Tacony ceramic precursor, tacony ceramic and preparation method

By controlling the reaction of tantalum pentachloride, citric acid monohydrate, and ethylene glycol, a stable TaC precursor solution was prepared. Combined with crosslinking curing and high-temperature treatment, the problems of complex process and low purity in TaC coating preparation were solved, and high-purity, low-cost TaC ceramic preparation was achieved.

CN118063215BActive Publication Date: 2026-04-24HUNAN JIUSHAN SEMICON TECH CO LTD
View PDF 1 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
HUNAN JIUSHAN SEMICON TECH CO LTD
Filing Date
2024-02-20
Publication Date
2026-04-24

AI Technical Summary

Technical Problem

In the existing technology, the preparation method of TaC coating has the problems of complex process, high cost and low purity, and the precursor solution has poor stability and is difficult to preserve for a long time.

Method used

Using tantalum pentachloride, citric acid monohydrate, and ethylene glycol as raw materials, a stable organic compound precursor was formed by controlling the water bath temperature and stirring speed. Subsequently, TaC ceramics were prepared under cross-linking curing and high-temperature treatment. The pyrolysis temperature and heating rate were controlled to ensure uniform dispersion and sufficient carbothermic reduction.

Benefits of technology

This method enables the high-purity preparation of TaC ceramics, reduces preparation costs, simplifies the process, and provides a precursor solution with good stability, making it suitable for long-term storage.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN118063215B_ABST
    Figure CN118063215B_ABST
Patent Text Reader

Abstract

The application belongs to the technical field of carbide ceramic preparation, and discloses a TaC ceramic precursor, a TaC ceramic and a preparation method. The preparation of the TaC ceramic precursor comprises the following steps: S1, adding monohydrated citric acid and a tantalum pentachloride powder into anhydrous ethanol, with a water bath temperature of 10-20 DEG C, to obtain a first solution; S2, heating the first solution obtained in S1 to 30-50 DEG C in a water bath, adding deionized water and continuously stirring, and keeping warm for 20-40 min to obtain a second solution; S3, adding ethylene glycol dropwise into the second solution obtained in S2, uniformly stirring and then standing for 20-30 min to obtain a third solution; and S4, heating the third solution obtained in S3 to 50-70 DEG C in a water bath, keeping warm for 0.5-2 h to obtain a precursor solution. The prepared precursor is a stable organic compound containing carbon and tantalum elements, can be stored for a long time, has simple preparation process and low production cost, and the finally obtained TaC ceramic has high purity.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of carbide ceramic preparation technology, specifically relating to a TaC ceramic precursor, TaC ceramic, and preparation method. Background Technology

[0002] Tantalum carbide (TaC) is a structural material with high strength, high hardness, and good physicochemical stability. Its melting point is as high as 3880℃, making it one of the highest-temperature resistant compounds known. Therefore, TaC has broad application prospects in the field of ultra-high temperature materials. In the semiconductor field, third-generation semiconductor materials such as SiC and GaN require single-crystal substrate fabrication temperatures as high as 2000–2500℃, and TaC is considered an ideal coating material for graphite components required for the growth of third-generation semiconductor single-crystal substrates.

[0003] Currently, chemical vapor deposition (CVD) is the most common method for preparing TaC coatings. However, this method is technically challenging, involves complex process control, and has high production costs, which greatly limits the application and development of TaC coatings. Precursor conversion is a novel method for preparing ceramic materials using the pyrolysis of organic precursor polymers. This method has a simple process and low production costs. The process generally involves first obtaining an organic polymer that can be converted into a ceramic material through chemical synthesis, and then pyrolyzing it under certain temperature conditions to obtain a ceramic material that is difficult to produce using traditional methods.

[0004] Existing technologies typically use physical methods to mix carbon source compounds and tantalum source compounds to obtain precursors. Since the two do not react chemically to form stable organic compounds, the final pyrolysis products contain a large number of impurities and have poor material properties. Alternatively, precursors containing carbon and tantalum elements are obtained through chemical synthesis, but the precursor solution has poor stability and cannot be stored for a long time. At the same time, the required pyrolysis temperature is high, usually above 1600℃. Summary of the Invention

[0005] The problem to be solved by the present invention is to provide a TaC ceramic precursor, TaC ceramic and preparation method. The prepared precursor is a stable organic compound containing carbon and tantalum elements, which can be stored for a long time. The preparation process is simple and the production cost is low. The final TaC ceramic has high purity.

[0006] The present invention includes a method for preparing a TaC ceramic precursor, comprising the following steps:

[0007] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol and the water bath temperature is 10-20℃ to obtain the first solution.

[0008] S2. Heat the first solution obtained in S1 to 30-50°C in a water bath, add deionized water and stir continuously, keep warm for 20-40 minutes to obtain the second solution;

[0009] S3. Add ethylene glycol dropwise to the second solution obtained in S2, stir well, and let stand for 20-30 minutes to obtain the third solution.

[0010] S4. Heat the third solution obtained in S3 to 50-70°C in a water bath and keep it at that temperature for 0.5-2 hours to obtain the precursor solution.

[0011] Furthermore, in the raw materials, the mass ratio of tantalum pentachloride to anhydrous ethanol is 4:(7-10).

[0012] Furthermore, in the raw materials, the mass ratio of tantalum pentachloride, citric acid monohydrate, and ethylene glycol is 4:(1-2):(1-2).

[0013] Furthermore, in S1, tantalum pentachloride is added slowly in multiple portions with continuous stirring. The amount added at one time is 1% to 5% of the mass of anhydrous ethanol, with an interval of 2 to 5 minutes between additions. The addition of tantalum pentachloride generates a large amount of heat. If the amount added at one time is too large, the solution temperature will rise rapidly, the solution properties will be unstable, and precipitation will easily form. Therefore, the addition rate should not be too fast, and the addition process can be carried out under a cold water bath.

[0014] Furthermore, in S2, deionized water is added slowly multiple times with continuous stirring until the heat preservation is completed. The amount added at one time is 2% to 4% of the mass of anhydrous ethanol, and the addition interval is 1 to 3 minutes.

[0015] As a general inventive concept, the present invention also includes a TaC ceramic precursor, which is prepared by any of the TaC ceramic precursor preparation methods described above.

[0016] As a general inventive concept, the present invention also includes a method for preparing TaC ceramics, which is prepared by any of the methods for preparing TaC ceramic precursors described above, or by preparing TaC ceramic precursors, comprising the following steps:

[0017] T1. Crosslink and cure the TaC ceramic precursor at a temperature of 120–200°C;

[0018] T2. The TaC ceramic precursor after cross-linking and curing in T1 is subjected to high-temperature treatment at 1400-1800℃ to obtain TaC ceramic.

[0019] Furthermore, in T1, the heating rate during the crosslinking and curing process is 0.5–1.5 °C / min, and the holding time is 0.5–2 h.

[0020] Furthermore, in T2, the high-temperature treatment process is carried out under vacuum or inert gas protection, with a heating rate of 4–8 °C / min and a holding time of 1–2 h.

[0021] Too rapid a heating rate will cause the volatile components in the precursor solution to evaporate quickly, which is not conducive to material preparation.

[0022] As a general inventive concept, the present invention also includes a TaC ceramic, which is prepared by the TaC ceramic preparation method described in any of the above claims.

[0023] The beneficial effects of this invention are:

[0024] This invention uses tantalum pentachloride as the tantalum source and citric acid monohydrate and ethylene glycol as the carbon source. Citric acid monohydrate and tantalum pentachloride are added to anhydrous ethanol to obtain a tantalum alcohol solution containing citric acid monohydrate. During the dropwise addition of deionized water, citric acid monohydrate reacts slowly with metal alkoxides to form a coordination intermediate. In the subsequent heating process, the coordination intermediate further reacts to form a stable chelate ring stereocoagulation structure. During the cross-linking and curing process, the formed chelate ring stereocoagulation structure undergoes an esterification reaction with ethylene glycol to form a macromolecular gel. At this point, Ta ions are uniformly dispersed in the system and are difficult to migrate. In the subsequent pyrolysis process, tantalum carbide is generated through a carbothermal reduction reaction. In this process, due to the uniform distribution of tantalum and carbon elements, the carbothermal reduction reaction is more complete, the required process temperature is lower, and the final product has higher purity.

[0025] Compared to chemical vapor deposition (CVD) for preparing TaC ceramics, the method provided in this invention is simpler and less expensive. The TaC precursor solution provided in this invention is stable and can be stored at room temperature for extended periods. TaC ceramics are obtained after high-temperature pyrolysis at 1400℃, a low pyrolysis temperature. The resulting TaC ceramics have high purity, and XRD analysis shows no diffraction peaks from other substances. The TaC precursor described in this invention can be used to successfully prepare TaC coatings on graphite surfaces and can also be introduced into porous C / C materials to generate high-temperature TaC matrices. Attached Figure Description

[0026] Appendix Figure 1 This is a flowchart illustrating the preparation process of the TaC ceramic precursor in one embodiment of the present invention;

[0027] Appendix Figure 2 A physical image of the precursor solution prepared in Example 1;

[0028] Appendix Figure 3 This is a photograph of the precursor after crosslinking and curing in Example 1;

[0029] Appendix Figure 4 The image shows a SEM image of the TaC material obtained in Example 1.

[0030] Appendix Figure 5 The XRD diffraction pattern of the TaC material obtained in Example 1;

[0031] Appendix Figure 6The XRD diffraction pattern of the TaC material obtained in Example 2;

[0032] Appendix Figure 7 SEM image of the TaC-coated graphite material obtained in Example 3;

[0033] Appendix Figure 8 SEM image of the C / C-TaC composite material obtained in Example 4;

[0034] Appendix Figure 9 A photograph of the precursor solution prepared for Comparative Example 1;

[0035] Appendix Figure 10 The XRD diffraction pattern of the ceramic material obtained in Comparative Example 3;

[0036] Appendix Figure 11 The XRD diffraction pattern of the ceramic material obtained in Comparative Example 4;

[0037] Appendix Figure 12 XRD diffraction patterns of ceramic materials were obtained for Comparative Example 5. Detailed Implementation

[0038] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.

[0039] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the specification of this invention is for the purpose of describing particular embodiments only and is not intended to limit the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items. Furthermore, the technical solutions of the various embodiments of this invention can be combined with each other, but only on the basis that they can be implemented by one of ordinary skill in the art. When the combination of technical solutions is contradictory or impossible to implement, such combination of technical solutions should be considered non-existent and not within the scope of protection claimed by this invention.

[0040] Example 1

[0041] As attached Figure 1 As shown, this embodiment provides a method for preparing a TaC precursor, wherein the mass ratio of tantalum pentachloride powder, anhydrous ethanol, citric acid monohydrate, and ethylene glycol is 4:10:1:2; the method includes the following steps:

[0042] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol to obtain the first solution; the tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0043] S2. Place the first solution in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours to obtain the second solution. Add approximately 50g of deionized water for every 100g of anhydrous ethanol.

[0044] S3. Add ethylene glycol dropwise to the second solution, stir well and let stand for 30 minutes to obtain the third solution;

[0045] S4. Place the third solution in a water bath and heat it to 50°C. After 2 hours of water bath heating, the TaC precursor solution is obtained.

[0046] This embodiment also provides a method for preparing TaC ceramics, including the following steps:

[0047] T1. Place the TaC precursor solution prepared above in an oven at 150°C for 1 hour to obtain the cross-linked and cured precursor.

[0048] T2. The cross-linked and cured precursor is placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature is 1800℃, the heating rate is 4℃ / min, and the holding time is 1h.

[0049] The TaC precursor solution obtained in this embodiment is shown in the attached figure. Figure 2 As shown, it is clear and transparent with good fluidity.

[0050] The precursor after crosslinking and curing in this embodiment is shown in the attached figure. Figure 3 As shown, after cross-linking and curing, the precursor solution is transformed into solid powder particles, which are pale yellow in color.

[0051] The SEM image of the TaC ceramic obtained after high-temperature treatment (T2) in this embodiment is attached. Figure 4 As shown, the obtained TaC ceramic consists of yellow solid particles with relatively dense grains. The XRD diffraction pattern is attached. Figure 5 As shown, the diffraction peaks are sharp and there are no other impurity peaks, indicating that the prepared TaC material has good crystallinity and high purity.

[0052] Example 2

[0053] This embodiment provides a method for preparing a TaC precursor, wherein the mass ratio of tantalum pentachloride powder, anhydrous ethanol, citric acid monohydrate, and ethylene glycol is 4:7:2:1; the method includes the following steps:

[0054] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol to obtain the first solution; the tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0055] S2. Place the first solution in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours to obtain the second solution. Add approximately 50g of deionized water for every 100g of anhydrous ethanol.

[0056] S3. Add ethylene glycol dropwise to the second solution, stir well and let stand for 20 minutes to obtain the third solution;

[0057] S4. Place the third solution in a water bath and heat it to 70°C. After 0.5 hours in the water bath, the precursor solution is obtained.

[0058] This embodiment also provides a method for preparing TaC ceramics, including the following steps:

[0059] T1. Place the TaC precursor solution prepared above in an oven at 120°C for 2 hours.

[0060] T2. The cross-linked and cured precursor is placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature is 1400℃, the heating rate is 8℃ / min, and the holding time is 2h.

[0061] The XRD diffraction pattern of the TaC ceramic material obtained after high-temperature treatment (T2) in this embodiment is attached. Figure 6 As shown, there are no other impurity peaks in the diffraction pattern, indicating that the obtained TaC ceramic has high purity.

[0062] Example 3

[0063] This embodiment provides a TaC coating, which uses the precursor solution prepared in Example 1 to coat the graphite surface, followed by crosslinking curing and high-temperature pyrolysis to obtain the TaC coated product. The specific steps are as follows:

[0064] 1) The precursor solution prepared in Example 1 was uniformly coated onto the graphite surface, where the graphite density was 1.72 g / cm³. 3 ;

[0065] 2) Place the graphite coated with the precursor solution in an oven for cross-linking and curing at 150°C for 1 hour.

[0066] 3) The cross-linked and cured sample was placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature was 1400℃, the heating rate was 4℃ / min, and the holding time was 1h to obtain TaC-coated graphite sample.

[0067] The SEM image of the TaC-coated graphite sample obtained in this embodiment is attached. Figure 7As shown, in this embodiment, a continuous TaC coating is prepared on the graphite surface. The coating has a good bonding effect with the graphite substrate, and the coating thickness is 46.5 μm.

[0068] Example 4

[0069] This embodiment provides a C / C-TaC composite material. The precursor solution prepared in Example 1 is introduced into a porous C / C material to obtain a C / C-TaC composite material with a high-temperature resistant matrix. The specific steps are as follows:

[0070] 1) The density is 1.1 g / cm³ 3 The C / C material is placed in a suitable sealed container, which is connected to a vacuum pump. The precursor solution prepared in Example 1 is injected into the container until the upper surface of the C / C material is completely submerged.

[0071] 2) Evacuate the container until the ultimate vacuum is reached, and continue evacuating for 30 minutes. Then turn off the vacuum pump and let it stand for 12 hours. Use vacuum impregnation to introduce the precursor solution into the C / C material.

[0072] 3) Take out the C / C material after vacuum impregnation treatment and place it in an oven for cross-linking and curing at 200℃ for 0.5h.

[0073] 4) The cross-linked and cured sample was placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature was 1800℃, the heating rate was 4℃ / min, and the holding time was 1h. After three cycles of vacuum impregnation-curing cross-linking-high-temperature pyrolysis process, a C / C-TaC composite material with a high-temperature resistant matrix was obtained.

[0074] The density of the C / C-TaC composite material obtained in this embodiment is 1.38 g / cm³. 3 The cross-sectional SEM image is attached. Figure 8 As shown in the figure, the precursor described in this invention was successfully infiltrated into the C / C material, and the resulting TaC ceramic phase was uniformly distributed in the pores inside the material.

[0075] Comparative Example 1

[0076] The preparation method of the tantalum carbide precursor in this comparative example is largely the same as that in Example 1, except for the water bath temperature and water bath time of the mixed solution. The specific steps are as follows:

[0077] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol. The tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0078] S2. Place the solution treated in S1 in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours. For every 100g of anhydrous ethanol, add approximately 50g of deionized water.

[0079] S3. Add ethylene glycol dropwise to the solution after S2 treatment, stir well and let stand for 20 minutes;

[0080] S4. Place the solution treated in S3 in a water bath and heat it to 80°C. After 1 hour in the water bath, the precursor solution is obtained, as shown in the attached figure. Figure 9 As shown;

[0081] In this comparative example, after the mixture was treated in an 80°C water bath for 1 hour, due to the high water bath temperature, some small molecules in the precursor solution underwent esterification and formed a gel, resulting in reduced solution fluidity and making it difficult to use for the subsequent preparation of TaC materials.

[0082] Comparative Example 2

[0083] The preparation method of the tantalum carbide precursor in this comparative example is largely the same as that in Example 1, except that the ratio of tantalum pentachloride powder, anhydrous ethanol, citric acid monohydrate, and ethylene glycol is 4:5:1:2, and the amount of anhydrous ethanol added is reduced. The specific steps are as follows:

[0084] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol. The tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0085] S2. Place the solution treated in S1 in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours. For every 100g of anhydrous ethanol, add approximately 50g of deionized water.

[0086] S3. Add ethylene glycol dropwise to the solution after S2 treatment, stir well and let stand for 20 minutes;

[0087] S4. The solution after S3 treatment is placed in a water bath and heated to 50°C. After 2 hours of water bath time, the precursor solution is obtained. The obtained precursor solution gels after standing for 24 hours, and the fluidity of the solution decreases.

[0088] In this comparative example, due to insufficient addition of anhydrous ethanol, tantalum pentachloride was not fully dissolved, resulting in a large amount of powder suspension in the obtained tantalum alcohol solution, which was retained in the final precursor solution. The presence of fine powder suspension in the solution promoted gelation of the solution, making it difficult for the precursor solution to remain stable for a long time.

[0089] Comparative Example 3

[0090] The preparation method of the tantalum carbide precursor in this comparative example is largely the same as that in Example 1, except that the ratio of tantalum pentachloride powder, anhydrous ethanol, citric acid monohydrate, and ethylene glycol is 4:10:0.75:2, and the amount of citric acid monohydrate added is reduced. The specific steps are as follows:

[0091] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol. The tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0092] S2. Place the solution treated in S1 in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours. For every 100g of anhydrous ethanol, add approximately 50g of deionized water.

[0093] S3. Add ethylene glycol dropwise to the solution after S2 treatment, stir well and let stand for 20 minutes;

[0094] S4. Place the solution treated in S3 in a water bath and heat it. Set the water bath temperature to 50°C and heat it for 2 hours to obtain the precursor solution.

[0095] The tantalum carbide precursor prepared using this comparative example is prepared using the following specific steps:

[0096] T1. Place the precursor solution prepared in this comparative example in an oven at 150°C for 1 hour to obtain the cross-linked and cured precursor.

[0097] T2. The cross-linked and cured precursor is placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature is 1800℃, the heating rate is 4℃ / min, and the holding time is 1h. TaC material is obtained after high-temperature treatment.

[0098] The XRD diffraction pattern of the TaC material obtained in this comparative example is attached. Figure 10 As shown, due to the reduction in the amount of citric acid monohydrate added, the carbon source of the prepared precursor solution was insufficient, and the final product after high-temperature pyrolysis was Ta2C.

[0099] Comparative Example 4

[0100] The preparation method of the tantalum carbide precursor in this comparative example is largely the same as that in Example 1, except that the high-temperature pyrolysis temperature is set to 1000℃. The specific steps are as follows:

[0101] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol. The tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0102] S2. Place the solution treated in S1 in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours. For every 100g of anhydrous ethanol, add approximately 50g of deionized water.

[0103] S3. Add ethylene glycol dropwise to the solution after S2 treatment, stir well and let stand for 20 minutes;

[0104] S4. Place the solution treated in S3 in a water bath and heat it. Set the water bath temperature to 50°C and heat it for 2 hours to obtain the precursor solution.

[0105] The tantalum carbide precursor prepared using this comparative example is prepared using the following specific steps:

[0106] T1. Place the precursor solution prepared in this comparative example in an oven at 150°C for 1 hour to obtain the cross-linked and cured precursor.

[0107] T2. The cross-linked and cured precursor is placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature is 1000℃, the heating rate is 4℃ / min, and the holding time is 2h. TaC material is obtained after high-temperature treatment.

[0108] The XRD diffraction pattern of the TaC material obtained in this comparative example is attached. Figure 11 As shown, due to the low high-temperature pyrolysis temperature, the carbothermic reduction reaction temperature was not reached, resulting in the pyrolysis products mainly being Ta2O5.

[0109] Comparative Example 5

[0110] The preparation method of the tantalum carbide precursor in this comparative example is largely the same as that in Example 1, except that the high-temperature pyrolysis temperature is set to 1200℃. The specific steps are as follows:

[0111] S1. Citric acid monohydrate and tantalum pentachloride powder are added to anhydrous ethanol. The tantalum pentachloride addition process is carried out in a cold water bath at a temperature of 20°C.

[0112] S2. Place the solution treated in S1 in a water bath and heat it to 40°C. Slowly add deionized water while stirring continuously. Keep it warm for 0.5 hours. For every 100g of anhydrous ethanol, add approximately 50g of deionized water.

[0113] S3. Add ethylene glycol dropwise to the solution after S2 treatment, stir well and let stand for 20 minutes;

[0114] S4. Place the solution treated in S3 in a water bath and heat it. Set the water bath temperature to 50°C and heat it for 2 hours to obtain the precursor solution.

[0115] The tantalum carbide precursor prepared using this comparative example is prepared using the following specific steps:

[0116] T1. The precursor solution was then placed in an oven at 150°C for 1 hour to obtain the cross-linked and cured precursor.

[0117] T2. The cross-linked and cured precursor is placed in a high-temperature pyrolysis furnace and subjected to high-temperature treatment under argon atmosphere protection. The treatment temperature is 1200℃, the heating rate is 4℃ / min, and the holding time is 2h. TaC material is obtained after high-temperature treatment.

[0118] The XRD diffraction pattern of the comparative TaC material is attached. Figure 12 As shown, in this comparative example, the high-temperature pyrolysis temperature is 1200℃. The metal oxide begins to undergo carbothermic reduction reaction and generates TaC. However, the carbothermic reduction reaction is insufficient, and the product still contains Ta2O5.

[0119] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0120] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

[0121] The contents not described in detail in this specification are existing technologies known to those skilled in the art.

Claims

1. A method for preparing TaC ceramics, characterized in that, Includes the following steps: Preparation of TaC ceramic precursors: S1. Add citric acid monohydrate and tantalum pentachloride powder to anhydrous ethanol, with a mass ratio of tantalum pentachloride to anhydrous ethanol of 4:(7~10), and a water bath temperature of 10~20℃ to obtain the first solution. S2. Heat the first solution obtained in S1 to 30~50℃ in a water bath, add deionized water and stir continuously, keep warm for 20~40min to obtain the second solution; S3. Add ethylene glycol dropwise to the second solution obtained in S2, stir evenly, and let stand for 20-30 minutes to obtain the third solution; the mass ratio of tantalum pentachloride, citric acid monohydrate and ethylene glycol is 4:(1-2):(1-2). S4. Heat the third solution obtained in S3 to 50~70℃ in a water bath and keep it at that temperature for 0.5~2h to obtain the precursor solution; Preparation of TaC ceramics: T1. Crosslink and cure the TaC ceramic precursor at a temperature of 120~200℃; T2. The TaC ceramic precursor after cross-linking and curing in T1 is subjected to high-temperature treatment at 1400~1800℃ to obtain TaC ceramic.

2. The method for preparing TaC ceramics as described in claim 1, characterized in that, In S1, tantalum pentachloride is added slowly in multiple portions with continuous stirring. The amount added at one time is 1% to 5% of the mass of anhydrous ethanol, and the interval between additions is 2 to 5 minutes.

3. The method for preparing TaC ceramics as described in claim 1, characterized in that, In S2, deionized water is added slowly in multiple batches with continuous stirring until the heat preservation is completed. The amount added at one time is 2% to 4% of the mass of anhydrous ethanol, and the interval between additions is 1 to 3 minutes.

4. The method for preparing TaC ceramics as described in claim 1, characterized in that, In T1, the heating rate during the crosslinking and curing process is 0.5~1.5℃ / min, and the holding time is 0.5~2h.

5. The method for preparing TaC ceramics as described in claim 1, characterized in that, In T2, the high-temperature treatment process is carried out under vacuum or inert gas protection, with a heating rate of 4~8℃ / min and a holding time of 1~2h.

Citation Information

Patent Citations

  • Preparation method of Ta4HfC5 precursor and prepared nano ceramic and high-temperature-resistant composite material

    CN117402336A