CN1176047C - Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics - Google Patents

Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics Download PDF

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Publication number
CN1176047C
CN1176047C CNB031482449A CN03148244A CN1176047C CN 1176047 C CN1176047 C CN 1176047C CN B031482449 A CNB031482449 A CN B031482449A CN 03148244 A CN03148244 A CN 03148244A CN 1176047 C CN1176047 C CN 1176047C
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laser
power density
sintering
continuously
initial value
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CN1460657A (en
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蒋毅坚
季凌飞
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Chengdu 3D Change Technology Co., Ltd.
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Beijing University of Technology
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Abstract

The present invention relates to a continuously adjustable and controllable power laser preparation method for high-dielectric constant Ta2O5 base ceramic, which belongs to the field of the preparation of ceramic materials. The present invention is characterized in that the present invention comprises: a high-power laser is used as a direct irradiation source to irradiate a Ta2O5 base ceramic body in an in-situ or scanning way, and the laser power density is continuously increased to the sintering power density value 640 to 1062 w/cm<2> from an initial value 20 to 40 w/cm<2> within the time of 10 to 60 seconds to start sintering; the laser power density value is continuously reduced to the initial value within the time of 10 to 60 seconds after the sintering for 3 to 60 seconds; Lasers are closed and samples are cooled into ceramic. The Ta2O5 base ceramic prepared by the present invention obviously enhance the dielectric constant, and the present invention has the advantages of less dielectric loss, short preparation time, easy control of process, high process repeatability, sintering without pollution, and high purity of prepared samples.

Description

The laser that adopts power to regulate and control continuously prepares high-k Ta 2O 5The method of base pottery
Technical field
The invention belongs to Ta 2O 5The preparation field of base ceramic material.
Background technology
At present, more and more higher in the microelectronics technology to the requirement of capacitor element capacitance density and reliability, the SiO that uses always in the existing technology 2Material, its relative permittivity is about 6, the limit effect that lower specific inductivity can cause device to produce because of specification further dwindles, the reliability of grievous injury device, the needs searching is a kind of to have the novel material of high-k to adapt to the development need of capacitor element microminiaturization.Ta 2O 5The relative dielectric constant of pottery is about 36, simultaneously, and than other dielectric material, Ta 2O 5Have and microelectronic processing technology compatible characteristics mutually, make it become the first-selected new material of development high-performance topographically elevated microelectronic capacitor spare of future generation.Preparation Ta 2O 5The existing technology of base pottery adopts the sintering furnace sintering technology more, and improves Ta by the method for doping vario-property 2O 5Dielectric constant, similarly bibliographical information is a lot of, " Enhancement of thedielectric constant of Ta among for example " NATURE " (" nature ") magazine nineteen ninety-five vol.377 2O 5Through substitution with TiO 2" (" by doped Ti O 2Improve Ta 2O 5Dielectric constant ") R.F.Cava that introduced U.S. AT﹠T Labs in the literary composition is by at Ta 2O 5Middle doping 8%TiO 2, make its dielectric constant be increased to 126.2 by 35.4.At existing Ta 2O 5In the base ceramics processing, sintering time needs a few hours usually at least, and sintering process is wayward, is difficult for obtaining Ta in the sintered sample 2O 5High dielectric phase in the ceramic phasor of base.
At present, existing technology adopts the sintering furnace sintering processing to prepare Ta more 2O 5The base pottery, prepared Ta 2O 5The relative dielectric constant of pottery is about 36, (Ta 2O 5) 0.92(TiO 2) 0.08The relative dielectric constant of pottery is about 126.2; And sintering time is longer, usually needs a few hours at least; Sintering process is wayward; Need to use crucible during sintering, the contaminating impurity when easily causing high temperature sintering.
Summary of the invention
The object of the present invention is to provide a kind of laser that adopts power to regulate and control continuously to prepare high-k Ta 2O 5The method of base pottery adopts high power laser as mode original position or the scanning and irradiation Ta of direct irradiation bomb with continuous regulation and control laser power 2O 5The base ceramic body is prepared fast and is had the more Ta of high-k 2O 5The base pottery.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
(1) adopt high power laser as direct irradiation bomb original position or scanning and irradiation Ta 2O 5The base ceramic body, in the time of 10～60s with laser power density from initial value 20～40w/cm 2Bring up to continuously sintering power density values 640～1062w/cm 2, the beginning sintering;
(2) behind the sintering through 3～60s, in the time of 10～60s, reduce laser power density continuously to initial value;
(3) laser closes light, and sample is cooled to porcelain.
Laser scanning speed is 0～50mm/s in the whole process of preparation; Scanning speed is that 0 o'clock laser irradiation is original position irradiation.
Described Ta 2O 5The base pottery comprises Ta 2O 5Pottery or (Ta 2O 5) 0.92(TiO 2) 0.08Pottery.
Compared with prior art, the invention has the beneficial effects as follows:
1. adopt the Ta of method preparation of the present invention 2O 5The dielectric constant of base pottery significantly improves Ta 2O 5The dielectric constant mean value of pottery is 61.6, (Ta 2O 5) 0.92(TiO 2) 0.08The dielectric constant mean value of pottery is 421.2, and dielectric loss factor mean value is 0.022, the dielectric properties of sample be improved significantly.
2. preparation time is short, and the average laser sintering time is 121s (the laser sintered time average of embodiment), and preparation efficiency improves greatly.
3. carry out under preparation technology's normal temperature, process controllability is strong, repeatability is high.
4. realize the pollution-free sintering of high-melting-point pottery, preparation sample purity height.
Embodiment
Be described in further detail below in conjunction with table 1 pair the specific embodiment of the present invention.
Laser provided by the invention prepares high-k Ta 2O 5The method of base pottery is carried out at normal temperatures; Adopt the dielectric properties of HP4284ALCR precision aid specimen under 25 ℃ of conditions, test frequency is 1MHz, and the dielectric properties measurement result sees Table 1.
Table 1 classify prepares high-k Ta by the present invention 2O 5The technological parameter of base pottery and the dielectric properties of respective sample.Wherein embodiment 15 to 18 is (Ta 2O 5) 0.92(TiO 2) 0.08Pottery, all the other embodiment are Ta 2O 5Pottery.
Adopt high power laser as mode original position or the scanning and irradiation Ta of direct irradiation bomb with continuous regulation and control laser power 2O 5The base ceramic body, at first in the time of 10～60s with laser power density from 20～40w/cm 2Initial value bring up to continuously 640～1062w/cm 2Carry out sintering, behind the sintering time through 3～60s, reduce continuously laser power to initial value in the time of 10～60s, laser closes light, and sample is cooled to porcelain.Laser scanning speed is 0～50mm/s in the irradiation process, and laser scanning speed is that 0 o'clock irradiation is meant original position irradiation.
Embodiment 1
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 850w/cm 2, this stage laser scanning speed is 2mm/s; Changing then laser scanning speed is 33mm/s, through behind the sintering time of 30s, reduces continuously laser power density to initial value in 60s again, and the laser scanning speed that power density reduces the stage is 2mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 2
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 850w/cm 2Through behind the sintering time of 10s, in 60s, reduce continuously again laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 2mm/s in the whole irradiation process.
Embodiment 3
Adopt high power laser as direct irradiation bomb original position irradiation Ta 2O 5Ceramic body.At first in 60s with laser power density from initial value 31w/cm 2Bring up to continuously sintering power density values 850w/cm 2Through behind the sintering time of 5s, in 60s, reduce continuously again laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 0mm/s in the whole irradiation process.
Embodiment 4
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 10s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 956w/cm 2Through behind the sintering time of 10s, in 10s, reduce continuously laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 17mm/s in the whole irradiation process.
Embodiment 5
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 10s with laser power density from initial value 31w/cm 2Bring up to continuously sintering power density values 1062w/cm 2, this stage laser scanning speed is 17mm/s; Changing then laser scanning speed is 33mm/s, through behind the sintering time of 5s, reduces continuously laser power density to initial value in 10s again, and the laser scanning speed that power density reduces the stage is 17mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 6
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 10s with laser power density from initial value 25w/cm 2Bring up to continuously sintering power density values 925w/cm 2, this stage laser scanning speed is 8mm/s; Changing then laser scanning speed is 33mm/s, through behind the sintering time of 3s, reduces continuously laser power density to initial value in 10s again, and the laser scanning speed that power density reduces the stage is 8mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 7
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 850w/cm 2, this stage laser scanning speed is 50mm/s; Changing then laser scanning speed is 33mm/s, through behind the sintering time of 30s, reduces continuously laser power density to initial value in 60s again, and the laser scanning speed that power density reduces the stage is 50mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 8
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 670w/cm 2, this stage laser scanning speed is 50mm/s; Changing then laser scanning speed is 17mm/s, through behind the sintering time of 60s, reduces continuously laser power density to initial value in 60s again, and the laser scanning speed that power density reduces the stage is 50mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 9
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 40w/cm 2Bring up to continuously sintering power density values 825w/cm 2, this stage laser scanning speed is 33mm/s; Changing then laser scanning speed is 8mm/s, through behind the sintering time of 40s, reduces continuously laser power density to initial value in 60s again, and the laser scanning speed that power density reduces the stage is 33mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 10
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 25w/cm 2Bring up to continuously sintering power density values 720w/cm 2Through behind the sintering time of 60s, in 60s, reduce continuously again laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 50mm/s in the whole irradiation process.
Embodiment 11
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 25w/cm 2Bring up to continuously sintering power density values 720w/cm 2, this stage laser scanning speed is 50mm/s; Changing then laser scanning speed is 33mm/s, through behind the sintering time of 50s, reduces continuously laser power density to initial value in 60s again, and the laser scanning speed that power density reduces the stage is 50mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 12
Adopt high power laser as direct irradiation bomb original position irradiation Ta 2O 5Ceramic body.At first in 60s with laser power density from initial value 25w/cm 2Bring up to continuously sintering power density values 720w/cm 2Through behind the sintering time of 30s, in 60s, reduce continuously again laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 0mm/s in the whole irradiation process.
Embodiment 13
Adopt high power laser as direct irradiation bomb original position irradiation Ta 2O 5Ceramic body.At first in 60s with laser power density from initial value 40w/cm 2Bring up to continuously sintering power density values 825w/cm 2Through behind the sintering time of 50s, in 60s, reduce continuously laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 0mm/s in the whole irradiation process.
Embodiment 14
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta 2O 5Ceramic body: at first in 60s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 670w/cm 2, this stage laser scanning speed is 50mm/s; Changing then laser scanning speed is 33mm/s, through behind the sintering time of 50s, reduces continuously laser power density to initial value in 60s, and the laser scanning speed that power density reduces the stage is 50mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 15
Adopt high power laser as direct irradiation bomb scanning and irradiation (Ta 2O 5) 0.92(TiO 2) 0.08Ceramic body: at first in 20s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 850w/cm 2Through behind the sintering time of 20s, in 20s, reduce continuously laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 2mm/s in the whole irradiation process.
Embodiment 16
Adopt high power laser as direct irradiation bomb scanning and irradiation (Ta 2O 5) 0.92(TiO 2) 0.08Ceramic body: at first in 40s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 640w/cm 2Through behind the sintering time of 20s, in 20s, reduce continuously laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 8mm/s in the whole irradiation process.
Embodiment 17
Adopt high power laser as direct irradiation bomb scanning and irradiation (Ta 2O 5) 0.92(TiO 2) 0.08Ceramic body: at first in 20s with laser power density from initial value 31w/cm 2Bring up to continuously sintering power density values 850w/cm 2, this stage laser scanning speed is 2mm/s; Changing then laser scanning speed is 8mm/s, through behind the sintering time of 60s, reduces continuously laser power density to initial value in 10s, and the laser scanning speed that power density reduces the stage is 2mm/s; Laser closes light, and sample is cooled to porcelain.
Embodiment 18
Adopt high power laser as direct irradiation source original position irradiation (Ta 2O 5) 0.92(TiO 2) 0.08Ceramic body.At first in 20s with laser power density from initial value 20w/cm 2Bring up to continuously sintering power density values 640w/cm 2Through behind the sintering time of 45s, in 20s, reduce continuously laser power density to initial value; Laser closes light, and sample is cooled to porcelain.Laser scanning speed is 0mm/s in the whole irradiation process.
Each embodiment has all carried out the process repeatability test in the table 1, and number of repetition is greater than 3 times.Wherein, the replica test number of times of optimum process condition embodiment is 5～8 times: embodiment 15 and 16 replica test number of times are 5 times, and the replica test number of times of embodiment 1 to 3 is 8 times.The dielectric constant of listed each embodiment and dielectric loss factor are the mean value of each routine process repeatability result of the test in the table.
Table 1 regulation and control laser power continuously prepares high-k Ta 2O 5The processing parameter and the sample dielectric properties of base pottery
Embodiment Power density initial value w/cm 2 Sintering power density w/cm 2 Improve power time s Sintering time s Reduce power time s Improve power density laser scanning speed mm/s Laser sintered scanning speed mm/s Reduce power density laser scanning speed mm/s Specific inductivity Dielectric loss factor
1 20 850 60 30 60 2 33 2 75.8 0.021
2 20 850 60 10 60 2 2 2 73.3 0.018
3 31 850 60 5 60 0 0 0 70.3 0.024
4 20 956 10 10 10 17 17 17 68.0 0.016
5 31 1062 10 5 10 17 33 17 65.4 0.019
6 25 925 10 3 10 8 33 8 62.6 0.018
7 20 850 60 30 60 50 33 50 60.9 0.031
8 20 670 60 60 60 50 17 50 59.4 0.022
9 40 825 60 40 60 33 8 33 59.2 0.024
10 25 720 60 60 60 50 50 50 56.0 0.022
11 25 720 60 50 60 50 33 50 55.8 0.030
12 25 720 60 30 60 0 0 0 55.4 0.019
13 40 825 60 50 60 0 0 0 55.0 0.033
14 20 670 60 50 60 50 33 50 54.2 0.023
15 20 850 20 20 20 2 2 2 499.0 0.023
16 20 640 40 20 20 8 8 8 442.3 0.018
17 31 850 20 60 10 2 8 2 386.5 0.024
18 20 640 20 45 20 0 0 0 357.1 0.012

Claims (3)

1, a kind of laser that adopts power to regulate and control continuously prepares high-k Ta 2O 5The method of base pottery is characterized in that it may further comprise the steps:
(1) adopt high power laser as direct irradiation bomb original position or scanning and irradiation Ta 2O 5The base ceramic body, in the time of 10～60s with laser power density from initial value 20～40w/cm 2Bring up to continuously sintering power density values 640～1062w/cm 2, the beginning sintering;
(2) behind the sintering through 3～60s, in the time of 10～60s, reduce laser power density continuously to initial value;
(3) laser closes light, and sample is cooled to porcelain.
2, the laser of the continuous regulation and control of employing power according to claim 1 prepares high-k Ta 2O 5The method of base pottery is characterized in that the laser scanning speed in the whole preparation process is 0～50mm/s, and laser scanning speed is that 0 o'clock irradiation is original position irradiation.
3, the laser of the continuous regulation and control of employing power according to claim 1 prepares high-k Ta 2O 5The method of base pottery is characterized in that described Ta 2O 5The base pottery is Ta 2O 5Pottery or (Ta 2O 5) 0.92(TiO 2) 0.08Pottery.
CNB031482449A 2003-07-04 2003-07-04 Continuously adjustable and controllable power laser preparation method by using high dielectric constant Ta2O5 base ceramics Expired - Fee Related CN1176047C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100420653C (en) * 2006-12-15 2008-09-24 北京工业大学 Laser prepn process of potassium/sodium niobtae no-lead piezoelectric ceramic
CN101439968B (en) * 2008-12-26 2011-07-20 北京工业大学 Method for realizing (Ta2O5)1-x(TiO2)x based ceramic dielectric temperature coefficient thermal compensation
CN108359394A (en) * 2017-12-30 2018-08-03 凤阳力拓新型材料有限公司 A kind of processing method for copper coated foil plate nano silicon micronization
CN109760173B (en) * 2019-03-07 2020-11-20 西北工业大学 Wall-like Al2O3-GdAlO3-ZrO2Laser melting forming method of ternary eutectic ceramics
CN109721353A (en) * 2019-03-15 2019-05-07 上海朗研光电科技有限公司 A kind of preparation method of huge dielectric constant CCTO based film material

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