CN116730740B - Preparation method of high-strength TiC-based porous ceramic - Google Patents
Preparation method of high-strength TiC-based porous ceramic Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000292 calcium oxide Substances 0.000 claims abstract description 28
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 28
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002131 composite material Substances 0.000 claims abstract description 9
- 238000011049 filling Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000011888 foil Substances 0.000 claims abstract description 8
- 239000011812 mixed powder Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 238000007731 hot pressing Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005498 polishing Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000007780 powder milling Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 8
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 5
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/04—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by dissolving-out added substances
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/5607—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides
- C04B35/5611—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on refractory metal carbides based on titanium carbides
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
A preparation method of high-strength TiC-based porous ceramic comprises the following steps: sequentially filling weighed titanium powder and graphite powder into a ball milling tank of a planetary ball mill, then ball milling for 4 hours on the ball mill, and finally sieving the ball milled powder and the grinding balls by using a stainless steel sieve, wherein the sieved powder is used as a raw material for preparing high-strength carbide; step (2), mixing the ball-milled titanium and carbon mixed powder with calcium oxide powder, and ball-milling for 10 minutes; filling the fully mixed powder into a graphite mold with the diameter of 25mm for hot-pressing sintering, and filling a layer of graphite foil in the graphite mold and at two ends of an upper ejector rod and a lower ejector rod to form a TiC/CaO composite material in the sintering process; and (4) taking out the sintered sample from the die, polishing the outer surface of the sample to remove graphite foil, and soaking the sample in hydrochloric acid until all calcium oxide is removed to form the porous carbide composite material mainly containing titanium carbide.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to a preparation technology of high-strength TiC-based porous ceramic.
Background
Ultra High Temperature Ceramics (UHTC) have received widespread and sustained attention for their excellent properties. TiC as a UHTC material exhibits a unique combination of qualities such as low thermal expansion, excellent thermal and chemical stability, excellent hardness, higher wear resistance, high melting point, low density, good electrical conductivity and suitable thermal conductivity. Because of its excellent combination of properties, this material can be an important candidate for high temperature structural applications, including hypersonic reentry vehicles, throat liners, beveled edge components, jet engine components, rocket nozzles, and the like. With the continuous development of high and new fields such as aerospace, energy chemical industry and the like, the demand for lightweight high-strength porous ceramic materials is increasing, and the demand for the performance of materials in service in polar environments is also increasing. In general, the temperature resistance limit of the traditional metal material is generally not more than 1000 ℃, and the material can be obviously softened at a higher temperature, so that the strength and hardness of the material are obviously reduced, and the high-temperature application of the metal material is limited; for some super-high temperature alloys, the temperature resistance limit can reach about 1200 ℃, but the application requirements can not be met in some special occasions. The melting point of titanium carbide can reach 3000 ℃, which is a good choice for high-temperature application above 1600 ℃.
Although UHTC such as TiC has excellent performance, porous ceramic materials prepared based on UHTC have generally low strength. This is mainly due to the difficulty in obtaining a high strength ceramic matrix by existing porous ceramic preparation technology routes (such as foaming method, etc.). In the common ceramic process, the porosity and strength of the sintered product can be controlled by adopting a method for adjusting the sintering temperature and time, but when the sintering temperature of the porous ceramic is too high, partial pores are closed or disappear, and when the sintering temperature is too low, the strength of the product is low, the porosity and strength cannot be considered, and the defect can be avoided by adopting a method for adding a pore-forming agent, so that the sintered product has high porosity and better strength. Hot press sintering is an effective means for preparing high strength ceramic matrix, however, there is no related technology for preparing high strength porous ceramic by hot press sintering process, and the key of the process method is the selection of the type and amount of pore-forming agent. The invention seeks to prepare a high strength TiC-based porous material by a hot press sintering process.
Disclosure of Invention
The invention aims to provide a preparation method of high-strength TiC-based porous ceramic.
The invention relates to a preparation method of high-strength TiC-based porous ceramic, which comprises the following specific steps:
weighing metal titanium powder with the particle size of 1000 meshes and graphite powder with the particle size of 1000 meshes according to an equimolar ratio, sequentially loading the weighed titanium powder and graphite powder into a ball milling tank of a planetary ball mill, then ball milling the titanium powder and the graphite powder on the ball mill for 4 hours (each 2 hours in forward rotation and reverse rotation), wherein the ball material ratio is 5:1, the rotating speed is 400r/min, and finally sieving the ball milled powder and the grinding balls by using a stainless steel sieve, wherein the sieved powder is used as a raw material for preparing high-strength carbide at the back;
mixing the ball-milled titanium and carbon mixed powder with calcium oxide powder, wherein the volume percentage of the calcium oxide is 40%, 45%, 50% and 55%, and the ball milling is carried out for ten minutes at the rotating speed of 400r/min, so that the powder is uniformly mixed;
filling fully mixed powder into a graphite mold with the diameter of 25mm for hot-pressing sintering, and filling a layer of graphite foil in the graphite mold and at two ends of an upper ejector rod and a lower ejector rod to prevent the raw materials from reacting with the graphite mold, wherein the sintering temperature is 1450-1650 ℃, the pressure is 20MPa, and the time is 30-120 min, so that a TiC/CaO composite material is formed in the sintering process;
and (4) taking out the sintered sample from the die, polishing the outer surface of the sample to remove graphite foil, and soaking the sample in hydrochloric acid with the concentration of 36-38% until all calcium oxide is removed to form the porous carbide composite material mainly containing titanium carbide.
The beneficial effects of the invention are as follows: the preparation method has the advantages that the process route is simple in the preparation process, only four steps are needed, and the technical process is greatly simplified; and the severity requirement on the equipment is low; the raw materials for preparing the porous material are low in cost and easy to obtain, and the preparation cost is greatly reduced in the aspects of raw materials, design of process routes and equipment conditions.
Drawings
FIG. 1 shows the phase composition of TiC-based porous material with 40% calcium oxide by volume before and after immersing hydrochloric acid in the embodiment of the invention. Fig. 2, 3 and 4 show SEM secondary electron images of TiC-based porous materials with a calcium oxide volume ratio of 40% in the examples of the present invention, with magnifications of 200 times, 1000 times and 5000 times, respectively. Fig. 5 is an SEM back-scattered electron image of a TiC-based porous material with a calcium oxide volume ratio of 40% in the embodiment of the present invention, and fig. 6, 7, and 8 are EDS point distribution spectra. Fig. 9 and 10 are bar charts of mechanical properties and displacement load graphs of samples prepared in examples of the present invention, respectively.
Detailed Description
The present invention will be described in further detail with reference to examples in order to make the objects and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Examples
The invention relates to a preparation method of high-strength TiC-based porous ceramic, which comprises the following specific steps:
s1, weighing metal titanium powder with the particle size of 1000 meshes and graphite powder with the particle size of 1000 meshes according to an equimolar ratio, sequentially loading the weighed titanium powder and graphite powder into a ball milling tank of a planetary ball mill, then ball milling the titanium powder and the graphite powder on the ball mill for 4 hours (each 2 hours in forward rotation and reverse rotation), wherein the ball-to-material ratio is 5:1, the rotating speed is 400r/min, and finally sieving the ball-milled powder and the grinding balls by using a stainless steel sieve, wherein the sieved powder is used as a raw material for preparing high-strength carbide at the back;
s2, mixing the ball-milled titanium and carbon mixed powder with calcium oxide powder, wherein the volume percentage of the calcium oxide is 40%, 45%, 50% and 55%, and the ball milling is carried out for ten minutes at the rotating speed of 400r/min, so that the powder is uniformly mixed;
s3, filling the fully mixed powder into a graphite mold with the diameter of 25mm for hot-pressing sintering, and filling a layer of graphite foil in the graphite mold and at the two ends of the upper ejector rod and the lower ejector rod to prevent the raw materials from reacting with the graphite mold, wherein the sintering temperature is 1450-1650 ℃, the pressure is 20MPa, the time is 30-120 min, and the TiC/CaO composite material is formed in the sintering process;
and S4, taking out the sintered sample from the die, polishing the outer surface of the sample to remove graphite foil, and soaking the sample in hydrochloric acid with the concentration of 36-38% until all calcium oxide is removed to form the porous carbide composite material mainly containing titanium carbide.
FIG. 1 shows the composition of TiC-based porous ceramic with 40% calcium oxide by volume, the phase of the soaked hydrochloric acid precursor mainly comprising TiC, C and CaO, and the phase of the soaked hydrochloric acid precursor mainly comprising TiC and C.
Fig. 2, 3 and 4 show SEM secondary electron images of TiC-based porous materials with a calcium oxide volume ratio of 40% in the examples of the present invention, with magnifications of 200 times, 1000 times and 5000 times, respectively. It can be seen from the figure that there are a number of cells of different sizes inside, which cells are formed by removal of calcium oxide as a pore-forming agent, and that the titanium particles and the carbon particles are joined together by hot-press sintering,
fig. 5 is an SEM back-scattered electron image of a TiC-based porous material with a calcium oxide volume ratio of 40% according to an embodiment of the present invention, and fig. 6, 7 and 8 are EDS point distribution spectra corresponding to fig. 5, respectively. The sample is mainly titanium and carbon, and combined with XRD, titanium reacts with carbon to generate TiC in the hot pressing process, and calcium oxide is removed by hydrochloric acid soaking when the contents of calcium and oxygen are small.
Fig. 9 and 10 are bar charts of mechanical properties and displacement load graphs of samples prepared in examples of the present invention, respectively. The following data were obtained by testing: tiC-based porous ceramic with calcium oxide volume ratio of 40% has compressive strength of 51.30MPa and volume density of 3.18g/cm 3 Specific compression strength of 16.1320 MPacm 3 /g; tiC-based porous ceramic with 45% calcium oxide volume ratio has compressive strength of 17.85MPa and volume density of 2.79g/cm 3 Specific compression strength of 6.3987 MPacm 3 /g; tiC-based porous ceramic with calcium oxide volume ratio of 50% has compressive strength of 11.85MPa and volume density of 2.67g/cm 3 Specific compression strength of 4.4382MPacm 3 /g; tiC-based porous ceramic with 55% calcium oxide volume ratio has compressive strength of 14.00MPa and volume density of 2.27g/cm 3 Specific compression strength of 6.1674MPacm 3 And/g. From its load-displacement curve, it can be derived that the fracture modes are basically pseudo-plastic fractures.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (3)
1. The preparation method of the high-strength TiC-based porous ceramic is characterized by comprising the following steps of:
weighing metal titanium powder with the particle size of 1000 meshes and graphite powder with the particle size of 1000 meshes according to an equimolar ratio, sequentially loading the weighed titanium powder and graphite powder into a ball milling tank of a planetary ball mill, then ball milling the ball milling tank on the ball mill for 4 hours, wherein the ball material ratio is 5:1, the rotating speed is 400r/min, and finally sieving the ball milling powder and the grinding balls by using a stainless steel sieve, wherein the sieved powder is used as a raw material for preparing high-strength carbide;
mixing the ball-milled titanium and carbon mixed powder with calcium oxide powder, wherein the volume percentage of the calcium oxide is 40%, 45%, 50% and 55%, and the ball milling is carried out for 10 minutes at the rotating speed of 400r/min; filling fully mixed powder into a graphite mold with the diameter of 25mm for hot-pressing sintering, and filling a layer of graphite foil in the graphite mold and at the two ends of an upper ejector rod and a lower ejector rod to prevent the raw materials from reacting with the graphite mold, wherein the sintering temperature is 1450-1650 ℃, the pressure is 20MPa, and the time is 30-120 min, so that a TiC/CaO composite material is formed in the sintering process;
and (4) taking out the sintered sample from the die, polishing the outer surface of the sample to remove graphite foil, and soaking the sample in hydrochloric acid with the concentration of 36-38% until all calcium oxide is removed to form the porous carbide composite material mainly containing titanium carbide.
2. The method for preparing high-strength TiC-based porous ceramic according to claim 1, wherein the sintering process condition in the step (3) is hot press sintering, the sintering temperature is 1450-1600 ℃, the pressure is 20MPa, and the time is 30-120 min.
3. The method of preparing a high strength TiC-based porous ceramic according to claim 1, wherein the hydrochloric acid in the step (4) is replaced every 24 hours.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04214076A (en) * | 1990-02-06 | 1992-08-05 | Senju Metal Ind Co Ltd | Tic sintered body and its manufacture |
| CN104141063A (en) * | 2014-07-31 | 2014-11-12 | 重庆大学 | Preparing method of in-situ synthesis titanium carbide enhanced titanium-based multi-hole materials |
| CN105274415A (en) * | 2015-10-10 | 2016-01-27 | 西安交通大学 | Manufacturing method for porous titanium carbide ceramics |
| CN106521219A (en) * | 2017-01-05 | 2017-03-22 | 重庆大学 | Preparation method for TiC particle reinforced titanium-based porous material |
| CN108585905A (en) * | 2018-04-16 | 2018-09-28 | 长兴科创科技咨询有限公司 | A kind of high-strength carborundum ceramics and preparation method thereof |
| CN111233478A (en) * | 2020-01-20 | 2020-06-05 | 北京交通大学 | Layered slurry preparation method of titanium carbide gradient porous ceramic |
-
2023
- 2023-06-25 CN CN202310745790.5A patent/CN116730740B/en active Active
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|---|---|---|---|---|
| JPH04214076A (en) * | 1990-02-06 | 1992-08-05 | Senju Metal Ind Co Ltd | Tic sintered body and its manufacture |
| CN104141063A (en) * | 2014-07-31 | 2014-11-12 | 重庆大学 | Preparing method of in-situ synthesis titanium carbide enhanced titanium-based multi-hole materials |
| CN105274415A (en) * | 2015-10-10 | 2016-01-27 | 西安交通大学 | Manufacturing method for porous titanium carbide ceramics |
| CN106521219A (en) * | 2017-01-05 | 2017-03-22 | 重庆大学 | Preparation method for TiC particle reinforced titanium-based porous material |
| CN108585905A (en) * | 2018-04-16 | 2018-09-28 | 长兴科创科技咨询有限公司 | A kind of high-strength carborundum ceramics and preparation method thereof |
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| Title |
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