CN109336609A - One kind is highly thermally conductive, be electrically insulated liquid phase sintering silicon carbide ceramic and its SPS preparation process - Google Patents
One kind is highly thermally conductive, be electrically insulated liquid phase sintering silicon carbide ceramic and its SPS preparation process Download PDFInfo
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Abstract
The present invention relates to a kind of highly thermally conductive, electrical isolation liquid phase sintering silicon carbide ceramic and its SPS preparation process.A kind of preparation method of glow discharge plasma liquid phase sintering silicon carbide ceramic includes: to mix SiC powder, rare earth oxide and solvent, and slurry is prepared, and the rare earth oxide is CeO2、Y2O3、Er2O3In at least two；Gained slurry is obtained into green body after drying, sieving, molding；Gained green body is subjected to glow discharge plasma sintering under pressurization, inert atmosphere conditions, obtains the glow discharge plasma liquid phase sintering silicon carbide ceramic.
Description
Technical field
The present invention relates to a kind of highly thermally conductive, electrical isolation liquid phase sintering silicon carbide (SiC) ceramics and preparation method thereof, belong to height
Thermal conductivity, electric insulation ceramics field.
Background technique
High thermal conductivity, electric insulation ceramics have wide in fields such as large scale integrated circuit, computer technology, hot industries
Application prospect by numerous studies and is applied to the fields such as electronics, aerospace.Currently, being widely used with good electrical exhausted
Alumina ceramics (the Al of edge and mechanical strength2O3) and beryllia ceramics (BeO).Al2O3Thermal conductivity it is relatively low (10~30W/mK),
It is not suitable for applying in high density, powerful device；BeO is most representative high heat-conducting ceramic, chemical stability, electricity
Insulating properties and heat resistance are all fabulous, but BeO has very strong toxicity, has now tapered off use in the industrial production.With
Semiconductor article develop to high-performance, miniaturization, high reliability direction, there is an urgent need to be provided simultaneously with good electrical insulation
(resistivity > 109Ω cm) and heat transfer, and thermal expansion coefficient is the same as new material similar in silicon semiconductor.
Silicon carbide (SiC) ceramics have high intensity, high rigidity, high thermal conductivity, high temperature resistant, corrosion-resistant, wear-resistant, performance is steady
The excellent performance such as fixed, non-aging, has been widely used in each industrial circle.According to the estimation of Slack, pure SiC single crystal
The intrinsic thermal conductivity of room temperature be 490W/ (mK)[7].But SiC ceramic is a kind of strongly covalent strong compound, to realize its densification
Sintering aid must be added by changing sintering, however, due to free crystal grain orientation, in crystal grain on lattice defect, stomata and crystal boundary
Second phase, the thermal conductivity of polycrystal carborundum ceramics is well below monocrystal SiC.Such as use 3~15wt%Al2O3-Y2O3As sintering
The thermal conductivity of the silicon carbide ceramics of auxiliary agent is usually 50~80W/ (mK).Therefore, for highly thermally conductive SiC, scholars carry out
A large amount of research.Nakano etc. prepares the liquid phase burning that thermal conductivity is 270W/ (mK) by adding 1wt%BeO hot pressed sintering
Tie SiC ceramic (LPS-SiC), this be have at present it is reported in the literature have highest thermal conductivity SiC ceramic.Kinoshita etc. passes through
Add 0.15wt%Al2O3Hot pressed sintering prepares LPS-SiC ceramics, and thermal conductivity is up to 235W/ (mK).The hot pressed sinterings such as Kim
SiC and 1vol%Y2O3-Sc2O3, prepare the LPS-SiC ceramics that room temperature thermal conductivity is 234W/ (mK).SiC is a kind of typical case
Semiconductor material, if requiring it to have certain electrical insulation capability for semiconductive material substrate, excessively low sintering aid is led
Cause its low resistivity, usually less than 106Ω·cm。
Summary of the invention
In view of the above-mentioned problems, it is an object of the invention to prepare a kind of while having highly thermally conductive, electrical insulation capability liquid phase
Sintered silicon carbon SiC ceramic and preparation method thereof.
On the one hand, the present invention provides a kind of preparation method of glow discharge plasma liquid phase sintering silicon carbide ceramic, comprising:
SiC powder, rare earth oxide and solvent are mixed, slurry is prepared, the rare earth oxide is CeO2、Y2O3、
Er2O3In at least two；
Gained slurry is obtained into green body after drying, sieving, molding；
Gained green body is subjected to glow discharge plasma sintering under pressurization, inert atmosphere conditions, obtains described glow discharge etc.
Ionic liquid phase sintered silicon carbide ceramics.
The present invention is by addition rare earth sintering aid (for example, Y2O3、Er2O3、CeO2In at least two), then put through aura
Glow discharge plasma LIQUID PHASE SINTERED SiC CERAMICS is obtained after electric plasma agglomeration.According to the binary or ternary system phase of oxide
Figure, the addition of two kinds and three kinds oxide sintering aids contribute to form crystal boundary eutectic phase or solid solution, are located at silicon carbide whisker
Intergranular, to promote the sintering densification of ceramics.Meanwhile the eutectic phase or solid solution of formation are still oxide phase, and aoxidize
Object has electrical insulation capability, to be conducive to the ceramics resistivity with higher of preparation, oxide is electrical insulator, can be true
Recognizing it, there are be conducive to improve the electrical insulation capability of material.The sintering aid Y selected in the present invention2O3、Er2O3、CeO2Y3+、
Er3+、Ce4+Ionic radius be all larger than Si4+Ionic radius, therefore the lattice of SiC is hardly entered, it is compared with system containing Al, it is brilliant
Grain defect is greatly reduced, and reduces phon scattering, to improve thermal conductivity.There is low frit using glow discharge plasma sintering
The advantages of temperature, Fast Sintering.
Preferably, the partial size of the SiC powder is 0.1~1.0 μm.
Preferably, the additive amount of the rare earth oxide account for SiC powder and rare earth oxide gross mass 3.0~
8.0wt%, preferably 3~6wt%.If sintering aid content is lower than 3.0wt%, too low auxiliary agent content is unfavorable for obtaining densification
Ceramic sintered bodies lead to the presence of a large amount of stomatas, and air is unfavorable for the conduction of heat, to reduce the thermal conductivity of prepared ceramics；
Excessively high sintering aid content leads to the presence of a large amount of oxides of silicon carbide ceramics crystal boundary, and oxide is the non-conductor of heat,
Also the thermal conductivity of prepared ceramics can be reduced.
Preferably, the solvent is dehydrated alcohol or/and water, the solid content of the slurry is 45~55wt%.It can lead to
Cross planetary ball mill mixing.
Preferably, the temperature of the glow discharge plasma sintering is 1850~1950 DEG C, preferably 1880~1930 DEG C, protect
The warm time is 10~30 minutes, preferably 10~20 minutes.
Preferably, the inert atmosphere is argon gas, the pressure of the pressurization is 20~30MPa.
Gained slurry can be obtained being packed into mold after powder is dry-pressing formed through drying, sieving, obtain green body.
On the other hand, the present invention also provides a kind of glow discharge plasma liquid-phase sintering carbon prepared according to the above method
SiClx ceramics, the resistivity of the glow discharge plasma liquid phase sintering silicon carbide ceramic is 1.0 × 109Ω cm or more.
The Y that the present invention passes through addition more amount2O3、Er2O3、CeO2Deng be used as sintering aid, and, using glow discharge etc. from
Highly thermally conductive SiC ceramic is prepared in sub- technique sintering, while the formation for the Grain-Boundary Phase that is electrically insulated has conducive to higher electricity is made it have
Resistance rate.
Detailed description of the invention
Fig. 1 is 1950 DEG C of embodiment 1 × 10min, 3wt%Y2O3-CeO2The microstructure of the SiC liquid phase ceramics of content；
Fig. 2 is 1950 DEG C of embodiment 2 × 10min, 3wt%Er2O3-CeO2The microstructure of the SiC liquid phase ceramics of content；
Fig. 3 is 1900 DEG C of embodiment 3 × 10min, 7wt%Y2O3-CeO2The microstructure of the SiC liquid phase ceramics of content；
Fig. 4 is 1900 DEG C of embodiment 4 × 10min, 7wt%Er2O3-CeO2The microstructure of the SiC liquid phase ceramics of content；
Fig. 5 is 1950 DEG C of embodiment 5 × 10min, 7wt%Er2O3-CeO2The microstructure of the SiC liquid phase ceramics of content；
Fig. 6 is 1850 DEG C of embodiment 6 × 20min, 7wt%Y2O3-CeO2The microstructure of the SiC liquid phase ceramics of content.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention relates to a kind of highly thermally conductive, electrical isolation liquid phase sintering silicon carbide (SiC) ceramics SPS (glow discharge etc. from
Son sintering) preparation method, by adding rare earth sintering aid, the acquisition liquid-phase sintered SiC pottery after glow discharge plasma is sintered
Porcelain.Preparation method includes the following steps: with SiC powder, RE oxide powder etc. for raw material, raw material mixing being matched and is slurried
Material；By mixed slurry drying and screening, obtained powder is fitted into mold；By mold in pressurization, brightness under inert atmosphere conditions
Light plasma discharging (SPS) sintering, sintering temperature are 1850~1950 DEG C, and soaking time is 10~30min, pressure 20-
30MPa.Preparation process of the invention is quick, preparation ceramic material is with fine grain structure, and carborundum grain is micro- less than 2
Rice, 90% less than 1 micron, while having highly thermally conductive, electrical insulation capability.
Illustrate to following exemplary highly thermally conductive, electrical isolation liquid phase sintering silicon carbide ceramic preparation side provided by the invention
Method.
The raw materials such as SiC powder, RE oxide powder are mixed into (for example, ball milling mixing etc.), slurry is prepared.This is dilute
Native oxide, can be by cerium oxide (CeO as sintering aid2), yttrium oxide (Y2O3), erbium oxide (Er2O3) etc. two kinds or more it is dilute
Native oxide composition.For example, using Y2O3-CeO2When sintering aid, Y2O3: CeO2Molar ratio can be (1-5): (1-3).Example
Such as, using Er2O3-CeO2When sintering aid, Er2O3: CeO2Molar ratio can be (1-5): (1-3).For example, using Y2O3-
Er2O3When sintering aid, Y2O3: Er2O3Molar ratio can be ((1-5): (1-3).For example, using CeO2-Y2O3-Er2O3Sintering
When auxiliary agent, CeO2: Y2O3: Er2O3Molar ratio can be (0.5-1.5): (1-5): (0.5-1.5).The addition of rare earth oxide
Amount can account for the 3.0~8.0wt%, preferably 3.0~6.0wt% of SiC powder and rare earth oxide gross mass.If sintering aid contains
Amount is lower than 3.0wt%, and too low auxiliary agent content is unfavorable for obtaining fine and close ceramic sintered bodies, leads to the presence of a large amount of stomatas, empty
Gas is unfavorable for the conduction of heat, to reduce the thermal conductivity of prepared ceramics；Excessively high sintering aid content, leads to silicon carbide ceramics
The presence of a large amount of oxides of crystal boundary, and oxide is the non-conductor of heat, can also reduce the thermal conductivity of prepared ceramics.It can incite somebody to action
Above-mentioned raw materials are made into slurry by ball milling mixing.The method that above-mentioned mixed method can be ball milling or stirring, SiC ball is as grinding
Medium.Wherein, SiC powder is high-purity alpha-SiC powder (oxygen content≤0.8wt%, Fe content≤0.02wt%).The SiC powder
Partial size can be 0.1~1.0 μm.The solvent can be dehydrated alcohol or water (such as deionized water).Finally control the slurry
Solid content reach 45~55wt%.
Then, mixed slurry is obtained into uniformly mixed powder by dry, sieving.The temperature of the drying can
It is 50~100 DEG C, the time can be 6~24 hours.The sieving can be the sieve of 100~200 mesh.
Then, by gained powder it is dry-pressing formed after be directly loadable into mold (for example, graphite jig etc.).Dry-pressing formed pressure
It can be 10~20MPa.
By mold (for example, graphite jig), glow discharge plasma is sintered under pressurization, inert atmosphere conditions.Wherein aura
The sintering temperature of discharge plasma sintering can be 1850~1950 DEG C.Consider sintering densification and liquid phase volatilization, preferably sintering temperature
Degree is 1880~1930 DEG C.Soaking time is 10~30 minutes, preferably 10~20 minutes.Inert atmosphere can be argon gas, be real
(furnace sintering is usually within 1 hour) is now densified quickly, in short-term, is added in glow discharge plasma sintering process
The pressure of pressure, pressurization can be 20~30MPa, to promote to densify.
As highly thermally conductive, electrical isolation liquid phase sintering silicon carbide ceramic preparation method a example, comprising: by material powder
(SiC powder, rare earth oxide) is added in water or dehydrated alcohol, uses SiC ball as mill ball, and mixing is made into slurry；Then will
Slurry is dry, sieving obtains uniformly mixed powder, is directly loadable into mold after the powder progress of acquisition is dry-pressing formed；Pressurization,
It is sintered under the conditions of argon gas, sintering temperature is 1850~1950 DEG C, and 10~30min of soaking time prepares sample.
By highly thermally conductive, electrical isolation liquid (high resistance) phase sintering silicon carbide ceramics after processing, its properties is tested.
The present invention measures highly thermally conductive, high resistance liquid phase sintering silicon carbide (SiC) ceramics the tool using laser thermal conductivity method
There is 80Wm-1·K-1Above thermal conductivity λ.
The present invention is measured described highly thermally conductive, high resistance liquid phase sintering silicon carbide (SiC) ceramics straight using DC resistance meter
Leakage resistance rate is 1.0 × 109Ω cm or more.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
97wt%SiC, 3wt%Y2O3-CeO2Sintering aid (Y2O3And CeO2Molar ratio is 1:1) total 100g, it takes water as a solvent, it will
Powder is made into the slurry that solid content is 45wt%, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then it dries
Sieving, obtained powder are packed into graphite jig.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1950 DEG C, soaking time
10min, moulding pressure 30MPa.Obtained SiC liquid phase ceramic density is 2.66gcm-3, Hv3.0=12.77 ± 0.15GPa.
The ceramics of acquisition are made to the sequin of Φ 10mm thickness 2.5mm, measuring its thermal conductivity λ is 84.18w/ (mK), and resistivity is
2.14×1010Ω cm, microstructure are shown in Fig. 1.
Embodiment 2
97wt%SiC, 3wt%Er2O3-CeO2The total 100g of sintering aid, takes water as a solvent, and powder is made into solid content and is
The slurry of 45wt%, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then drying and screening, obtained powder
It is packed into graphite jig.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1950 DEG C, soaking time 10min, and moulding pressure is
30MPa.Obtained SiC liquid phase ceramic density is 2.89gcm-3, Hv3.0=13.25 ± 0.23GPa.The ceramics of acquisition are made
The sequin of Φ 10mm thickness 2.5mm, measuring its thermal conductivity λ is 88.62w/ (mK), and resistivity is 3.37 × 109Ω cm,
Its microstructure is shown in Fig. 2.
Embodiment 3
93wt%SiC, 7wt%Y2O3-CeO2The total 100g of sintering aid, takes water as a solvent, and it is 55wt% that powder, which is made into solid content,
Slurry, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then drying and screening, obtained powder are packed into stone
Black mold.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1900 DEG C, soaking time 10min, moulding pressure 30MPa.
Obtained SiC liquid phase ceramic density is 3.28gcm-3, Hv3.0=17.82 ± 0.12GPa.Φ 10mm is made in the ceramics of acquisition
The sequin of thickness 2.5mm, measuring its thermal conductivity λ is 87.11w/ (mK), and resistivity is 1.41 × 109Ω cm, it is microcosmic
Structure is shown in Fig. 3.
Embodiment 4
93wt%SiC, 7wt%Er2O3-CeO2The total 100g of sintering aid, takes water as a solvent, and powder is made into solid content and is
The slurry of 45wt%, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then drying and screening, obtained powder
It is packed into graphite jig.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1900 DEG C, soaking time 10min, and moulding pressure is
30MPa.Obtained SiC liquid phase ceramic density is 3.20gcm-3, Hv3.0=15.32 ± 0.17GPa.The ceramics of acquisition are made
The sequin of Φ 10mm thickness 2.5mm, measuring its thermal conductivity λ is 80.75w/ (mK), and resistivity is 1.96 × 109Ω cm,
Its microstructure is shown in Fig. 4.
Embodiment 5
93wt%SiC, 7wt%Er2O3-CeO2The total 100g of sintering aid, takes water as a solvent, and powder is made into solid content and is
The slurry of 45wt%, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then drying and screening, obtained powder
It is packed into graphite jig.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1950 DEG C, soaking time 10min, and moulding pressure is
30MPa.Obtained SiC liquid phase ceramic density is 3.21gcm-3, Hv3.0=16.55 ± 0.16GPa.The ceramics of acquisition are made
The sequin of Φ 10mm thickness 2.5mm, measuring its thermal conductivity λ is 93.28w/ (mK), and resistivity is 5.19 × 109Ω cm,
Its microstructure is shown in Fig. 5.
Embodiment 6
93wt%SiC, 7wt%Y2O3-CeO2The total 100g of sintering aid, takes water as a solvent, and it is 45wt% that powder, which is made into solid content,
Slurry, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then drying and screening, obtained powder are packed into stone
Black mold.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1850 DEG C, soaking time 20min, moulding pressure 30MPa.
Obtained SiC liquid phase ceramic density is 3.19gcm-3.The ceramics of acquisition are made to the sequin of Φ 10mm thickness 2.5mm, are surveyed
Obtaining its thermal conductivity λ is 80.08w/ (mK), and resistivity is 1.20 × 109Ω cm, microstructure are shown in Fig. 6.
Embodiment 7
95wt%SiC, 5wt%Y2O3-Er2O3The total 100g of sintering aid, takes water as a solvent, and powder is made into solid content and is
The slurry of 45wt%, using 200g SiC ball as ball-milling medium, planetary ball mill mixing 4h.Then drying and screening, obtained powder
It is packed into graphite jig.Then SPS is sintered under an ar atmosphere, and sintering temperature is 1950 DEG C, soaking time 30min, and moulding pressure is
20MPa.Obtained SiC liquid phase ceramic density is 3.28gcm-3.The ceramics of acquisition are made to the roundlet of Φ 10mm thickness 2.5mm
Piece, measuring its thermal conductivity λ is 97.95w/ (mK), and resistivity is 2.08 × 109Ω·cm。
Claims (8)
1. a kind of preparation method of glow discharge plasma liquid phase sintering silicon carbide ceramic characterized by comprising
SiC powder, rare earth oxide and solvent are mixed, slurry is prepared, the rare earth oxide is CeO2、Y2O3、Er2O3
In at least two；
Gained slurry is obtained into green body after drying, sieving, molding；
Gained green body is subjected to glow discharge plasma sintering under pressurization, inert atmosphere conditions, obtains described glow discharge etc.
Ionic liquid phase sintered silicon carbide ceramics.
2. preparation method according to claim 1, which is characterized in that the partial size of the SiC powder is 0.1~1.0 μm.
3. preparation method according to claim 1 or 2, which is characterized in that the additive amount of the rare earth oxide accounts for SiC powder
3.0~8.0wt% of body and rare earth oxide gross mass.
4. preparation method according to any one of claim 1-3, which is characterized in that the solvent be dehydrated alcohol or
Water, the solid content of slurry are 45~55wt%.
5. preparation method described in any one of -4 according to claim 1, which is characterized in that the glow discharge plasma sintering
Temperature be 1850~1950 DEG C, soaking time be 10~30 minutes.
6. preparation method according to any one of claims 1-5, which is characterized in that the inert atmosphere is argon gas, institute
The pressure for stating pressurization is 20~30MPa.
7. preparation method according to claim 1 to 6, which is characterized in that by gained slurry through drying, sieving
It obtains being packed into mold after powder is dry-pressing formed, obtains green body.
8. a kind of glow discharge plasma liquid-phase sintering carbon of the preparation of preparation method described in any one of -7 according to claim 1
SiClx ceramics, which is characterized in that the resistivity of the glow discharge plasma liquid phase sintering silicon carbide ceramic is 1.0 × 109
Ω cm or more.
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| CN201811339714.XA CN109336609B (en) | 2018-11-12 | 2018-11-12 | High-thermal-conductivity and electric-insulation liquid-phase sintered silicon carbide ceramic and SPS (semi-sintering) process preparation method thereof |
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| CN201811339714.XA CN109336609B (en) | 2018-11-12 | 2018-11-12 | High-thermal-conductivity and electric-insulation liquid-phase sintered silicon carbide ceramic and SPS (semi-sintering) process preparation method thereof |
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| CN114516756A (en) * | 2022-03-14 | 2022-05-20 | 台州学院 | Silicon carbide composite ceramic material and preparation method and application thereof |
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| CN114516756A (en) * | 2022-03-14 | 2022-05-20 | 台州学院 | Silicon carbide composite ceramic material and preparation method and application thereof |
| CN114516756B (en) * | 2022-03-14 | 2022-10-18 | 台州学院 | Silicon carbide composite ceramic material and preparation method and application thereof |
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