CN102659106A - Pressureless sintering method for synthesizing high-purity Ti3SiC2 powder - Google Patents
Pressureless sintering method for synthesizing high-purity Ti3SiC2 powder Download PDFInfo
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- CN102659106A CN102659106A CN2011103842648A CN201110384264A CN102659106A CN 102659106 A CN102659106 A CN 102659106A CN 2011103842648 A CN2011103842648 A CN 2011103842648A CN 201110384264 A CN201110384264 A CN 201110384264A CN 102659106 A CN102659106 A CN 102659106A
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Abstract
The invention discloses a pressureless sintering method for synthesizing high-purity Ti3SiC2 powder, comprising the following steps of: (1) adding element powders of Ti, Si, C and Al into a container, adding alcohol and heating and stirring the solution for more than 1h at a controlled temperature of 70 DEG C until the alcohol is totally evaporated so that residual powder is obtained, wherein the molar ratio of Ti, Si, C and Al is 3:1:2:0.1; (2) transferring the residual powder to a tubular furnace, sintering the residual powder at 1420 DEG C for 2 to 2.5h in an atmosphere of argon, and cooling the obtained product naturally so that Ti3SiC2 powder is obtained. Element substances of Ti, Si, C and Al are used as raw materials in the invention, and a synthesis of high-purity (96.7 %) Ti3SiC2 powder is achieved by means of optimized mixing and by using a pressureless sintering method at 1420 DEG C under the protection of argon. The method of the invention provides a good practicability, good economic prospects and good social benefits.
Description
Technical field
The present invention relates to a kind of novel stupalith, be specifically related to a kind of pressureless sintering synthesis of high purity Ti
3SiC
2The method of powder.
Background technology
Ti
3SiC
2As a kind of novel stupalith,, receive increasing extensive concern recently in conjunction with a lot of premium propertiess of metal with pottery.Ti
3SiC
2Belong to ternary layered compound, the general formula of this compounds is M
N+1AX
N(N=1 in the formula, 2,3; M is a transition metal, and A is IIIA family or IVA family element, and X is carbon or nitrogen element).Good heat conduction, electroconductibility like their existing and metallographic phase; The workability soft relatively, that plasticity-is good and superior; The physical and chemical performance close with stupalith arranged, like HMP, anti-oxidant, resistance to chemical attack, high temperature resistant and good thermal shock resistance etc. again.
Both at home and abroad to Ti
3SiC
2Powder and block carried out big quantity research, prepare Ti at present
3SiC
2Method meteorological synthesis method, self propagating high temperature synthesis method, hot isostatic pressing method and discharge plasma sintering etc. are arranged.Usefulness liquid phase reaction sintering such as Zou go out the very high Ti of purity
3SiC
2Powder, usefulness Ti such as Sun, Si, TiC, Al powder synthesize high purity Ti at 1300 ℃ with pressureless sintering method
3SiC
2Powder.But their synthesis technique mostly comprises ball mill mixing, has that production efficiency is low, complicated operating process, raw material be prone to deficiencies such as oxidation and length consuming time, and in industry, can't realize producing in enormous quantities.
Summary of the invention
Goal of the invention: the deficiency to existing in the prior art the purpose of this invention is to provide a kind of pressureless sintering synthesis of high purity Ti
3SiC
2The method of powder, simple to operate to realize, weak point consuming time, product purity advantages of higher.
Technical scheme: in order to realize the foregoing invention purpose, the technical scheme that the present invention adopts is following:
A kind of pressureless sintering synthesis of high purity Ti
3SiC
2The method of powder, step is following:
(1) in container, add Ti, Si, C and Al simple substance powder, add alcohol, 70 ℃ of temperature controls, clean more than the heated and stirred 1h until vaporized alcohol, get residual powder; Wherein, the mol ratio of Ti, Si, C and Al is 3:1:2:0.1;
(2) change residual powder to tube furnace, under argon gas atmosphere, 1420 ℃ of sintering 2 ~ 2.5h, cooling obtains Ti naturally
3SiC
2Powder.
In the step (2), be heated to 1420 ℃, sintering 2h with the speed of 10 ℃/min.
The prepared Ti that goes out
3SiC
2Powder thickness is 10 ~ 20nm.
Beneficial effect: the present invention is a raw material with simple substance such as Ti, Si, C, Al, through optimizing hybrid mode, adopts the pressureless sintering method under 1420 ℃ and argon shield, to synthesize high purity (96.7%) Ti
3SiC
2Powder has good practicability, and good economic outlook is arranged, and can produce good social benefit.
Description of drawings
Fig. 1 is mix X-ray energy spectrum (EDS) spectrogram of two selenizing tungsten nanometer sheet of the solid lubrication oil additive molybdenum of embodiment 1.
Fig. 2 is the solid lubrication oil additive molybdenum of the embodiment 1 microscopic appearance picture under the two selenizing tungsten nanometer sheet Electronic Speculum (SEM) that mixes.
Embodiment
Below in conjunction with specific embodiment the present invention is done further explanation.
Embodiment 1
Simple substance powder such as Ti, Si, C, Al with mol ratio Ti:Si:C:Al=3:1:2:0.1 weighing, are poured into raw material powder in the beaker, added an amount of alcohol, then beaker is placed on the constant temperature blender with magnetic force, 70 ℃ of Heating temperatures, and constantly stir.Alcohol is evaporated in heat-processed, and approximately through 1 hour, vaporized alcohol was clean.Remaining powder is put into crucible, and put sintering in the tube furnace into, the speed with 10 ℃/min under argon gas atmosphere is heated to 1420 ℃, insulation 2h, and the furnace cooling room temperature obtains the very high Ti of purity
3SiC
2Powder.Through XRD diffraction picture, as shown in Figure 1, the composition that can find out sample is the very high Ti of purity
3SiC
2Powder, purity is up to 96.7%.Can see that through the SEM picture microscopic appearance of sample is lamellated structure, as shown in Figure 2, Ti
3SiC
2The nanometer sheet surface very smooth smooth, the size of nanometer sheet is bigger, thickness is about 10 to 20nm.
Embodiment 2
Simple substance powder such as Ti, Si, C, Al with mol ratio Ti:Si:C:Al=2.9:1.1:2.1:0.11 weighing, are poured into raw material powder in the beaker, added an amount of alcohol, then beaker is placed on the constant temperature blender with magnetic force, 70 ℃ of Heating temperatures, and constantly stir.Alcohol is evaporated in heat-processed, approximately passes through 1h, and vaporized alcohol is clean.Remaining powder is put into crucible, and put sintering in the tube furnace into, the speed with 10 ℃/min under argon gas atmosphere is heated to 1420 ℃, insulation 2.5h, and the furnace cooling room temperature obtains the very high Ti of purity
3SiC
2Powder.Purity is up to 95.3%.
Embodiment 3
Simple substance powder such as Ti, Si, C, Al with mol ratio Ti:Si:C:Al=3.1:0.9:1.9:0.09 weighing, are poured into raw material powder in the beaker, added an amount of alcohol, then beaker is placed on the constant temperature blender with magnetic force, 70 ℃ of Heating temperatures, and constantly stir.Alcohol is evaporated in heat-processed, and approximately through 1 hour, vaporized alcohol was clean.Remaining powder is put into crucible, and put sintering in the tube furnace into, the speed with 10 ℃/min under argon gas atmosphere is heated to 1420 ℃, insulation 2h, and the furnace cooling room temperature obtains the very high Ti of purity
3SiC
2Powder.Purity is up to 96.5%.
Claims (3)
1. pressureless sintering synthesis of high purity Ti
3SiC
2The method of powder is characterized in that, step is following:
(1) in container, add Ti, Si, C and Al simple substance powder, add alcohol, 70 ℃ of temperature controls, clean more than the heated and stirred 1h until vaporized alcohol, get residual powder; Wherein, the mol ratio of Ti, Si, C and Al is 3:1:2:0.1;
(2) change residual powder to tube furnace, under argon gas atmosphere, 1420 ℃ of sintering 2 ~ 2.5h, cooling obtains Ti naturally
3SiC
2Powder.
2. pressureless sintering synthesis of high purity Ti according to claim 1
3SiC
2The method of powder is characterized in that: in the step (2), be heated to 1420 ℃, sintering 2h with the speed of 10 ℃/min.
3. pressureless sintering synthesis of high purity Ti according to claim 1
3SiC
2The method of powder is characterized in that: the prepared Ti that goes out
3SiC
2Powder thickness is 10 ~ 20nm.
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| CN2011103842648A CN102659106A (en) | 2011-11-28 | 2011-11-28 | Pressureless sintering method for synthesizing high-purity Ti3SiC2 powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058749A (en) * | 2013-03-21 | 2014-09-24 | 中国科学院宁波材料技术与工程研究所 | Method for preparing titanium silicon carbon ceramic block material by pressureless sintering |
| CN104404426A (en) * | 2014-11-17 | 2015-03-11 | 苏州大学 | Ti3SiC2-based composite-material coating on surface of large-sized workpiece and method for preparing coating through plasma surfacing |
| CN105777127A (en) * | 2016-02-29 | 2016-07-20 | 东南大学 | Preparation method of high-purity Ti2SnC powder |
| RU2610380C2 (en) * | 2015-07-13 | 2017-02-09 | федеральное государственное бюджетное образовательное учреждение высшего образования "Пермский национальный исследовательский политехнический университет" | Method of producing titanium carbosilicide-based composite |
| CN109666815A (en) * | 2018-12-28 | 2019-04-23 | 西安交通大学 | A kind of MAX phase enhances the preparation method and applications of nickel-base high-temperature lubricating composite |
| WO2019181604A1 (en) * | 2018-03-23 | 2019-09-26 | 日清エンジニアリング株式会社 | Composite particles and method for producing composite particles |
Citations (3)
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| WO2001046083A1 (en) * | 1999-12-22 | 2001-06-28 | Drexel University | Process for forming 312 phase materials and process for sintering the same |
| CN1609055A (en) * | 2004-09-21 | 2005-04-27 | 北京交通大学 | Ti-Si carbide powder and its normal pressure synthesis process with Al as reaction assistant |
| CN1966409A (en) * | 2005-11-19 | 2007-05-23 | 中国科学技术大学 | Process for synthesizing carbon titanium silicide powder |
-
2011
- 2011-11-28 CN CN2011103842648A patent/CN102659106A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001046083A1 (en) * | 1999-12-22 | 2001-06-28 | Drexel University | Process for forming 312 phase materials and process for sintering the same |
| CN1609055A (en) * | 2004-09-21 | 2005-04-27 | 北京交通大学 | Ti-Si carbide powder and its normal pressure synthesis process with Al as reaction assistant |
| CN1966409A (en) * | 2005-11-19 | 2007-05-23 | 中国科学技术大学 | Process for synthesizing carbon titanium silicide powder |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058749A (en) * | 2013-03-21 | 2014-09-24 | 中国科学院宁波材料技术与工程研究所 | Method for preparing titanium silicon carbon ceramic block material by pressureless sintering |
| CN104404426A (en) * | 2014-11-17 | 2015-03-11 | 苏州大学 | Ti3SiC2-based composite-material coating on surface of large-sized workpiece and method for preparing coating through plasma surfacing |
| RU2610380C2 (en) * | 2015-07-13 | 2017-02-09 | федеральное государственное бюджетное образовательное учреждение высшего образования "Пермский национальный исследовательский политехнический университет" | Method of producing titanium carbosilicide-based composite |
| CN105777127A (en) * | 2016-02-29 | 2016-07-20 | 东南大学 | Preparation method of high-purity Ti2SnC powder |
| WO2019181604A1 (en) * | 2018-03-23 | 2019-09-26 | 日清エンジニアリング株式会社 | Composite particles and method for producing composite particles |
| US20210024423A1 (en) * | 2018-03-23 | 2021-01-28 | Nisshin Engineering Inc. | Composite particles and method for producing composite particles |
| JPWO2019181604A1 (en) * | 2018-03-23 | 2021-03-18 | 日清エンジニアリング株式会社 | Composite particles and methods for producing composite particles |
| JP7159293B2 (en) | 2018-03-23 | 2022-10-24 | 日清エンジニアリング株式会社 | Composite particles and method for producing composite particles |
| CN109666815A (en) * | 2018-12-28 | 2019-04-23 | 西安交通大学 | A kind of MAX phase enhances the preparation method and applications of nickel-base high-temperature lubricating composite |
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Application publication date: 20120912 |