CN1233591C - Laser preparing method for Ta2O5 base transparent ceramics - Google Patents
Laser preparing method for Ta2O5 base transparent ceramics Download PDFInfo
- Publication number
- CN1233591C CN1233591C CN 200410050131 CN200410050131A CN1233591C CN 1233591 C CN1233591 C CN 1233591C CN 200410050131 CN200410050131 CN 200410050131 CN 200410050131 A CN200410050131 A CN 200410050131A CN 1233591 C CN1233591 C CN 1233591C
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- CN
- China
- Prior art keywords
- ta2o5
- preparation
- ceramic
- laser
- base
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title abstract description 8
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 title abstract 4
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 14
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 14
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- 235000015895 biscuits Nutrition 0.000 abstract 2
- 238000005245 sintering Methods 0.000 description 13
- 239000011222 crystalline ceramic Substances 0.000 description 11
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 7
- 239000013078 crystal Substances 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 235000012054 meals Nutrition 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 241000707825 Argyrosomus regius Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a Ta2O5-base transparent ceramic product and high-speed laser preparation method thereof, which belongs to the field of ceramic material preparation. The ceramic preparation method comprises the following steps that Ta2O5 powder materials or Ta2O5 and TiO2 powder materials mixed according to a stoichiometric ratio of 92:8 are presintered for 4.8 to 5.6 hours at a temperature of 1200 to 1350 DEG C, and then pressed into Ta2O5-base ceramic biscuit; the Ta2O5 base ceramic biscuit is preheated through the irradiation of laser with 800 to 1250 w/cm<2> in power density for 50 to 90s; and when the preheating is completed, the test samples are cooled to the room temperature after being sintered by laser with 4800 to 5700 w/cm<2> in power density for 30 to 50s. The preparation method has the advantages that the Ta2O5-base transparent ceramic (as shown in the figure) has high density, the minimum relative density is greater than 97%, the average relative density approximates to the theoretical density, ordinary industrial powder materials can be used as raw material powder, and the preparation method has simple process, low energy consumption, time saving and low preparation cost.
Description
Technical field
The invention belongs to Ta
2O
5The base transparent ceramic preparation field.
Background technology
Ta
2O
5The base pottery is a kind of dielectric material that is applied to capacitor dielectric storage and integrated circuit.In the page 5 the 24th～26 of " crystalline ceramics " book that is edited by works such as USSR (Union of Soviet Socialist Republics) г .A. Wei Delike, Chen Wanhua translation, high Long Qiao of publishing in 1980 is capable, point out that " transparent ceramic material can be used as the microwave substrate and the surface-mounted integrated circuit of storing device.With almost completely not having leachy high density transparent ceramic material can obtain high-quality integrated circuit.", but up to now, be showed no relevant transparent Ta both at home and abroad
2O
5The report of base pottery and preparation method thereof.Transparent Ta
2O
5Simple, the free from admixture of base ceramic phase, the function course in the material such as phase transformation, crystal boundary migration etc. are all easily directly observed at microscopically, therefore, very are suitable for carrying out the basic research of ceramic functional characteristic.In addition, in conjunction with its intrinsic dielectric property, transparent Ta
2O
5The base pottery also has a good application prospect in the function elements such as photoelectricity storage.
Pottery is transparent must possess high density, mutually simple, the porosity is extremely low, crystal boundary free from admixture, the equal condition of no glass.The present technology adopts the sintering furnace sintering processing to prepare Ta more
2O
5Base pottery, relative density are difficult to reach the transparent needed approximation theory density of pottery and the extremely low porosity less than 95%.And for other class pottery that obtains transparent article, its existing complicated process of preparation must adopt the technologies such as sintering aid, atmosphere sintering or hot pressed sintering usually, to improve ceramic density, the porosity in the reduction sintered body and sintering temperature etc.; Strict to raw meal, as generally to adopt special chemical technology to prepare powder, the preparation cost height; Sintering time long (general several hours even tens hours), energy consumption is big; Need to use crucible or closed agglomerating plant etc. during sintering, can't directly observe sintering process, preparation technology is difficult to control.
Summary of the invention
The objective of the invention is to overcome the shortcoming of said method, adopt laser as direct heat source, in room temperature, atmospheric air environment, fast prepare high density Ta with powder as raw meal with general industry
2O
5Base transparent ceramic (minimum relative density is greater than 97%).
Ta provided by the invention
2O
5The laser preparation method of base transparent ceramic is characterized in that, it may further comprise the steps:
1. with Ta
2O
5Powder or press the Ta that stoichiometric 92: 8 mixes
2O
5And TiO
2Powder 1200～1350 ℃ of pre-burnings 4.8～5.6 hours, is pressed into Ta then
2O
5Base ceramic blank material;
2. in the time, adopt power density 800～1250w/cm at 50～90s
2The above-mentioned Ta of laser irradiation
2O
5Base ceramic blank material carries out preheating;
3. after above-mentioned preheating finishes, adopt power density 4800～5700w/cm
2Laser sintered 30～50s after, sample is cooled to room temperature.
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. the Ta for preparing
2O
5Base transparent ceramic density height, relative density can reach approximation theory density, and metallographic and X-ray diffraction analysis show does not almost completely have pore in the ceramic sintered body, mutually pure, free from admixture.
2. raw material powder of the present invention adopts the general industry powder, and is loose to the raw material powder requirement, reduces preparation cost greatly.
3. the preparation method can carry out under the non-pressurized air ambient in room temperature, work simplification, and the time is short, and average laser irradiation preparation time is 113s (the laser irradiation time average of embodiment), and preparation efficiency significantly improves.
4. preparation technology need not crucible, does not use closed agglomerating plant, and whole sintering process can intuitively be observed, and process controllability is strong, is easy to realize serialization production.
5. method technology of the present invention is suitable for preparing other oxide ceramic material equally.
Description of drawings
Fig. 1 is embodiment 1Ta
2O
5The crystalline ceramics design sketch;
Fig. 2 is embodiment 1Ta
2O
5Crystalline ceramics printing opacity microscope metallograph;
Fig. 3 is embodiment 2 (Ta
2O
5)
0.92(TiO
2)
0.08The crystalline ceramics design sketch;
Fig. 4 is embodiment 3 (Ta
2O
5)
0.92(TiO
2)
0.08Crystalline ceramics X-ray diffraction spectrogram.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Embodiment 1:
With Ta
2O
5Powder is pressed into the base material then 1350 ℃ of pre-burnings 4.8 hours; Adopt laser as direct heat source, in room temperature, the atmospheric air environment, with 1250w/cm
2Power density 90s in the time to this Ta
2O
5The ceramic blank material carries out preheating; Preheating is adjusted to 5700w/cm with laser power density after finishing
2Sintering 50s, laser closes light, and sample is cooled to room temperature, makes transparent Ta
2O
5Sample.The transparent sample bulk density is 8.396g/cm
3, relative density is 99.95%.
From Fig. 1: Ta
2O
5Can find out the Ta that makes in the crystalline ceramics design sketch
2O
5Crystalline ceramics possesses good light transmission.
From Fig. 2: Ta
2O
5Can find out in the crystalline ceramics printing opacity microscope metallograph that the sample porosity that makes is extremely low, crystal grain is grown fairly perfect, and big or small homogeneous is arranged closely, and crystal boundary is meagre, no glassy phase.This structure provides good basis for the light transmission of pottery.
Embodiment 2
Will be by 92: 8 Ta of stoichiometric
2O
5And TiO
2Powder is pressed into the base material then 1200 ℃ of pre-burnings 5 hours; Adopt laser as direct heat source, in room temperature, the atmospheric air environment, with 800w/cm
2Power density 50s in the time to this (Ta
2O
5)
0.92(TiO
2)
0.08The ceramic blank material carries out preheating; Preheating is adjusted to 5200w/cm with laser power density after finishing
2Sintering 30s, laser closes light, and sample is cooled to room temperature, makes transparent (Ta
2O
5)
0.92(TiO
2)
0.08Ceramic sample.The transparent sample bulk density is 8.239g/cm
3, relative density is 98.08%.
From Fig. 3: (Ta
2O
5)
0.92(TiO
2)
0.08In the crystalline ceramics design sketch as can be seen, (the Ta that makes
2O
5)
0.92(TiO
2)
0.08Crystalline ceramics possesses good light transmittance.
Embodiment 3
Will be by 92: 8 Ta of stoichiometric
2O
5And TiO
2Powder is pressed into the base material then 1250 ℃ of pre-burnings 5.6 hours; Adopt laser as direct heat source, in room temperature, the atmospheric air environment, with 1150w/cm
2Power density 70s in the time to this (Ta
2O
5)
0.92(TiO
2)
0.08The ceramic blank material carries out preheating; Preheating is adjusted to 4800w/cm with laser power density after finishing
2Sintering 40s, laser closes light, and sample is cooled to room temperature, makes transparent (Ta
2O
5)
0.92(TiO
2)
0.08Ceramic sample.The transparent sample bulk density is 8.218g/cm
3, relative density is 97.83%.
Fig. 4: (Ta
2O
5)
0.92(TiO
2)
0.08Characteristic peak is sharp-pointed shown in the crystalline ceramics X-ray diffraction spectrogram, does not have assorted peak, shows that the sample that makes is mutually pure, and inclusion-free is the phase structure of homogeneous.
Claims (1)
1, a kind of Ta
2O
5The laser preparation method of base transparent ceramic is characterized in that, it may further comprise the steps:
Step 1. is with Ta
2O
5Powder or press the Ta that stoichiometric 92: 8 mixes
2O
5And TiO
2Powder 1200～1350 ℃ of pre-burnings 4.8～5.6 hours, is pressed into Ta then
2O
5Base ceramic blank material;
Step 2. in the time, adopts power density 800～1250w/cm at 50～90s
2The above-mentioned Ta of laser irradiation
2O
5Base ceramic blank material carries out preheating;
After the above-mentioned preheating of step 3. finishes, adopt power density 4800～5700w/cm
2Laser sintered 30～50s after, sample is cooled to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410050131 CN1233591C (en) | 2004-06-28 | 2004-06-28 | Laser preparing method for Ta2O5 base transparent ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410050131 CN1233591C (en) | 2004-06-28 | 2004-06-28 | Laser preparing method for Ta2O5 base transparent ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1587200A CN1587200A (en) | 2005-03-02 |
| CN1233591C true CN1233591C (en) | 2005-12-28 |
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ID=34602168
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410050131 Expired - Fee Related CN1233591C (en) | 2004-06-28 | 2004-06-28 | Laser preparing method for Ta2O5 base transparent ceramics |
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| Country | Link |
|---|---|
| CN (1) | CN1233591C (en) |
Families Citing this family (6)
| 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 |
| CN1300050C (en) * | 2005-04-22 | 2007-02-14 | 北京工业大学 | Technique for quick sintering ceramics in (Ta2O5)1-x(TiO2)x system |
| CN1305804C (en) * | 2005-05-13 | 2007-03-21 | 北京工业大学 | Process for raising dielectric coefficient of (Ta2O5) 1-x (TiO2) ceramics |
| 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 |
| CN102881572A (en) * | 2011-07-11 | 2013-01-16 | 刘莹 | Method for preparing crystalline silicon battery back electrode by laser sintering |
| CN107522465B (en) * | 2017-09-19 | 2018-08-24 | 界首市伟盛古窑彩陶制作发展有限公司 | A kind of preparation method of high-quality ceramics seal |
-
2004
- 2004-06-28 CN CN 200410050131 patent/CN1233591C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1587200A (en) | 2005-03-02 |
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Effective date of registration: 20131022 Address after: 610000, No. 199, West Avenue, hi tech Zone, Sichuan, Chengdu Patentee after: Chengdu 3D Change Technology Co., Ltd. Address before: 100022 No. 100 Chaoyang District Ping Tian Park, Beijing Patentee before: Beijing University of Technology |
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