CN101734923A - Aluminum nitride porous ceramic and preparation method thereof - Google Patents
Aluminum nitride porous ceramic and preparation method thereof Download PDFInfo
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- CN101734923A CN101734923A CN200910219299A CN200910219299A CN101734923A CN 101734923 A CN101734923 A CN 101734923A CN 200910219299 A CN200910219299 A CN 200910219299A CN 200910219299 A CN200910219299 A CN 200910219299A CN 101734923 A CN101734923 A CN 101734923A
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Abstract
The invention discloses an aluminum nitride porous ceramic and a preparation method thereof. The aluminum nitride porous ceramic comprises the following components by weight percent: 60-72 percent of aluminum oxide, 1-10 percent of sintering assistant, 18-30 percent of carbon black and 1-10 percent of aluminum nitride seed crystal. The preparation method comprises the following steps of: carrying out ball milling mixture on the components with a wetting method to obtain mixed powder; carrying out mould pressing on the components for forming; placing a forming body into an atmosphere furnace, heating the forming body to 1650-1750 DEG C when the nitrogen pressure is higher than one pressure atmosphere and keeping the temperature for 1-4 hours to obtain a sintering body. The aluminum oxide and the carbon black with low cost are used as raw materials to prepare the aluminum nitride porous ceramic with high porosity, therefore, the invention can overcome the defects of the complicated process of preparing the aluminum nitride porous ceramic by using the traditional method and the excessive cost, and can be widely applied in photoelectricity fields of high-temperature electronic devices, microwave integrated circuits, mixed integrated circuits, power electronic modules, laser diodes and the like as well as reinforced phases of metal-based composite materials.
Description
Technical field
The present invention relates to a kind of porous ceramics and preparation method thereof, particularly a kind of aluminum nitride porous ceramic and preparation method thereof.
Background technology
In recent years, the research of porous semi-conductor material has caused the very big interest of scientists.Porous III-V group iii v compound semiconductor material shows many new and quite interesting performances, since vesicular structure, the intensity of its photoluminescence, the quantum effect of photoresponse, secondary harmonic generation (SHG) has all had raising significantly, and the performance of scattering of light and refraction of light all has tangible change.The nitride porous aluminum has the semiconductor material with wide forbidden band of direct band gap as typical III-V family covalent compound, very high thermal conductivity is arranged, good high-temperature insulating property and dielectric properties, heat shock resistance resistance height, the strength of materials is big under the high temperature, the hardness height, nontoxicity, thermal expansivity is low, especially its thermal expansivity and semiconductor silicon material are complementary, thereby at the high-temperature electronic device, microwave integrated circuit, hybrid integrated circuit, electric power electronic module, laser diode, and be used widely in the medium many fields of the wild phase of metal-base composites.According to the difference of used initial powder, existing aluminum nitride porous ceramic preparation methods has following two kinds:
1) atmosphere sintering method is referring to Boey F Y C.Porous AlN ceramic substrates byreaction sintering.Journal of Materials Processing Technology, 2003,140:413-419.Use aluminum nitride particle as initial feed, molding is heated in nitrogen, form aluminum nitride porous ceramic.The molding that perhaps will contain the mixed powder formation of aluminum nitride particle and oxidesintering auxiliary agent heats in nitrogen, and the addition of control sintering temperature and sintering aid obtains the aluminum nitride porous ceramic material.Shortcoming is to need a large amount of aluminium nitride as main raw material, and the preparation cost of aluminium nitride is higher, so cost an arm and a leg, causes the raw materials cost of atmosphere sintering method too high, is unfavorable for suitability for industrialized production,
2) direct nitridation method is that main raw material is made porous formed body earlier with the metallic aluminium powder, is placed on the method manufacturing aluminum nitride porous ceramic (referring to Japanese Patent 1987-217633) that direct reaction carries out nitrogenize in the nitrogen again.The reaction formula of metallic aluminium nitrogenize is Al+N → AlN.The shortcoming of direct nitridation method is to be that main raw material is made porous formed body earlier with the metallic aluminium powder, causes complex manufacturing, and in order to obtain the tiny aluminum nitride porous ceramic of crystal grain, the metallic aluminium powder preparation cost that required particle diameter is tiny is higher.
Summary of the invention
The objective of the invention is to improve the existing existing defective of aluminum nitride porous ceramic preparation method, a kind of method of utilizing carbothermic method to prepare aluminum nitride porous ceramic is provided, have excellent product performance, production technique is simple, the characteristics that preparation cost is low.
For reaching above purpose, the present invention takes following technical scheme to be achieved:
A kind of aluminum nitride porous ceramic, by weight percentage, comprise following component: aluminum oxide 60～72%, sintering aid 1～10%, carbon black 18～30%, aln seed crystal 1～10%, wherein sintering aid is selected from any of Ia family oxide compound, IIa family oxide compound, IIIa family oxide compound, rare earth oxide or fluorochemical.
In the above scheme, the mass ratio of described aluminum oxide and carbon black is 2～4.Described aluminum oxide, its Al
2O
3Content＞95% weight, median size is at 0.2～2 μ m.Described aln seed crystal, its AlN content＞95% weight, particle diameter d
50＜1.2 μ m.Described carbon black, its C content＞95% weight, particle diameter d
50＜80nm.
The preparation method of aforementioned aluminum nitride porous ceramic comprises the steps:
(1) percentage ratio by weight: aluminum oxide 60～72%, sintering aid 1～10%, carbon black 18～30%, aln seed crystal 1～10% carry out weighing respectively, are prepared into mixed powder after the wet ball grinding drying;
(2) mixed powder is sieved make the granulation material;
(3) select mould according to required article shape, above-mentioned granulation material is packed in the mold cavity, die forming is a blank;
(4) blank is rapidly heated under nitrogen atmosphere 1200 ℃, be warmed up to 1600 ℃ more at a slow speed, the heat-up rate with 0.6 ℃/min is warmed up to 1650～1750 ℃ of following insulations 1～4 hour then, feeds flowing nitrogen in the sintering process all the time, last furnace cooling promptly obtains aluminum nitride porous ceramic.
In the aforesaid method, the quality ratio of aluminum oxide and carbon black is 2～4 in the step (1).
Nitrogen atmosphere pressure is＞1 normal atmosphere in the described step (4).The flow of flowing nitrogen is 3L/min.Be rapidly heated is that heat-up rate with 20 ℃/min carries out; Heat up at a slow speed is that heat-up rate with 1.6 ℃/min carries out.
According to method of the present invention, form the aluminum nitride porous ceramic that can obtain having different void content and mechanical property by adjusting prescription.This preparation technology is because utilize the advantage of carbothermic method, thereby is that main raw material further reduces production costs with alumina powder, the carbon black of cheapness.This preparation technology compares with the preparation technology of existing other aluminum nitride porous ceramic, and it is simple to have production technique, the advantage that preparation cost is low.It is tiny that the aluminum nitride porous ceramic of this prepared has crystal grain, the characteristics of even air hole distribution.Owing to superior economy and the reliability of product, can be widely used in the fields such as strengthening material of high-temperature electronic device, microwave integrated circuit, hybrid integrated circuit, electric power electronic module, laser diode and metal-base composites.
Description of drawings
Fig. 1 is the microstructure photo behind embodiment 8 sintering.
Fig. 2 is the microstructure photo behind embodiment 9 sintering.
Fig. 3 is the microstructure photo behind embodiment 10 sintering.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
Aluminum nitride porous ceramic, its composition is as shown in table 1, in the embodiment shown in the table 1 1～21, the median size of forming aluminum oxide generally is controlled at 0.2～2 μ m, if during less than 0.2 μ m, powder is reunited easily, be unfavorable for carbothermic reduction reaction, too high greater than the aluminum nitride porous ceramic void content that 2 μ m form, crystal grain is thick, mechanical properties decrease.Therefore the median size of aluminum oxide preferably is controlled between 0.2～2 μ m.
The quality ratio of aluminum oxide and carbon black is preferably 2～4, if greater than 4 o'clock, aluminum oxide is residual in sintered compact.The thermotolerance of the porous ceramics that obtains and erosion resistance can reduce; If less than 2 o'clock, carbon is residual in sintered compact, influences the mechanical property of porous ceramics.Carbon can be the carbon of arbitrary shape attitude, charcoal for example, and carbon black comprises also and the presoma of carbon such as various resins, also can utilize the mixture of the presoma of carbon black and carbon that table 1 embodiment adopts carbon black, its C content＞95% weight, particle diameter d
50＜80nm.
The addition of the sintering aid during table 1 is formed is 1～10%, surpasses 10%, and the shrinking percentage of porous ceramics strengthens, and causes reducing and a large amount of intergranular glassy phases of void content.If can cause the sintering densification degree low less than 1%, mechanical properties decrease.Sintering aid described here mainly is meant the metal oxide that is varied to glass in agglomerating high temperature field, and the oxide compound that also comprises a kind of or several compositions can become the mixture of glassy phase and some fluorochemicals by reaction.Such sintering aid is selected from the oxide compound Li of Ia family as described in table 1 embodiment
2O, the oxide M gO of IIa family, the oxide compound B of IIIa family
2O
3, rare earth oxide Yb
2O
3, Lu
2O
3, La
2O
3, Y
2O
3Or fluorochemical YF
3, CaF
2Any.The addition of aln seed crystal is 1～10%, its AlN content＞95% weight, median size d
50＜1.2 μ m.Surpass 10%, the void content of porous ceramics reduces, and raw materials cost increases.If can cause carbothermic reduction reaction incomplete less than 1%.
The composition of table 1 aluminum nitride porous ceramic of the present invention and sintering condition
The preparation method of the aluminum nitride porous ceramic that table 1 embodiment forms, earlier alumina powder, aln seed crystal, carbon black, sintering aid are pressed the weighing respectively of different compositions shown in the table 1, and add respectively in the ball mill of packing into behind the dehydrated alcohol and carry out wet mixing, obtain uniform mixed powder after the drying.Then each composition mixed powder is crossed 40 mesh sieves and make the granulation material, put into the green compact sample that the metal die press forming obtains embodiment 1～21 respectively, respectively shaped blanks is put into atmosphere furnace at last, heat-up rate with 20 ℃/min under nitrogen atmosphere is warmed up to 1200 ℃ gradually, heat-up rate with 1.6 ℃/min is warmed up to 1600 ℃ gradually, heat-up rate with 0.6 ℃/min is warmed up to 1650～1750 ℃ of following insulations 1～4 hour gradually, obtains sintered compact.All the time feed flowing nitrogen in the sintering process, the flow of flowing nitrogen is 3L/min, and nitrogen atmosphere pressure is 1 more than the normal atmosphere.
If sintering temperature is less than 1650 ℃, carbothermic reduction reaction can not thoroughly be finished.If sintering temperature surpasses 1750 ℃, aluminum nitride grain is grown up unusually, cause mechanical properties decrease.Heat-up rate preferably is warmed up to 1200 ℃ gradually with the heat-up rate of 20 ℃/min, heat-up rate with 1.6 ℃/min is warmed up to 1600 ℃ gradually, is warmed up to 1650～1750 ℃ gradually with the heat-up rate of 0.6 ℃/min, is lower than above heat-up rate, can increase sintering time, reduce production efficiency.Be higher than above heat-up rate, may cause blank cracking, carbothermic reduction reaction is incomplete.Soaking time was less than 1 hour, and the sintering densification degree is low, mechanical properties decrease, and greater than 4 hours, microstructure changed little, causes energy dissipation.Therefore soaking time is preferably in 1～4 hour.
By the three-point bending strength under the aluminum nitride porous ceramic sintered compact mensuration room temperature of aforesaid method acquisition, shrinking percentage, reaction is weightless.Archimedes's drainage is measured the ventilate rate.Scanning electronic microscope is observed microstructure on sample section.The results of property of these void content and flexural strength is as shown in table 2.Wherein the microstructure picture of embodiment 8-10 as shown in Figure 1-Figure 3.
At 1650～1750 ℃ temperature sintering, material has shown very high flexural strength in the void content scope of 45.8-75.5%, reach as high as 39.2MPa as can be seen from Table 2.
From Fig. 1, Fig. 2 and Fig. 3 as can be seen, it is tiny that the microtexture of the nitride porous aluminium pottery of carbothermic reduction reaction preparation has crystal grain, the characteristics of even air hole distribution.
The performance of table 2 aluminum nitride porous ceramic sintered compact of the present invention
| Shrinking percentage (%) | Weightless (%) | Ventilate rate (%) | Bending strength (MPa) | |
| Embodiment 1 | ??10 | ??32 | ??63.2 | ??7.9 |
| Embodiment 2 | ??9 | ??32 | ??61.7 | ??8.6 |
| Embodiment 3 | ??4 | ??33 | ??68.5 | ??2.1 |
| Embodiment 4 | ??5 | ??32 | ??70.3 | ??1.6 |
| Embodiment 5 | ??4 | ??34 | ??72.9 | ??1.5 |
| Embodiment 6 | ??3 | ??34 | ??75.5 | ??0.9 |
| Embodiment 7 | ??12 | ??31 | ??58.1 | ??17.4 |
| Embodiment 8 | ??6 | ??34 | ??66.9 | ??2.7 |
| Embodiment 9 | ??14 | ??35 | ??56.6 | ??19.9 |
| Embodiment 10 | ??10 | ??32 | ??60.8 | ??9.2 |
| Shrinking percentage (%) | Weightless (%) | Ventilate rate (%) | Bending strength (MPa) | |
| Embodiment 11 | ??5 | ??40 | ??71.5 | ??0.5 |
| Embodiment 12 | ??13 | ??28 | ??53.2 | ??26.1 |
| Embodiment 13 | ??3 | ??32 | ??68.2 | ??1.9 |
| Embodiment 14 | ??15 | ??33 | ??51.7 | ??25.2 |
| Embodiment 15 | ??12 | ??37 | ??62.2 | ??5.6 |
| Embodiment 16 | ??7 | ??30 | ??52.1 | ??28.9 |
| Embodiment 17 | ??15 | ??37 | ??53.1 | ??16.2 |
| Embodiment 18 | ??7 | ??30 | ??61.5 | ??8.9 |
| Embodiment 19 | ??21 | ??36 | ??45.8 | ??39.2 |
| Embodiment 20 | ??10 | ??32 | ??63.7 | ??11.7 |
| Embodiment 21 | ??12 | ??33 | ??58.7 | ??8.6 |
Claims (9)
1. aluminum nitride porous ceramic, it is characterized in that, by weight percentage, comprise following component: aluminum oxide 60～72%, sintering aid 1～10%, carbon black 18～30%, aln seed crystal 1～10%, wherein sintering aid is selected from any of Ia family oxide compound, IIa family oxide compound, IIIa family oxide compound, rare earth oxide or fluorochemical.
2. aluminum nitride porous ceramic as claimed in claim 1 is characterized in that, the quality ratio of described aluminum oxide and carbon black is 2～4.
3. aluminum nitride porous ceramic as claimed in claim 1 is characterized in that, described aluminum oxide, its Al
2O
3Content＞95% weight, median size is at 0.2～2 μ m; Described aln seed crystal, its AlN content＞95% weight, particle diameter d
50＜1.2 μ m; Described carbon black, its C content＞95% weight, particle diameter d50＜80nm.
4. aluminum nitride porous ceramic as claimed in claim 1 is characterized in that, described Ia family oxide compound is Li
2O; Described IIa family oxide compound is MgO; Described IIIa family oxide compound is B
2O
3; Described rare earth oxide is Yb
2O
3, Lu
2O
3, La
2O
3Or Y
2O
3Described fluorochemical is YF
3Or CaF.
5. the preparation method of an aluminum nitride porous ceramic is characterized in that, comprises the steps:
(1) percentage ratio by weight: aluminum oxide 60～72%, sintering aid 1～10%, carbon black 18～30%, aln seed crystal 1～10% carry out weighing respectively, are prepared into mixed powder after the wet ball grinding drying;
(2) mixed powder is sieved make the granulation material;
(3) select mould according to required article shape, above-mentioned granulation material is packed in the mold cavity, die forming is a blank;
(4) blank is rapidly heated under nitrogen atmosphere 1200 ℃, be warmed up to 1600 ℃ more at a slow speed, the heat-up rate with 0.6 ℃/min is warmed up to 1650～1750 ℃ of following insulations 1～4 hour then, feeds flowing nitrogen in the sintering process all the time, last furnace cooling promptly obtains aluminum nitride porous ceramic.
6. as the preparation method of aluminum nitride porous ceramic as described in the claim 5, it is characterized in that the quality ratio of aluminum oxide and carbon black is 2～4 in the step (1).
7. as the preparation method of aluminum nitride porous ceramic as described in the claim 5, it is characterized in that described aluminum oxide, its Al
2O
3Content＞95% weight, median size is at 0.2～2 μ m; Described aln seed crystal, its AlN content＞95% weight, particle diameter d
50＜1.2 μ m; Described carbon black, its C content＞95% weight, particle diameter d50＜80nm.
8. as the preparation method of aluminum nitride porous ceramic as described in the claim 5, it is characterized in that described Ia family oxide compound is Li
2O; Described IIa family oxide compound is MgO; Described IIIa family oxide compound is B
2O
3; Described rare earth oxide is Yb
2O
3, Lu
2O
3, La
2O
3Or Y
2O
3Described fluorochemical is YF
3Or CaF
2
9. as the preparation method of aluminum nitride porous ceramic as described in the claim 5, it is characterized in that nitrogen atmosphere pressure is＞1 normal atmosphere in the described step (4); The flow of flowing nitrogen is 3L/min; Described being rapidly heated is that heat-up rate with 20 ℃/min carries out; Heat up at a slow speed is that heat-up rate with 1.6 ℃/min carries out.
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| CN105084904A (en) * | 2015-08-10 | 2015-11-25 | 哈尔滨工业大学 | Preparing method for aluminum nitride ceramic material |
| CN104968601B (en) * | 2013-02-04 | 2018-02-16 | 德山株式会社 | The manufacture method of aluminium nitride sintered particles |
| CN110194441A (en) * | 2019-05-29 | 2019-09-03 | 北京科技大学 | The preparation method of hollow ball shape aluminium nitride powder material and aluminum nitride porous ceramic |
| CN110903092A (en) * | 2019-12-13 | 2020-03-24 | 苏州纳迪微电子有限公司 | High-purity porous AlN ceramic and preparation method thereof |
| CN111825066A (en) * | 2020-07-31 | 2020-10-27 | 山东恒晶新材料有限公司 | Preparation method of autocatalytic high-purity aluminum nitride |
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| CN115745623A (en) * | 2022-11-23 | 2023-03-07 | 郑州大学 | Aluminum nitride composite material, preparation method and application thereof |
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| CN104968601B (en) * | 2013-02-04 | 2018-02-16 | 德山株式会社 | The manufacture method of aluminium nitride sintered particles |
| CN105084904A (en) * | 2015-08-10 | 2015-11-25 | 哈尔滨工业大学 | Preparing method for aluminum nitride ceramic material |
| CN110194441A (en) * | 2019-05-29 | 2019-09-03 | 北京科技大学 | The preparation method of hollow ball shape aluminium nitride powder material and aluminum nitride porous ceramic |
| CN110903092A (en) * | 2019-12-13 | 2020-03-24 | 苏州纳迪微电子有限公司 | High-purity porous AlN ceramic and preparation method thereof |
| CN111825066A (en) * | 2020-07-31 | 2020-10-27 | 山东恒晶新材料有限公司 | Preparation method of autocatalytic high-purity aluminum nitride |
| CN113045320A (en) * | 2021-03-04 | 2021-06-29 | 杭州安誉科技有限公司 | High-heat-dissipation metal substrate for LED and preparation method thereof |
| CN113045320B (en) * | 2021-03-04 | 2022-08-09 | 杭州安誉科技有限公司 | High-heat-dissipation metal substrate for LED and preparation method thereof |
| CN116410001A (en) * | 2021-12-31 | 2023-07-11 | 江苏博睿光电股份有限公司 | Substrate, preparation method and application |
| CN114506828A (en) * | 2022-01-19 | 2022-05-17 | 福建华清电子材料科技有限公司 | Low-cost aluminum nitride powder preparation process |
| CN114506828B (en) * | 2022-01-19 | 2024-02-27 | 福建华清电子材料科技有限公司 | Low-cost aluminum nitride powder preparation process |
| CN115141022A (en) * | 2022-07-28 | 2022-10-04 | 江苏正力新能电池技术有限公司 | Preparation method of porous ceramic bottom supporting plate, porous ceramic bottom supporting plate and battery |
| CN115745623A (en) * | 2022-11-23 | 2023-03-07 | 郑州大学 | Aluminum nitride composite material, preparation method and application thereof |
| CN115745623B (en) * | 2022-11-23 | 2024-02-06 | 郑州大学 | Aluminum nitride composite material, preparation method and application thereof |
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Application publication date: 20100616 |