CN101265106A - Method for preparing nano/nano-type Si3N4/SiC nano multi-phase ceramic - Google Patents

Method for preparing nano/nano-type Si3N4/SiC nano multi-phase ceramic Download PDF

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CN101265106A
CN101265106A CN 200810086327 CN200810086327A CN101265106A CN 101265106 A CN101265106 A CN 101265106A CN 200810086327 CN200810086327 CN 200810086327 CN 200810086327 A CN200810086327 A CN 200810086327A CN 101265106 A CN101265106 A CN 101265106A
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nano
nanometer
sic
sintering
ceramic
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杨为佑
王华涛
高凤梅
谢志鹏
安立楠
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Tsinghua University
Ningbo University of Technology
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Tsinghua University
Ningbo University of Technology
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Abstract

The invention provides a novel method for producing nanometer/nanometer-type Si3N4/SiC nanometer multiphase ceramics. The method comprises the following steps: (1) low-temperature cross-linking and solidification: organic precursors undergo low-temperature cross-linking and solidification in the protective atmosphere to produce a non-crystalline solid; (2) ball mill pulverization: the non-crystalline solid is ground with a ball mill; (3) high-temperature thermal decomposition: the resulting mixture produced by ball milling undergoes high-temperature thermal decomposition in the protective atmosphere to produce SiCN powder; (4) ball mill pulverization: the SiCN powder is further ground with the ball mill while introducing a sintering aid; (5) spark plasma sintering (SPS): the mixture produced by high-energy ball milling undergoes SPS, to produce nanometer/nanometer-type Si3N4/SiC nanometer multiphase ceramic. Compared with the prior art, the method overcomes the problems in the conventional powder processing, can change the composition, structure and performance of the final product by controlling the atom size of the organic precursors, and ensures the final product to meet the performance requirements for various materials.

Description

A kind of nanometer/Nano type Si for preparing 3N 4The method of/SiC nano heterogeneous ceramic
Technical field
The present invention relates to a kind of nanometer/Nano type Si for preparing 3N 4The method of/SiC nano heterogeneous ceramic belongs to technical field of material.
Technical background
Nano heterogeneous ceramic is the method for a kind of new raising Mechanical Property of Ceramics that rose in recent years, and different from traditional micron order polycrystalline ceramics, nano ceramics microstructure to material on nanoscale is regulated and control, and then improves the combination property of pottery.Studies show that, the nano heterogeneous ceramic of different series, breaking tenacity improves 2～3 times, and fracture toughness property improves 2～4 times, and use temperature improves greatly.Nano heterogeneous ceramic has now become an important channel of improving ceramic material property, becomes one of focus of current high-temperature structural ceramics research.
Si 3N 4/ SiC complex phase ceramic is than single-phase Si 3N 4Or single-phase SiC has better performance, and the fracture toughness as more much higher than SiC material compares Si 3N 4The better elevated temperature strength of material, creep resistance and high-temperature oxidation resistance, wear-resistant, corrosion-resistant etc., in high-technology field and modern industry production, have broad application prospects.Be that raw material is prepared nano SiC granule and strengthened Si since the people such as Japanese Niihara adopt the non-crystalline flour of SiCN 3N 4The Si of matrix 3N 4/ SiC complex phase ceramic, and find that its mechanical property significantly improves, bending strength reaches 1550MPa, Si 3N 4/ SiC nano heterogeneous ceramic becomes at first system of high-temperature structural ceramics of future generation with its excellent mechanical property.
In existing research work, be to adopt nano SiC crystal grain and sub-micron Si mostly 3N 4Powder, or nanometer SiCN end and sub-micron Si 3N 4Powder mixes, and introduces Y 2O 3, Al 2O 3, La 2O 3, the sintering aids such as MgO, sintering forms under 1750 ℃～1900 ℃ high temperature, and what finally obtain is the intracrystalline that forms of nano particle and micron particles/crystal boundary type Nanocomposite material.And, existing research work is directly to adopt nano powder (such as nano SiC), this method exist some subject matters as: the nano SiC powder that introduce (1) is difficult to Uniform Dispersion, thereby causes easily the material microstructure inhomogeneous, is Si such as the nano SiC enrichment of some reunion 3N 4Grain boundaries; (2) because the huge specific surface of Nanosize powder forms reunion (hard aggregation or soft-agglomerated) easily, cause compact density lower; The temperature (1750～1900 ℃) that (3) the follow-up sintering of this method need to be high and long-time insulation (2～4h), cause crystal grain too to be grown up.Thereby finally prepd nano heterogeneous ceramic be actually the Nano/micron type but not the two-phase crystallite dimension all less than the Si of nanometer/Nano type of 100nm 3N 4/ SiC nano heterogeneous ceramic.
Summary of the invention
Technical problem to be solved by this invention provides a kind of nanometer/Nano type Si for preparing 3N 4The new method of/SiC complex phase ceramic.Method of the present invention can overcome some problems of bringing on direct employing nanometer, the submicron powder technology, and Fast Sintering is prepared the two-phase crystallite dimension all less than the nanometer of 100nm/Nano type Si under relatively low sintering temperature 3N 4/ SiC nano heterogeneous ceramic.
The present invention solves the problems of the technologies described above the technical scheme that adopts: this preparation nanometer/Nano type Si 3N 4The method of/SiC nano heterogeneous ceramic, it comprises following concrete steps:
1) crosslinked at low temperature solidifies: organic precursor solidifies in carrying out crosslinked at low temperature under protective atmosphere, obtains non-crystalline solids;
2) high-energy ball milling is pulverized: non-crystalline solids are packed into carry out dry ball milling in the nylon resin ball grinder in high energy ball mill and pulverize;
3) high temperature pyrolysis: the mixture behind the high-energy ball milling carries out high temperature pyrolysis, obtains the SiCN powder at certain pyrolysis temperature pyrolysis certain hour under protective atmosphere.
4) high-energy ball milling is pulverized: the SiCN powder is packed into carry out dry ball milling in the nylon resin ball grinder in high energy ball mill and pulverize, introduce sintering aid in the time of ball milling, make non-crystalline state powder and sintering aid mix;
5) discharge plasma sintering (SPS): the mixture behind the high-energy ball milling carries out the SPS Fast Sintering, obtains the two-phase crystallite dimension all less than the nanometer of 100nm/Nano type Si 3N 4/ SiC nano heterogeneous ceramic.
In the described step (1), the raw material that uses is polysilazane, thereby also can adopt the organic precursor of other chemical ingredientss to prepare the nano heterogeneous ceramic of other materials system.
In described step (1) and (3), the pyrolysis plant that uses be the pipe type atmosphere sintering stove, also can adopt other atmosphere sintering furnaces.For anti-oxidation and pollution, the shielding gas of employing is N 2, also can adopt NH 3With rare gas elementes such as Ar.
In described step (2) and (4), employed ball milling method is high-energy ball milling, and the mill of preferentially selecting is situated between and is Si 3N 4Ceramic Balls, the ball grinder that uses is the nylon resin ball grinder, also can use the Ceramic Balls grinding jar, avoids using the metal ball grinding jar such as stainless steel to introduce other contaminating impurities to reduce.
In the described step (4), the sintering aid of introducing is Y 2O 3, also can adopt other sintering aids such as Al 2O 3Deng.
In the described step (5), the agglomerating plant that is adopted is the discharge plasma sintering oven.
Compared with prior art, the invention has the advantages that:
1. the present invention can prepare the two-phase crystallite dimension less than the nanometer of 100nm/Nano type Si 3N 4/ SiC nano heterogeneous ceramic and unconventional intracrystalline/crystal boundary type Nanocomposite material.
2. the present invention can overcome direct employing nanometer, sub-micrometer SiC and Si 3N 4Some problems of bringing on the powder technology are low etc. such as the inhomogeneous and compact density of the dispersion of powder.
3. the present invention adopts organic precursor method to prepare Si 3N 4Pyrolytic reaction and the sintering temperature of system's pottery are low, be usually less than 1650 ℃, and the sintering temperature of traditional handicraft are 1750 ℃～1900 ℃.
4. the present invention can satisfy the performance requriements of differing materials to change product component, structure and character, thereby be particularly suitable for making ceramic matric composite by the design of organic precursor at atomic scale.
Description of drawings
Fig. 1 is the embodiment of the invention one prepared Si 3N 4/ SiC nano heterogeneous ceramic fracture ESEM (SEM) figure;
Fig. 2 is the embodiment of the invention two prepared Si 3N 4/ SiC nano heterogeneous ceramic fracture ESEM (SEM) figure;
Fig. 3 is the embodiment of the invention three prepared Si 3N 4/ SiC nano heterogeneous ceramic fracture ESEM (SEM) figure;
Fig. 4 is the embodiment of the invention one～three prepared Si 3N 4/ SiC nano heterogeneous ceramic X-ray diffraction (XRD) figure;
Fig. 5 is the embodiment of the invention four prepared Si 3N 4/ SiC nano heterogeneous ceramic fracture ESEM (SEM) figure;
Fig. 6 is the embodiment of the invention five prepared Si 3N 4/ SiC nano heterogeneous ceramic fracture ESEM (SEM) figure;
Fig. 7 is the embodiment of the invention six prepared Si 3N 4/ SiC nano heterogeneous ceramic fracture ESEM (SEM) figure;
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment one
Take by weighing initial feed polysilazane 10g and place 99 alumina-ceramic crucibles, at the N of 0.1MPa 2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing with 10 ℃/min.The solid particle that obtains packed into carry out the dry method high-energy ball milling in the nylon resin ball grinder and pulverize and be placed in the 99 aluminium oxide ceramics crucibles, at N in 24 hours 2Be warmed up to 1000 ℃ with 10 ℃/min from room temperature under the atmosphere protection in pipe type sintering furnace, be incubated 2 hours and carry out pyrolysis, the amorphous SiCN powder that obtains is introduced the Y of 3wt% 2O 3The high-energy ball milling of packing in the nylon resin ball grinder was further pulverized after 12 hours, the powder that obtains packed into place the SPS sintering furnace in the graphite jig, after 600 ℃ of 300 ℃/min intensifications, then heat up 1600 ℃ with 100 ℃/min and under the pressure of 80MPa, in vacuum environment, carry out SPS Fast Sintering 5min, powered-down is with the stove cool to room temperature, obtains to have the nanometer of nanoscale/Nano type Si 3N 4/ SiC complex phase ceramic, its microstructure as shown in Figure 1.Microstructure shows that prepared nano heterogeneous ceramic grain size is comparatively even, is equiax crystal, and the average crystal grain size is～60nm that compact structure, employing drainage detect its density and be～2.89g/cm 3
Embodiment two
Take by weighing initial feed polysilazane 10g and place 99 alumina-ceramic crucibles, at the N of 0.1MPa 2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing with 10 ℃/min.The solid particle that obtains packed into carry out the dry method high-energy ball milling in the nylon resin ball grinder and pulverize and be placed in the 99 aluminium oxide ceramics crucibles, at N in 24 hours 2Be warmed up to 1000 ℃ with 10 ℃/min from room temperature under the atmosphere protection in pipe type sintering furnace, be incubated 2 hours and carry out pyrolysis, the amorphous SiCN powder that obtains is introduced the Y of 3wt% 2O 3The high-energy ball milling of packing in the nylon resin ball grinder was further pulverized after 12 hours, the powder that obtains packed into place the SPS sintering furnace in the graphite jig, after 600 ℃ of 300 ℃/min intensifications, then heat up 1600 ℃ with 100 ℃/min and under the pressure of 80MPa, in vacuum environment, carry out SPS Fast Sintering 10min, powered-down is with the stove cool to room temperature, obtains to have the nanometer of nanoscale/Nano type Si 3N 4/ SiC complex phase ceramic, its microstructure as shown in Figure 2.Microstructure shows that prepared nano heterogeneous ceramic grain size is comparatively even, is equiax crystal, and the average crystal grain size is～90nm that compact structure, employing drainage detect its density and be～2.96g/cm 3
Embodiment three
Take by weighing initial feed polysilazane 10g and place 99 alumina-ceramic crucibles, at the N of 0.1MPa 2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing with 10 ℃/min.The solid particle that obtains packed into carry out the dry method high-energy ball milling in the nylon resin ball grinder and pulverize and be placed in the 99 aluminium oxide ceramics crucibles, at N in 24 hours 2Be warmed up to 1000 ℃ with 10 ℃/min from room temperature under the atmosphere protection in pipe type sintering furnace, be incubated 2 hours and carry out pyrolysis, the amorphous SiCN powder that obtains is introduced the Y of 3wt% 2O 3The high-energy ball milling of packing in the nylon resin ball grinder was further pulverized after 12 hours, the powder that obtains packed into place the SPS sintering furnace in the graphite jig, after 600 ℃ of 300 ℃/min intensifications, then heat up 1600 ℃ with 100 ℃/min and under the pressure of 80MPa, in vacuum environment, carry out SPS Fast Sintering 15min, powered-down is with the stove cool to room temperature, obtains to have the nanometer of nanoscale/Nano type Si 3N 4/ SiC complex phase ceramic, its microstructure as shown in Figure 3.Microstructure shows that prepared nano heterogeneous ceramic grain size is comparatively even, is equiax crystal, and the average crystal grain size is～110nm that compact structure, employing drainage detect its density and be～2.98g/cm 3Fig. 4 is the prepared nanometer of the embodiment of the invention one～three/Nano type Si 3N 4The XRD collection of illustrative plates of/SiC complex phase ceramic shows that the main phase of the complex phase ceramic of preparation consists of β-SiC (JCPDS Card No.29-1129), α-Si 3N 4(JCPDS Card No.41-0360) and β-Si 3N 4(JCPDS CardNo.33-1160), and a small amount of α-Y is arranged 2Si 2O 7(JCPDS Card No.38-0223), α-Y 2Si 2O 7Mainly be because being added in the middle of the high-temperature sintering process of sintering aid forms.
Embodiment four
Take by weighing initial feed polysilazane 10g and place 99 alumina-ceramic crucibles, at the N of 0.1MPa 2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing with 10 ℃/min.The solid particle that obtains packed into carry out the dry method high-energy ball milling in the nylon resin ball grinder and pulverize and be placed in the 99 aluminium oxide ceramics crucibles, at N in 24 hours 2Be warmed up to 1000 ℃ with 10 ℃/min from room temperature under the atmosphere protection in pipe type sintering furnace, be incubated 2 hours and carry out pyrolysis, the amorphous SiCN powder that obtains is introduced the Y of 3wt% 2O 3The high-energy ball milling of packing in the nylon resin ball grinder was further pulverized after 12 hours, the powder that obtains packed into place the SPS sintering furnace in the graphite jig, after 600 ℃ of 300 ℃/min intensifications, then heat up 1550 ℃ with 100 ℃/min and under the pressure of 80MPa, in vacuum environment, carry out SPS Fast Sintering 10min, powered-down is with the stove cool to room temperature, obtains to have the nanometer of nanoscale/Nano type Si 3N 4/ SiC complex phase ceramic, its microstructure as shown in Figure 5.Microstructure shows that prepared nano heterogeneous ceramic grain size is comparatively even, is equiax crystal, and the average crystal grain size is～80nm that compact structure, employing drainage detect its density and be～2.91g/cm 3
Embodiment five
Take by weighing initial feed polysilazane 10g and place 99 alumina-ceramic crucibles, at the NH of 0.1MPa 3In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing with 10 ℃/min.The solid particle that obtains packed into carry out the dry method high-energy ball milling in the nylon resin ball grinder and pulverize and be placed in the 99 aluminium oxide ceramics crucibles, at N in 24 hours 2Be warmed up to 1000 ℃ with 10 ℃/min from room temperature under the atmosphere protection in pipe type sintering furnace, be incubated 2 hours and carry out pyrolysis, the amorphous SiCN powder that obtains is introduced the Y of 3wt% 2O 3The high-energy ball milling of packing in the nylon resin ball grinder was further pulverized after 12 hours, the powder that obtains packed into place the SPS sintering furnace in the graphite jig, after 600 ℃ of 300 ℃/min intensifications, then heat up 1600 ℃ with 200 ℃/min and under the pressure of 80MPa, in vacuum environment, carry out SPS Fast Sintering 10min, powered-down is with the stove cool to room temperature, obtains to have the nanometer of nanoscale/Nano type Si 3N 4/ SiC complex phase ceramic, its microstructure as shown in Figure 6.Microstructure shows that prepared nano heterogeneous ceramic grain size is comparatively even, is equiax crystal, and the average crystal grain size is～80nm that compact structure, employing drainage detect its density and be～2.96g/cm 3
Embodiment six
Take by weighing initial feed polysilazane 10g and place 99 alumina-ceramic crucibles, at the N of 0.1MPa 2In the tubular type sintering oven, be warmed up to 260 ℃ from room temperature under the gas shiled atmosphere, be incubated 0.5 hour and carry out crosslinking curing with 10 ℃/min.The solid particle that obtains packed into carry out the dry method high-energy ball milling in the nylon resin ball grinder and pulverize and be placed in the 99 aluminium oxide ceramics crucibles, at N in 24 hours 2Be warmed up to 1000 ℃ with 10 ℃/min from room temperature under the atmosphere protection in pipe type sintering furnace, be incubated 2 hours and carry out pyrolysis, the amorphous SiCN powder that obtains is introduced the Y of 3wt% 2O 3The high-energy ball milling of packing in the nylon resin ball grinder was further pulverized after 12 hours, the powder that obtains packed into place the SPS sintering furnace in the graphite jig, after 600 ℃ of 300 ℃/min intensifications, then heat up 1600 ℃ with 100 ℃/min and under the pressure of 60MPa, in vacuum environment, carry out SPS Fast Sintering 10min, powered-down is with the stove cool to room temperature, obtains to have the nanometer of nanoscale/Nano type Si 3N 4/ SiC complex phase ceramic, its microstructure as shown in Figure 7.Microstructure shows that prepared nano heterogeneous ceramic grain size is comparatively even, is equiax crystal, and the average crystal grain size is～100nm that compact structure, employing drainage detect its density and be～2.89g/cm 3
The present invention proposes a kind of new employing organic precursor pyrolysis in conjunction with the method for SPS sintering, can prepare the two-phase crystallite dimension all less than the nanometer of 100nm/Nano type Si by regulation and control SPS sintering process parameter 3N 4/ SiC nano heterogeneous ceramic, and the prepared intracrystalline of unconventional direct employing nano powder (such as nano SiC)/crystal boundary type Nanocomposite material.Method of the present invention can overcome some problems such as the initial raw material nano powder that bring on the conventional powder technology and disperse temperature (1750～1900 ℃) inhomogeneous, that compact density is lower and high and long-time insulation (2～4h).Simultaneously the present invention can satisfy the performance requirement of different materials by the design of organic precursor at atomic scale to change product component, structure and character, be particularly suitable for making ceramic matric composite.

Claims (5)

1, a kind of nanometer/Nano type Si for preparing 3N 4The new method of/SiC nano heterogeneous ceramic, it comprises following concrete steps:
(1) crosslinked at low temperature solidifies: organic precursor solidifies in carrying out crosslinked at low temperature under protective atmosphere, obtains non-crystalline solids;
(2) ball mill pulverizing: non-crystalline solids are carried out ball mill pulverizing in ball mill;
(3) high temperature pyrolysis: the mixture behind the ball milling carries out high temperature pyrolysis, obtains the SiCN powder at certain pyrolysis temperature pyrolysis certain hour under protective atmosphere.
(4) ball mill pulverizing: with the further ball mill pulverizing of SiCN powder, introduce sintering aid in the time of ball milling, make non-crystalline state powder and sintering aid mix;
(5) discharge plasma sintering (SPS): the mixture behind the high-energy ball milling carries out the SPS Fast Sintering, obtains nanometer/Nano type Si 3N 4/ SiC nano heterogeneous ceramic.
2, preparation nanometer according to claim 1/Nano type Si 3N 4The method of/SiC nano heterogeneous ceramic is characterized in that: the raw material that uses in the described step (1) is organic precursor.
3, preparation nanometer according to claim 2/Nano type Si 3N 4The method of/SiC nano heterogeneous ceramic is characterized in that: in described step (1) and (3), curing and the pyrolysis plant of using is atmosphere sintering furnace, and the protective gas of employing is N 2, also can adopt NH 3With gases such as Ar.
4, preparation nanometer according to claim 2/Nano type Si 3N 4The method of/SiC nano heterogeneous ceramic is characterized in that: in described step (2) and (4), the mill of preferentially selecting is situated between and is Si 3N 4Ceramic Balls, the ball grinder that uses is the nylon resin ball grinder, also can use the Ceramic Balls grinding jar, avoids using the metal ball grinding jars such as stainless steel to avoid introducing other contaminating impurities.
5, preparation nanometer according to claim 4/Nano type Si 3N 4The method of/SiC nano heterogeneous ceramic is characterized in that: in the described step (5), employed sintering method is discharge plasma sintering (SPS).
CN 200810086327 2008-03-24 2008-03-24 Method for preparing nano/nano-type Si3N4/SiC nano multi-phase ceramic Pending CN101265106A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN103641484A (en) * 2013-12-16 2014-03-19 武汉科技大学 Method for preparing Si3N4/SiC composite ceramic powder from biomass power plant ash
CN108147822A (en) * 2017-12-26 2018-06-12 天津大学 A kind of heat conduction silicon nitride-based material and preparation method thereof
JPWO2020032036A1 (en) * 2018-08-08 2021-08-10 京セラ株式会社 Housing
JPWO2020032035A1 (en) * 2018-08-08 2021-08-12 京セラ株式会社 substrate
JPWO2020032037A1 (en) * 2018-08-08 2021-08-26 京セラ株式会社 Holding member for optical products
JPWO2020032034A1 (en) * 2018-08-08 2021-08-26 京セラ株式会社 Shading member
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641484A (en) * 2013-12-16 2014-03-19 武汉科技大学 Method for preparing Si3N4/SiC composite ceramic powder from biomass power plant ash
CN108147822A (en) * 2017-12-26 2018-06-12 天津大学 A kind of heat conduction silicon nitride-based material and preparation method thereof
JPWO2020032036A1 (en) * 2018-08-08 2021-08-10 京セラ株式会社 Housing
JPWO2020032035A1 (en) * 2018-08-08 2021-08-12 京セラ株式会社 substrate
JPWO2020032037A1 (en) * 2018-08-08 2021-08-26 京セラ株式会社 Holding member for optical products
JPWO2020032034A1 (en) * 2018-08-08 2021-08-26 京セラ株式会社 Shading member
JP7150026B2 (en) 2018-08-08 2022-10-07 京セラ株式会社 substrate
JP7150025B2 (en) 2018-08-08 2022-10-07 京セラ株式会社 light shielding material
CN115354322A (en) * 2022-08-05 2022-11-18 佳木斯大学 Preparation method of high-porosity thermal barrier coating
CN115354322B (en) * 2022-08-05 2023-06-23 佳木斯大学 Preparation method of high-pore thermal barrier coating

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