CN1278992C - Method of metchanically actiratee low temperature synthesis of tin titanium carbide - Google Patents
Method of metchanically actiratee low temperature synthesis of tin titanium carbide Download PDFInfo
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- CN1278992C CN1278992C CN 200510011932 CN200510011932A CN1278992C CN 1278992 C CN1278992 C CN 1278992C CN 200510011932 CN200510011932 CN 200510011932 CN 200510011932 A CN200510011932 A CN 200510011932A CN 1278992 C CN1278992 C CN 1278992C
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Abstract
The present invention relates to a method for synthesizing tin-titanium carbide at a low temperature through mechanical activation. In the method, titanium, tin and graphite are used as raw materials to be compounded according to the molar ratio of 2: (0.7 to 1.3): (0.6 to 1) and then put in a ball milling pot, the pot is vacuumized, and the ratio of milling media to material is 10:1 to 50:1; the rotary speed of the ball mill big disc is 150 to 350 r/min; the milling ball is stainless steel; at the room temperature, the raw materials are treated by ball milling for 0.5 to 3h into superfine alloy powder with a submicron or nano level structure; the powder is pressed into blocks at 10 to 50MPa and put in a high-temperature furnace, in the atmosphere of vacuum, the furnace temperature is raised to 650 to 850 DEG C at the speed of 10 to 40 DEG C /min and preserved for 5 to 30 min, and tin-titanium carbide is obtained. The method has the advantages of low sintering temperature, short preparation time and low cost.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic powder, particularly a kind of mechanical activation low temperature is synthesizing tin-titanium carbide Ti in batches
2The preparation method of SnC.
Background technology
Ti
2SnC is a kind of novel ternary layered compound, and it integrates the advantage of metal and pottery, as has high conductivity, high-modulus, self-lubricating, easily processing, characteristics such as corrosion-resistant.This novel material has caused investigator's great attention and high research interest.Ti
2SnC is with a wide range of applications, as can be used as and flowed friction means, conductivity ceramics spare, corrosion-resistant parts etc.In addition, Ti
2The SnC powder also can be used as toughener, not only can improve the intensity and the modulus of matrix material, and again can its conductivity of corresponding raising.Therefore synthetic Ti
2The SnC powder has crucial scientific research meaning.
But correlative study shows, synthetic at present Ti
2SnC adopts quiet sintering technologies such as hot pressing or heat usually, not only apparatus expensive, and synthesis temperature height, and temperature is generally at 1200～1250 ℃; Soaking time is long, is generally 2～6h.Adopt above-mentioned technology, increased preparation cost, influenced the application of its large-scale production.If adopt normal pressure-sintered technology, also will be at 1200 ℃, insulation 6h, synthetic Ti
2SnC.As document 1 Scrip.Mater., 1997,37 (10): on 1583, disclosed is to utilize hot isostatic pressing technique at 1250 ℃, and under the 40MPa pressure, insulation 4h has synthesized Ti
2SnC.Document 2 Mat.Res.Innovat., 2002, on the 6:219, disclosed is to utilize the solid-liquid reaction method at 1250 ℃, under the 30MPa pressure, insulation 2h, argon gas is a protective atmosphere, has synthesized Ti
2SnC.Document 3Mater.Sci.Eng.A., 1998, on the 256:83, disclosed is at 1200 ℃, insulation 6h has synthesized Ti
2SnC.
Summary of the invention
Technical problem to be solved by this invention is that (Mechanically ActivatedLow-temperature Synthesis MALS), realizes synthetic Ti of low temperature short period of time to utilize mechanical activation low temperature synthetic technology
2SnC.Solve sintering temperature height in the prior art, preparation time is long, the problem that cost is high.MALS combines the advantage of mechanical alloying and non-pressure sintering technology.In the high-energy ball milling process, the Ti/Sn/C composite powder is through cold welding-breaking-down process repeatedly, and particle size constantly diminishes; Powdered alloy constantly is squeezed and impacts simultaneously, serious viscous deformation has taken place, a large amount of strains, defective and nano level microstructure have been introduced in crystal grain inside, make these powder have good sintering activity, can make the later stage synthesis temperature reduce (with respect to the powder sintered temperature of routine) greatly, obtain even size distribution, have the product of hyperfine structure.
Technical scheme of the present invention is:
(1) ma process: titanium Ti, tin Sn and graphite C are pressed 2: (0.7～1.3): the molar ratio ingredient of (0.6～1), put into ball grinder then, the ratio of grinding media to material scope is 10: 1～50: 1, ball grinder vacuumizes; High energy ball mill deep bid rotating speed is 150～350r/min; Mill ball is stainless steel or Wimet.At room temperature, mixed through the ball milling of 0.5～3h, grain fineness number is in submicron or nano level ultrafine powder.
(2) low-temperature sintering process: with superfine alloy powder briquetting under 10～50MPa pressure, place High Temperature Furnaces Heating Apparatus, under vacuum or argon shield atmosphere, with the temperature rise rate of 10～40 ℃/min furnace temperature is risen to 650～850 ℃, soaking time is 5～30min.Promptly make Ti
2SnC.
The present invention compares the beneficial effect that is had with prior art and is:
Present technique combines the advantage of mechanical alloying and non-pressure sintering technology, realized low temperature, in short-term, low-cost synthetic Ti
2SnC.
(1) the present invention adopt the time of high-energy ball-milling process synthesizing superfine powder short (0.5～3h), improved the preparation efficiency of product greatly, and avoided coming from impurity introducing chances mutually such as mill ball and jar, ultrafine powder is pure, and is pollution-free.
(2) sintering activity of prepared powdered alloy improves greatly.Because the Ti/Sn/C mixed powder experiences cold welding-breaking-down process repeatedly through high-energy ball milling, particle size constantly diminishes; Powder is through the strong extruding and the impact of mill ball simultaneously, serious viscous deformation having taken place, introduced a large amount of strains, defective and nano level microstructure in crystal grain inside, makes these powder have good sintering activity, therefore, synthesis temperature reduces greatly the later stage.
(3) synthetic Ti
2SnC is normal pressure-sintered, and the used time is short, is 5～30min; Especially synthesis temperature is low, about 650 ℃, well below the synthesis temperature (1200～1250 ℃) of report, reduces temperature and reaches 600 degree, and this has great importance for cutting down the consumption of energy.
(4) Ti of Huo Deing
2The particle mean size of SnC is about 5 μ m, and pattern is the sheet crystalline substance, is a kind of good second phase toughener;
(5) the present invention is applicable to large-scale production, and is easy to operate, and equipment used is simple, less investment, and the synthetic powder cost is low.
Description of drawings
Fig. 1 is mechanical activation low temperature synthetic Ti of the present invention
2The SnC stereoscan photograph.
Embodiment
Embodiment one:
Press Ti: Sn: C=2: 1: 1 molar ratio ingredient, take by weighing Ti powder 8.46 grams, Sn powder 10.48 grams, C powder 1.06 grams, put into ball grinder, ratio of grinding media to material is 20: 1, and ball grinder vacuumizes, and vacuum tightness is less than 10Pa.Planetary high-energy ball mill deep bid rotating speed is 250r/min.At room temperature, through behind the high-energy ball milling of 1h, obtain superfine alloy powder.With ultrafine powder briquetting under 40MPa pressure, place High Temperature Furnaces Heating Apparatus, argon shield atmosphere rises to 750 ℃ with the temperature rise rate of 40 ℃/min with furnace temperature, and soaking time is 30min, promptly makes Ti
2SnC, its productive rate are 90%.
Embodiment two:
Press Ti: Sn: C=2: 0.9: 0.8 molar ratio ingredient, take by weighing Ti powder 4.51 grams, Sn powder 5.04 grams, C powder 0.45 gram, put into ball grinder, ratio of grinding media to material is 40: 1, and ball grinder vacuumizes, and vacuum tightness is less than 10Pa.Planetary high-energy ball mill deep bid rotating speed is 300r/min.At room temperature, the high-energy ball milling through 40min obtains superfine alloy powder.With ultrafine powder briquetting under 50MPa pressure, place High Temperature Furnaces Heating Apparatus, argon shield atmosphere rises to 650 ℃ with the temperature rise rate of 20 ℃/min with furnace temperature, and soaking time is 15min, promptly makes Ti
2SnC, its productive rate are 94%.
Prepared Ti
2SnC powder granule pattern is seen accompanying drawing 1.As can be seen from the figure, particle all is the sheet crystalline substance, smooth surface.The size of sheet crystalline substance is about 5 μ m, and thickness is below 1 μ m.
Claims (1)
1. the method for metchanically actiratee low temperature synthesis of tin titanium carbide is characterized in that, the step of this method:
Step (1) is a raw material with titanium, tin and graphite, presses titanium: tin: graphite=2: (0.7～1.3): the molar ratio ingredient of (0.6～1);
Step (2) is put into ball grinder with batching, and the ratio of grinding media to material scope is 10: 1～50: 1, and ball grinder vacuumizes; High energy ball mill deep bid rotating speed is 150～350r/min; Mill ball is stainless steel or Wimet, at room temperature, is mixed through the ball milling of 0.5～3h, has the superfine alloy powder of submicron or nanoscale structures;
Step (3) with superfine alloy powder briquetting under 10～50MPa pressure, places High Temperature Furnaces Heating Apparatus with briquetting then; under vacuum or argon shield atmosphere; temperature rise rate with 10～40 ℃/min rises to 650～850 ℃ with furnace temperature, and soaking time is 5～30min, promptly makes tin-titanium carbide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510011932 CN1278992C (en) | 2005-06-15 | 2005-06-15 | Method of metchanically actiratee low temperature synthesis of tin titanium carbide |
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| CN 200510011932 CN1278992C (en) | 2005-06-15 | 2005-06-15 | Method of metchanically actiratee low temperature synthesis of tin titanium carbide |
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| CN1724468A CN1724468A (en) | 2006-01-25 |
| CN1278992C true CN1278992C (en) | 2006-10-11 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331759C (en) * | 2006-03-21 | 2007-08-15 | 北京交通大学 | Method for synthesizing tin-titanium carbide at low temperature |
| CN101462163A (en) * | 2009-01-16 | 2009-06-24 | 江西稀有稀土金属钨业集团有限公司 | Ball mill technique for preparing carbide alloy mixture |
| CN102744691B (en) * | 2012-07-16 | 2015-08-12 | 中原工学院 | A kind of tin titanium carbide binder diamond composite and preparation method thereof |
| CN104557045B (en) * | 2015-02-05 | 2016-06-15 | 安徽工程大学 | A kind of tin-titanium carbide material normal pressure low temperature preparation method |
| CN104557044A (en) * | 2015-02-05 | 2015-04-29 | 安徽工程大学 | Preparation method of titanium tin carbide |
| CN105777127A (en) * | 2016-02-29 | 2016-07-20 | 东南大学 | Preparation method of high-purity Ti2SnC powder |
| CN114890413B (en) * | 2022-04-15 | 2023-09-01 | 中南大学 | Graphite @ Ti 2 SnC powder particles and preparation method thereof |
| CN116924804B (en) * | 2023-09-18 | 2023-11-21 | 成都金钨硬质合金有限公司 | Binding phase-free ultrafine ultra-fine grain hard alloy and preparation method thereof |
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