CN1480427A - Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant - Google Patents
Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant Download PDFInfo
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- CN1480427A CN1480427A CNA031482457A CN03148245A CN1480427A CN 1480427 A CN1480427 A CN 1480427A CN A031482457 A CNA031482457 A CN A031482457A CN 03148245 A CN03148245 A CN 03148245A CN 1480427 A CN1480427 A CN 1480427A
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- laser
- sintering
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- pottery
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Abstract
A process for preparing Ta2O5-base ceramics with high dielectric constant by instaneous regulation of laser power includes using high-power laser to irradiate the raw Ta2O5-base ceramics at 190-350 W/sq.cm of power density for 30-185 s in order to preheat it, instantaneously regulating the laser powre density to 850-1405 W/sq.cm, sintering it for 25-95s, and cooling. Its advantages are high dielectric constant, short period, easy control, and high purity of product.
Description
Technical field
The invention belongs to high-k Ta
2O
5The preparation field of base pottery.
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, compares and 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 technology of preparing of base pottery, 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 high-k Ta
2O
5The instantaneous regulation and control power laser preparation method of base pottery adopts high power laser as mode original position or the scanning and irradiation Ta of direct irradiation bomb with instantaneous 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 is with 190～350w/cm
2Low power density 30～185s in the time to Ta
2O
5The base ceramic body carries out the laser irradiation preheating;
2. after preheating finishes, regulate the instantaneous sintering power density values 850～1405w/cm that is raised to of laser power density
2, carry out sintering;
3. behind the sintering time through 25～95s, laser closes light, and sample is cooled to porcelain.
Scanning speed during the laser irradiation preheating is 0～33mm/s; Scanning speed during sintering is 0～50mm/s; 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 58.1, (Ta
2O
5)
0.92(TiO
2)
0.8The dielectric constant mean value of pottery is 397.25, and dielectric loss factor mean value is 0.020, the dielectric properties of sample be improved significantly.
2. preparation time is short, and the average laser sintering time is 76s (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 6, embodiment 7, embodiment 8, embodiment 9 are (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 instantaneous regulation and control laser power
2O
5The base ceramic body is at first with 190～350w/cm
2Low power density 30～185s in the time to Ta
2O
5The base ceramic body carries out the laser irradiation preheating, after preheating finishes, regulates the instantaneous sintering power density values 850～1405w/cm that is raised to of laser power density
2, behind the sintering time through 25～95s, laser closes light, and sample is cooled to porcelain.Scanning speed during the laser irradiation preheating is 0～33mm/s, and the scanning speed during sintering is 0～50mm/s, and scanning speed is that 0 o'clock laser irradiation is original position irradiation.
Embodiment 1
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta
2O
5Ceramic body: at first with 350w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 30s, this stage laser scanning speed is 33mm/s; After preheating finishes, regulate the instantaneous sintering power density values 1405w/cm that is raised to of laser power density
2, and to change laser scanning speed be 50mm/s, and through behind the sintering time of 60s, 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 with 215w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 185s, this stage laser scanning speed is 1mm/s; After preheating finishes, regulate the instantaneous sintering power density values 925w/cm that is raised to of laser power density
2, and to change laser scanning speed be 5mm/s, and through behind the sintering time of 65s, laser closes light, and sample is cooled to porcelain.
Embodiment 3
Adopt high power laser as direct irradiation bomb original position irradiation Ta
2O
5Ceramic body: at first with 215w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 45s; After preheating finishes, regulate the instantaneous sintering power density values 925w/cm that is raised to of laser power density
2, through behind the sintering time of 45s, 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 with 215w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 185s, this stage laser scanning speed is 8mm/s; After preheating finishes, regulate the instantaneous sintering power density values 925w/cm that is raised to of laser power density
2, and to change laser scanning speed be 17mm/s, and through behind the sintering time of 95s, laser closes light, and sample is cooled to porcelain.
Embodiment 5
Adopt high power laser as direct irradiation bomb scanning and irradiation Ta
2O
5Ceramic body: at first with 215w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 140s, this stage laser scanning speed is 5mm/s; After preheating finishes, regulate the instantaneous sintering power density values 925w/cm that is raised to of laser power density
2, and to change laser scanning speed be 33mm/s, and through behind the sintering time of 25s, laser closes light, and sample is cooled to porcelain.
Embodiment 6
Adopt high power laser as direct irradiation source scanning and irradiation (Ta
2O
5)
0.92(TiO
2)
0.08Ceramic body: at first with 190w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 45s, this stage laser scanning speed is 1mm/s; After preheating finishes, regulate the instantaneous sintering power density values 850w/cm that is raised to of laser power density
2, and to change laser scanning speed be 2mm/s, and through behind the sintering time of 35s, laser closes light, and sample is cooled to porcelain.
Embodiment 7
Adopt high power laser as direct irradiation source scanning and irradiation (Ta
2O
5)
0.92(TiO
2)
0.08Ceramic body: at first with 190w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 30s; After preheating finishes, regulate the instantaneous sintering power density values 850w/cm that is raised to of laser power density
2, through behind the sintering time of 35s, laser closes light, and sample is cooled to porcelain.Laser scanning speed is 5mm/s in the whole irradiation process.
Embodiment 8
Adopt high power laser as direct irradiation source scanning and irradiation (Ta
2O
5)
0.92(TiO
2)
0.08Ceramic body: at first with 190w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 100s, this stage laser scanning speed is 8mm/s; After preheating finishes, regulate the instantaneous sintering power density values 850w/cm that is raised to of laser power density
2, and to change laser scanning speed be 2mm/s, and through behind the sintering time of 35s, laser closes light, and sample is cooled to porcelain.
Embodiment 9
Adopt high power laser as direct irradiation source original position irradiation (Ta
2O
5)
0.92(TiO
2)
0.08Ceramic body: at first with 190w/cm
2Low power density this ceramic body is carried out laser irradiation preheating 70s; After preheating finishes, regulate the instantaneous sintering power density values 850w/cm that is raised to of laser power density
2, through behind the sintering time of 35s, laser closes light, and sample is cooled to porcelain.Laser scanning speed is 0mm/s in the whole irradiation process.
All embodiment have all carried out the process repeatability test, and number of repetition is greater than 3 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.
The instantaneous regulation and control laser power of table 1 prepares high-k Ta
2O
5The processing parameter and the sample dielectric properties of base pottery
| Embodiment | Preheating power density w/cm 2 | Sintering power density w/cm 2 | Warm up time s | Sintering time s | Laser preheating scanning speed mm/s | Laser sintered scanning speed mm/s | Specific inductivity | Dielectric loss factor |
| ?1 | ?350 | ?1405 | ?30 | ?60 | ?33 | ?50 | ?63.3 | ?0.016 |
| ?2 | ?215 | ?925 | ?185 | ?65 | ?1 | ?5 | ?57.1 | ?0.023 |
| ?3 | ?215 | ?925 | ?45 | ?45 | ?0 | ?0 | ?57.0 | ?0.010 |
| ?4 | ?215 | ?925 | ?185 | ?95 | ?8 | ?17 | ?56.6 | ?0.014 |
| ?5 | ?215 | ?925 | ?140 | ?25 | ?5 | ?33 | ?56.4 | ?0.020 |
| ?6 | ?190 | ?850 | ?45 | ?35 | ?1 | ?2 | ?449.9 | ?0.027 |
| ?7 | ?190 | ?850 | ?30 | ?35 | ?5 | ?5 | ?421.6 | ?0.021 |
| ?8 | ?190 | ?850 | ?100 | ?35 | ?8 | ?2 | ?386.2 | ?0.027 |
| ?9 | ?190 | ?850 | ?70 | ?35 | ?0 | ?0 | ?331.3 | ?0.024 |
Claims (3)
1, a kind of high-k Ta
2O
5The instantaneous regulation and control power laser preparation 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 is with 190～350w/cm
2Low power density 30～185s in the time to Ta
2O
5The base ceramic body carries out the laser irradiation preheating;
(2), after preheating finishes, regulate the instantaneous sintering power density values 850～1405w/cm that is raised to of laser power density
2, carry out sintering;
(3), behind the sintering through 25～95s, laser closes light, sample is cooled to porcelain.
2, high-k Ta according to claim 1
2O
5The instantaneous regulation and control power laser preparation method of base pottery is characterized in that, the sweep speed during the middle laser irradiation preheating of step (1) is 0～33mm/s; Sweep speed during step (2) sintering is 0～50mm/s.
3, high-k Ta according to claim 1
2O
5The instantaneous regulation and control power laser preparation 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03148245 CN1199910C (en) | 2003-07-04 | 2003-07-04 | Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03148245 CN1199910C (en) | 2003-07-04 | 2003-07-04 | Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1480427A true CN1480427A (en) | 2004-03-10 |
| CN1199910C CN1199910C (en) | 2005-05-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03148245 Expired - Fee Related CN1199910C (en) | 2003-07-04 | 2003-07-04 | Method of instantaneous controlling laser power for preparing ceramics in base of Ta2O5 with high dielectric constant |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329341C (en) * | 2005-03-07 | 2007-08-01 | 北京工业大学 | Process for laser preparation of hexagonal phase barium titanate ceramic |
| 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 |
-
2003
- 2003-07-04 CN CN 03148245 patent/CN1199910C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1329341C (en) * | 2005-03-07 | 2007-08-01 | 北京工业大学 | Process for laser preparation of hexagonal phase barium titanate ceramic |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN1199910C (en) | 2005-05-04 |
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