CN106431417A - High-hardness high-toughness B4C-W2B5-C composite ceramic and preparation method thereof - Google Patents
High-hardness high-toughness B4C-W2B5-C composite ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-hardness high-toughness B4C-W2B5-C composite ceramic. W2B5 and C are uniformly distributed in the matrix B4C, wherein the mole ratio of the B4C to the W2B5 is 1:4, and the C accounts for 5-10 vol% of the total product. The preparation method comprises the following steps: weighing boron powder, graphite powder and WC powder according to the mole ratio of 17:2:2, adding graphite powder which accounts for 5-10 vol% of the total powder above, carrying out dry milling by using a ball mill, and carrying out pre-press forming; and finally, putting in a sintering furnace, keeping the temperature at 1000-1200 DEG C for 3-5 minutes while ensuring the sintering pressure at 30 MPa, keeping the temperature at 1400-1550 DEG C for 3-5 minutes, and keeping the temperature at 1700 DEG C for 6-10 minutes. The compaction temperature of the composite ceramic is 1700 DEG C, and the fracture toughness is up to 7.8-11.9 MPa.mm<1/2>.
Description
Technical field
The invention belongs to composite ceramic material technical field is and in particular to a kind of high hardness high toughness B4C-W2B5- C is combined
Pottery, further relates to the preparation method of this composite ceramics.
Background technology
Boron carbide (B4C) pottery is important wear-resistant and high rigidity structural ceramic material in new ceramics, is a kind of weight
The engineering material wanted, its hardness is only second to diamond and cubic boron nitride, because boron and carbon are all nonmetalloid, and atom
Radius is close, and its combination is different from general interstitial compound, and therefore boron carbide ceramics has high-melting-point (2450 DEG C), superelevation
Hardness (>30GPa), low-density (2.52g/cm3), is the 1/3 of iron and steel, and elastic modelling quantity is high, is 450GPa, its thermal coefficient of expansion
Low, thermal conductivity is higher, many unique excellent properties such as wear-resistant and corrosion-resistant, in national defence, nuclear energy, Aero-Space, machinery, resistance to
The fields such as mill technology, are just increasingly showing its wide development and application prospect.
But, the densification sintering of pure boron carbide is extremely difficult, because the covalent linkage content of boron carbide is very high
(93.9%), higher than other structures pottery, such as SiC (88%), Si3N4 (70%) etc., plasticity is very poor in addition, crystal boundary moving resistance
Greatly, surface tension very little during solid-state, atom activation energy is high, and sintering activating energy is low, makes elimination, crystal boundary and the body of boron carbide inner air vent
The mechanism of mass transmission of long-pending diffusion need to be more than 2000 DEG C, thus determining boron carbide is a kind of ceramic material of extremely difficult sintering.Normal pressure
Under be typically only capable to obtain the relative density of 80%-87% in 2300 DEG C of sintering, sinter at such high temperatures, crystal grain can be quick
It is roughened and grows up, be unfavorable for the exclusion of pore, will result in substantial amounts of Residual Pores makes material density be restricted, product mechanical property
Can poor, in addition sintering temperature is too high, fracture toughness low it is impossible to meet practical application, therefore, determine boron carbide apply core ask
Topic is exactly the densification process of material and reduces sintering temperature, improves fracture toughness.
Most researcheres are by adding the second toughness mutually to strengthen boron carbide, such as SiC at presentW、TiB2Deng employing no
Pressure sintering, the method such as hot pressed sintering, but sintering temperature is still higher, and densification temperature reaches 1900 DEG C -2200 DEG C, exists hard
Degree and toughness can not reach balance, and the problem of high cost.
Content of the invention
It is an object of the invention to provide a kind of high hardness high toughness B4C-W2B5- C composite ceramicses, it has high-compactness, height
Hardness, the feature of high tenacity, solve existing B4C ceramic post sintering and densification temperature are high, and the shortcoming that toughness is low.
It is a further object of the present invention to provide above-mentioned B4C-W2B5The preparation method of-C composite ceramicses.
A technical scheme of the present invention is, a kind of high hardness high toughness B4C-W2B5- C composite ceramicses, W2B5And C
It is uniformly distributed in matrix B4In C, wherein B4C and W2B5Mol ratio be 1:4, C volume account for product cumulative volume 5～
10vol%.
W2B5And B4The particle diameter of C is respectively 0.2-0.6 μm and 0.2-0.5 μm, and C is list structure, and length is about 0.6～
1.5um, width is about 45～58nm.
Another technical scheme of the present invention is, above-mentioned B4C-W2B5The preparation method of-C composite ceramicses, including with
Lower step：
Step 1, is 17 according to mol ratio:2:2 ratio weighs B powder (boron powder), C powder (graphite powder) and WC powder, Ran Houzai
Add the C powder (graphite powder) of above total powder volume 5～10vol%, dry grinded using ball mill, the abrasive material being uniformly mixed；
Step 2, by the abrasive material pre-molding of mix homogeneously；
Step 3, the abrasive material of pre-molding is placed in sintering furnace it is ensured that sintering pressure be 30Mpa, first 1000 DEG C～
1200 DEG C of scope inside holding 3-5min, then in 1400～1550 DEG C of scope inside holding 3-5min, are finally incubated 6- at 1700 DEG C
10min, obtains B4C-W2B5- C composite ceramicses.
Above-mentioned preparation method also has the characteristics that：
The B powder footpath of step 1 is 10-20 μm, and C powder adopts the graphite powder that particle diameter is 20-30 μm, the particle diameter of WC powder<10μm.
Dry grinded using tungsten-carbide ball grinding jar in step 2, ratio of grinding media to material be (8～12): 1wt%, Ball-milling Time be 10～
14 hours, rotating speed was 150～200 revs/min.
In step 3, heating rate is：0～(1000 DEG C -1200 DEG C) is (100 DEG C～120 DEG C)/min, (1000 DEG C -
1200 DEG C)-(1400 DEG C～1550 DEG C) be 50 DEG C/min, -1700 DEG C of (1400 DEG C～1550 DEG C) are 20～25 DEG C/min.
The preparation method of the present invention is in-situ synthesis, and its principle is：
(1) (B+C) and (B+WC) are reaction in-situ, through following calculation of thermodynamics, temperature 298k-2000k it
Between, Gibbs free energyIllustrate that this reaction is a kind of self- propagating exothermic reaction, reacting driving force is big, it is possible to use
Reaction in-situ liberated heat reduces sintering temperature, in addition, using in-situ reactive synthesis method so that C, B4C and W2B5Between
Clean interfaces, be well combined, determined basis for good mechanical property pad.
4B+C=B4C (a)
5B+2WC=W2B5+2C (b)
Can be obtained by the reaction enthalpy and Gibbs free energy calculating reaction equation (a) (b)：
ΔH(2200K)1=-81.42kJ/mol (c)
ΔH(2200K)2=-508.86kJ/mol (d)
In 298K-2000KCan be seen that from thermodynamic (al) calculating, in this temperature range,
The Gibbs free energy of reaction is less than zero, and reaction is exothermic reaction, illustrates that reaction can be carried out.
(2) B+C reaction in-situ can adjust the ratio of B and C, controls the C in product
B+C+WC→W2B5+B4C+C
Advantage using in-situ synthetic method is：The ratio of B and C being adjusted, thus controlling the C content in product, entering
And can get the preferable composite of mechanical property.Traditional method directly adopts B4The former powder sintering of C, will generate one in product
Quantitative C, and uncontrollable content, so can affect the correlated performance of composite.
The invention has the beneficial effects as follows, this invention employs the preparation method of fabricated in situ, the heat released using its reaction
Amount reduces sintering temperature, and the present invention sinters at 1700 DEG C, you can reach 100% densification, and traditional sintering method and former powder
Sintering, densification sintering temperature is at 1900～2200 DEG C.The B of present invention preparation4C-W2B5Composite ceramicses have excellent comprehensive
Energy：Only 1700 DEG C of densification temperature, high-fracture toughness (7.8～11.9MPa mm1/2).
Brief description
Fig. 1 is the B of the present invention4C-W2B5The XRD (X-ray diffractogram) of-C composite ceramicses；Wherein, (a) 4B4C+W2B5, (b)
4B4C+W2B5+ 5%C, (c) 4B4C+W2B5+ 10%C；
Fig. 2 is the B of the present invention4C-W2B5Scanning electron microscope micro- (SEM) photo of-C composite ceramicses fracture；
Fig. 3 is the B of the present invention4C-W2B5Projection Electronic Speculum (TEM) photo of-C composite ceramicses.
Specific embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings, but the present invention is not limited to this
A little embodiments.
Embodiment 1
According to required sintered specimen a size of Φ 20mm × 22mm, weigh boron powder 10.75g, graphite powder 1.138g, WC powder
(mol ratio is 21 to 18.55g:2:2), add the graphite powder of above total powder volume 5vol%.Boron powder footpath is 10-20 μm,
Graphite powder adopts the graphite powder that particle diameter is 20-30 μm, the particle diameter of WC powder<10μm.Tungsten carbide ball milling is put in the mixing of above powder
In tank, add tungsten carbide milling balls, ratio of grinding media to material is 10: 1wt%, ball milling 12 hours on PM100 planetary ball mill, rotating speed is
200 revs/min, rested 20 minutes every 1 hour, prevent Ball-milling Time long and lead to the ball grinder every 4 hour medications of heating
The powder being bonded on ball grinder and abrading-ball is separated by spoon.The good mixed-powder of ball milling is loaded into a size of Φ 20..4mm
In the graphite jig of × 40mm, the inwall of graphite grinding tool needs the graphite paper of one layer of 0.2mm of pad, and the two ends of graphite pressure head also need
Graphite paper on pad, prevents sample in sintering process from adhering on graphite jig inwall and pressure head, is then compacted with Manual tablet pressing machine, then
The powder being compacted and graphite grinding tool are put into sintering in LABOX-330 type discharge plasma sintering stove, sintering temperature is 1700 DEG C,
Using the sintering parameter of 1100 DEG C of three step thermal-insulating method (insulation 5min) -1550 DEG C (insulation 5min) -1700 DEG C (insulation 6min), burn
Knot pressure is by force 30MPa, and heating rate is：0-1100 DEG C is 100 DEG C/min, and 1100 DEG C -1550 DEG C is 50 DEG C/min, 1500 DEG C -
1700 DEG C is 25 DEG C/min.After sintering completes, reuse Manual tablet pressing machine by the sample demoulding, obtain B through above-mentioned steps4C-
W2B5The volume fraction shared by C in-C composite ceramicses, wherein product is 5vol%.
The reactive mode of the present embodiment is：
21B+2C+2WC→W2B5+4B4C+C (1)
Embodiment 2
According to required sintered specimen a size of Φ 20mm × 22mm, weigh the boron powder of size same as Example 1
(mol ratio is 21 for 10.75g, graphite powder 1.138g, WC powder 18.55g:2:2), add the stone of above total powder volume 7vol%
Powdered ink, then repeats the operating procedure of embodiment 1, wherein, operating parameter is：Ratio of grinding media to material is 8: 1wt%, and ball milling 10 hours turns
180 revs/min of speed；Using -1700 DEG C of (insulations of -1400 DEG C of 1000 DEG C of three step thermal-insulating method (insulation 5min) (insulation 5min)
Sintering parameter 10min), sintering pressure is 30MPa.Heating rate is：0-1000 DEG C is 120 DEG C/min, 1000 DEG C -1450 DEG C
For 50 DEG C/min, 1450 DEG C -1700 DEG C is 25 DEG C/min.Obtain B through above-mentioned steps4C-W2B5- C composite ceramicses.Wherein in product
Volume fraction shared by C is 7vol%.
The reactive mode of the present embodiment is：
21B+2C+2WC→W2B5+4B4C+C (2)
Embodiment 3
According to required sintered specimen a size of Φ 20mm × 22mm, weigh the boron powder of size same as Example 1
(mol ratio is 21 for 10.75g, graphite powder 1.138g, WC powder 18.55g:2:2), add above total powder volume 10vol%'s
Graphite powder, then repeats the operating procedure of embodiment 1, wherein, operating parameter is：Ratio of grinding media to material is 12: 1wt%, ball milling 14 hours,
150 revs/min of rotating speed；Using -1700 DEG C of (insulations of -1550 DEG C of 1200 DEG C of three step thermal-insulating method (insulation 3min) (insulation 3min)
Sintering parameter 6min), sintering pressure is 30MPa.Heating rate is：0-1200 DEG C is 100 DEG C/min, 1200 DEG C -1400 DEG C
For 50 DEG C/min, 1400 DEG C -1700 DEG C is 20 DEG C/min.Obtain B through above-mentioned steps4C-W2B5- C composite ceramicses.Wherein in product
Volume fraction shared by C is 10vol%.
The reactive mode of the present embodiment is：
21B+2C+2WC→W2B5+4B4C+C (3)
Comparative example
According to required sintered specimen a size of Φ 20mm × 22mm, weigh boron powder 10.75g, graphite powder 1.138g, WC powder
(mol ratio is 21 to 18.55g:2:2), obtain B4C-W2B5Composite ceramicses.W in this material2B5And B4The mol ratio of C is 1:4, product
In there is no carbon.
The reaction equation of comparative example is：
21B+2C+2WC=W2B5+4B4C (4)
Embodiment is observed using XRD-7000 type X-ray diffractometer and JSM-6700F type field emission scanning electron microscope
The thing phase of product and microstructure, XRD figure is shown in Fig. 1, and be can be seen that by figure increases with C content, and the diffraction maximum of C gradually strengthens,
Illustrate in product, there is remaining C.In XRD spectrum, B4The diffraction maximum of C is relatively low, this is because B and C are light element relative to W, spreads out
Penetrate low intensity, therefore B4The diffraction maximum of C reduces.Its SEM figure is shown in Fig. 2, can be seen that composite ceramicses microstructure of the present invention by figure
Matrix B by black4C and C, the W of Lycoperdon polymorphum Vitt strip2B5Composition, and be evenly distributed.In addition it can also be seen that having from fracture photo
W2B5The extracting of granule, this is also the main cause that fracture toughness increases.W2B5And B4The particle diameter of C be respectively 0.2-0.6 μm and
0.2-0.5 μm of other C is list structure, and length is about 0.6-1.5um, and width is about 45-58nm.Transmission photo as Fig. 3 can
Find out, the method makes C, B4C and W2B5Between clean interfaces, be well combined.
B by embodiment4C-W2B5- C composite ceramicses and the B of comparative example4C pottery through linear cutter for 2mm × 4mm ×
20mm, central indentation is the bar-shaped sample of 2mm, by SANS universal testing machine, sample is carried out with performance test, and processing is remaining
Sample carries out the test such as hardness；Density measurement is carried out using Archimedes's drainage；Using the fracture of three-point bending method test galley proof
Toughness；With B4C-W2B5Pottery carries out performance comparison, B for matched group4C-W2B5- C composite ceramicses and B4C-W2B5The densification of pottery
Degree, hardness, fracture toughness the results are shown in Table 1.
Technique and properties of sample that each embodiment of table 1 adopts
From result above, by aforementioned proportion, using discharge plasma sintering, three step thermal-insulating method preparation B4C-W2B5-
C composite ceramicses, can a step lifting B4C-W2B5Toughness, hardness be 19.3～30.2GPa, fracture toughness be 9.5-11.9MPa
mm1/2.Especially, when adding the C of 5vol%, combination property is the most excellent, and hardness is 30.2GPa, and fracture toughness can reach
11.9MPa·mm1/2, the B of preparation is sintered with same procedure4C-W2B5Compare, fracture toughness is greatly improved.
Claims (6)
1. a kind of high hardness high toughness B4C-W2B5- C composite ceramicses are it is characterised in that W2B5It is uniformly distributed in matrix B with C4In C,
Wherein B4C and W2B5Mol ratio be 1:4, C volume accounts for 5～10vol% of product cumulative volume.
2. high hardness high toughness B according to claim 14C-W2B5- C composite ceramicses are it is characterised in that described W2B5With
B4The particle diameter of C is respectively 0.2-0.6 μm and 0.2-0.5 μm, and C is list structure, and length is about 0.6-1.5um, and width is about 45-
58nm.
3. a kind of B as claimed in claim 14C-W2B5The preparation method of-C composite ceramicses is it is characterised in that include following walking
Suddenly：
Step 1, is 17 according to mol ratio:2:2 ratio weighs boron powder, graphite powder and WC powder, then adds above powder more total
The graphite powder of volume 5～10vol%, is dry grinded using ball mill, the abrasive material being uniformly mixed；
Step 2, by the abrasive material pre-molding of mix homogeneously；
Step 3, the abrasive material of pre-molding is placed in sintering furnace it is ensured that sintering pressure is 30Mpa, first 1000 DEG C～1200
DEG C scope inside holding 3-5min, then in 1400～1550 DEG C of scope inside holding 3-5min, is finally incubated 6- at 1700 DEG C
10min, obtains B4C-W2B5- C composite ceramicses.
4. B according to claim 34C-W2B5The preparation method of-C composite ceramicses is it is characterised in that described boron powder footpath
For 10-20 μm, graphite powder particle diameter is 20-30 μm, the particle diameter of WC powder<10μm.
5. B according to claim 34C-W2B5The preparation method of-C composite ceramicses is it is characterised in that described dry grinding uses
Tungsten-carbide ball grinding jar is carried out, ratio of grinding media to material be (8～12): 1wt%, Ball-milling Time be 10～14 hours, rotating speed be 150～200 turns/
Minute.
6. B according to claim 34C-W2B5The preparation method of-C composite ceramicses is it is characterised in that the liter of described sintering
Warm speed is：0～(1000 DEG C -1200 DEG C) is (100 DEG C～120 DEG C)/min, (1000 DEG C -1200 DEG C)-(1400 DEG C～1550
DEG C) it is 50 DEG C/min, -1700 DEG C of (1400 DEG C～1550 DEG C) are 20～25 DEG C/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142473A (en) * | 2020-09-29 | 2020-12-29 | 东北大学 | B4C-based double-layer ceramic composite material and preparation method thereof |
| CN113387704A (en) * | 2021-06-24 | 2021-09-14 | 武汉理工大学 | Boron carbide-titanium boride light high-strength composite ceramic material and preparation method thereof |
| CN113894461A (en) * | 2021-10-12 | 2022-01-07 | 广州汉源新材料股份有限公司 | Glass-based sealing composition, sealing slurry, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112142473A (en) * | 2020-09-29 | 2020-12-29 | 东北大学 | B4C-based double-layer ceramic composite material and preparation method thereof |
| CN113387704A (en) * | 2021-06-24 | 2021-09-14 | 武汉理工大学 | Boron carbide-titanium boride light high-strength composite ceramic material and preparation method thereof |
| CN113894461A (en) * | 2021-10-12 | 2022-01-07 | 广州汉源新材料股份有限公司 | Glass-based sealing composition, sealing slurry, and preparation method and application thereof |
| CN113894461B (en) * | 2021-10-12 | 2023-01-03 | 广州汉源新材料股份有限公司 | Glass-based sealing composition, sealing slurry, and preparation method and application thereof |
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