CN1648103A - Method of preparing high dielectric constant AL203 base ceramics with power regulating laser - Google Patents

Method of preparing high dielectric constant AL203 base ceramics with power regulating laser Download PDF

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Publication number
CN1648103A
CN1648103A CN 200510000295 CN200510000295A CN1648103A CN 1648103 A CN1648103 A CN 1648103A CN 200510000295 CN200510000295 CN 200510000295 CN 200510000295 A CN200510000295 A CN 200510000295A CN 1648103 A CN1648103 A CN 1648103A
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China
Prior art keywords
laser
sintering
pottery
dielectric constant
ceramic
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Chinese (zh)
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蒋毅坚
于振龙
王伟
季凌飞
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The present invention is the preparation process of high dielectric constant Al2O3 base ceramic with power regulating laser, and belongs to the field of ceramic material preparing technology. The present invention features using great laser as heat source for preparing the ceramic material, and the production process includes the following steps: setting Al2O3 ceramic blank on rotary work bench, raising laser power from 0 to 630-1030 w/sq cm in 30-60 s for sintering, sintering for 60-300 s, lowering the laser power to initial value in 60-300 s, turning off laser and cooling to form ceramic. Compared with common furnace sintering process, the said process has obviously raised dielectric constant of the Al2O3 base ceramic product, short preparation time, easy control of process, high technological repeatability, no pollution in sintering, and high purity of product.

Description

High-k Al 2O 3The regulating power laser preparation method of base pottery
Technical field:
The invention belongs to Al 2O 3The preparation field of base ceramic material.
Background technology:
At present, capacitance density and reliability requirement to capacitor element in the microelectronics technology are more and more higher, the SiO that commonly uses in the existing technology 2Material, its relative dielectric constant is about 6, the limit effect that lower dielectric constant can cause device to produce because specification further dwindles, grievous injury device reliability.Al 2O 3The relative dielectric constant of pottery is about 10, and cheap, is widely used in microelectronic.Preparation Al 2O 3The ceramic existing technology of base adopts the sintering furnace sintering technology more.
At present, existing technology adopts the sintering furnace sintering processing to prepare Al more 2O 3The base pottery, the Al of preparation 2O 3The relative dielectric constant of pottery is about 10, and sintering time is longer, needs a few hours at least; Sintering process is wayward; Contaminating impurity when easily causing high temperature sintering.
Summary of the invention:
The object of the present invention is to provide a kind of high-k Al 2O 3The regulating power laser preparation method of base pottery adopts high power laser as heating source, to regulate laser power and to be aided with the mode of rotary table, prepares fast the Al with high-k 2O 3The base pottery.
The present invention is achieved by the following technical solutions:
(1) with Al 2O 3The base ceramic body places on the rotary table, makes laser power density reach 630-1030w/cm in the time of 30-60s 2, begin simultaneously sintering;
(2) through behind the sintering of 60-300s, reducing continuously laser power density in the time of 60-300s is zero;
(3) laser closes light, and sample is cooled to porcelain.
The rotating speed of the rotary table in the whole process of preparation is 10 ° of-50 °/s.
Described Al 2O 3The base pottery is Al 2O 3Pottery or (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Pottery.
Compared with prior art, the invention has the beneficial effects as follows:
1. adopt the Al of this method preparation 2O 3The dielectric constant of base pottery significantly improves, especially with Al 2O 3Pottery and (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006The change in dielectric constant of pottery is the most remarkable.The Al of conventional sintering 2O 3Pottery and (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006The dielectric constant mean value of pottery is respectively 9.8 and 10.5.And the Al after laser sintered 2O 3The dielectric constant mean value of pottery is 14.2, (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006The dielectric constant mean value of pottery is 34.3, and dielectric loss factor mean value is respectively 0.0039 and 0.1636.
2. because the beam quality of laser instrument and inhomogeneous, all the light cost is higher if laser beam carried out, and adopts rotary table can avoid the inhomogeneous problem of beam quality, effect is relatively good in experiment, find in the experiment that when turntable speed was 10 ° of-50 °/s, effect was better.
3. preparation time is short, and preparation efficiency improves greatly.
4. carry out under preparation technology's normal condition, process controllability is strong, and repeatability is high.
5. owing to do not need crucible, the pottery preparation is pollution-free, preparation sample purity height.
Embodiment
Laser provided by the invention prepares high-k Al 2O 3The method of base pottery is carried out at normal temperatures; Adopt the dielectric properties of HP4284ALCR fine measuring instrument specimen under 25 ℃ of conditions, test frequency is 1MHz, and the dielectric properties measurement result sees Table 1.
Table 1 classify prepares high-k Al by the present invention 2O 3The dielectric properties of the technological parameter of base pottery and response sample.Wherein embodiment 9, and embodiment 10 is Al 2O 3Pottery, all the other embodiment are (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Pottery.
The laser apparatus that the present invention uses is German Rofin-sina RS2500 CO 2Laser apparatus.
With Al 2O 3The base ceramic body places on the rotary table, makes laser power density reach 630-1030w/cm in the time of 30-60s 2, begin simultaneously sintering; Through behind the sintering of 60-300s, reducing continuously laser power density in the time of 60-300s is zero; Laser closes light, and sample is cooled to porcelain.The rotating speed of rotary table is 10 ° of-50 °/s in the sintering process.
Embodiment 1
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 60s, laser power density is brought up to sintering power density values 850w/cm continuously from 0 2, the rotary table rotating speed is 50 °/s, through behind the sintering time of 90s, reduces then laser power to zero in 60s; Laser closes light.Sample is cooled to porcelain.
Embodiment 2
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 60s, laser power density is brought up to sintering power density values 850w/cm continuously from zero 2, the rotary table rotating speed is 50 °/s, through behind the sintering time of 300s, reduces then laser power to zero in 300s; Laser closes light.Sample is cooled to porcelain.
Embodiment 3
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 30s, laser power density is brought up to sintering power density values 630w/cm continuously from zero 2, the rotary table rotating speed is 25 °/s, through behind the sintering time of 150s, reduces then laser power to zero in 150s; Laser closes light.Sample is cooled to porcelain.
Embodiment 4
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 40s, laser power density is brought up to sintering power density values 1030w/cm continuously from zero 2, the rotary table rotating speed is 25 °/s, through behind the sintering time of 210s, reduces then laser power to zero in 180s; Laser closes light.Sample is cooled to porcelain.
Embodiment 5
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 50s, laser power density is brought up to sintering power density values 1030w/cm continuously from zero 2, the rotary table rotating speed is 50 °/s, through behind the sintering time of 300s, reduces then laser power to zero in 60s; Laser closes light.Sample is cooled to porcelain.
Embodiment 6
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 60s, laser power density is brought up to sintering power density values 630w/cm continuously from zero 2, the rotary table rotating speed is 10 °/s, through behind the sintering time of 300s, reduces then laser power to zero in 300s; Laser closes light.Sample is cooled to porcelain.
Embodiment 7
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 30s, laser power density is brought up to sintering power density values 750w/cm continuously from zero 2, the rotary table rotating speed is 10 °/s, through behind the sintering time of 180s, reduces then laser power to zero in 210s; Laser closes light.Sample is cooled to porcelain.
Embodiment 8
Adopt German Rofin-sina RS2500 laser illumination (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Ceramic body; At first in 45s, laser power density is brought up to sintering power density values 950w/cm continuously from zero 2, the rotary table rotating speed is 25 °/s, through behind the sintering time of 60s, reduces then laser power to zero in 250s; Laser closes light.Sample is cooled to porcelain.
Embodiment 9
Adopt German Rofin-sina RS2500 laser illumination Al 2O 3Ceramic body; At first in 40s, laser power density is brought up to sintering power density values 900w/cm continuously from zero 2, the rotary table rotating speed is 10 °/s, through behind the sintering time of 180s, reduces then laser power to zero in 300s; Laser closes light.Sample is cooled to porcelain.
Embodiment 10
Adopt German Rofin-sina RS2500 laser illumination Al 2O 3Ceramic body; At first in 50s, laser power density is brought up to sintering power density values 900w/cm continuously from zero 2, the rotary table rotating speed is 25 °/s, through behind the sintering time of 210s, reduces then laser power to zero in 240s; Laser closes light.Sample is cooled to porcelain.
Table 1 is regulated power laser and is prepared Al 2O 3The processing parameter and the sample dielectric properties of base pottery
Embodiment Sintering power density w/cm 2 Improve power time s Sintering time s Reduce power time s Turntable speed °/s Specific inductivity Dielectric loss factor
1 ??850 ??60 ??90 ??60 ??50 ??33.322 ??0.1630
2 ??850 ??60 ??300 ??300 ??50 ??34.211 ??0.1521
3 ??630 ??30 ??150 ??150 ??25 ??33.234 ??0.1431
4 ??1030 ??40 ??210 ??180 ??25 ??34.189 ??0.1580
5 ??1030 ??50 ??300 ??60 ??50 ??34.174 ??0.1621
6 ??630 ??60 ??300 ??300 ??10 ??33.752 ??0.1623
7 ??750 ??30 ??180 ??210 ??10 ??33.840 ??0.1589
8 ??950 ??45 ??60 ??250 ??25 ??33.568 ??0.1596
9 ??900 ??40 ??180 ??300 ??10 ??14.240 ??0.0038
10 ??1030 ??50 ??210 ??240 ??25 ??14.246 ??0.0039

Claims (3)

1. high-k Al 2O 3The regulating power laser preparation method of base pottery is characterized in that it may further comprise the steps:
(1) with Al 2O 3The base ceramic body places on the rotary table, makes laser power density rise to 630-1030w/cm in the time of 30-60s 2, begin simultaneously sintering;
(2) through behind the sintering of 60-300s, reducing laser power close in the time of 60-300s is zero;
(3) laser closes light, and sample is cooled to porcelain.
2. high-k Al according to claim 1 2O 3The regulating power laser preparation method of base pottery is characterized in that the rotating speed of the rotary table in the whole preparation process is 10 ° of-50 °/s.
3. high-k Al according to claim 1 2O 3The regulating power laser preparation method of base pottery is characterized in that described Al 2O 3The base pottery is Al 2O 3Pottery or (Al 2O 3) 0.988(Fe 2O 3) 0.006(FeTiO 3) 0.006Pottery.
CN 200510000295 2005-01-10 2005-01-10 Method of preparing high dielectric constant AL203 base ceramics with power regulating laser Pending CN1648103A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101845652A (en) * 2010-03-17 2010-09-29 中国船舶重工集团公司第十二研究所 Method for preparing micro-arc oxide film layer
CN103771835A (en) * 2012-10-24 2014-05-07 天津城市建设学院 Hot pressure casting moulding method of laser pumping cavity Al2O3 ceramic reflector

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101845652A (en) * 2010-03-17 2010-09-29 中国船舶重工集团公司第十二研究所 Method for preparing micro-arc oxide film layer
CN101845652B (en) * 2010-03-17 2012-01-11 中国船舶重工集团公司第十二研究所 Method for preparing micro-arc oxide film layer
CN103771835A (en) * 2012-10-24 2014-05-07 天津城市建设学院 Hot pressure casting moulding method of laser pumping cavity Al2O3 ceramic reflector

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