CN103880435A - Microwave rapid sintering method for high-quality aluminum nitride ceramic substrates - Google Patents
Microwave rapid sintering method for high-quality aluminum nitride ceramic substrates Download PDFInfo
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Abstract
The invention discloses a microwave rapid sintering method for high-quality aluminum nitride ceramic substrates. The method belongs to microwave firing of ceramic materials and comprises the following steps: after discharging glue, putting aluminum nitride ceramic substrate blanks into an auxiliary heating insulation structure in a microwave sintering cavity, uniformly spraying boron nitride powder among the blanks, wherein the aluminum nitride ceramic substrate blanks are overlapped orderly and the auxiliary heating insulation structure comprises an aluminum nitride fiber plate, a boron nitride sagger and a high-purity graphite plate; sintering in a nitride atmosphere containing 6-10% of hydrogen under the conditions that the microwave sintering frequency is 2.45GHz, the normal-pressure microwave sintering temperature is 1700-1750 DEG C and the heating rate is 8-10 DEG C per minute; preserving the heat for two hours, cooling along with a furnace, opening the furnace and taking out the aluminum nitride ceramic substrate blanks when the temperature is below 400 DEG C, thus obtaining high-quality aluminum nitride ceramic substrate sintering bodies which are small in deformation and has a heat conductivity being greater than 150W/(m K). Different from a conventional methods adopting a convection, conduction or radiation heating manner, the method adopts a heating manner that the microwave with a special waveband is used to be coupled with basic structures of the materials so as to generate heat and the materials are heated completely by adopting medium loss of the materials; and in combination with special microwave sintering structures and sintering process, the method is capable of rapidly and uniformly sintering the materials and has the advantages of low sintering temperature, short time, low energy consumption, high quality and high efficiency.
Description
Technical field
The present invention relates to a kind of sintering method of ceramic aluminium nitride ceramics, particularly relate to a kind of Rapid Microwave Sintering method of high quality aluminium nitride ceramic substrate.
Background technology
Aluminium nitride ceramics is a kind of new ceramic material growing up in recent years, because its thermal conductivity is high and good insulation preformance has a wide range of applications it in a lot of fields, its good thermal characteristics, mechanical property make it be used as high heat-radiating substrate in fields such as high power package and multi-chip assemblings, there is greatly the trend that replaces beryllium oxide, silicon carbide and aluminum oxide, have broad application prospects in fields such as microelectronics, photoelectron, power electronics and power electronics.From growth rate of market, it is one of fastest-rising stupalith of existing market, according to Keramont corporate statistics, the demand increase rate of the aluminium nitride chip of Europe, the United States, Deng state is respectively 60%, 80% and 40%, and the growth rate of market of encapsulation approaches 100%.At home, the market requirement of aluminium nitride chip is also in sharp increase.
Aluminium nitride ceramics is as a kind of novel high heat conduction non-oxide ceramic material, and at present domestic also do not have for maturation process and the processing unit used for reference, to report little abroad to AlN synthesis technology yet.Aluminium nitride ceramics is a kind of non-oxidized substance material of hard-to-sinter, at high temperature without fusing point, directly distillation, the sintering of aluminium nitride ceramics conventionally adopt add sintering aid normal pressure-sintered or under the hot pressing condition of high-temperature pressurizing sintering form.The equipment cost of hot pressed sintering is high and once sintered amount is less, and the sintering period is long and sintering loss is larger, causes the high expensive of aluminium nitride ceramic substrate, is difficult to adapt to fierce market competition.Normal pressure-sintered required equipment is relatively simple, and production cost is low, but sintering temperature is high, yielding, is difficult for densification, causes the quality of aluminium nitride ceramic substrate to ensure.
Summary of the invention
The technical problem to be solved in the present invention is, the defect existing for prior art, a kind of flash sintering method of new high quality aluminium nitride ceramic substrate is proposed, adopt this method, can accelerate sintering process, within lower temperature, shorter time, under normal pressure, sintering goes out fine and close high quality aluminium nitride ceramic substrate.Have heat-up rate fast, sintering temperature is low, and soaking time is short, better performances, and save energy, the feature that production efficiency is high, is applicable to scale operation.
Technical solution of the present invention is, the flash sintering method of described high quality aluminium nitride ceramic substrate is: the auxiliary hot insulation construction of the aluminium nitride ceramic substrate base substrate after binder removal being put into microwave sintering chamber, stack neat, between sheet and sheet, sprinkle uniformly boron nitride powder, auxiliary hot insulation construction is by sapphire whisker plate, boron nitride saggar and high purity graphite plate form, microwave sintering frequency is 2.45GHz, pass into hydrogeneous 6～10% nitrogen atmosphere, 1700～1750 ℃ of normal pressure microwave sintering temperatures, temperature rise rate is 8～10 ℃/min, be incubated 2 hours, furnace cooling, blow-on is taken out to below 400 ℃ time, obtain fine and close high quality aluminium nitride ceramic substrate sintered compact.
Principle of work of the present invention is: utilize micro-wave energy to be converted into kinetic energy and the heat energy of molecule, with a kind of " mode of body heating " overall homogeneous heating, not yielding, and due to the activation performance of microwave, at lower temperature dense sintering aluminium nitride ceramic substrate, cost significantly declines, then in conjunction with the microwave reflection effect of high purity graphite plate and exciting of reducing atmosphere, purify at the crystal boundary in sintering later stage by hydrogeneous nitrogen atmosphere, finally obtain high-quality aluminium nitride ceramic substrate.
The invention has the beneficial effects as follows, microwave sintering is to utilize microwave heating to carry out sintering to material, it is with traditional type of heating difference, traditional heating is to rely on heating that heat energy is passed to heated material by convection current, conduction or method of radiating to reach a certain temperature, heat transmits from outside to inside, sintering time is long, and energy consumption is high; And microwave sintering is utilize the basic structure coupling of special wave band that microwave has and material and produce heat, the dielectric loss of material makes a kind of type of heating of its material monolithic heating, again in conjunction with special microwave sintering structure and sintering process Quick uniform sintering, thereby there are a series of advantages such as sintering temperature is low, soaking time is short, improve sintering environment, energy consumption is low.Therefore the efficiency of microwave heating is high, than traditional method power saving 30～70%, greatly reduce production cost, and industrial microwave oven is simple in structure, automatic operating, is easy to safeguard.
Accompanying drawing explanation
In order to be illustrated more clearly in embodiments of the invention, to needing the accompanying drawing using to do simple introduction in embodiment, apparently, accompanying drawing described below is only some embodiments of the present invention, can not think the restriction to protection scope of the present invention below.
Fig. 1 is schematic diagram when sintering in the microwave oven of aluminium nitride ceramic substrate in the Rapid Microwave Sintering method of high quality aluminium nitride ceramic substrate of the embodiment of the present invention.
Embodiment
Aluminium nitride ceramic substrate base substrate after binder removal is put into the auxiliary hot insulation construction in microwave sintering chamber, stacked neatly, between sheet and sheet, sprinkle uniformly boron nitride powder.The overall dimension of aluminium nitride ceramic substrate base substrate is no more than 150mm.Microwave sintering chamber is similar spherical or cylindrical shape cavity, and at the uniform velocity rotates with the speed of 30 turn/min.Auxiliary hot insulation construction is made up of sapphire whisker plate, boron nitride saggar and high purity graphite plate, as shown in Figure 1, high purity graphite plate overall dimension is consistent with the overall dimension of aluminium nitride ceramic substrate base substrate, can cover whole aluminium nitride ceramic substrate base substrate, and upper graphite cake is directly pressed on aluminium nitride ceramic substrate base substrate, the distance range between two blocks of high purity graphite plates is that graphite cake maximum sized 1/2 is to graphite cake overall dimension.Microwave sintering frequency is 2.45GHz, passes into hydrogeneous 6～10% nitrogen atmosphere, 1700～1750 ℃ of normal pressure microwave sintering temperatures, temperature rise rate is 8～10 ℃/min, is incubated 2 hours, furnace cooling, blow-on is taken out to below 400 ℃ time, obtains fine and close high quality aluminium nitride ceramic substrate sintered compact.
Below in conjunction with embodiment, the invention will be further described.
embodiment 1:
Aluminium nitride ceramic substrate base substrate 1 after binder removal is put into the auxiliary hot insulation construction in microwave sintering chamber, stack neat, between sheet and sheet, sprinkle uniformly boron nitride powder, aluminium nitride ceramic substrate base substrate 1 is of a size of 150mm × 150mm × 3mm, microwave sintering chamber is spherical cavity, at the uniform velocity rotates with the speed of 30 turn/min.Auxiliary hot insulation construction is made up of sapphire whisker plate 2, boron nitride saggar 3 and high purity graphite plate 4, as shown in Figure 1, the inside dimension of boron nitride saggar 3 is 180mm × 180mm × 100mm, high purity graphite plate 4 is of a size of 150mm × 150mm × 8mm, distance between upper and lower graphite cake is 75mm, and upper graphite cake is directly pressed on aluminium nitride ceramic substrate base substrate 1.Microwave sintering frequency is 2.45GHz, passes into hydrogeneous 10% nitrogen atmosphere, 1750 ℃ of normal pressure microwave sintering temperatures, temperature rise rate is 10 ℃/min, is incubated 2 hours, furnace cooling, blow-on is taken out to below 400 ℃ time, obtains fine and close high quality aluminium nitride ceramic substrate sintered compact.The density of the aluminium nitride ceramic substrate making after measured, is 3.26g/cm
3, bending strength is 448MPa, and thermal conductivity is 178 W/ (mK), and sintering rear surface is highly polished, is light yellow, color even.
embodiment 2:
Aluminium nitride ceramic substrate base substrate 1 after binder removal is put into the auxiliary hot insulation construction in microwave sintering chamber, stack neat, between sheet and sheet, sprinkle uniformly boron nitride powder, aluminium nitride ceramic substrate base substrate is of a size of Φ 80mm × 2mm, microwave sintering chamber is circular cylindrical cavity, at the uniform velocity rotates with the speed of 30 turn/min.Auxiliary hot insulation construction is made up of sapphire whisker plate 2, boron nitride saggar 3 and high purity graphite plate 4, as shown in Figure 1, the inside dimension of boron nitride saggar 3 is Φ 100mm × 60mm, high purity graphite plate 4 is of a size of Φ 80mm × 5mm, distance between upper and lower graphite cake is 40mm, and upper graphite cake is directly pressed on aluminium nitride ceramic substrate base substrate.Microwave sintering frequency is 2.45GHz, passes into hydrogeneous 6% nitrogen atmosphere, 1700 ℃ of normal pressure microwave sintering temperatures, temperature rise rate is 8 ℃/min, is incubated 2 hours, furnace cooling, blow-on is taken out to below 400 ℃ time, obtains fine and close high quality aluminium nitride ceramic substrate sintered compact.The density of the aluminium nitride ceramic substrate making after measured, is 3.25g/cm
3, bending strength is 396MPa, and thermal conductivity is 152 W/ (mK), and sintering rear surface is highly polished, is light yellow, color even.
Claims (4)
1. the Rapid Microwave Sintering method of a high quality aluminium nitride ceramic substrate, it is characterized in that, aluminium nitride ceramic substrate base substrate after binder removal is put into the auxiliary hot insulation construction in microwave sintering chamber, stack neat, between sheet and sheet, sprinkle uniformly boron nitride powder, auxiliary hot insulation construction is by sapphire whisker plate, boron nitride saggar and high purity graphite plate form, microwave sintering frequency is 2.45GHz, pass into hydrogeneous 6～10% nitrogen atmosphere, 1700～1750 ℃ of normal pressure microwave sintering temperatures, temperature rise rate is 8～10 ℃/min, be incubated 2 hours, furnace cooling, blow-on is taken out to below 400 ℃ time, obtain fine and close high quality aluminium nitride ceramic substrate sintered compact.
2. the Rapid Microwave Sintering method of high quality aluminium nitride ceramic substrate according to claim 1, is characterized in that, the overall dimension of described aluminium nitride ceramic substrate base substrate is no more than 150mm.
3. the Rapid Microwave Sintering method of high quality aluminium nitride ceramic substrate according to claim 1, is characterized in that, described microwave sintering chamber is similar spherical or cylindrical shape cavity, and at the uniform velocity rotates with the speed of 30 turn/min.
4. the Rapid Microwave Sintering method of high quality aluminium nitride ceramic substrate according to claim 1, it is characterized in that, described high purity graphite plate overall dimension is consistent with the overall dimension of aluminium nitride ceramic substrate base substrate, can cover whole aluminium nitride ceramic substrate base substrate, and upper graphite cake is directly pressed on aluminium nitride ceramic substrate base substrate, the distance range between two blocks of high purity graphite plates is that graphite cake maximum sized 1/2 is to graphite cake overall dimension.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163640A (en) * | 2014-07-22 | 2014-11-26 | 衡阳凯新陶瓷科技有限公司 | Microwave sintering preparation method of high purity silicon nitride ceramic lift tube for low-pressure casting |
| CN109987944A (en) * | 2019-03-06 | 2019-07-09 | 清华大学 | A kind of high thermal conductivity silicon nitride ceramic substrate and preparation method thereof |
| CN112212693A (en) * | 2019-07-09 | 2021-01-12 | 郑州大学 | Microwave glue removing method for paster electronic element blank |
| CN112759401A (en) * | 2020-12-02 | 2021-05-07 | 兆山科技（北京）有限公司 | Method for preparing high-entropy boron ceramic surface material by microwave sintering |
| CN115321993A (en) * | 2022-10-17 | 2022-11-11 | 江苏富乐华功率半导体研究院有限公司 | Method for quickly discharging PVB (polyvinyl butyral) adhesive from ceramic body |
| WO2023184934A1 (en) * | 2022-04-02 | 2023-10-05 | 中材高新氮化物陶瓷有限公司 | Dynamic sintering method for nitride ceramic substrate |
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2014
- 2014-04-04 CN CN201410133055.XA patent/CN103880435A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163640A (en) * | 2014-07-22 | 2014-11-26 | 衡阳凯新陶瓷科技有限公司 | Microwave sintering preparation method of high purity silicon nitride ceramic lift tube for low-pressure casting |
| CN109987944A (en) * | 2019-03-06 | 2019-07-09 | 清华大学 | A kind of high thermal conductivity silicon nitride ceramic substrate and preparation method thereof |
| CN109987944B (en) * | 2019-03-06 | 2020-09-01 | 清华大学 | High-thermal-conductivity silicon nitride ceramic substrate and preparation method thereof |
| CN112212693A (en) * | 2019-07-09 | 2021-01-12 | 郑州大学 | Microwave glue removing method for paster electronic element blank |
| CN112759401A (en) * | 2020-12-02 | 2021-05-07 | 兆山科技（北京）有限公司 | Method for preparing high-entropy boron ceramic surface material by microwave sintering |
| WO2023184934A1 (en) * | 2022-04-02 | 2023-10-05 | 中材高新氮化物陶瓷有限公司 | Dynamic sintering method for nitride ceramic substrate |
| CN115321993A (en) * | 2022-10-17 | 2022-11-11 | 江苏富乐华功率半导体研究院有限公司 | Method for quickly discharging PVB (polyvinyl butyral) adhesive from ceramic body |
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Application publication date: 20140625 |