difficulties in dispersion and boron carbide ceramics.Dual temperature proposed by the present invention is quick
Heat pressing process can obviously reduce long-time heating temperature, and graphene uniform is scattered in boron carbide, and crystal boundary structure is complete, fine and close, from
And the graphene/carbon boron ceramic composite of function admirable is obtained, and this material is applied to bulletproof armour or wearable device
Part.
The technical scheme is that be achieved by following processing steps：
Crystalline flake graphite is heated expansion, heating power 900W by step 1 in micro-wave oven, and heating time is 20~40s,
Obtained thermal expansion graphite is add to deionized water again, and carries out ultrasonic agitation dispersion, expanded graphite is shredded as sheet
Graphene；
Boron carbide powder is added in flake graphite alkene suspension in step 2, and high energy ball is carried out in planetary ball mill
20~40h is ground, after ball milling mixing is uniform, mist projection granulating obtains powder；
Step 3, by step 2 obtain powder be put into graphite jig, under vacuum conditions, first with 70~100 DEG C/
The speed of min is warming up to 2250 DEG C, and after keeping the temperature 5min, fast cooling keeps the temperature 30~60min to 2050 DEG C, is entirely being sintered
Apply the pressure of 30~50MPa in the process.
Preferably, boron carbide described in step 2 is made of two kinds of boron carbide powders of thickness, and the average particle size particle size of coarse powder is 3
~8 μm, the average particle size particle size of fine powder is 0.2~0.5 μm, and the mass ratio of coarse powder and fine powder is 1:(2~3).
A kind of boron carbide ceramics composite material described in this patent is made of boron carbide matrix phase and graphene, it is preferred that
The proportion of the graphene in the material is 0.5~5wt%.
Compared with the existing technology, the present invention has the following advantages that：
1. heat pressing process proposed by the present invention can reduce the long-time heating temperature of boron carbide ceramics, graphene uniform dispersion
In boron carbide, the tissue that crystal boundary is complete, crystal grain is tiny is obtained, crystal boundary structure is complete, fine and close；This material has excellent power
Performance is learned, can be used for armour or wear resistant appliance.
2. present invention process can effectively improve flake graphite alkene dispersing uniformity in boron carbide, and be easy progress industry and put
Greatly, it is suitable for large-scale production.
3. graphene/carbon boron ceramic composite intensity prepared by the present invention is high, toughness is big, especially suitable for special purpose vehicle
Protection field.
Specific embodiment
Below in conjunction with two specific embodiments, exemplary illustration and help further understand the present invention.But embodiment is specific
Details does not represent whole technical solutions under present inventive concept merely to illustrate the present invention, therefore should not be construed as to this
The restriction of the technical solution of invention.Some unsubstantialities without departing from present inventive concept are changed, such as with same or similar
The technical characteristic of technical effect simply changes or replaces, and belongs to rights protection scope of the present invention.
Embodiment 1
A kind of preparation method of graphene/carbon boron ceramic composite, preparation process include the following steps：
Crystalline flake graphite, is heated expansion by step 1 in micro-wave oven, and heating power 900W, heating time 30s are obtained
Thermal expansion graphite；It weighs 1 part (mass fraction) to be added in 10 parts of deionized waters, 2h is stirred by ultrasonic, obtains flake graphite alkene
Suspension；
99 parts of boron carbide powder (mass fraction), celestial body of being expert at is added in step 2 in above-mentioned sheet graphene suspension
High-energy ball milling 40h is carried out in grinding machine, after ball milling mixing is uniform, mist projection granulating obtains powder；Wherein, boron carbide is by two kinds of thickness
Powder constituent, the average particle size particle size of coarse powder are 8 μm, and the average particle size particle size of fine powder is 0.5 μm, the mass ratio of coarse powder and fine powder
It is 1:2.
The powder that step 2 obtains is put into graphite jig by step 3, under vacuum conditions, first with 100 DEG C/min's
Speed is warming up to 2250 DEG C, and after keeping the temperature 5min, fast cooling keeps the temperature 45min to 2050 DEG C, applies in entire sintering process
The pressure of 50MPa.
Step 4 after sintered heat insulating, turns off heating power supply, fine and close graphene/carbon boron is made in furnace cooling
Ceramic composite.The bending strength of gained composite material is greater than 450MPa, and fracture toughness is greater than 6.5MPam1/2, Vickers hardness
Greater than 31GPa.
Embodiment 2
A kind of preparation method of graphene/carbon boron ceramic composite, preparation process include the following steps：
Crystalline flake graphite, is heated expansion by step 1 in micro-wave oven, and heating power 900W, heating time 40s are obtained
Thermal expansion graphite；It weighs 2 parts (mass fractions) to be added in 15 parts of deionized waters, 2h is stirred by ultrasonic, obtains flake graphite alkene
Suspension；
98 parts of boron carbide powder (mass fraction), celestial body of being expert at is added in step 2 in above-mentioned sheet graphene suspension
High-energy ball milling 40h is carried out in grinding machine, after ball milling mixing is uniform, mist projection granulating obtains powder；Wherein, boron carbide is by two kinds of thickness
Powder constituent, the average particle size particle size of coarse powder are 6 μm, and the average particle size particle size of fine powder is 0.4 μm, the mass ratio of coarse powder and fine powder
It is 1:2.
The powder that step 2 obtains is put into graphite jig by step 3, under vacuum conditions, first with the speed of 80 DEG C/min
Degree is warming up to 2250 DEG C, and after keeping the temperature 5min, fast cooling keeps the temperature 60min to 2050 DEG C, applies in entire sintering process
The pressure of 40MPa.
Step 4 after sintered heat insulating, turns off heating power supply, fine and close graphene/carbon boron is made in furnace cooling
Ceramic composite.The bending strength of gained composite material is greater than 420MPa, and fracture toughness is greater than 7.5MPam1/2, Vickers hardness
Greater than 30GPa.
Claims (4)
1. a kind of graphene/carbon boron ceramic composite, it is characterised in that：The composite material is by boron carbide matrix phase and graphite
Alkene composition, the proportion of the graphene in the material are 0.5~5wt%.
2. the preparation method of graphene/carbon boron ceramic composite as described in claim 1, it is characterized in that preparation method packet
Include following steps：
Crystalline flake graphite is heated expansion, heating power 900W by step 1 in micro-wave oven, and heating time is 20~40s, then
Obtained thermal expansion graphite is add to deionized water, and carries out ultrasonic agitation dispersion, and expanded graphite is shredded as flake graphite
Alkene；
Step 2 is added boron carbide powder in obtained flake graphite alkene suspension, and carries out high energy in planetary ball mill
20~40h of ball milling, after ball milling mixing is uniform, mist projection granulating obtains powder；
The powder that step 2 obtains is put into graphite jig by step 3, under vacuum conditions, first with 70~100 DEG C/min's
Speed is warming up to 2150 DEG C, and after keeping the temperature 5min, fast cooling keeps the temperature 30min, apply 30 in entire sintering process to 1950 DEG C
The pressure of~50MPa.
3. the preparation method of graphene/carbon boron ceramic composite as claimed in claim 2, it is characterised in that：Step 2
Described in boron carbide be made of two kinds of boron carbide powders of thickness, the average particle size particle size of coarse powder is 3~8 μm, average of fine powder
Particle size is 0.2~0.5 μm, and the mass ratio of coarse powder and fine powder is 1:2~3.
4. graphene/carbon boron ceramic composite as described in claim 1 is for making armour or wear resistant appliance.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111766184A (en) * | 2020-06-30 | 2020-10-13 | 吉林大学 | Method for measuring particle size distribution of titanium hydride powder compact |
| CN111943679A (en) * | 2020-08-10 | 2020-11-17 | 宁波普莱斯帝金属制品有限公司 | Preparation method and application of boron-rich boron carbide material |
| CN113788681A (en) * | 2021-10-12 | 2021-12-14 | 景德镇学院 | Boron carbide light bulletproof material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383527A (en) * | 2018-03-21 | 2018-08-10 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of graphene/carbon boron ceramic composite |
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- 2018-07-24 CN CN201810820900.9A patent/CN108863373A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108383527A (en) * | 2018-03-21 | 2018-08-10 | 浙江立泰复合材料股份有限公司 | A kind of preparation method of graphene/carbon boron ceramic composite |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111766184A (en) * | 2020-06-30 | 2020-10-13 | 吉林大学 | Method for measuring particle size distribution of titanium hydride powder compact |
| CN111943679A (en) * | 2020-08-10 | 2020-11-17 | 宁波普莱斯帝金属制品有限公司 | Preparation method and application of boron-rich boron carbide material |
| CN113788681A (en) * | 2021-10-12 | 2021-12-14 | 景德镇学院 | Boron carbide light bulletproof material and preparation method thereof |
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Application publication date: 20181123 |