CN101070247A - Silicon-aluminium titanium carbonate solid-solution material and preparing method - Google Patents
Silicon-aluminium titanium carbonate solid-solution material and preparing method Download PDFInfo
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- CN101070247A CN101070247A CN 200610046560 CN200610046560A CN101070247A CN 101070247 A CN101070247 A CN 101070247A CN 200610046560 CN200610046560 CN 200610046560 CN 200610046560 A CN200610046560 A CN 200610046560A CN 101070247 A CN101070247 A CN 101070247A
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- 239000006104 solid solution Substances 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims description 41
- KNVIEQLRCVAUGJ-UHFFFAOYSA-L aluminum silicon(4+) titanium(4+) carbonate Chemical compound C([O-])([O-])=O.[Ti+4].[Al+3].[Si+4] KNVIEQLRCVAUGJ-UHFFFAOYSA-L 0.000 title claims description 15
- 238000000034 method Methods 0.000 title description 24
- 238000005245 sintering Methods 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004411 aluminium Substances 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 11
- 239000010439 graphite Substances 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 8
- 238000010297 mechanical methods and process Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000010936 titanium Substances 0.000 claims description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 235000013312 flour Nutrition 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 4
- 229910052710 silicon Inorganic materials 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 abstract description 4
- 238000011065 in-situ storage Methods 0.000 abstract description 3
- -1 silicon-aluminium titanium Chemical compound 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000005226 mechanical processes and functions Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000009747 press moulding Methods 0.000 abstract 1
- 239000011863 silicon-based powder Substances 0.000 abstract 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 13
- 239000012535 impurity Substances 0.000 description 8
- 238000009413 insulation Methods 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000012071 phase Substances 0.000 description 5
- 229910010271 silicon carbide Inorganic materials 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- FOZHTJJTSSSURD-UHFFFAOYSA-J titanium(4+);dicarbonate Chemical compound [Ti+4].[O-]C([O-])=O.[O-]C([O-])=O FOZHTJJTSSSURD-UHFFFAOYSA-J 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 1
- 229910002796 Si–Al Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910021341 titanium silicide Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
This invention relates to a silicon-aluminium titanium carbide zirconium solid solution stuff and preparation method by in situ thermocompression / solid- liquid phase reaction. The invention adopts element powder in situ synthesize silicon aluminium titanium carbide zirconium ( ( Ti1 - xZrx) 3 ( Si1 - yAly) C2) solid solution, the X is greater than zero and not greater than 0.07, Y is greater than zero and not greater than 0.10. The concrete preparation method is: takes titanium powder, zirconium powder, silicon powder, aluminium powder and graphite powder as raw material, mix 10 to 25 hours by physical mechanical process, enclose graphite tooting for cold-press moulding, applied pressure is 5 to 20MPa, sinter in hot pressing furnace that has shielding gas atmosphere, heating rate is 5 to 50 deg per minute, sintering temperature is 1400 to 1600deg, sintering time is 0.5 to 2 hours, sintering pressure 20 to 40 MPa.
Description
Technical field
The present invention relates to ceramic solid-solution material and preparation method, be specially a kind of silicon-aluminium titanium carbonate solid-solution ((Ti
1-xZr
x)
3(Si
1-yAl
y) C
2) material and preparation method thereof.
Background technology
Ti
3SiC
2It is a kind of novel ternary layered ceramic material.U.S. pottery (the Journal of theAmerican Ceramic Society 79 of association journal, 1953 (1996)) studies show that in that it combines the plurality of advantages of pottery and metal, have low density, high-modulus, high strength, high specific conductivity and thermal conductivity and easy characteristics such as processing, thereby have broad application prospects.But as a kind of structured material, Ti
3SiC
2Hardness and more than 1100 ℃ antioxidant property on the low side, limited its widespread use.Usually be feedstock production silicon titanium carbide (Ti with titanium valve, silica flour and Graphite Powder 99
3SiC
2) can there be impurity phase titanium carbide (TiC) in the process.In material journal (ActaMaterialia 49,4347 (2001)), point out that titanium carbide is disadvantageous to the high-temperature oxidation resistance of silicon titanium carbide.At material journal (Acta Materialia 52,3631 (2004)) and studies show that in the investigation of materials innovation (Material ResearchInnovations 8,97 (2004)) that the silicon by replacing in the silicon titanium carbide with an amount of aluminium forms silicon aluminum titanium carbide sosoloid (Ti
3Si (Al) C
2) method can remove impurity phase titanium carbide (TiC), and because the content that has increased aluminium (Al) can significantly improve its antioxidant property.In the Ti-Si-C system, if utilize element Zr can replace the titanium of part, improve the good mechanical property that can also keep other after its hardness in the position of Ti, then might reach the effect of solution strengthening.
Summary of the invention
The object of the present invention is to provide that a kind of mechanical property is good, high-temperature oxidation resistance is good, purity is high, simple to operate, easy control of process conditions, silicon-aluminium titanium carbonate solid-solution ((Ti that cost is low
1-xZr
x)
3(Si
1-yAl
y) C
2) material and preparation method thereof.
Technical scheme of the present invention is:
A kind of original position synthesizing Si-Al titanium carbonate solid-solution ((Ti
1-xZr
x)
3(Si
1-yAl
y) C
2) material, the span that Zr replaces the atomic molar replacement amount x of Ti is 0＜x≤0.07, the span that Al replaces the atomic molar replacement amount y of Si is 0＜y≤0.10.
Described silicon-aluminium titanium carbonate solid-solution ((Ti
1-xZr
x)
3(Si
1-yAl
y) C
2) preparation methods, with simple substance titanium valve, zirconium powder, silica flour, aluminium powder and Graphite Powder 99 as raw material.(Ti
1-xZr
x)
3(Si
1-yAl
y) C
2(Ti in the sosoloid
1-xZr
x): (Si
1-yAl
y): the mol ratio of C is 3.0: (1～1.2): 2.0, wherein the span of the atomic molar replacement amount x of Zr replacement Ti is 0＜x≤0.07, the span that Al replaces the atomic molar replacement amount y of Si is 0＜y≤0.10.The confected materials powder mixed 10～25 hours through physical mechanical method; the coldmoulding in the graphite jig of packing into; the pressure that applies is 5～20MPa; sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere; temperature rise rate is 5～50 ℃/minute, and sintering temperature is that 1400～1600 ℃, sintering time are that 0.5～2 hour, sintering pressure are 20～40MPa.Thereby, prepare have high purity, superior the silicon-aluminium titanium carbonate solid-solution ((Ti of over-all properties such as high rigidity, high strength, high elastic coefficient, high tenacity and high-temperature oxidation resistance are good
1-xZr
x)
3(Si
1-yAl
y) C
2) material.
The titanium valve of described adding, zirconium powder, silica flour, aluminium powder, Graphite Powder 99 size range are 200～400 orders; Described sintering processing is hot pressed sintering or HIP sintering; Described rare gas element is argon gas, helium or neon; Described physical mechanical method mixes the ball milled that adopts under the alcohol medium.
The present invention's design and the silicon-aluminium titanium carbonate solid-solution ((Ti for preparing
1-xZr
x)
3(Si
1-yAl
y) C
2) material, because the solid solution of aluminium (Al) can have been eliminated impurity phase titanium carbide, the amount that has increased aluminium simultaneously can improve its high-temperature oxidation resistance on the one hand; On the other hand because the solid solution of zirconium can improve silicon aluminum titanium carbide sosoloid (Ti
3Si (Al) C
2) hardness, and other performance such as Young's modulus, flexural strength, fracture toughness property etc. are all and Ti
3SiC
2Quite.
Advantage of the present invention is:
1, the purity height, mechanical property is good, high-temperature oxidation resistance is good.Adopt the silicon-aluminium titanium carbonate solid-solution ((Ti of the inventive method preparation
1-xZr
x)
3(Si
1-yAl
y) C
2) material do not contain other impurity mutually as titanium carbide or titanium silicide etc.Owing to do not had impurity phase titanium carbide to the oxidation susceptibility adverse influence, can improve the antioxidant property of material in high temperature is used.Silicon-aluminium titanium carbonate solid-solution ((Ti
1-xZr
x)
3(Si
1-yAl
y) C
2) the pure Ti of hardness ratio of material
3Si (Al) C
2Improved many, and its Young's modulus, flexural strength, fracture toughness property etc. all with pure Ti
3Si (Al) C
2Quite.With (Ti
0.93Zr
0.07)
3(Si
0.95Al
0.05) C
2Be example, the hardness of material is 6.5GPa, compares Ti
3Si (Al) C
2Hardness improved 62.5%; The Young's modulus of material reaches 329GPa, and fracture toughness property is 6.23MPam
1/2, flexural strength is 473MPa, these performances all with pure Ti
3Si (Al) C
2Performance suitable.
2, technology is simple, and cost is low.The present invention is that sintering and densification are carried out simultaneously by in-situ hot pressing/solid-liquid phase reaction.Because the appearance of liquid phase is arranged in sintering process, utilize the quick mass transfer process of liquid phase, chemical time is shortened greatly, make densification process become very easy again, technical process is become simply, saved expense again.
Description of drawings
Fig. 1 is the replacement amount asynchronous (TiZr) that zirconium (Zr) replaces titanium (Ti)
3(SiAl) C
2The X-ray diffractogram of solid-solution material.Wherein the replacement amount of aluminium (Al) replacement silicon (Si) is fixed as 0.05.
Fig. 2 is (Ti
0.93Zr
0.07)
3(Si
0.95Al
0.05) C
2Backscattered electron photo after the solid-solution material corrosion.
Fig. 3 is (TiZr)
3(SiAl) C
2The relation of the Vickers' hardness of solid-solution material and Zr solid solution capacity.
Fig. 4 is (TiZr)
3(SiAl) C
2Relation between room temperature bending strength and the fracture toughness property Zr solid solution capacity.Crossbeam speed is 0.5mm/min when surveying intensity, and crossbeam speed is 0.05mm/min when surveying fracture toughness property.
Embodiment
Below by example in detail the present invention is described in detail.
With size range is that (stoichiometric ratio is (Ti for 200～400 purpose titanium valves, 133.38 grams, zirconium powder 2.57 grams, silica flour 30.02 grams, aluminium powder 0.62 gram and graphite 22.52 grams
0.99Zr
0.01)
3(Si
0.98Al
0.02) C
2) ball milling 10 hours in the alcohol medium, coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 10 ℃/minute, is heated to 1550 ℃ of insulations 1 hour, and pressure is added to 25MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 25MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is (TiZr) through X-ray diffraction analysis
3Si (Al) C
2The density that Archimedes's method records is 4.49g/cm
3, be 98.9% of theoretical density.(Ti
0.99Zr
0.01)
3(Si
0.98Al
0.02) C
2) Vickers' hardness of solid-solution material is 4.29GPa; Young's modulus is 337GPa; Fracture toughness property is 6.35MPa.m
1/2, flexural strength is 470MPa.
With size range is that (stoichiometric ratio is (Ti for 200～400 purpose titanium valves, 129.02 grams, zirconium powder 7.6 grams, silica flour 28.14 grams, aluminium powder 3.00 grams and graphite 22.24 grams
0.97Zr
0.03)
3(Si
0.90Al
0.10) C
2) ball milling 15 hours in the alcohol medium, coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 5MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 15 ℃/minute, is heated to 1560 ℃ of insulations 1 hour, and pressure is added to 30MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 30MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is (TiiZr) through X-ray diffraction analysis
3Si (Al) C
2The density that Archimedes's method records is 4.52g/cm
3, be 98.6% of theoretical density.(Ti
0.97Zr
0.03)
3(Si
0.90Al
0.10) C
2Vickers' hardness be 4.71GPa; Young's modulus is 334GPa; Fracture toughness property is 6.30MPam
1/2, flexural strength is 476MPa.
With size range is that (stoichiometric ratio is (Ti for 200～400 purpose titanium valves, 120.64 grams, zirconium powder 17.30 grams, silica flour 30.12 grams, aluminium powder 0.29 gram and graphite 21.64 grams
0.93Zr
0.07)
3(Si
0.99Al
0.01) C
2) ball milling 20 hours in the alcohol medium, coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 10MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 20 ℃/minute, is heated to 1600 ℃ of insulations 1 hour, and pressure is added to 30MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 40MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is (TiZr) through X-ray diffraction analysis
3Si (Al) C
2The density that Archimedes's method records is 4.59g/cm
3, be 98.4% of theoretical density.(Ti
0.93Zr
0.07)
3(Si
0.99Al
0.01) C
2Vickers' hardness be 6.51GPa; Young's modulus is 330GPa; Fracture toughness property is 6.26MPam
1/2, flexural strength is 480MPa.
With size range is that (stoichiometric ratio is (Ti for 200～400 purpose titanium valves, 120.64 grams, zirconium powder 17.30 grams, silica flour 28.77 grams, aluminium powder 1.46 grams and graphite 21.64 grams
0.93Zr
0.07)
3(Si
0.95Al
0.05) C
2) ball milling 20 hours in the alcohol medium, coldmoulding in the graphite jig of packing into afterwards, the pressure that applies is 15MPa, puts into the hot pressing furnace hot pressed sintering.Temperature rise rate is 15 ℃/minute, is heated to 1550 ℃ of insulations 1 hour, and pressure is added to 25MPa gradually simultaneously.Temperature is reduced to 1400 ℃ then, and 1400 ℃ of insulations 0.5 hour, the pressure in the whole insulating process all maintained 25MPa.Whole sintering process all is to carry out under argon shield, and the reaction product of acquisition is (TiZr) through X-ray diffraction analysis
3Si (Al) C
2The density that Archimedes's method records is 4.59g/cm
3, be 98.4% of theoretical density.(Ti
0.93Zr
0.07)
3(Si
0.95Al
0.05) C
2Vickers' hardness be 6.50GPa; Young's modulus is 329GPa; Fracture toughness property is 6.25MPam
1/2, flexural strength is 464MPa.
Comparative example
The pure Ti that adopted the prepared identical with embodiment 3
3Si
0.95Al
0.05C
2, the density that Archimedes's method records is 4.47g/cm
3, be 98.7% of theoretical density; Vickers' hardness is 4.02GPa; Young's modulus is 336GPa; Fracture toughness property is 6.24MPam
1/2Except hardness (TiZr)
3Si (Al) C
2Beyond solid-solution material is on the low side, all the other every mechanical performance indexs all with (TiZr)
3Si (Al) C
2Solid-solution material is suitable.Show (TiZr)
3Si (Al) C
2Solid-solution material is keeping Ti
3(SiAl) C
2In the mechanical property, also improved its hardness effectively preferably.Below with (Ti
0.93Zr
0.07)
3(Si
0.95Al
0.05) C
2Solid-solution material is an example, and its tissue and performance variation are described.
Fig. 1 is the replacement amount asynchronous (TiZr) that zirconium (Zr) replaces titanium (Ti)
3(SiAl) C
2The X-ray diffractogram of solid-solution material.Wherein aluminium (Al) the replacement amount that replaces silicon (Si) is fixed as 0.05,0%, 1%, 3%, 5%, 7% represents zirconium (Zr) to replace the atomic molar replacement amount of titanium (Ti) respectively among the figure.Has only Ti as seen from the figure
3Si (Al) C
2Diffraction peak, and skew has taken place left, illustrate that Zr has been solidly soluted into Ti
3Si (Al) C
2In.Do not find the diffraction peak of impurity phase titanium carbide (TiC) etc. simultaneously.Fig. 2 is (Ti
0.93Zr
0.07)
3(Si
0.95Al
0.05) C
2Backscattered electron photo after the solid-solution material corrosion.Mainly form as seen from the figure by the lath-shaped crystal.Do not find any other impurity mutually as TiC etc., this point can be eliminated titanium carbide (TiC) impurity with a spot of aluminium of the interpolation of above mentioning and be consistent mutually.Fig. 3 is (TiZr)
3(SiAl) C
2The relation of the vickers hardness number of solid-solution material and Zr solid solution capacity.As seen the solid solubility along with zirconium increases, (TiZr)
3(SiAl) C
2The hardness of solid-solution material increases gradually.This explanation can improve Ti more significantly by the method that forms sosoloid
3Si (Al) C
2Hardness.Fig. 4 is (TiZr)
3(SiAl) C
2Relation between room temperature bending strength and the fracture toughness property Zr solid solution capacity.As seen no matter be after aluminium solid solution or the zirconium solid solution, (TiZr)
3(SiAl) C
2The room temperature bending strength of solid-solution material and fracture toughness property all do not have too big variation, all with pure Ti
3Si
0.95Al
0.05C
2Performance suitable.
By embodiment 1, embodiment 2, embodiment 3, embodiment 4 and comparative example as seen, (TiZr) of present method preparation
3(SiAl) C
2Advantages such as solid-solution material has purity height, density height, hardness height, mechanical property is good, high-temperature oxidation resistance is good.
Claims (7)
1, a kind of silicon-aluminium titanium carbonate solid-solution material is characterized in that: the chemical formula of described solid-solution material is (Ti
1-xZr
x)
3(Si
1-yAl
y) C
2, the span that Zr replaces the atomic molar replacement amount x of Ti is 0＜x≤0.07, the span that Al replaces the atomic molar replacement amount y of Si is 0＜y≤0.10.
2, according to the preparation method of the described silicon-aluminium titanium carbonate solid-solution material of claim 1, it is characterized in that: with simple substance titanium valve, zirconium powder, silica flour, aluminium powder and Graphite Powder 99 is raw material; (Ti
1-xZr
x)
3(Si
1-yAl
y) C
2(Ti in the sosoloid
1-xZr
x): (Si
1-yAl
y): the mol ratio of C is 3.0: (1～1.2): 2.0, wherein the span of the atomic molar replacement amount x of Zr replacement Ti is 0＜x≤0.07, the span that Al replaces the atomic molar replacement amount y of Si is 0＜y≤0.10; Raw material powder is behind uniform mixing; the coldmoulding in the graphite jig of packing into; the pressure that applies is 5～20MPa; sintering in the hot pressing furnace that is connected with protection of inert gas atmosphere; temperature rise rate is 5～50 ℃/minute, and sintering temperature is that 1400～1600 ℃, sintering time are that 0.5～2 hour, sintering pressure are 20～40MPa.
3, according to the preparation method of the described silicon-aluminium titanium carbonate solid-solution material of claim 2, it is characterized in that: the titanium valve of described adding, zirconium powder, silica flour, aluminium powder, Graphite Powder 99 size range are 200～400 orders.
4, according to the preparation method of the described silicon-aluminium titanium carbonate solid-solution material of claim 2, it is characterized in that: described sintering processing is hot pressed sintering or HIP sintering.
5, according to the preparation method of the described silicon-aluminium titanium carbonate solid-solution material of claim 2, it is characterized in that: described rare gas element is argon gas, helium or neon.
6, according to the preparation method of the described silicon-aluminium titanium carbonate solid-solution material of claim 2, it is characterized in that: raw material powder was mixed 10～25 hours through physical mechanical method.
7, according to the preparation method of the described silicon-aluminium titanium carbonate solid-solution material of claim 6, it is characterized in that: described physical mechanical method mixes employing ball milling in the alcohol medium.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531602A (en) * | 2010-12-09 | 2012-07-04 | 中国科学院金属研究所 | Zirconium niobium aluminum silicon carbon solid solution material and preparation method thereof |
| CN102557638A (en) * | 2010-12-09 | 2012-07-11 | 中国科学院金属研究所 | Zirconium titanium aluminum silicon carbon solid-solution material and preparation method |
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| CN116121701A (en) * | 2023-03-03 | 2023-05-16 | 青岛大学 | Modified composite three-layer coating of fuel cell metal connector and preparation method thereof |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1234641C (en) * | 2003-05-28 | 2006-01-04 | 中国科学院金属研究所 | Preparing method for Ti3 SiC2 material without TiC impurity |
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| CN102531602A (en) * | 2010-12-09 | 2012-07-04 | 中国科学院金属研究所 | Zirconium niobium aluminum silicon carbon solid solution material and preparation method thereof |
| CN102557638A (en) * | 2010-12-09 | 2012-07-11 | 中国科学院金属研究所 | Zirconium titanium aluminum silicon carbon solid-solution material and preparation method |
| CN102557638B (en) * | 2010-12-09 | 2014-02-12 | 中国科学院金属研究所 | Zirconium titanium aluminum silicon carbon solid-solution material and preparation method |
| CN104387067A (en) * | 2014-10-23 | 2015-03-04 | 西安电子科技大学 | Method for preparing high dielectric loss titanium silicon carbon microwave absorbent powder |
| CN104387067B (en) * | 2014-10-23 | 2016-04-20 | 西安电子科技大学 | The preparation method of high dielectric loss titanium silicon-carbon powder microwave absorption |
| CN108083278A (en) * | 2017-12-26 | 2018-05-29 | 佛山科学技术学院 | A kind of titanium aluminium tin carbon-coating shape solid solution powder and preparation method thereof |
| CN116121701A (en) * | 2023-03-03 | 2023-05-16 | 青岛大学 | Modified composite three-layer coating of fuel cell metal connector and preparation method thereof |
| CN116178021A (en) * | 2023-03-03 | 2023-05-30 | 青岛大学 | Ceramic connector material of solid oxide fuel cell |
| CN116178020A (en) * | 2023-03-03 | 2023-05-30 | 青岛大学 | Ceramic connector material of solid oxide fuel cell and preparation method thereof |
| CN116178020B (en) * | 2023-03-03 | 2024-07-23 | 青岛大学 | Ceramic connector material of solid oxide fuel cell and preparation method thereof |
| CN116178021B (en) * | 2023-03-03 | 2024-07-23 | 青岛大学 | Ceramic connector material of solid oxide fuel cell |
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