CN100467424C - Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, and preparation method - Google Patents
Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, and preparation method Download PDFInfo
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- CN100467424C CN100467424C CNB2007100645478A CN200710064547A CN100467424C CN 100467424 C CN100467424 C CN 100467424C CN B2007100645478 A CNB2007100645478 A CN B2007100645478A CN 200710064547 A CN200710064547 A CN 200710064547A CN 100467424 C CN100467424 C CN 100467424C
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Abstract
This invention discloses a method for preparing Ti-Si-Al-C lamellar solid solution powder. The powder is composed of: Ti3Siy-xAlxCz (wherein, 0 less than x less than y; y is 1-1.2; z is 1.8-2) higher than 96 vol.%, and impurities lower than 4 vol.%. Ti3Siy-xAlxCz has the same lamellar crystal structure as Ti3SiC2 and Ti3AlC2. Si and Al atoms are set between two Ti3Cz lamellae. The crystal constants c and a increase with the increase of x. The method comprises: mixing Ti, Si, Al and graphite powder at a mol. ratio of 3.0:(0.1-1.1):(0.1-1.1):(1.8-2.0), ball-milling, pressing into a block, placing in a high-temperature furnace, calcining at 1400-1500 deg.C under Ar protection, keeping the temperature for 5-10 min, cooling to obtain loose block product, pulverizing, and ball-milling. The powder can be used to prepare composite or mono-phase Ti-Si-Al-C block material.
Description
Technical field
The present invention relates to a kind of powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon and preparation method thereof, belong to the new ceramic material field.
Background technology
Solid-solution material generally has than its solvent material or solute material excellent comprehensive performances or certain property, and the practical metallic substance overwhelming majority is as basis or the complete alloy material of being made up of sosoloid with sosoloid; Some have the stupalith of excellent properties, as Sialon, partially stabilized ZrO
2, also form by sosoloid.
The titanium silicon carbide is respectively by W.Jeitschko ﹠amp with " 312 " titanium aluminium carbide mutually; H.Nowotny (Monatsh Chem, 1967[98]: 329-337) with Pietzka ﹠amp; Schuster (J.Phase Equilib, 1994[15]: 392) the novel tertiary carbide of Fa Xianing, they have identical layered crystal structure and close lattice parameter, high conductivity and workability with extraordinary stupalith have potential use widely in fields such as machinery, electrician and metallurgy.In order to obtain highly purified titanium silicon carbide material, suppress the generation of impurity phases such as deleterious TiC in its building-up reactions product, people such as Zhai Hongxiang successively invented a kind of titanium silicon carbide powder and with aluminium be reaction promoter atmospheric synthesizing method (patent No.: ZL200410009589.8.) and a kind of be the titanium silicon-carbon block materials and preparation method thereof (patent No.: ZL200410009243.8) of additive with aluminium.With a spot of aluminium is the purity that reaction promoter or additive have improved titanium silicon carbide synthetic product effectively, but the performance of synthetic titanium silicon carbide is not changed basically.
In view of the titanium aluminium carbide of titanium silicon carbide and " 312 " phase has identical layered crystal structure and close lattice parameter, titanium aluminium carbide with titanium silicon carbide or " 312 " phase is solvent or solute, change their natural characteristics by the interlayer solid solution, thereby the type material of obtained performance excellence all is feasible on Materials science and material preparation technology.The adding of opposite sex atom changes the chemical relationship of interlayer, thereby some characteristic of sosoloid, and as high temperature oxidation resistance, comparable titanium silicon carbide significantly strengthens with " 312 " titanium aluminium carbide mutually.
Summary of the invention
The object of the present invention is to provide a kind of powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon and preparation method thereof.
Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon of the present invention, its composition is as follows:
(1) Ti
3Si
Y-xAl
xC
zVolume content 96%, in the expression formula: 0＜x＜y, 1≤y≤1.2,1.8≤z≤2;
(2) volume content of TiC impurity phase＜4%;
(3) Ti
3Si
Y-xAl
xC
zHave and Ti
3SiC
2Or Ti
3AlC
2Identical layered crystal structure, Si atom and Al atom coexist as two-layer Ti
3C
zBetween the layer, lattice parameter c and a increase with the x value.
Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon of the present invention, its crystalline structure is as follows:
(1) has and Ti
3SiC
2And Ti
3AlC
2Identical layered crystal structure;
(2) Si atom and Al atom coexist as two-layer Ti
3C
zBetween;
(3) Ti
3Si
Y-xAl
xC
zThe lattice parameter c of phase and a increase with the x value.
A kind of powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon preparation method of the present invention comprises following each step:
(1) batching: with Ti powder, Si powder, Al powder and Graphite Powder 99 Ti:Si:Al:C=3.0:(0.1～1.1 in molar ratio): (0.1～1.1): the ratio batching of (1.8～2.0);
(2) batch mixing: add 70～100 milliliters dehydrated alcohol, the agate ball or the alumina balls of 200～250 grams in the above-mentioned batching of per 100 grams, ball milling 2～4 hours, 60～70 ℃ of oven dry in baking oven with the mixing raw material grinding of oven dry, are crossed 70～100 mesh sieves;
(3) precompressed: the base substrate that the dried feed behind the above-mentioned batch mixing is pressed into Any shape;
(4) calcining: the mixing raw material base substrate of above-mentioned precompressed is put into plumbago crucible, place high temperature sintering furnace, under argon shield, temperature rise rate by 10～40 ℃/min, furnace temperature is risen to 1400～1500 ℃, and insulation 5～10min postcooling obtains fluffy block reaction product;
(5) with reaction product pulverizing, ball milling, promptly obtain powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon of the present invention.
The invention has the beneficial effects as follows, prepare powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon with method of the present invention, method is simple, reliable, is easy to suitability for industrialized production; Prepared powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon does not contain or only contains dephasigns such as a spot of TiC, and available its is the matrix material or the monophasic titanium sial carbon block material of feedstock production various uses.
Description of drawings
The x-ray diffraction pattern that Fig. 1 is that the x value of one group of principal phase Ti3Siy-xAlxCz of the present invention is 0.2,0.4,0.6,0.8 and 1.0, the y value is 1.2, the z value is 1.8 titanium sial carbon sosoloid powder; The diffraction peak that is labeled as Cr among the figure is the diffraction peak of the chromium metal of demarcation in being used for.
Embodiment
Embodiment 1
Take by weighing Ti powder 14.455 grams, Si powder 2.827 grams, Al powder 0.543 gram, Graphite Powder 99 2.175 grams; mix the back and add 15 milliliters of dehydrated alcohols and 40 gram agate balls; ball mill mixing 2 hours; 70 ℃ of oven dry in baking oven then, grind; be pressed into block base substrate after crossing 100 mesh sieves; move into High Temperature Furnaces Heating Apparatus after putting into plumbago crucible; under argon shield; speed with 20 ℃/min is warming up to 1470 ℃; insulation 5min postcooling; the loose block product that reaction is generated takes out, pulverizing, ball milling, and promptly obtaining principal phase of the present invention is Ti
3Si
1.0Al
0.2C
1.8Titanium sial carbon sosoloid powder.
Embodiment 2
Take by weighing Ti powder 14.471 grams, Si powder 2.264 grams, Al powder 1.087 grams, Graphite Powder 99 2.178 grams; mix the back and add 15 milliliters of dehydrated alcohols and 40 gram agate balls; ball mill mixing 2 hours; 70 ℃ of oven dry in baking oven then, grind; be pressed into sheet-shaped blank after crossing 100 mesh sieves; move into High Temperature Furnaces Heating Apparatus after putting into plumbago crucible; under argon shield; speed with 20 ℃/min is warming up to 1450 ℃; insulation 5min postcooling; the loose block product that reaction is generated takes out, pulverizing, ball milling, and promptly obtaining principal phase of the present invention is Ti
3Si
0.8Al
0.4C
1.8Titanium sial carbon sosoloid powder.
Embodiment 3
Take by weighing Ti powder 14.487 grams, Si powder 1.70 grams, Al powder 1.63 grams, Graphite Powder 99 2.18 grams; mix the back and add 15 milliliters of dehydrated alcohols and 40 gram agate balls; ball mill mixing 3 hours; 70 ℃ of oven dry in baking oven, grinding then, be pressed into block base substrate after crossing 70 mesh sieves; move into High Temperature Furnaces Heating Apparatus after putting into plumbago crucible; under argon shield; speed with 30 ℃/min is warming up to 1450 ℃; insulation 5min postcooling; the loose block product that reaction is generated takes out; pulverizing, ball milling, promptly obtaining principal phase of the present invention is Ti
3Si
0.6Al
0.6C
1.8Titanium sial carbon sosoloid powder.
Embodiment 4
Take by weighing Ti powder 21.755 grams, Si powder 1.702 grams, Al powder 3.269 grams, Graphite Powder 99 3.274 grams; mix the back and add 25 milliliters of dehydrated alcohols and 60 gram agate balls; ball mill mixing 4 hours; 60 ℃ of oven dry in baking oven, grinding then, be pressed into block base substrate after crossing 100 mesh sieves; move into High Temperature Furnaces Heating Apparatus after putting into plumbago crucible; under argon shield; speed with 40 ℃/min is warming up to 1430 ℃; insulation 5min postcooling; the loose block product that reaction is generated takes out; pulverizing, ball milling, promptly obtaining principal phase of the present invention is Ti
3Si
0.4Al
0.8C
1.8Titanium sial carbon sosoloid powder.
Embodiment 5
Take by weighing Ti powder 21.779 grams, Si powder 0.852 gram, Al powder 4.091 grams, Graphite Powder 99 3.278 grams; mix the back and add 25 milliliters of dehydrated alcohols and 60 gram agate balls; ball mill mixing 4 hours; 60 ℃ of oven dry in baking oven, grinding then, be pressed into block base substrate after crossing 100 mesh sieves; move into High Temperature Furnaces Heating Apparatus after putting into plumbago crucible; under argon shield; speed with 40 ℃/min is warming up to 1400 ℃; insulation 5min postcooling; the loose block product that reaction is generated takes out; pulverizing, ball milling, promptly obtaining principal phase of the present invention is Ti
3Si
0.2Al
1.0C
1.8Titanium sial carbon sosoloid powder.
Claims (2)
1. powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, it is characterized in that: its composition is as follows:
(1) Ti
3Si
Y-xAl
xC
zVolume content 96%, in the expression formula: 0＜x＜y, 1≤y≤1.2,1.8≤z≤2;
(2) volume content of impurity phase＜4%;
(3) Ti
3Si
Y-xAl
xC
zHave and Ti
3SiC
2Or Ti
3AlC
2Identical layered crystal structure, Si atom and Al atom coexist as two-layer Ti
3C
zBetween the layer, lattice parameter c and a increase with the x value.
2. one kind prepares powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon preparation method as claimed in claim 1, it is characterized in that: this method comprises following each step:
(1) batching: with Ti powder, Si powder, Al powder and Graphite Powder 99 Ti:Si:Al:C=3.0:(0.1～1.1 in molar ratio): (0.1～1.1): the ratio batching of (1.8～2.0);
(2) batch mixing: add 70～100 milliliters dehydrated alcohol, the agate ball or the alumina balls of 200～250 grams in the above-mentioned batching of per 100 grams, ball milling 2～4 hours, 60～70 ℃ of oven dry in baking oven with the mixing raw material grinding of oven dry, are crossed 70～100 mesh sieves;
(3) precompressed: the base substrate that the dried feed behind the above-mentioned batch mixing is pressed into Any shape;
(4) calcining: the mixing raw material base substrate of above-mentioned precompressed is put into plumbago crucible, place high temperature sintering furnace, under argon shield, temperature rise rate by 10～40 ℃/min, furnace temperature is risen to 1400～1500 ℃, and insulation 5～10min postcooling obtains fluffy block reaction product;
(5) with reaction product pulverizing, ball milling, promptly obtain powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon as claimed in claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100645478A CN100467424C (en) | 2007-03-20 | 2007-03-20 | Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100645478A CN100467424C (en) | 2007-03-20 | 2007-03-20 | Powder body of solid solution among interlayer of titanium, silicon, aluminum, carbon, and preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101050116A CN101050116A (en) | 2007-10-10 |
| CN100467424C true CN100467424C (en) | 2009-03-11 |
Family
ID=38781748
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|---|---|---|---|
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102117907B (en) * | 2009-12-31 | 2013-10-16 | 中国科学院金属研究所 | Preparation method of solid oxide fuel cell connector material used in fuel cell |
| CN102345144B (en) * | 2010-07-30 | 2014-02-26 | 中国科学院金属研究所 | Method for preparing nickel/titanium silicon aluminum carbon composite coating by using electrochemical co-deposition method |
| CN102345152A (en) * | 2010-07-30 | 2012-02-08 | 中国科学院金属研究所 | Method for preparing Ti-Si-Al-C ceramic coating through electrophoretic deposition |
| CN107827477B (en) * | 2017-10-27 | 2020-09-08 | 兰州理工大学 | Based on Ti3SiC2Reaction diffusion bonding method for carbon-carbon composite material with-Al mixed powder as intermediate layer |
| CN110054496B (en) * | 2018-01-18 | 2020-09-18 | 北京交通大学 | Titanium-aluminum-silicon-tin-carbon three-phase interlayer solid solution powder and preparation method thereof |
| CN108341670B (en) * | 2018-02-02 | 2020-08-04 | 西南科技大学 | Single phase Ti3SiC2Method for preparing metal ceramic |
| CN109836157A (en) * | 2019-03-28 | 2019-06-04 | 北京交通大学 | A kind of titanium aluminium silicon-carbon solid solution block materials preparation method with high intensity and superior abrasion resistance |
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