CN104058749A - Method for preparing titanium silicon carbon ceramic block material by pressureless sintering - Google Patents
Method for preparing titanium silicon carbon ceramic block material by pressureless sintering Download PDFInfo
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- CN104058749A CN104058749A CN201310093359.3A CN201310093359A CN104058749A CN 104058749 A CN104058749 A CN 104058749A CN 201310093359 A CN201310093359 A CN 201310093359A CN 104058749 A CN104058749 A CN 104058749A
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Abstract
The invention provides a method for preparing a titanium silicon carbon ceramic block material by pressureless sintering, which particularly comprises the following steps: putting raw materials in a mold, performing cold pressing at a pressure of 20 MPa-80 MPa to form a blank, then performing cold isostatic pressing molding at a pressure of 150 MPa-300 MPa, embedding the molded sample in titanium silicon carbon powder or SiC powder, then putting into a pressureless sintering furnace, heating to 1200 DEG C-1700 DEG C under an inert gas protection condition or under a vacuum condition and with a heating speed of 2 DEG C/min-100 DEG C/min, and performing sintering for 0.1-4 hours to obtain the titanium silicon carbon ceramic block material. Tests prove that with the combination with processes of cold pressing for blank formation, cold isostatic pressing molding, and pressureless sintering, the method of the invention prepares the compact titanium silicon carbon ceramic block material with low cost and low energy consumption; the block material is diverse in shape; and the preparation method has good application prospects.
Description
Technical field
The present invention relates to the technology of preparing of high-temperature structural ceramics, provide especially a kind of pressureless sintering to prepare the method for titanium silicon carbide ceramics block materials.
Background technology
Ternary layered MAX phase (wherein M is transiting group metal elements, and A is IIIA HuoIVA family element, and X is C or N) pottery is a class high temperature structural material, receives much concern in recent years.This class Ceramic bond many good characteristics of metal and pottery, as low density, high strength, high-modulus, conduction, heat conduction, can process, good anti-damage tolerance and thermal shock resistance, good high-temperature oxidation resistance and chemical stability etc.These excellent performances make MAX phase ceramics have broad application prospects in high-tech sectors such as chemical industry, machinery, electronics and aerospace, for example turbine blade and the stator for aircraft engine as high-temperature structural material; As self-lubricating material, be made into the brush of alternating current machine of new generation; And use as the electrode materials of smelting metal.Current research also shows: MAX multiphase ceramics material is (as Ti
3alC
2and Ti
3siC
2) there is good radiation hardness, be expected to be applied in nuclear reactor of new generation as first wall material and Divertor Materials.
Yet block materials is often prepared difficulty, this has limited the widespread use of MAX phase ceramics to a great extent.The preparation of MAX phase ceramics block materials is at present accompanied by larger pressure conventionally, as hot pressing (HP), hot isostatic pressing (HIP), discharge plasma sintering (SPS) etc.These method costs are high, energy consumption is large, and are difficult to prepare abnormal member, are difficult to accomplish scale production.Therefore,, in order to promote the further application of MAX phase ceramics, developing low-cost preparation technology's (as dead size moulding and pressureless sintering) becomes pressing issues urgently to be resolved hurrily.
Ti
3siC
2be in MAX phase ceramics, to study to obtain one of material the most widely, up to now, still there is larger difficulty in the pressureless sintering of this pottery, how to suppress Ti in sintering process
3siC
2decomposition be the key point of dealing with problems.
Summary of the invention
Technical purpose of the present invention be in the preparation process of existing MAX phase ceramics block materials due to problems such as the cost that need to cause compared with large hot pressing are high, energy consumption is large, provide a kind of pressureless sintering to prepare titanium silicon-carbon (Ti
3siC
2) method of ceramic block material, the method can reduce preparation cost and the energy consumption of titanium silicon carbide ceramics block materials greatly, to realize the scale operation of titanium silicon carbide ceramics block materials.
The present invention realizes the technical scheme that above-mentioned technical purpose adopts: the method for titanium silicon carbide ceramics block materials is prepared in a kind of pressureless sintering, and concrete steps are as follows:
The titanium silicon-carbon powder of take is raw material; raw material is packed in mould; under the pressure of 20MPa～80MPa, be cold-pressed into base substrate; then cold isostatic compaction under the pressure of 150MPa～300MPa; after again the sample after moulding being embedded in titanium silicon-carbon powder or SiC powder, put into non-pressure sintering furnace; temperature rise rate with 2 ℃/min～100 ℃/min under protection of inert gas conditioned disjunction vacuum condition is heated to 1200 ℃/min～1700 ℃ sintering 0.1 hour～4 hours, obtains titanium silicon carbon block stupalith.
The quality purity of described titanium silicon-carbon raw material powder is preferably greater than and equals 95%, can comprise a small amount of impurity, such as solid solution aluminium, TiC impurity etc.;
Described titanium silicon-carbon raw material powder granularity is preferably 50～1000 orders;
Described moulding stock is not limit, and includes but not limited to stainless steel etc.
Described non-pressure sintering furnace refers to the agglomerating plant of in sintering process, agglomerated material not being exerted pressure, and includes but not limited to tube furnace, retort furnace, microwave agglomerating furnace etc.
Described rare gas element includes but not limited to argon gas, helium etc.;
As preferably, under the pressure of 30MPa～50MPa, be cold-pressed into base substrate;
As preferably, cold isostatic compaction under the pressure of 200MPa～300MPa;
As preferably, described temperature rise rate is 5 ℃/min～50 ℃/min, more preferably 10 ℃/min～30 ℃/min;
As preferably, described Heating temperature is 1300 ℃/min～1500 ℃, and described sintering time is 0.5 hour～2 hours.
In sum, the present invention is with Ti
3siC
2powder is raw material, in conjunction with being cold-pressed into base, cold isostatic compaction, and the technique of pressureless sintering, by Optimizing Technical, made fine and close titanium silicon carbide ceramics block materials, meanwhile, in order to have suppressed Ti in sintering process
3siC
2decomposition, adopt the titanium silicon-carbon sample after moulding to be embedded in Ti
3siC
2method in powder or SiC powder and obtained highly purified titanium silicon carbide ceramics block materials.Experiment confirms, adopt method of the present invention to make fine and close titanium silicon carbide ceramics block materials under the condition of low cost, less energy-consumption, its grain-size reaches 5 μ m～100 μ m, and the shape of block materials is various, can make the ceramic block material of the various shapes such as sheet, strip, ring-type, wherein the size of flaky material can reach Φ (13～100) * (2～50) mm
3.Therefore, compare with existing preparation method, preparation method provided by the invention greatly reduces preparation cost and the energy consumption of titanium silicon carbide ceramics block materials, and has realized the shape variation of this block materials, is a kind of preparation method with applications well prospect.
Accompanying drawing explanation
Fig. 1 is the outside drawing of the titanium silicon carbide ceramics block materials that makes in the embodiment of the present invention 1;
Fig. 2 is the X-ray diffracting spectrum of the titanium silicon carbide ceramics block materials that makes in the embodiment of the present invention 1;
Fig. 3 is the fracture stereoscan photograph of the titanium silicon carbide ceramics block materials that makes in the embodiment of the present invention 1.
Embodiment
Below in conjunction with accompanying drawing, embodiment is described in further detail the present invention, it is pointed out that the following stated embodiment is intended to be convenient to the understanding of the present invention, and it is not played to any restriction effect.
Embodiment 1:
It is the titanium silicon-carbon powder of 300 order left and right that raw material adopts granularity, this titanium silicon-carbon powder quality purity is 95%, wherein, containing a small amount of solid solution aluminium impurity, raw material is packed in the cylinder shape stainless steel mould that diameter is 15mm, under the pressure of 50MPa, be cold-pressed into base substrate, then cold isostatic compaction under 250MPa pressure.Sample after moulding is embedded in titanium silicon-carbon powder; put into microwave agglomerating furnace; be heated to 1400 ℃ being connected with the temperature rise rate with 20 ℃/min under the condition of argon shield; sintering 1 hour; obtain titanium silicon-carbon sheet block materials as shown in Figure 1, because sample diameter after sintering is slightly shunk, the diameter of this block materials is 13.5mm; thickness is 3.2mm, is of a size of Φ 13.5 * 3.2mm
3.
The above-mentioned titanium silicon carbon block material making is carried out to X-ray diffraction analysis, and as shown in Figure 2, its main component is Ti to result
3siC
2, also have in addition a small amount of oxide compound to exist, do not find Ti
3siC
2degradation production TiC.
The fracture stereoscan photograph of the above-mentioned titanium silicon carbon block material making as shown in Figure 3, can be found out this block agglomerated material compact structure.This titanium silicon carbon block material is carried out to density measurement, and testing method is Archimedes's method, and the density that obtains this block sintered product is 95.15%.
Embodiment 2:
It is the titanium silicon-carbon powder of 300 order left and right that raw material adopts granularity, this titanium silicon-carbon powder quality purity is 96%, wherein, containing a small amount of TiC impurity, raw material is packed in the cylinder shape stainless steel mould that diameter is 15mm, under the pressure of 30MPa, be cold-pressed into base substrate, then cold isostatic compaction under 300MPa pressure.After being embedded in titanium silicon-carbon powder, sample after moulding puts into non-pressure sintering furnace; be heated to 1600 ℃ being connected with the temperature rise rate with 10 ℃/min under the condition of argon shield; sintering 2 hours; obtain sheet titanium silicon carbon block material similar to Figure 1, this block materials is of a size of Φ 13.3 * 3.3mm
3.
The above-mentioned titanium silicon carbon block material making is carried out to X-ray diffraction analysis, and result is similar to Figure 2, and its main component is Ti
3siC
2, also have in addition a small amount of oxide compound to exist, Ti
3siC
2do not decompose.
The fracture stereoscan photograph of the above-mentioned titanium silicon carbon block material making is similar to Figure 3, can find out this block agglomerated material compact structure.This titanium silicon carbon block material is carried out to density measurement, and testing method is for being Archimedes's method, and obtaining this block sintered product density is 95.27%.
Embodiment 3:
It is the titanium silicon-carbon powder of 300 order left and right that raw material adopts granularity, and this titanium silicon-carbon powder quality purity is 95%, wherein containing a small amount of solid solution aluminium impurity.Raw material is packed in the cylinder shape stainless steel mould that diameter is 25mm, under the pressure of 50MPa, be cold-pressed into base substrate, then cold isostatic compaction under 300MPa pressure.After being embedded in carborundum powder, sample after moulding puts into microwave agglomerating furnace vacuum sintering, temperature rise rate with 30 ℃/min is heated to 1500 ℃ of sintering 2 hours, obtain sheet titanium silicon carbon block material similar to Figure 1, this block materials is of a size of Φ 22.5 * 4.2mm
3.
The above-mentioned titanium silicon carbon block material making is carried out to X-ray diffraction analysis, and result is similar to Figure 2, and it is mainly Ti
3siC
2, also have in addition a small amount of oxide compound to exist, do not find Ti
3siC
2degradation production TiC.
The fracture stereoscan photograph of the above-mentioned titanium silicon carbon block material making is similar to Figure 3, can find out this block agglomerated material compact structure.This titanium silicon carbon block material is carried out to density measurement, and testing method is Archimedes's method, and obtaining this block sintered product density is 91.46%.
Embodiment 4:
In the present embodiment, raw material and preparation method are basic identical with embodiment 1, and difference is that mould is that cross section is rectangular columnar structure, and the titanium silicon carbon block material obtaining is list structure.
Embodiment 5:
In the present embodiment, raw material and preparation method are basic identical with embodiment 1, and difference is that mould is that cross section is annular ring texture, and the titanium silicon carbon block material obtaining is structure in the form of a ring.
Above-described embodiment has been described in detail technical scheme of the present invention; be understood that and the foregoing is only specific embodiments of the invention; be not limited to the present invention; all any modifications of making within the scope of principle of the present invention, supplement or similar fashion substitutes etc., within all should being included in protection scope of the present invention.
Claims (10)
1. the method for titanium silicon carbide ceramics block materials is prepared in a pressureless sintering, it is characterized in that: the titanium silicon-carbon powder of take is raw material, raw material is packed in mould, under the pressure of 20MPa～80MPa, be cold-pressed into base substrate, then cold isostatic compaction under the pressure of 150MPa～300MPa, after again the sample after moulding being embedded in titanium silicon-carbon powder or SiC powder, put into non-pressure sintering furnace, temperature rise rate with 2 ℃/min～100 ℃/min under protection of inert gas conditioned disjunction vacuum condition is heated to 1200 ℃/min～1700 ℃ sintering 0.1 hour～4 hours, obtain titanium silicon carbon block stupalith.
2. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: the quality purity of described titanium silicon-carbon raw material powder is more than or equal to 95%.
3. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: the granularity of described titanium silicon-carbon raw material powder is 50～1000 orders.
4. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: described non-pressure sintering furnace comprises tube furnace, retort furnace, microwave agglomerating furnace.
5. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: under the pressure of 30MPa～50MPa, be cold-pressed into base substrate.
6. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: cold isostatic compaction under the pressure of 200MPa～300MPa.
7. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: described temperature rise rate is 5 ℃/min～50 ℃/min.
8. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: described temperature rise rate is 10 ℃/min～30 ℃/min.
9. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: described Heating temperature is 1300 ℃/min～1500 ℃.
10. the method for titanium silicon carbide ceramics block materials is prepared in pressureless sintering according to claim 1, it is characterized in that: described sintering time is 0.5 hour～2 hours.
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Cited By (7)
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| CN105149592A (en) * | 2015-09-29 | 2015-12-16 | 东风商用车有限公司 | Warm-pressing manufacturing method for high-strength aluminum alloy |
| CN107778009A (en) * | 2016-08-26 | 2018-03-09 | 辽宁省轻工科学研究院 | A kind of pressure-bearing prepares Ti3SiC2The reverse thermal expansion synthetic method of ceramics |
| CN108585889A (en) * | 2018-04-28 | 2018-09-28 | 武汉科技大学 | A kind of rodlike zirconium boride-sheet-shaped silicon carbide monocrystalline composite granule and preparation method thereof |
| CN110330339A (en) * | 2019-07-05 | 2019-10-15 | 北京科技大学 | A kind of large scale MAX phase ceramics impeller preparation method |
| CN116121701A (en) * | 2023-03-03 | 2023-05-16 | 青岛大学 | Modified composite three-layer coating of fuel cell metal connector and preparation method thereof |
| CN116178020A (en) * | 2023-03-03 | 2023-05-30 | 青岛大学 | Ceramic connector material of solid oxide fuel cell and preparation method thereof |
| CN116178019A (en) * | 2022-09-08 | 2023-05-30 | 合肥工业大学 | Method for preparing porous MAX phase ceramic material by pressureless wrapping calcination |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105149592A (en) * | 2015-09-29 | 2015-12-16 | 东风商用车有限公司 | Warm-pressing manufacturing method for high-strength aluminum alloy |
| CN107778009A (en) * | 2016-08-26 | 2018-03-09 | 辽宁省轻工科学研究院 | A kind of pressure-bearing prepares Ti3SiC2The reverse thermal expansion synthetic method of ceramics |
| CN107778009B (en) * | 2016-08-26 | 2021-04-20 | 辽宁省轻工科学研究院有限公司 | Pressure-bearing preparation of Ti3SiC2Method for synthesizing ceramics by reverse thermal expansion |
| CN108585889A (en) * | 2018-04-28 | 2018-09-28 | 武汉科技大学 | A kind of rodlike zirconium boride-sheet-shaped silicon carbide monocrystalline composite granule and preparation method thereof |
| CN110330339A (en) * | 2019-07-05 | 2019-10-15 | 北京科技大学 | A kind of large scale MAX phase ceramics impeller preparation method |
| CN116178019A (en) * | 2022-09-08 | 2023-05-30 | 合肥工业大学 | Method for preparing porous MAX phase ceramic material by pressureless wrapping calcination |
| CN116178019B (en) * | 2022-09-08 | 2023-12-22 | 合肥工业大学 | Method for preparing porous MAX phase ceramic material by pressureless wrapping calcination |
| CN116121701A (en) * | 2023-03-03 | 2023-05-16 | 青岛大学 | Modified composite three-layer coating of fuel cell metal connector and preparation method thereof |
| CN116178020A (en) * | 2023-03-03 | 2023-05-30 | 青岛大学 | Ceramic connector material of solid oxide fuel cell and preparation method thereof |
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