CN102745992B - (ZrB2+ZrC)/Zr3[Al(Si)]4C6Complex phase ceramic material and preparation method thereof - Google Patents
(ZrB2+ZrC)/Zr3[Al(Si)]4C6Complex phase ceramic material and preparation method thereof Download PDFInfo
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- CN102745992B CN102745992B CN201210259673.XA CN201210259673A CN102745992B CN 102745992 B CN102745992 B CN 102745992B CN 201210259673 A CN201210259673 A CN 201210259673A CN 102745992 B CN102745992 B CN 102745992B
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 229910007948 ZrB2 Inorganic materials 0.000 title abstract 3
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 6
- 238000007731 hot pressing Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000010297 mechanical methods and process Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000000137 annealing Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000009413 insulation Methods 0.000 claims description 5
- 230000001186 cumulative effect Effects 0.000 claims description 4
- 230000007246 mechanism Effects 0.000 abstract description 6
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 229910000568 zirconium hydride Inorganic materials 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000013001 point bending Methods 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention relates to an in-situ (ZrB)2+ZrC)/Zr3[Al(Si)]4C6A complex phase ceramic material and a preparation method thereof. The complex phase ceramic material is prepared from ZrB2ZrC reinforcing phase and Zr3[Al(Si)]4C6A matrix composition of which ZrB27.08-21.23% of the total volume of the material, and ZrC 2.92-8.77% of the total volume of the material. Raw material ZrH2Powder, Al powder, Si powder, graphite powder, B4Weighing the C powder according to the molar ratio of 3 to (2.04-3.00) to (0.28-0.42) to (3.28-4.83) to (0.18-0.49), uniformly mixing the raw materials by a physical mechanical method, then putting the mixture into a graphite die coated with BN for cold press molding, and sintering the mixture in a hot pressing furnace with protective atmosphere. The invention has simple process, can synthesize the multi-element complex phase ceramic material by one step, and has excellent comprehensive performance due to the synergistic effect of two different toughness phases and a reinforcing and toughening mechanism in the material.
Description
Technical field:
The present invention relates to ceramic matric composite and preparation method thereof.Be specially a kind of by ZrB
2with the collaborative (ZrB strengthening of the many units of ZrC
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material and preparation method thereof.
Background technology:
Zr
3[Al (Si)]
4c
6it is a kind of novel quaternary stratiform carbide ceramics material, there is high-modulus, high rigidity, anti-oxidant, corrosion-resistant, high conductivity, high heat conductance, stronger advantages such as destruction tolerance, especially its Young's modulus can remain to 1600 ℃, at high-technology fields such as Aeronautics and Astronautics, nuclear industry, ultrahigh-temperature structural parts, has wide practical use.But its intensity and toughness are still on the low side, wear resistance and antioxidant property are poor, and this has seriously limited its application.Complex phase, from Reinforced structure, be the effective way of improving mechanical property, realizing strengthening and toughening.At present existing SiC is introduced in quaternary Zr as wild phase
2[Al (Si)]
4c
5in pottery, its mechanical property and antioxidant property (Guiqing Chen, Rubing Zhang, Xinghong Zhang, Wenbo Han. hot pressing Zr have significantly been improved
2[Al (Si)]
4c
5/ SiC and microstructure and properties thereof [J]. alloy and compound journal .2009,481 (1-2): 877-880; Ling-Feng He, Fang-Zhi Li, Xin-Po Lu, Yi-Wang Bao, Yan-Chun Zhou. in-situ hot pressing is prepared Zr
2[Al (Si)]
4c
5-SiC and microtexture thereof, mechanical property, thermal characteristics and oxidation susceptibility [J]. the magazine .2010 of European Ceramic Society, 30 (11): 2147-2154; Guiqing Chen, Rubing Zhang, Ping Hu and Wenbo Han.Zr
2[Al (Si)]
4c
5antioxidant property [J] the .Scripta material .2009 of base complex phase ceramic under ultra-high temperature condition, 61 (7): 697-700; Ling Wu, Ling-Feng He, Ji-Xin Chen, Xin-Po Lu, and Yan-Chun Zhou, Zr
2[Al (Si)]
4c
5and Zr
2[Al (Si)]
4c
5– SiC is at Si
3n
4reciprocating friction under abrading-ball and friction behavior [J]. U.S. ceramics meeting magazine .2010,30 (11): 2147-2154; ).ZrB
2there is high-melting-point, high rigidity, corrosion-resistant, oxidation resistant characteristic and good heat-conductivity conducting performance, have report to Zr
2al
3c
4in pottery, introduce ZrB
2after wild phase, the density of material, hardness and Young's modulus are all improved, and have than single-phase Zr
2al
3c
4the thermal conductivity that pottery is higher and better oxidation-resistance (Guo Qilong, Yang Yahui, Li Junguo, Shen Qiang, Zhang Lianmeng.Zr
2al
3c
4/ ZrB
2the original position of matrix material is synthesized and performance [J]. material and design, 2011,32 (8-9): 4289-4294).But adopt a kind of tough phase, strengthening and toughening mechanism is single, and modified effect is limited, and there is no at present relevant by complex phase to Zr
3[Al (Si)]
4c
6pottery carries out the report of highly malleablized.
Summary of the invention:
The invention provides that a kind of cost is low, mechanical property good, processing condition are simple and hold manageable original position (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material, another object of the present invention is to provide the preparation method of above-mentioned materials; ZrB
2, two kinds of wild phases of ZrC are collaborative strengthens, bending strength and the fracture toughness property of material significantly improve.
Technical scheme of the present invention is: utilize the synthetic method preparation (ZrB of original position
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material, its ultimate principle is ZrH
2at high temperature decompose and produce Zr, then Zr reacts with Al, Si, C and generates Zr
3[Al (Si)]
4c
6matrix, meanwhile, Zr also with B
4c generates ZrB by reaction original position
2with the associating wild phase of two kinds of different-shapes of ZrC and yardstick, different enhanced mechanism, thereby a step makes (ZrB
2+ ZrC) strengthen Zr
3[Al (Si)]
4c
6composite diphase material.(the ZrB being recorded by Archimedes's method
2+ ZrC)/Zr
3[Al (Si)]
4c
6the density of block materials is greater than 99%.
Concrete technical scheme of the present invention is: a kind of (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material, is characterized in that: by ZrB
2, ZrC wild phase and Zr
3[Al (Si)]
4c
6matrix composition, wherein ZrB
2account for 7.08 ~ 21.23% of material cumulative volume, ZrC accounts for 2.92 ~ 8.77% of material cumulative volume.
The present invention also provides the preparation method who prepares above-mentioned matrix material, and its concrete steps are: by raw material ZrH
2powder, Al powder, Si powder, Graphite Powder 99 and B
4c powder is 3:(2.04 ~ 3.00 according to mole proportioning): (0.28 ~ 0.42): (3.28 ~ 4.83): (0.18 ~ 0.49) weighs; after mixing, physical mechanical method packs coldmoulding in the graphite jig that inwall scribbles BN into; sintering in being connected with the hot pressing furnace of protective atmosphere; then annealing insulation; last power-off, furnace cooling.
ZrH preferably
2powder Particle Size is-400 orders; Described Al powder and Si Powder Particle Size are-300 orders; Described Graphite Powder 99 size range is 5 ~ 20 μ m; Described B
4c Powder Particle Size scope is 3 ~ 10 μ m.
Preferably coldmoulding pressure is 1 ~ 3MPa.Preferably in sintering process, temperature rise rate is 15 ~ 25 ℃/min; Sintering temperature is 1850 ~ 1950 ℃; The sintered heat insulating time is 1 ~ 1.5 hour, and sintering pressure is 25 ~ 30MPa; Preferably rate of temperature fall is 15 ~ 30 ℃/min, and annealing holding temperature is 1600 ~ 1650 ℃, and annealing soaking time is 20 ~ 40 minutes, protects annealing temperature and pressure and maintains by force 25 ~ 30MPa; Preferably the protective atmosphere in sintering process is argon gas.
Preferably described physical mechanical mixing method is barreling.
The invention provides the densification (ZrB that a kind of mechanical property is good, technique is simple, cost is low
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material and in-situ preparation method thereof, contain ZrB in material
2with two kinds of wild phases of ZrC and corresponding two kinds of mechanism and enhancement mechanism.
Beneficial effect:
1. with ZrH
2powder is as the raw material that Zr source is provided, it decomposes produce pure, tiny, highly active Zr powder completely in heat-processed before 900 ℃, avoided traditional and directly usingd Zr powder during as zirconium source, Zr powder is the disadvantageous effect of oxidation to material composition, structure and performance inevitably.Meanwhile, ZrH
2powder price is low and be easy to preserve compared with Zr powder.
2.ZrH
2decompose and produce pure, tiny, highly active Zr powder, in heat-processed subsequently, react with Al, Si, C and generate Zr
3[Al (Si)]
4c
6matrix, while and B
4the synthetic ZrB of C reaction original position
2with two kinds of wild phases of ZrC, thereby a step makes (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material, technique is simple, and cost is low.
3. (the ZrB making
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material uniform microstructure, by Zr
3[Al (Si)]
4c
6crystal grain, ZrB
2crystal grain and ZrC crystal grain form, and crystal boundary is clean, ZrB
2with interaction between two kinds of tough phases of ZrC, two kinds of collaborative couplings of strengthening and toughening mechanism, bending strength and the fracture toughness property of material significantly improve.
4. utilize ZrB
2with the feature of ZrC high rigidity, (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6the hardness of composite diphase material significantly improves, and utilizes ZrB in high-speed friction process
2the low melting point B that oxidation produces
2o
3, can form one deck self-lubricating film at surface of friction, further improve the friction and wear behavior of material.
5. utilize respectively ZrB
2and Zr
3[Al (Si)]
4c
6in B element, Al element, Si element, (the ZrB making
2+ ZrC)/Zr
3[Al (Si)]
4c
6composite diphase material can generate fine and close boroaluminosilicate protective membrane when oxidation, thereby improves the oxidation-resistance of material.
Accompanying drawing explanation:
Fig. 1 is embodiment 1 gained (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6the XRD figure spectrum of diphase ceramic material, wherein ● represent Zr
3[Al (Si)]
4c
6,
represent ZrB
2,
represent ZrC;
Fig. 2 is embodiment 1 gained (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6the back scattering stereoscan photograph of the glazed surface of diphase ceramic material.
Embodiment:
Embodiment 1:
N (ZrH in molar ratio
2): n (Al): n (Si): n (C): n (B
4c)=3:2.04:0.28:3.28:0.49 takes raw material ZrH
2powder (400 order), Al powder (300 order), Si powder (300 order), Graphite Powder 99 (10 μ m), B
4after C powder (5 μ m), be placed in polyethylene ball grinder, in vacuum glove box, operate, make ball grinder be full of argon gas, mix and be placed on coldmoulding (pressure is 1 ~ 3MPa) in the graphite jig that surface scribbles BN, hot pressed sintering in argon atmospher, speed with 15 ℃/min is warming up to 1850 ℃, arrive after sintering temperature point, pressure adds to 30MPa gradually, is incubated 1.5 hours, then with the speed of 15 ℃/min, lower the temperature, at 1600 ℃, under 30MPa pressure, annealing insulation is 40 minutes, finally turns off power supply furnace cooling.That obtain is 30vol.% (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6matrix material, wherein ZrB
2be respectively 21.23% and 8.77% with the volume fraction of ZrC, the density of material reaches 99.9%, and on universal testing machine, the three-point bending resistance intensity of test material reaches 625MPa, adopts the fracture toughness property of monolateral breach beam method test material to reach 6.04MPam
1/2.The product making is carried out to XRD analysis, and as shown in Figure 1, product is by Zr
3[Al (Si)]
4c
6, ZrB
2form with ZrC.The glazed surface of sample is carried out to sem analysis, and as shown in Figure 2, the crystal grain of three kinds of thing phases is high-visible, and material structure is fine and close, and crystal grain is tiny.
Embodiment 2:
N (ZrH in molar ratio
2): n (Al): n (Si): n (C): n (B
4c)=3:2.49:0.35:4.01:0.34 takes raw material ZrH
2powder (400 order), Al powder (300 order), Si powder (300 order), Graphite Powder 99 (5 μ m), B
4after C powder (3 μ m) powder, be placed in polyethylene ball grinder, in vacuum glove box, operate, make ball grinder be full of argon gas, mix and be placed on coldmoulding (pressure is 1 ~ 3MPa) in the graphite jig that surface scribbles BN, hot pressed sintering in argon atmospher, speed with 20 ℃/min is warming up to 1900 ℃, arrive after sintering temperature, pressure adds to 25MPa gradually, is incubated 1 hour, then with the speed of 25 ℃/min, lower the temperature, at 1650 ℃, under 25MPa pressure, annealing insulation is 0.5 hour, finally turns off power supply furnace cooling.That obtain is 20vol.% (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6matrix material, wherein ZrB
2be respectively 14.15% and 5.85% with the volume fraction of ZrC, the density of material reaches 99.8%, and on universal testing machine, the three-point bending resistance intensity of test material reaches 550MPa, adopts the fracture toughness property of monolateral breach beam method test material to reach 5.46MPam
1/2.
Embodiment 3:
N (ZrH in molar ratio
2): n (Al): n (Si): n (C): n (B
4c)=3:3.00:0.42:4.83:0.18 takes raw material ZrH
2powder (400 order), Al powder (300 order), Si powder (300 order), Graphite Powder 99 (20 μ m), B
4after C powder (10 μ m), be placed in polyethylene ball grinder, in vacuum glove box, operate, make ball grinder be full of argon gas, be dry mixed the even coldmoulding (pressure is 1 ~ 3MPa) in the graphite jig that surface scribbles BN that is placed on, hot pressed sintering in argon atmospher, speed with 25 ℃/min is warming up to 1950 ℃, arrive after sintering temperature, pressure adds to 30MPa gradually, is incubated 1 hour, then with the speed of 30 ℃/min, lower the temperature, at 1600 ℃, under 30MPa pressure, annealing insulation is 20 minutes, finally turns off power supply furnace cooling.That obtain is 10vol.% (ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6matrix material, wherein ZrB
2be respectively 7.08% and 2.92% with the volume fraction of ZrC, the density of material reaches 99.9%, and on universal testing machine, the three-point bending resistance intensity of test material reaches 507MPa, adopts the fracture toughness property of monolateral breach beam method test material to reach 4.99MPam
1/2.
Claims (6)
1. (a ZrB
2+ ZrC)/Zr
3[Al (Si)]
4c
6diphase ceramic material, is characterized in that: by ZrB
2, ZrC wild phase and Zr
3[Al (Si)]
4c
6matrix composition, wherein ZrB
2account for 7.08～21.23% of material cumulative volume, ZrC accounts for 2.92～8.77% of material cumulative volume.
2. prepare (ZrB as claimed in claim 1 for one kind
2+ ZrC)/Zr
3[Al (Si)]
4c
6the method of diphase ceramic material, its concrete steps are: by raw material ZrH
2powder, Al powder, Si powder, Graphite Powder 99 and B
4c powder is 3:(2.04～3.00 according to mole proportioning): (0.28～0.42): (3.28～4.83): (0.18～0.49) weighs, after mixing, physical mechanical method packs coldmoulding in the graphite jig that inwall scribbles BN into, sintering in being connected with the hot pressing furnace of protective atmosphere, then annealing insulation, last power-off, furnace cooling; Wherein in sintering process, temperature rise rate is 15～25 ℃/min; Sintering temperature is 1850～1950 ℃; The sintered heat insulating time is 1～1.5 hour; Then with the rate of temperature fall of 15～30 ℃/min, be down to 1600～1650 ℃ and anneal, be incubated 20～40 minutes.
3. in accordance with the method for claim 2, it is characterized in that described ZrH
2powder Particle Size is-400 orders; Described Al powder and Si Powder Particle Size are-300 orders; Described Graphite Powder 99 size range is 5～20 μ m; Described B
4c Powder Particle Size scope is 3～10 μ m.
4. in accordance with the method for claim 2, it is characterized in that described coldmoulding pressure is 1～3MPa.
5. in accordance with the method for claim 2, it is characterized in that the pressure in sintering process and annealing insulating process all maintains 25～30MPa.
6. in accordance with the method for claim 2, it is characterized in that protective atmosphere is argon gas.
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|---|---|---|---|---|
| CN109467435A (en) * | 2018-11-02 | 2019-03-15 | 常熟理工学院 | A kind of tough oxidation resistant Zr3 [Al (Si)] 4C6 based ultra-high temperature ceramic material and preparation method thereof |
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|---|---|---|---|---|
| CN101824576A (en) * | 2009-03-04 | 2010-09-08 | 中国科学院金属研究所 | Zirconium-aluminum-silicon-carbon-silicon carbide composite material and preparation method thereof |
| CN102515870A (en) * | 2011-12-10 | 2012-06-27 | 西北工业大学 | Preparation method of C/SiC-ZrB2-ZrC ultrahigh-temperature ceramic-based composite material |
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| CN101824576A (en) * | 2009-03-04 | 2010-09-08 | 中国科学院金属研究所 | Zirconium-aluminum-silicon-carbon-silicon carbide composite material and preparation method thereof |
| CN102515870A (en) * | 2011-12-10 | 2012-06-27 | 西北工业大学 | Preparation method of C/SiC-ZrB2-ZrC ultrahigh-temperature ceramic-based composite material |
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| Title |
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| Qu Qiang et al..In situ synthesis mechanism and characterization of ZrB2-ZrC-SiC ultra high-temperature ceramics.《Materials Chemistry and Physics》.2008,第110卷第216页右栏第2段,第217页2.试验步骤部分. |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467435A (en) * | 2018-11-02 | 2019-03-15 | 常熟理工学院 | A kind of tough oxidation resistant Zr3 [Al (Si)] 4C6 based ultra-high temperature ceramic material and preparation method thereof |
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