CN115959668A - Full-liquid state synthetic Ti 3 SiC 2 Ceramic and preparation method thereof - Google Patents
Full-liquid state synthetic Ti 3 SiC 2 Ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic materials, and discloses a full-liquid state synthesized Ti 3 SiC 2 The ceramic and the preparation method thereof are as follows: according to the molar ratio of Ti to Si being 3 2 Uniformly mixing the powder and LPCS to obtain a precursor material; in an inert atmosphere, curing the precursor material at 110-130 ℃, and then performing ball milling, drying and pyrolysis in sequence to obtain the Ti 3 SiC 2 A ceramic. The preparation method is simple and convenient to operate; and LPCS and TiH 2 The powder can form a full liquid system, a high-content target product can be guaranteed without adding other additives, and the full liquid system has good fluidity and is convenient to be combined with a porous material through impregnation to prepare a composite material meeting the use conditions of the high-speed railway pantograph.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to a full-liquid state synthesized Ti 3 SiC 2 Ceramics and a method for preparing the same.
Background
With the rapid development of high-speed railways in China, the electric locomotive is ensured to obtain sufficient and stable electric power from a railway contact network power supply system, and the method is one of key factors for ensuring the safe and reliable operation of the electric locomotive. The pantograph slide plate is a key current collecting element for obtaining power of the electric locomotive, and the current collecting quality of the pantograph slide plate directly influences the running speed, the smoothness and the safety of the electric locomotive.
Ti 3 SiC 2 The MAX phase material has excellent conductivity, and the MAX phase material can be used as a preferred material of a new-generation pantograph pan by being combined with a C/C composite material with carbon fibers as a reinforcement.
In the prior art, when the MAX phase material modified C/C composite material is prepared, methods such as solid powder embedding or reaction infiltration are generally adopted, however, these methods generally require a plurality of powder raw materials and additives to participate in the preparation, not only the process is complex, but also the MAX phase material with higher content can be generated by pressurizing or higher temperature in the sintering process; in addition, the method can only generate MAX phase materials on the surface of the C/C composite material, and the MAX phase materials are difficult to enter the porous material, so that the improvement on the performance of the C/C composite material matrix is very limited; when the C/C composite material prepared by the method is used as a pantograph material, the conductivity can meet the requirement of power transmission because the MAX material on the surface is not lost in the initial use stage; however, when the surface layer is consumed, the conductivity of the surface layer is greatly reduced, and finally the use requirement cannot be met.
Therefore, the invention provides a fully liquid state synthetic Ti 3 SiC 2 Ceramics and a method for preparing the same.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a full liquid state synthetic Ti 3 SiC 2 The preparation method of the invention is easier to be dipped into the porous material to generate MAX phase material to satisfy the severe service environment.
The invention relates to a full liquid state synthetic Ti 3 SiC 2 The ceramic and the preparation method thereof are realized by the following technical scheme:
first object of the inventionIt is to provide a fully liquid state synthesized Ti 3 SiC 2 The preparation method of the ceramic comprises the following steps:
step 1, according to the molar ratio of Ti to Si of 1.2-1.7, adding TiH into a mixture of Ti and Si in a molar ratio of 3 2 Uniformly mixing the powder with LPCS (liquid polycarbosilane) to obtain a precursor material;
step 2, curing the precursor material at 110-130 ℃ in an inert atmosphere, and then performing ball milling, drying and pyrolysis in sequence to obtain the Ti 3 SiC 2 A ceramic.
Further, stirring the TiH 2 The powder and the LPCS are mixed evenly, the stirring speed is 900-1100 r/min, and the stirring time is 8-12 h.
Furthermore, the time of the curing treatment is 2-6 h, and the temperature rise rate of the curing treatment is 3-7 ℃/min.
Further, the ball milling treatment is wet ball milling, the ball-material ratio is 1-3, the ball milling rotation speed is 400-600 r/min, and the ball milling time is 16-24 h.
Furthermore, the temperature of the drying treatment is 60-80 ℃, and the drying time is 6-12 h.
Further, the pyrolysis treatment process comprises the following steps:
the first stage heat preservation treatment is carried out on the dried product at 650-750 ℃, then the second stage heat preservation treatment is carried out at 1050-1150 ℃, and then the third stage heat preservation treatment is carried out at 1450-1550 ℃.
Further, the vacuum degree of the pyrolysis treatment is less than or equal to 100Pa.
Further, the heat preservation time of the first stage heat preservation treatment is 4-10h;
the heat preservation time of the second stage heat preservation treatment is 1.5-2.5 h;
the heat preservation time of the third stage heat preservation treatment is 3-5 h.
Further, the heating rates of the first stage heat preservation treatment, the second stage heat preservation treatment and the third stage heat preservation treatment are all 3-7 ℃/min.
The second purpose of the invention is to provide Ti prepared by the preparation method 3 SiC 2 A ceramic.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses TiH 2 Mixing the powder and LPCS (liquid polycarbosilane) serving as raw materials to form a precursor material of a full liquid system, crosslinking and curing the precursor material at 110-130 ℃, and then placing a product obtained by crosslinking and curing in a graphite crucible under the protection of inert gas for high-temperature reaction, wherein the LPCS is converted from organic to inorganic and pyrolyzed into a SiC ceramic phase and C; at the same time, tiH 2 Dehydrogenation to Ti also occurs at high temperatures, and this transformation results in Ti being more reactive than Ti powder; with further increase in temperature, siC, C react with the dehydrogenated Ti formed in the precursor material to form Ti 3 SiC 2 Phase thereby preparing Ti 3 SiC 2 A material.
Ti provided by the invention 3 SiC 2 The ceramic preparation method has simple principle and convenient operation; precursors LPCS and TiH 2 The powder can form a full liquid system, and not only can a target product with higher content be ensured, but also good fluidity can be ensured under the condition that other additives are not needed; therefore, the composite material can be combined with the porous material through impregnation to prepare the composite material meeting the use conditions of the high-speed railway pantograph.
And Ti prepared by the invention 3 SiC 2 In the material Ti 3 SiC 2 The mass percentage of the titanium dioxide can reach 33-81 percent, and the titanium dioxide also contains a small amount of TiC which can form TiO at high temperature 2 Thereby acting as a barrier to oxidation of the protective material itself. Thus, ti can be prepared as a fully liquid system 3 SiC 2 The material is applied to severer service environment.
Drawings
FIG. 1 shows Ti prepared in example 1 3 SiC 2 An XRD pattern of (a);
FIG. 2 shows Ti prepared in example 2 3 SiC 2 An XRD pattern of (a);
FIG. 3 is T prepared in example 3i 3 SiC 2 An XRD pattern of (a);
FIG. 4 shows Ti prepared in example 1 3 SiC 2 SEM photograph of (a);
FIG. 5 shows Ti prepared in example 2 3 SiC 2 SEM photograph of (a);
FIG. 6 shows Ti prepared in example 3 3 SiC 2 SEM photograph of (b).
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. In the following examples of the present invention, LPCS used was VHPCS-1 LPCS provided by the institute of chemistry of the chinese academy of sciences.
The invention provides a Ti synthesized in a full liquid state 3 SiC 2 The ceramic is prepared by the following steps:
step 1, reacting TiH 2 Uniformly mixing the powder with LPCS (liquid polycarbosilane) to obtain a precursor material;
in the present invention, tiH is preferably added in a molar ratio of Ti: si of 3 2 And uniformly mixing the powder and the LPCS to obtain a fully liquid precursor material.
The invention is not limited to TiH 2 The powder and the LPCS may be mixed in a manner that the powder and the LPCS can be uniformly mixed. In the invention, preferably, the mixing is carried out by adopting a stirring mode, the stirring speed is 900-1100 r/min, and the stirring time is 8-12 h, so that TiH can be ensured 2 Mixing the powder with LPCS.
Step 2, solidifying the precursor material in an inert atmosphere, and then performing ball milling treatment, drying treatment and pyrolysis treatment in sequence to obtain Ti 3 SiC 2 A ceramic;
in the present invention, it is preferable that the temperature of the curing treatment is 110 to 130 ℃, the curing time is 2 to 6 hours, and the temperature rise rate of the curing treatment is 3 to 7 ℃/min. The invention carries out curing treatment under the process condition, the temperature is relatively low, and the temperature rise is relatively gentle; so as to ensure the solidification of the sample and avoid the phenomenon that a large amount of small molecule gas is discharged to leave a large amount of bubbles in the sample to influence the uniformity of the sample due to high temperature.
The invention avoids the possible presence of TiH in the cured product 2 And the distribution is uneven, and ball milling treatment and drying treatment are sequentially carried out before pyrolysis treatment is carried out on a product obtained by curing treatment so as to ensure that all materials in the cured product are fully and uniformly mixed. In the invention, the ball milling is preferably carried out by adopting a wet ball milling method, ethanol is taken as a ball milling auxiliary agent, and the materials are as follows: ethanol: the mass ratio of the ball is 1:0.5:1 to 3, the ball milling rotating speed is 400 to 600r/min, and the ball milling time is 16 to 24 hours. In the invention, the drying temperature is 60-80 ℃, and the drying time is 6-12 h.
In the invention, the pyrolysis treatment is preferably carried out by adopting a gradual temperature rise mode, and the pyrolysis treatment process comprises the following steps: the dried product is firstly preserved for 4-10h at 650-750 ℃, then preserved for 1.5-2.5 h at 1050-1150 ℃ and preserved for 3-5 h at 1450-1550 ℃, and the heating rate of each stage is 3-7 ℃/min. Wherein, the invention ensures TiH through the first stage heat preservation treatment 2 Completely dehydrogenated to be converted into Ti, thereby providing a Ti source with high activity for subsequent reaction. And then, carrying out second-stage heat preservation treatment to ensure that the LPCS is completely transformed into SiC and C in a ceramic way. Then, carrying out a third stage heat preservation treatment to enable the high-activity Ti source, siC and C obtained by the first two stages of heat preservation treatment to generate Ti at 1450-1550 DEG C 3 SiC 2 (ii) a Thereby leading each raw material to fully react through the step-by-step temperature rise treatment, and finally generating Ti 3 SiC 2 A material.
Example 1
This example provides a Ti 3 SiC 2 The material and the preparation method thereof are as follows:
s101: preparation of precursor Material
According to the molar ratio of Ti to Si =3, 84.49g of TiH is accurately weighed out 2 Powder, 35.01g lpcs;
weighing the TiH 2 Mixing the powder and the LPCS in a magnetic stirring cup at controlled rotation speedAnd (5) performing magnetic stirring for 10 hours under the condition of 1000r/min to obtain the all-liquid precursor material.
S102: solidifying, ball milling and drying
Placing the precursor material prepared in the step S101 in a forced air drying oven, wherein the curing temperature is 120 ℃, the heating rate is 5 ℃/min, and the time is 4h; pretreating a cured product, wherein the raw materials are as follows: ethanol: the ball mass ratio is 1:0.5:2, wet grinding is carried out under the condition of 500r/min, and the wet grinding time is 20h; then putting the mixture into a blast drying oven for drying at the temperature of 70 ℃ for 8h.
S103: preparation of Ti 3 SiC 2 Material
Putting the solidified product treated in the step S102 into a box type sintering furnace for cracking, sequentially vacuumizing to be below 100Pa, introducing argon for protection, heating to 700 ℃, and preserving heat for 4-10h; keeping the temperature at 1100 ℃ for 2h; preserving heat for 4 hours at 1500 ℃; cooling to room temperature to obtain Ti 3 SiC 2 Ceramic, wherein the heating rate is 5 ℃/min.
Example 2
This example provides a Ti 3 SiC 2 The material and the preparation method thereof are as follows:
s101: preparation of precursor Material
According to the molar ratio of Ti to Si =3, 80.65g of TiH is accurately weighed 2 Flour, 41.78g lpcs;
weighing the TiH 2 And mixing the powder and the LPCS, placing the mixture in a magnetic stirring cup, and performing magnetic stirring for 10 hours under the condition of controlling the rotating speed to be 1000r/min to obtain the all-liquid precursor material.
S102: curing and pretreatment
Placing the precursor material prepared in the step S101 in a forced air drying oven, wherein the curing temperature is 120 ℃, the heating rate is 5 ℃/min, and the time is 4h; pretreating a cured product, wherein the raw materials are as follows: ethanol: the ball mass ratio is 1:0.5:2, wet grinding is carried out under the condition of 500r/min, and the wet grinding time is 20h; then putting the mixture into a blast drying oven for drying at the temperature of 70 ℃ for 8h.
S103: preparation of Ti 3 SiC 2 Material
Will be processed in step S102Putting the solidified product into a box type sintering furnace for cracking, sequentially vacuumizing to below 100Pa, introducing argon for protection, heating to 700 ℃, and preserving heat for 4-10h; keeping the temperature at 1100 ℃ for 2h; preserving heat for 4 hours at 1500 ℃; cooling to room temperature to obtain Ti 3 SiC 2 Ceramic, wherein the heating rate is 5 ℃/min.
Example 3
This example provides a Ti 3 SiC 2 The material and the preparation method thereof are as follows:
s101: preparation of precursor Material
According to the molar ratio of Ti to Si =3, 78.28g of TiH is accurately weighed 2 Powder, 45.96g of LPCS;
weighing the TiH 2 And mixing the powder and the LPCS, placing the mixture in a magnetic stirring cup, and performing magnetic stirring for 10 hours under the condition of controlling the rotating speed to be 1000r/min to obtain the all-liquid precursor material.
S102: curing and pretreatment
Placing the precursor material prepared in the step S101 in a forced air drying oven, wherein the curing temperature is 120 ℃, the heating rate is 5 ℃/min, and the time is 4h; pretreating a cured product, wherein the raw materials are as follows: ethanol: the ball mass ratio is 1:0.5:2, wet grinding is carried out under the condition of 500r/min, and the wet grinding time is 20h; then putting the mixture into a blast drying oven for drying at the temperature of 70 ℃ for 8h.
S103: preparation of Ti 3 SiC 2 Material
Putting the cured product treated in the step S102 into a box type sintering furnace for cracking, sequentially vacuumizing to be less than 100Pa, introducing argon for protection, heating to 700 ℃, and preserving heat for 4-10 hours; keeping the temperature at 1100 ℃ for 2h; preserving the heat for 4 hours at 1500 ℃; cooling to room temperature to obtain Ti 3 SiC 2 Ceramic, wherein the heating rate is 5 ℃/min.
Example 4
This example provides a Ti 3 SiC 2 The material, and its preparation method differs from example 1 only in that:
the temperature of the curing treatment is 110 ℃, the time of the curing treatment is 2h, and the heating rate of the curing treatment is 3 ℃/min;
the stirring speed is 900r/min, and the stirring time is 12h;
the ball-material ratio of ball-milling treatment is 1, the ball-milling rotation speed is 400r/min, and the ball-milling time is 16h;
the drying treatment temperature is 60 ℃, and the drying time is 6h;
the pyrolysis treatment process comprises the following steps: preserving the heat of the dried product at 650 ℃ for 4h, then preserving the heat at 1050 ℃ for 1.5h, and then preserving the heat at 1450 ℃ for 3h; and the heating rate of each stage is 3 ℃/min.
Example 5
This example provides a Ti 3 SiC 2 The material, and the preparation method thereof differs from example 1 only in that:
the temperature of the curing treatment is 130 ℃, the time of the curing treatment is 6h, and the heating rate of the curing treatment is 7 ℃/min;
the stirring speed is 1100r/min, and the stirring time is 8h;
the ball-material ratio of the ball milling treatment is 1;
the drying temperature is 80 ℃, and the drying time is 12h;
the pyrolysis treatment process comprises the following steps: the dried product is firstly insulated at 750 ℃ for 10h, then at 1150 ℃ for 2.5h and then at 1550 ℃ for 5h; and the heating rate of each stage is 7 ℃/min.
Experimental part
(I) XRD test
Ti of the invention prepared in examples 1-3 3 SiC 2 For example, XRD tests were performed respectively, and the test results are shown in fig. 1, fig. 2 and fig. 3, respectively. Wherein FIG. 1 shows Ti prepared in example 1 3 SiC 2 An XRD pattern of the material; FIG. 2 shows Ti prepared in example 2 3 SiC 2 An XRD pattern of the material; FIG. 3 shows Ti prepared in example 3 3 SiC 2 XRD pattern of material.
As can be seen from FIGS. 1 to 3, ti prepared in example 1 3 SiC 2 The material contains Ti 5 Si 3 And TiC, wherein Ti 5 Si 3 Due to the fact thatThe carbon content in the system is lacked so as to remain; examples 2 and 3 contained a large amount of Ti 3 SiC 2 In addition, small amounts of TiC are also present; indicating that TiC is used as a part of the intermediate product to continue reacting to generate Ti 3 SiC 2 The other part is remained; the residual TiC can generate TiO under the high-temperature use environment 2 The protective material prevents further oxidation.
(II) SEM scanning Electron microscopy image analysis
Ti of the invention prepared in examples 1-3 3 SiC 2 For example, SEM image analysis was performed on the materials, and the test results are shown in fig. 4, fig. 5, and fig. 6, respectively. Wherein, FIG. 4 shows Ti prepared in example 1 3 SiC 2 SEM pictures of the material; FIG. 5 Ti prepared in example 2 3 SiC 2 SEM pictures of the material; FIG. 6 Ti prepared in example 3 3 SiC 2 SEM pictures of the materials.
As can be seen from FIG. 4, except for Ti of a layered structure 3 SiC 2 In addition, tiC still exists; from FIGS. 5 and 6, it can be seen that a large amount of Ti is contained 3 SiC 2 Layered structure and less intermediate products.
It is to be understood that the above-described embodiments are only some of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. Full liquid state synthetic Ti 3 SiC 2 The preparation method of the ceramic is characterized by comprising the following steps:
step 1, according to the molar ratio of Ti to Si being 1.2-1.7, mixing TiH 2 Uniformly mixing the powder and liquid polycarbosilane to obtain a precursor material;
step 2, curing the precursor material at 110-130 ℃ in an inert atmosphere, and then performing ball milling, drying and pyrolysis in sequence to obtain the Ti 3 SiC 2 A ceramic.
2. The method of claim 1, wherein the TiH is agitated to form the TiH 2 The powder and the liquid polycarbosilane are uniformly mixed, the stirring speed is 900-1100 r/min, and the stirring time is 8-12 h.
3. The method according to claim 1, wherein the curing treatment time is 2 to 6 hours, and the temperature increase rate of the curing treatment is 3 to 7 ℃/min.
4. The preparation method of claim 1, wherein the ball milling treatment is wet ball milling, the ball-to-material ratio is 1-3, the ball milling rotation speed is 400-600 r/min, and the ball milling time is 16-24 h.
5. The method according to claim 1, wherein the drying treatment is carried out at a temperature of 60 to 80 ℃ for 6 to 12 hours.
6. The method of claim 1, wherein the pyrolysis treatment comprises:
the first stage heat preservation treatment is carried out on the dried product at 650-750 ℃, then the second stage heat preservation treatment is carried out at 1050-1150 ℃, and then the third stage heat preservation treatment is carried out at 1450-1550 ℃.
7. The method according to claim 6, wherein the degree of vacuum of the pyrolysis treatment is 100Pa or less.
8. The preparation method according to claim 6, wherein the first-stage heat-insulating treatment is carried out for a heat-insulating time of 4 to 10 hours;
the heat preservation time of the second stage heat preservation treatment is 1.5-2.5 h;
the heat preservation time of the third stage heat preservation treatment is 3-5 h.
9. The method according to claim 6, wherein the first-stage heat-retaining treatment, the second-stage heat-retaining treatment and the third-stage heat-retaining treatment are performed at a temperature increase rate of 3 to 7 ℃/min.
10. Ti prepared by the preparation method of any one of claims 1 to 9 3 SiC 2 A ceramic.
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| CN202211590500.6A CN115959668A (en) | 2022-12-12 | 2022-12-12 | Full-liquid state synthetic Ti 3 SiC 2 Ceramic and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530945A (en) * | 2011-12-15 | 2012-07-04 | 中国科学院上海硅酸盐研究所 | Method for preparing high-purity Ti3SiC2 powder |
| CN103341291A (en) * | 2013-06-30 | 2013-10-09 | 成都易态膜分离技术有限公司 | Sintered porous material and filter element using same |
| CN111675541A (en) * | 2020-05-10 | 2020-09-18 | 华北理工大学 | Preparation method of carbon-containing MAX phase material |
| CN114315394A (en) * | 2021-12-21 | 2022-04-12 | 西北工业大学 | By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102530945A (en) * | 2011-12-15 | 2012-07-04 | 中国科学院上海硅酸盐研究所 | Method for preparing high-purity Ti3SiC2 powder |
| CN103341291A (en) * | 2013-06-30 | 2013-10-09 | 成都易态膜分离技术有限公司 | Sintered porous material and filter element using same |
| CN111675541A (en) * | 2020-05-10 | 2020-09-18 | 华北理工大学 | Preparation method of carbon-containing MAX phase material |
| CN114315394A (en) * | 2021-12-21 | 2022-04-12 | 西北工业大学 | By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material |
Non-Patent Citations (1)
| Title |
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| JINSHAN YANG ET AL.，: "Fabrication of Ti3SiC2 powders using TiH2 as the source of Ti", 《CERAMICS INTERNATIONAL》, pages 3509 - 3512 * |
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