CN1807347A - Boride-silicon carbide multiple phase ceramic and its preparation method - Google Patents
Boride-silicon carbide multiple phase ceramic and its preparation method Download PDFInfo
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Abstract
The invention provides a preparation method for the boride-silicon carbide multiple-phase ceramic by thermal pressing at 1700~1900Deg with 1-12wt% zirconium boride, titanium boride and hafnium boride by the activity of silicon carbide from polysilane cracking. Wherein, the active carbon is packed and combines with the bride. This invention needs not other auxiliary-fire agent to ensure material performance at high temperature, and improves the composite material properties.
Description
Technical field
The present invention relates to boride-silicon carbide multiple phase ceramic and preparation method thereof, comprise titanium boride-silicon carbide (TiB
2-SiC) complex phase ceramic, zirconium boride 99.5004323A8ure-silicon carbide (ZrB
2-SiC) complex phase closes pottery and hafnium boride-silicon carbide (HfB
2-SiC) complex phase ceramic and preparation method thereof.Belong to non-oxidized substance complex phase ceramic field.
Background technology
The transition metal boride pottery is with its high-melting-point; high rigidity; premium propertiess such as high conductivity and anti-glass and metal melt corrosion; at the space flight and aviation superhigh temperature ceramic material; cutting tool and high-abrasive material; electrode materials, and purposes is widely arranged with glass and the contacted container of metal melt and protecting materials aspect.If can improve the performance of boride ceramics by certain approach, improve its oxidation-resistance mutually as adding silicon carbide second, then can make the boride composite ceramics of acquisition have purposes widely.The boride complex phase ceramic generally by direct mixing method preparation, is opened clear 61-72687 as the spy, and the spy opens clear 61-21980, and the spy opens shown in the communique such as flat 5-319936, at ZrB
2In directly add SiC, B
4C, carbide such as TiC second phase, or open clear 61-48484 as the spy, the spy opens shown in the communiques such as clear 61-63573, at ZrB
2In directly add TiN, nitride such as BN second phase obtains sintered compact by hot pressing or normal pressure-sintered method then.
But, resemble ZrB
2, SiC, B
4C, TiC, TiN, the self-diffusion coefficient of non-oxide ceramicses such as BN is very little, even hot pressing also is difficult to obtain fine and close sintered compact, the intensity of material, erosion resistance etc. are difficult to reach service requirements.Add resembling Ni on a small quantity, the metal that Fe is the same can significantly improve sintering character, opens shown in the flat 05-132363 as the spy.But these metal additives can remain in the crystal boundary place of pottery, thereby reduce the mechanical behavior under high temperature and the corrosion resistance of material.
Following reusable space vehicle and hypersonic plane must adopt the novel thermal protection system material of not ablating for a long time or seldom ablating, i.e. ultrahigh-temperature pottery (UHTC) material under ultrahigh-temperature (more than 2500～2700 ℃) aerobic Service Environment.Superhigh temperature ceramic material mainly comprises ZrB
2, HfB
2, ZrC and HfC etc. with and various matrix material.But single boride ceramics can't satisfy desired physics, chemistry, mechanics and structure properties under ultrahigh-temperature simultaneously.So, select different materials to carry out reasonable combination from the material design angle, be the unique channel that addresses this problem.At present, the boride ceramics that contains SiC has become the main flow of research.
In order to obtain the material of ultrahigh-temperature excellent property, must adopt the sintering aid that high-temperature behavior is not had an influence even not add sintering aid, but must realize densification sintering.
Therefore, the research of boride-silicon carbide multiple phase ceramic and preparation method thereof has become an important branch of current non-oxidized substance complex phase ceramic area research.
Summary of the invention
The object of the present invention is to provide class boride-silicon carbide multiple phase ceramic and preparation method thereof.In the present invention, the inventor proposes to adopt the organic precursor pyrolysis method to come original position to generate SiC second phase, utilizes the high reactivity of generated in-situ SiC to promote boride ceramics densification sintering at a lower temperature and suppress growing up of boride crystal grain simultaneously.
Specifically, the organic precursor of the present invention's employing is Polycarbosilane (PCS).Its molecular formula is (SiH (CH
3)-CH
2) n, molecular weight is～1250.Carbon silicon in the split product changes than the difference with cracking temperature, and cracking temperature is when 500 ℃～1300 ℃ change, and carbon silicon is than changing between 1.72～1.44, as seen with the raising carbon silicon of cracking temperature than descending, Zong weightlessness is about 40%.Explanation will have residual carbon and occur in cracking process, scission reaction is:
So, when this PCS is added to boride (for sake of convenience following, all with ZrB
2Be example) in the pottery time, it is characterized in that the phase composite of the composite diphase material that obtains is ZrB after cracking
2-SiC-C, reaction formula is as follows:
。
The existence of carbon can stop the sintering densification of material to a certain extent in the material, but this influence is not really remarkable when the addition of PCS hangs down.The existence of carbon can improve the thermomechanical property of composite diphase material to a certain extent conversely, as heat-shock resistance etc.
In addition, the carbon that produces in cracking process also can absorb by other metallic elements that add 1-12wt%, for example, can obtain ZrB when adding metal zirconium
2-SiC-ZrC composite diphase material then can obtain ZrB when adding silicon
2-SiC complex phase ceramic:
Also can add the metal hafnium and absorb residual carbon, that at this moment form is ZrB
2-SiC-HfC composite ceramics:
Can also add metal titanium and absorb residual carbon, that at this moment form is ZrB
2-SiC-TiC composite ceramics:
In this case, because ZrB
2Will change TiB at a certain temperature into TiC
2And ZrC, reaction process is further activated, thereby the acceleration of sintering densification improve the mechanical property and the antioxidant property of material.
But itself antioxidant property of the boride of the titanium that produces when adding metal titanium or carbide is relatively poor, and too much interpolation can reduce the antioxidant property of material.So, Zr, Hf, the compound interpolation of Ti and Si will provide a valid approach for the matrix material that obtains good sintering densification performance and antioxidant property.On the other hand, complicated phase composite can improve phase composite and the microstructure stability of complex phase ceramic under ultra-high temperature condition to a certain extent, creates better condition for this class material can use under ultrahigh-temperature.
Most representative compound interpolation reaction is in above-mentioned reaction:
More than every in used metal-powder raw material, even it is characterized in that using thick and than the raw material of low-purity, also can obtain to have the matrix material at fine microstructure and pure interface, its reason be thing new in the reaction process generate mutually and in this course from purification effect.
More than every in employed boride (ZrB
2, TiB
2And HfB
2) raw material powder, even it is characterized in that using thicker raw material, it is to not significantly influence of sintering densification, because the active SiC that whole sintering process produces when mainly relying on the PCS cracking realizes.
In sum, be the split product-active carbide silicon-combination under mild temperature that utilizes Polycarbosilane by boride-silicon carbide multiple phase ceramic provided by the invention, by the hot pressed sintering densification, it is characterized in that
The active carbide silicon product that is produced by the Polycarbosilane cracking is wrapped in the surface of boride particle, in hot pressing in conjunction with boride particle.Silicon-carbide particle and residual carbon that cracking produces are distributed at the interface, and inside is the crystal grain of boride.The volume content of interfacial phase silicon carbide and residual carbon is 2% to 35%, is difficult to obtain fine and close sintered compact when surpassing this scope.
The silicon that in preparation process, adds 1～12wt%, zirconium, titanium, metal-powders such as hafnium, the perhaps arbitrary combination of these metal-powders is to absorb the residual carbon in the Polycarbosilane cracking process.The silicon-carbide particle that cracking produces and by the silicon of residual carbon and interpolation, zirconium, titanium, metal-powders such as hafnium, perhaps the arbitrary combination of the silicon carbide that arbitrary combination generated of these metal-powders or zirconium carbide or titanium carbide or hafnium carbide or these carbide is distributed at the interface, and inside is the crystal grain of boride.
The preparation method of boride-silicon carbide composite ceramics of the present invention, it is characterized in that earlier Polycarbosilane being wrapped in the surface of boride particle, obtain the boride composite powder of cleaved product parcel then through cracking, or obtain the boride composite powder of cleaved product parcel by the direct mixture of boride powder and Polycarbosilane powder through cracking.The mixed powder that obtains is prepared fine and close sintered compact through hot pressed sintering.
The cracking process of the Polycarbosilane by being wrapped in the boride particle surface in advance, generate the mix products of active carbide silicon and carbon on the boride particle surface, its volume content is between 2% to 35%, this mix products evenly is wrapped in the surface of boride particle, makes this boride powder that has wrapped up active carbide silicon and carbon have good sintering activity.
The present invention is based on the hard-to-sinter that improves existing boride ceramics and suppresses crystal grain and too grow up and improve its antioxidant property and propose.The invention is characterized in the densification sintering that under mild temperature, to realize boride ceramics.
Boride (ZrB used in the present invention
2, TiB
2And HfB
2) raw material is the powder less than 10 microns, even hot pressing can only not obtain the sintered compact of about 80% density yet when not adding sintering aid.The molecular weight of the Polycarbosilane (PCS) that uses is～1250.Other raw materials Zr, Hf, Ti and Si are 320 purposes (≤45 μ m) powders, and wherein the largest particle particle diameter is about 50 microns.
Various raw material powders are prepared burden according to a certain ratio, add to have dissolved in the gasoline solution of a certain amount of PCS.Ball milling mixed 12 hours then, and compound is dry while stirring in air, obtained evenly to apply the mixed powder of PCS, as shown in Figure 1.Mixed powder carries out cracking under 600-1200 ℃ of temperature, obtain the potteryization mixed powder.The characteristics of this potteryization mixed powder are, at boride (ZrB
2, TiB
2And HfB
2) the particulate surface-coated the split product SiC+C of layer of even PCS, as shown in Figure 2.The mixed powder that obtains after the cracking hot pressed sintering under 1700-1900 ℃ differing temps of packing in the graphite jig, the protective atmosphere during hot pressing is an argon gas.Sample after dry-pressing formed also can carry out sintering densification by the normal pressure method.The microstructure of the sintered compact that obtains as shown in Figure 3, the SiC+C that reaction generates, perhaps at the Zr that adds 1-12wt%, Hf, the SiC+ZrC that Ti or Si generate when absorbing C, SiC+HfC, SiC+TiC or have only SiC, be evenly distributed between the ZrB2 particle and form three-dimensional network, and rely on the high reactivity that reacts the thing phase that generates boride (ZrB
2, TiB
2And HfB
2) particle combines and form fine and close sintered compact.The ZrB of Fig. 4 for obtaining
2The X-ray diffraction spectrum of-SiC-C matrix material demonstrates and designs the corresponding to phase composite of phase composite.Pressure is 20MPa during hot pressed sintering, is incubated 60 minutes.
Even though use the thicker Zr of raw material particle size, Hf, Ti and Si powder also can obtain to have the matrix material at fine microstructure and pure interface, but, when the addition of these powders hanged down, thick excessively particle was difficult to obtain uniform dispersion, finally is difficult to obtain the uniform sintered compact of phase composite.Because the addition of these raw materials is lower among the present invention, for this reason, also used the tiny Zr of particle diameter among the present invention, Hf, Ti and Si powder compare experiment, and their particle diameter is between the 5-10 micron.
Because the sintering densification process among the present invention does not rely on boride (ZrB
2, TiB
2And HfB
2) activity, so the particle diameter of boride raw material is not the significant effects factor, this point has great importance for the sintering of boride coarse grain powder.
Boride-silicon carbide multiple phase ceramic of the present invention has the advantage of easy-sintering densification under 1700-1900 ℃ of temperature, compares with traditional technology and can reduce sintering temperature, reduces the preparation energy consumption, has very strong industrial applicibility.Simultaneously by adding separately or compound interpolation zirconium, hafnium, metal-powder such as titanium or silicon absorbs or partially absorbs the carbon that produces because of the Polycarbosilane cracking, can conveniently regulate the mechanics and the thermal property of composite diphase material, and the Properties Control approach of a flexibility is provided for industrial applications.The composite diphase material of preparation has excellent mechanical property and thermal property, for material application at high temperature provides the assurance on the rerum natura.Boride-silicon carbide multiple phase ceramic of the present invention is particularly suitable for the industrial application under the high temperature corrosion condition.Therefore industrial applicibility of the present invention is conspicuous.
Description of drawings
Fig. 1 applies the boride powder of PCS (with ZrB
2Be example)
The boride powder that cleaved product S iC+C coats after Fig. 2 PCS cracking is (with ZrB
2Be example)
The microstructure synoptic diagram of Fig. 3 sintered compact
The ZrB that Fig. 4 prepares with method provided by the present invention
2The X-ray diffraction spectrum of-SiC-C matrix material
The ZrB that Fig. 5 embodiment 1 obtains
2The scanning electron microscope pattern of-SiC-C matrix material
Embodiment
The present invention will describe in detail with the following examples, but the present invention is not limited by the following examples.
For preparation contains ZrB
2-(SiC+C) composite diphase material of 20% volume content is with ZrB
2Powder 8.8 gram adds in the gasoline solution that is dissolved with 1.2 gram PCS, with zirconia ball mix grinding 12 hours, pours in the kiver limit then into and stirs and allow gasoline vaporising, obtains to apply ZrB
2Powder.This coating powders carries out cracking under 800 ℃ in the argon gas atmosphere that flows, obtain the potteryization mixed powder.The 1800 ℃ of hot pressed sinterings in argon shield atmosphere of then this powder being packed in the graphite jig, hot pressing pressure is 20MPa, soaking time is 60min.The performance of the material that obtains is listed in the table 1.
Embodiment 2
For preparation contains ZrB
2-(SiC+C) composite diphase material of 20% volume content, with 1.2 gram PCS powder directly with 8.8 gram ZrB
2Powder mixes.This mixed powder carries out cracking under 800 ℃ in the argon gas atmosphere that flows, obtain the potteryization mixed powder.The 1800 ℃ of hot pressed sinterings in argon shield atmosphere of then this powder being packed in the graphite jig, hot pressing pressure is 20MPa, soaking time is 60min.The performance of the material that obtains is listed in the table 1.
By obtaining sample with example 1 identical mode, different is at 1700 ℃ of hot pressed sinterings.The performance of the material that obtains is listed in the table 1.
Embodiment 4
By obtaining sample with example 1 identical mode, different is the residual carbon that generates when adding 0.3 gram, 320 purpose silica flours with absorption PCS cracking in compound, and generates the SiC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 5
By obtaining sample with example 1 identical mode, different is the residual carbon that generates when adding 1 gram, 320 purpose zirconium powders with absorption PCS cracking in compound, and generates the ZrC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 6
By obtaining sample with example 1 identical mode, different is the residual carbon that generates when adding 0.5 gram, 320 purpose titanium valves with absorption PCS cracking in compound, and generates the TiC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 7
By obtaining sample with example 1 identical mode, different is the residual carbon that generates when adding 0.9 gram, 320 purpose hafnium powder with absorption PCS cracking in compound, and generates the HfC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 8
By obtaining sample with example 1 identical mode, the residual carbon that different is adds 0.3 gram 5-10 micron in compound silica flour generates when absorbing the PCS cracking, and generate the SiC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 9
By obtaining sample with example 1 identical mode, the residual carbon that different is adds 1 gram 5-10 micron in compound zirconium powder generates when absorbing the PCS cracking, and generate the ZrC phase.The performance of the material that obtains is listed in the table 1.
By obtaining sample with example 1 identical mode, the residual carbon that different is adds 0.5 gram 5-10 micron in compound titanium valve generates when absorbing the PCS cracking, and generate the TiC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 11
By obtaining sample with example 1 identical mode, the residual carbon that different is adds 0.9 gram 5-10 micron in compound hafnium powder generates when absorbing the PCS cracking, and generate the HfC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 12
By obtaining sample with example 1 identical mode, different is only to add 2% volume (SiC+C) in compound.The performance of the material that obtains is listed in the table 1.
Embodiment 13
By obtaining sample with example 1 identical mode, different is to add 35% volume (SiC+C) in compound.The performance of the material that obtains is listed in the table 1.
Embodiment 14
For preparation contains TiB
2-(SiC+C) composite diphase material of 20% volume content is with TiB
2Powder 8.5 gram adds in the gasoline solution that is dissolved with 1.5 gram PCS, with zirconia ball mix grinding 12 hours, pours in the shallow beaker limit then into and stirs and allow gasoline vaporising, obtains to apply TiB
2Powder.This coating powders carries out cracking under 800 ℃ in the argon gas atmosphere that flows, obtain the potteryization mixed powder.The 1800 ℃ of hot pressed sinterings in argon shield atmosphere of then this powder being packed in the graphite jig, hot pressing pressure is 20MPa, soaking time is 60min.The performance of the material that obtains is listed in the table 1.
Embodiment 15
By obtaining sample with example 14 identical modes, the residual carbon that different is adds 0.3 gram 5-10 micron in compound silica flour generates when absorbing the PCS cracking, and generate the SiC phase.The performance of the material that obtains is listed in the table 1.
Embodiment 16
The composite diphase material that contains HfB2-(SiC+C) 20% volume content for preparation, HfB2 powder 9.3 grams are added in the gasoline solution that is dissolved with 0.7 gram PCS, with zirconia ball mix grinding 12 hours, pour in the shallow beaker limit then into and stir and allow gasoline vaporising, obtain to apply the HfB2 powder.This coating powders carries out cracking under 800 ℃ in the argon gas atmosphere that flows, obtain the potteryization mixed powder.The 1800 ℃ of hot pressed sinterings in argon shield atmosphere of then this powder being packed in the graphite jig, hot pressing pressure is 20MPa, soaking time is 60min.The performance of the material that obtains is listed in the table 1.
Embodiment 17
By obtaining sample with example 16 identical modes, the residual carbon that different is adds 0.3 gram 5-10 micron in compound silica flour generates when absorbing the PCS cracking, and generate the SiC phase.The performance of the material that obtains is listed in the table 1.
Table 1
| Embodiment | Phase composite | Density (%TD) | Hardness (GPa) | Flexural strength (MPa) |
| 1 | ZrB 2，SiC，C | 98.5 | 13 | 356 |
| 2 | ZrB 2，SiC，C | 96.8 | 12 | 323 |
| 3 | ZrB 2，SiC，C | 95.1 | 10 | 261 |
| 4 | ZrB 2，SiC | 99.3 | 16 | 482 |
| 5 | ZrB 2，SiC，ZrC | 99.1 | 15.6 | 463 |
| 6 | ZrB 2，SiC，TiC | 99.2 | 15.5 | 487 |
| 7 | ZrB 2，SiC，HfC | 99.2 | 15.5 | 458 |
| 8 | ZrB 2，SiC | 99.7 | 17 | 512 |
| 9 | ZrB 2，SiC，ZrC | 99.3 | 16.3 | 485 |
| 10 | ZrB 2，SiC，TiC | 99.5 | 16.2 | 498 |
| 11 | ZrB 2，SiC，HfC | 99.4 | 16.3 | 471 |
| 12 | ZrB 2，SiC，C | 89.2 | 5.1 | 127 |
| 13 | ZrB 2，SiC，C | 82.7 | 4.3 | 113 |
| 14 | TiB 2，SiC，C | 92.3 | 9.0 | 265 |
| 15 | TiB 2，SiC | 98.7 | 18.1 | 521 |
| 16 | HfB 2，SiC，C | 99.1 | 17.2 | 435 |
| 17 | HfB 2，SiC | 99.8 | 17.8 | 482 |
Claims (6)
1. boride-carborundum composite-phase ceramic is characterized in that:
1. the active carbide silicon product that is produced by the Polycarbosilane cracking is wrapped in the surface of boride particle, in hot pressing in conjunction with boride particle; Silicon-carbide particle and residual carbon that cracking produces are distributed at the interface, and inside is the crystal grain of boride;
2. adding weight percentage in preparation process is the silicon of 1-12%, zirconium, any one metal-powder of titanium and hafnium or their arbitrary combination generate silicon carbide, zirconium carbide, titanium carbide and hafnium carbide, or the arbitrary combination of these carbide is distributed at the interface, and inside is the crystal grain of boride.
2. by the described boride-carborundum composite-phase ceramic of claim 1, it is characterized in that the silicon carbide of Polycarbosilane cracking generation and the volume content of residual carbon are 2-35%.
3. by the described boride-carborundum composite-phase ceramic of claim 1, it is characterized in that the ZrB that uses
2, TiB
2And HfB
2Raw material particle size is less than 10 microns; The particle diameter of Zr, Hf, Ti and Si≤45 μ m is 50 μ m to the maximum.
4. by the described boride-carborundum composite-phase ceramic of claim 1, the molecular weight that it is characterized in that Polycarbosilane is 1250.
5. prepare boride-carborundum composite-phase ceramic as claimed in claim 1, it is characterized in that earlier Polycarbosilane being wrapped in the surface of boride particle, obtain the boride composite powder of cleaved product parcel then through cracking, or obtain the boride composite powder of cleaved product parcel by the direct mixture of boride powder and Polycarbosilane powder through cracking; The mixed powder that obtains is prepared fine and close sintered compact through hot pressed sintering, and processing step is:
1. various raw material powders add and have dissolved in the gasoline solution of aequum Polycarbosilane by required proportion ingredient, and ball milling mixed 12 hours then, and compound is dry while stirring in air, obtain evenly to apply the mixed powder of Polycarbosilane;
2. mixed powder carries out cracking under 600-1200 ℃ of temperature, obtains the potteryization mixed powder, makes it in the surface-coated of boride particle the split product SiC+C of layer of even Polycarbosilane;
3. the mixed powder that obtains after the cracking is packed in the graphite jig at 1700-1900 ℃ 1700-1900 ℃ of hot pressed sintering, and the protective atmosphere during hot pressing is an argon gas; Perhaps at the Zr that adds 1-12wt%, Hf generates when Ti or Si absorption C;
Described required proportioning is that the volume of mixture content that makes the Polycarbosilane cracking generate SiC and C on boride particle surface is between the 2-35%;
The Zr that comprises weight percent 1-12% in the described proportioning, Hf, when absorbing C, Ti or Si generate SiC+ZrC, SiC+HfC, SiC+TiC or have only SiC, be evenly distributed between the ZrB2 particle and form three-dimensional network, and rely on the high reactivity of the thing phase of reaction generation boride particle to be combined the sintered compact that forms densification.
6. by the preparation method of the described boride-carborundum composite-phase ceramic of claim 5, pressure is 20MPa when it is characterized in that hot pressed sintering, and the time is 60min.
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| CN1240640C (en) * | 2004-04-14 | 2006-02-08 | 哈尔滨工业大学 | Method preparing BN/SiO2 composite ceramics through dipping, and cracking precursor body |
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