CN101935220A - Carbon nanofiber reinforced aluminum nitride composite ceramic and preparation method thereof - Google Patents
Carbon nanofiber reinforced aluminum nitride composite ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to carbon nanofiber reinforced aluminum nitride composite ceramic, which is characterized by being prepared from the following components in percentage by weight: 1-5 percent of carbon nanofibers, 90-97 percent of aluminum nitride, 1-3 percent of calcium fluoride and 1-2 percent of yttria. The preparation method of the carbon nanofiber reinforced aluminum nitride composite ceramic comprises the following steps of: ultrasonically dispersing the carbon nanofibers, the aluminum nitride and a sintering assistant respectively, mixing dispersed slurry and continuing to ultrasonically disperse the dispersed slurry; then, dispersing into mixed slurry through ball milling, drying and sieving the mixed slurry, and carrying out plasma activated sintering so as to finally prepare the carbon nanofiber reinforced aluminum nitride composite ceramic. The carbon nanofiber reinforced aluminum nitride composite ceramic of the invention has the advantages of preferable mechanical performance and conductive performance, simple preparation process, short preparation time and low cost.
Description
Technical field:
The invention belongs to new material technology field, particularly a kind of carbon nanofiber strengthen aluminium nitride complex phase ceramic and preparation method thereof.
Background technology:
One of of paramount importance III group-III nitride of aluminium nitride (AlN), because of having broad-band gap, high heat conductance, high insulating coefficient, low-k, can being widely used in aspect (L.M.Sheppard such as high-temperature electronic device, electronic material, photodiode (LED), advanced ceramics parts and thermal component with a series of good characteristics such as silicon matched coefficient of thermal expansion, excellent mechanical property and chemical stabilities, " Aluminumnitride:a versatile but challenging material ", Am.Ceram.Soc.Bull.69, (1990) 1801).Yet, because lower intensity the essential fragility of aluminium nitride ceramics material and relative other stupalith (as silicon nitride, zirconium white etc.) has limited it and has used widely.In addition, the aluminium nitride ceramics of high-insulativity is in some application such as functional areas such as absorbing material, ion etching electrode materials, electromachining baseplate material, electric heating materials, usually need it to have certain electric conductivity (T.Kusunose, T.Sekino, K.Niihara, " Production of a grainboundary phase as conducting pathway in insulating AlN ceramics ", ActaMaterialia, 55, (2007) 6170).
China's CN101100386 patent disclosure a kind of hot-pressing sintering method prepare carbon nano-tube enhanced aluminum nitride composite material, the adding of this carbon nanotube can promote the mechanical property of aluminium nitride, but this preparation method still exists certain problem, is mainly reflected in the following aspects: one, the cost of carbon nanotube is higher; Two, the chemical activity of carbon nano-tube height causes its purity lower, need carry out chemical purification before using and handle; Three, carbon nanotube needs the long dispersion treatment time (ultra-sonic dispersion needs 1～24 hour, Ball milling needs 12～48 hours) because of its bad dispersibility before the use; Four, adopt hot pressing sintering method temperature rise rate slow (about 1～3 hour), soaking time long (1～4 hour consuming time).Below what time make this complicated process of preparation, the production cycle is long, cost is high, is unfavorable for practical application.
Summary of the invention:
The object of the present invention is to provide the carbon nanofiber of a kind of mechanical property that can improve aluminium nitride ceramics and conductivity to strengthen aluminium nitride complex phase ceramic and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is: provide a kind of carbon nanofiber to strengthen the aluminium nitride complex phase ceramic, this complex phase ceramic is that 1～5% carbon nanofiber, mass percent are that 90～97% aluminium nitride, mass percent are that 1～3% Calcium Fluoride (Fluorspan) and mass percent are that 1～2% yttrium oxide is formed by mass percent.
For achieving the above object, the technical solution adopted in the present invention is: a kind of method that carbon nanofiber strengthens the aluminium nitride complex phase ceramic for preparing is provided, this method comprises behind carbon nanofiber, aluminium nitride and the sintering aid difference ultra-sonic dispersion, dispersed paste is mixed and the continuation ultra-sonic dispersion, Ball milling becomes mixed slurry subsequently, mixed slurry through super-dry, sieve, carry out plasma activated sintering again, prepare carbon nanofiber enhanced aluminium nitride complex phase ceramic at last.
The described method for preparing carbon nanofiber enhancing aluminium nitride complex phase ceramic specifically may further comprise the steps:
1) carbon nanofiber, aluminium nitride and sintering aid are carried out ultra-sonic dispersion respectively: taking by weighing mass percent and be 1～5% carbon nanofiber, is medium with the dehydrated alcohol, and ultra-sonic dispersion 20～30 minutes obtains suspension one; Take by weighing mass percent and be 90～97% aluminium nitride, mass percent is that 1～3% Calcium Fluoride (Fluorspan) and mass percent are 1～2% yttrium oxide, is medium with the dehydrated alcohol, and ultra-sonic dispersion 20～30 minutes obtains suspension two; Suspension one and suspension two are mixed, continued ultra-sonic dispersion 20～30 minutes, obtain suspension three;
2) batch mixing Ball milling: suspension three is poured in the ball grinder, and rotational speed of ball-mill is 100～200 rev/mins, disperses to obtain mixed slurry after 6～24 hours;
3) the batch mixing drying, sieve: mixed slurry is put into vacuum drying oven, and holding temperature is 70～90 degree, dry 6～10 hours, cross 100～200 mesh sieves then, obtain mixed powder;
4) plasma activated sintering: mixed powder is packed in the graphite jig, be placed on subsequently in the plasma activated sintering stove, predetermined fixed pressure 30～50MPa, vacuumize furnace chamber air pressure is in below the 6Pa, energising heating, with 100～200 degree/minute speed be warmed up to 1600～1800 degree and carry out sintering, sintered heat insulating 5～10 minutes, furnace cooling obtains fine and close carbon nanofiber and strengthens the aluminium nitride complex phase ceramic to room temperature subsequently.
Wherein said carbon nanofiber diameter is 60～200 nanometers, and length-to-diameter ratio was at least 10: 1, and purity is greater than 99%.
The invention has the beneficial effects as follows: adopt carbon nanofiber as wild phase, have the following advantages compared to carbon nanotube: one, at first carbon nanofiber than the cost of carbon nanotube low (80～150 dollars/gram of carbon nanofiber, 1000～2000 dollars/gram of carbon nanotube); Two, the activity of carbon nanofiber is lower, makes it have higher purity, thus do not need to carry out chemical purification before using, thereby reduced the purification processes operation compared to prior art; Three, carbon nanofiber makes that compared to easier dispersive characteristic of having of carbon nanotube and high chemical stability the jitter time among the preparation technology shortens greatly.Adopt the plasma activated sintering method to prepare carbon nanofiber in addition and strengthen the aluminium nitride complex phase ceramic, shortened sintering time, reduced sintering temperature, controlled production cost.The carbon nanofiber of the present invention's preparation strengthens the material densification of aluminium nitride complex phase ceramic, has mechanical property such as flexural strength, fracture toughness property preferably, and has specific conductivity preferably.
Description of drawings
Fig. 1 is the X-ray diffractogram that the carbon nanofiber of embodiment 1 strengthens the aluminium nitride complex phase ceramic;
Fig. 2 is the sem photograph that the carbon nanofiber of embodiment 1 strengthens the aluminium nitride complex phase ceramic;
Fig. 3 is the X-ray diffractogram that the carbon nanofiber of embodiment 4 strengthens the aluminium nitride complex phase ceramic;
Fig. 4 is the sem photograph that the carbon nanofiber of embodiment 4 strengthens the aluminium nitride complex phase ceramic;
Embodiment:
Embodiment 1:
Taking by weighing mass percent and be 2% carbon nanofiber (diameter 60～200, length-to-diameter ratio＞10: 1, purity＞99%), is medium with the dehydrated alcohol, and 1. ultra-sonic dispersion 30 minutes obtains suspension; Take by weighing mass percent and be 94% aluminium nitride, mass percent is that 2% Calcium Fluoride (Fluorspan) and mass percent are 2% yttrium oxide, is medium with the dehydrated alcohol, and 2. ultra-sonic dispersion 30 minutes obtains suspension; Subsequently 1. and 2. suspension mixed, continued ultra-sonic dispersion 30 minutes, obtain suspension 3..3. suspension poured in the ball grinder, and rotational speed of ball-mill is 120 rev/mins, disperses to obtain mixed slurry 4. after 12 hours.4. mixed slurry is put into vacuum drying oven, and holding temperature is 70 degree, dry 10 hours, cross 100 mesh sieves then, and obtain mixed powder.Mixed powder is packed in the graphite jig, be placed on subsequently in the plasma activated sintering stove, predetermined fixed pressure 35MPa, vacuumize furnace chamber air pressure is in below the 6Pa, energising heating, with 150 degree/minute speed be warmed up to 1700 degree and carry out sintering, sintered heat insulating 5 minutes, furnace cooling obtains fine and close carbon nanofiber and strengthens the aluminium nitride complex phase ceramic to room temperature subsequently.After measured, flexural strength is 354MPa, and fracture toughness property is 5.03MPam
1/2, specific conductivity is 0.2Sm
-1
Utilize X-ray diffractometer (XRD), field emission scanning electron microscope (FESEM) that resulting sample is characterized.Fig. 1 is the X-ray diffractogram of gained sample, can see that principal crystalline phase is the aluminium nitride (AlN) of hexagonal wurtzite structure, and the yttrium-calcium aluminate (CaYAlO that minute quantity is formed by the sintering aid reaction occurred
4) and yttrium aluminium monocline phase (Y
4Al
2O
9) liquid phase, the formation of these liquid phases has promoted the densification performance of material.But because the finiteness of XRD analysis methods analyst precision, the diffraction peak of carbon nanofiber is also not obvious.Fig. 2 is the sem photograph of gained sample, can see, material is very fine and close, and carbon nanofiber is evenly dispersed in the aluminium nitride matrix, has greatly promoted the lifting of mechanical property and specific conductivity.
Embodiment 2:
Taking by weighing mass percent and be 1% carbon nanofiber (diameter 60～200, length-to-diameter ratio＞10: 1, purity＞99%), is medium with the dehydrated alcohol, and 1. ultra-sonic dispersion 20 minutes obtains suspension; Take by weighing mass percent and be 97% aluminium nitride, mass percent is that 1% Calcium Fluoride (Fluorspan) and mass percent are 1% yttrium oxide, is medium with the dehydrated alcohol, and 2. ultra-sonic dispersion 20 minutes obtains suspension; Subsequently 1. and 2. suspension mixed, continued ultra-sonic dispersion 20 minutes, obtain suspension 3..3. suspension poured in the ball grinder, and rotational speed of ball-mill is 100 rev/mins, disperses to obtain mixed slurry 4. after 24 hours.4. mixed slurry is put into vacuum drying oven, and holding temperature is 70 degree, dry 6 hours, cross 100 mesh sieves then, and obtain mixed powder.Mixed powder is packed in the graphite jig, be placed on subsequently in the plasma activated sintering stove, predetermined fixed pressure 30MPa, vacuumize furnace chamber air pressure is in below the 6Pa, energising heating, with 200 degree/minute speed be warmed up to 1600 degree and carry out sintering, sintered heat insulating 5 minutes, furnace cooling obtains fine and close carbon nanofiber and strengthens the aluminium nitride complex phase ceramic to room temperature subsequently.After measured, flexural strength is 322MPa, and fracture toughness property is 4.75MPam
1/2, specific conductivity is 0.002Sm
-1
Embodiment 3:
Taking by weighing mass percent and be 3% carbon nanofiber (diameter 60～200, length-to-diameter ratio＞10: 1, purity＞99%), is medium with the dehydrated alcohol, and 1. ultra-sonic dispersion 30 minutes obtains suspension; Take by weighing mass percent and be 92% aluminium nitride, mass percent is that 3% Calcium Fluoride (Fluorspan) and mass percent are 2% yttrium oxide, is medium with the dehydrated alcohol, and 2. ultra-sonic dispersion 25 minutes obtains suspension; Subsequently 1. and 2. suspension mixed, continued ultra-sonic dispersion 25 minutes, obtain suspension 3..3. suspension poured in the ball grinder, and rotational speed of ball-mill is 150 rev/mins, disperses to obtain mixed slurry 4. after 8 hours.4. mixed slurry is put into vacuum drying oven, and holding temperature is 80 degree, dry 7 hours, cross 100 mesh sieves then, and obtain mixed powder.Mixed powder is packed in the graphite jig, be placed on subsequently in the plasma activated sintering stove, predetermined fixed pressure 40MPa, vacuumize furnace chamber air pressure is in below the 6Pa, energising heating, with 120 degree/minute speed be warmed up to 1750 degree and carry out sintering, sintered heat insulating 8 minutes, furnace cooling obtains fine and close carbon nanofiber and strengthens the aluminium nitride complex phase ceramic to room temperature subsequently.After measured, flexural strength is 302MPa, and fracture toughness property is 4.52MPam
1/2, specific conductivity is 0.5Sm
-1
Embodiment 4:
Taking by weighing mass percent and be 5% carbon nanofiber (diameter 60～200, length-to-diameter ratio＞10: 1, purity＞99%), is medium with the dehydrated alcohol, and 1. ultra-sonic dispersion 30 minutes obtains suspension; Take by weighing mass percent and be 90% aluminium nitride, mass percent is that 3% Calcium Fluoride (Fluorspan) and mass percent are 2% yttrium oxide, is medium with the dehydrated alcohol, and 2. ultra-sonic dispersion 30 minutes obtains suspension; Subsequently 1. and 2. suspension mixed, continued ultra-sonic dispersion 30 minutes, obtain suspension 3..3. suspension poured in the ball grinder, and rotational speed of ball-mill is 200 rev/mins, disperses to obtain mixed slurry 4. after 10 hours.4. mixed slurry is put into vacuum drying oven, and holding temperature is 90 degree, dry 12 hours, cross 100 mesh sieves then, and obtain mixed powder.Mixed powder is packed in the graphite jig, be placed on subsequently in the plasma activated sintering stove, predetermined fixed pressure 50MPa, vacuumize furnace chamber air pressure is in below the 6Pa, energising heating, with 100 degree/minute speed be warmed up to 1800 degree and carry out sintering, sintered heat insulating 10 minutes, furnace cooling obtains fine and close carbon nanofiber and strengthens the aluminium nitride complex phase ceramic to room temperature subsequently.After measured, flexural strength is 270MPa, and fracture toughness property is 3.95MPam
1/2, specific conductivity is 1.2Sm
-1
Fig. 3 is the X-ray diffractogram of gained sample, can see that principal crystalline phase is the aluminium nitride (AlN) of hexagonal wurtzite structure, and the yttrium-calcium aluminate (CaYAlO that minute quantity is formed by the sintering aid reaction occurred
4) and yttrium aluminium monocline phase (Y
4Al
2O
9) liquid phase, the formation of these liquid phases has promoted the densification performance of material.In addition, Fig. 3 can see that the diffraction peak (26.6 °) of carbon nanofiber occurs, and illustrates that preparation method used in the present invention can be stored in carbon nanotube in the aluminium nitride matrix well.Fig. 4 is the sem photograph of gained sample, can see, even the content of carbon nanofiber reaches 5% massfraction, preparation method used in the present invention still can be evenly dispersed in carbon nanofiber aluminium nitride matrix inside well, and has very high density.
Adopt carbon nanofiber as wild phase, carbon nanofiber has characteristics such as higher length-to-diameter ratio, low density, high strength, high thermal conductance and specific conductivity because of it not only can improve the mechanical property of matrix, and has improved the conductivity of matrix.And carbon nanofiber also has higher purity, easier dispersive characteristic and high chemical stability, and making does not need to carry out purification processes among the preparation technology and jitter time shortens greatly.Adopt the plasma activated sintering method to prepare carbon nanofiber in addition and strengthen the aluminium nitride complex phase ceramic, shortened sintering time, reduced sintering temperature, controlled production cost; Simultaneously, the carbon nanofiber of preparation strengthens mechanics and the conductivity that the aluminium nitride complex phase ceramic has excellence, the range of application of having widened this material.
Claims (5)
1. a carbon nanofiber strengthens the aluminium nitride complex phase ceramic, it is characterized in that: this complex phase ceramic is that 1～5% carbon nanofiber, mass percent are that 90～97% aluminium nitride, mass percent are that 1～3% Calcium Fluoride (Fluorspan) and mass percent are that 1～2% yttrium oxide is formed by mass percent.
2. carbon nanofiber as claimed in claim 1 strengthens the aluminium nitride complex phase ceramic, and it is characterized in that: described carbon nanofiber diameter is 60～200 nanometers, and length-to-diameter ratio was at least 10: 1, and purity is greater than 99%.
3. one kind prepares the method that carbon nanofiber as claimed in claim 1 strengthens the aluminium nitride complex phase ceramic, it is characterized in that: behind carbon nanofiber, aluminium nitride and sintering aid difference ultra-sonic dispersion, dispersed paste is mixed and the continuation ultra-sonic dispersion, Ball milling becomes mixed slurry subsequently, mixed slurry through super-dry, sieve, carry out plasma activated sintering again, prepare carbon nanofiber at last and strengthen the aluminium nitride complex phase ceramic.
4. the method for preparing carbon nanofiber enhancing aluminium nitride complex phase ceramic as claimed in claim 3, it is characterized in that: described method may further comprise the steps:
1) taking by weighing mass percent is 1～5% carbon nanofiber, is medium with the dehydrated alcohol, and ultra-sonic dispersion 20～30 minutes obtains suspension one; Take by weighing mass percent and be 90～97% aluminium nitride, mass percent is that 1～3% Calcium Fluoride (Fluorspan) and mass percent are 1～2% yttrium oxide, is medium with the dehydrated alcohol, and ultra-sonic dispersion 20～30 minutes obtains suspension two; Suspension one and suspension two are mixed, continued ultra-sonic dispersion 20～30 minutes, obtain suspension three;
2) suspension three is poured in the ball grinder, rotational speed of ball-mill is 100～200 rev/mins, disperses to obtain mixed slurry after 6～24 hours;
3) mixed slurry is put into vacuum drying oven, holding temperature is 70～90 degree, dry 6～10 hours, cross 100～200 mesh sieves then, and obtain mixed powder;
4) mixed powder is packed in the graphite jig, be placed on subsequently in the plasma activated sintering stove, predetermined fixed pressure 30～50MPa, vacuumize furnace chamber air pressure is in below the 6Pa, energising heating, with 100～200 degree/minute speed be warmed up to 1600～1800 degree and carry out sintering, sintered heat insulating 5～10 minutes, furnace cooling obtains fine and close carbon nanofiber and strengthens the aluminium nitride complex phase ceramic to room temperature subsequently.
5. the method for preparing carbon nanofiber enhancing aluminium nitride complex phase ceramic as claimed in claim 4 is characterized in that described carbon nanofiber diameter is 60～200 nanometers, and length-to-diameter ratio was at least 10: 1, and purity is greater than 99%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502538A (en) * | 2011-11-08 | 2012-06-20 | 中国计量学院 | Method for synthesizing ultrafine aluminum nitride powder at low temperature under assistance of calcium |
| CN110981528A (en) * | 2019-12-06 | 2020-04-10 | 西安交通大学 | Directional porous aluminum nitride ceramic and rapid preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100386A (en) * | 2007-07-20 | 2008-01-09 | 中国人民解放军国防科学技术大学 | Carbon nano-tube enhanced aluminum nitride composite material and preparation method thereof |
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2010
- 2010-08-31 CN CN 201010268201 patent/CN101935220A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100386A (en) * | 2007-07-20 | 2008-01-09 | 中国人民解放军国防科学技术大学 | Carbon nano-tube enhanced aluminum nitride composite material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502538A (en) * | 2011-11-08 | 2012-06-20 | 中国计量学院 | Method for synthesizing ultrafine aluminum nitride powder at low temperature under assistance of calcium |
| CN110981528A (en) * | 2019-12-06 | 2020-04-10 | 西安交通大学 | Directional porous aluminum nitride ceramic and rapid preparation method thereof |
| CN110981528B (en) * | 2019-12-06 | 2021-02-26 | 西安交通大学 | Directional porous aluminum nitride ceramic and rapid preparation method thereof |
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Application publication date: 20110105 |