CN118619677B - A preparation method of LiBaF3 microwave dielectric ceramics - Google Patents
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- 239000000919 ceramic Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 62
- 239000000843 powder Substances 0.000 claims abstract description 59
- 238000001354 calcination Methods 0.000 claims abstract description 46
- 238000000227 grinding Methods 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000280 densification Methods 0.000 claims abstract description 12
- 238000003825 pressing Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 229910001632 barium fluoride Inorganic materials 0.000 claims abstract 4
- 239000000463 material Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 22
- 239000012535 impurity Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000005416 organic matter Substances 0.000 claims 1
- 238000004891 communication Methods 0.000 abstract description 10
- 239000003989 dielectric material Substances 0.000 abstract description 9
- 238000009694 cold isostatic pressing Methods 0.000 abstract description 8
- 238000005516 engineering process Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000008054 signal transmission Effects 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010344 co-firing Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
本发明公开了一种LiBaF3微波介质陶瓷的制备方法，涉及微波通讯领域及低温共烧陶瓷介质材料领域，包括将LiF和BaF2粉末分别放于加热炉中进行一次煅烧、一次研磨、一次干燥、二次煅烧、二次研磨、二次干燥、过筛造粒；将制得的粉体原料压制成圆柱体，并冷等静压；最终烧结2小时以实现致密化，得到致密化的LiBaF3；本发明中LiBaF3微波介质材料的制备方法可以在较低温度下实现致密化；在该制备条件下，LiBaF3微波介质陶瓷具有较低的介电常数13.72，较高的品质73000GHz和近零的谐振频率温度系数‑35.74×10‑6/℃；同时，该LiBaF3微波介质陶瓷可以与Ag低温共存，是一种颇具应用潜力的新型微波介质材料。
The invention discloses a preparation method of LiBaF3 microwave dielectric ceramics, which relates to the field of microwave communication and the field of low-temperature co-fired ceramic dielectric materials. The method comprises the following steps: placing LiF and BaF2 powders in a heating furnace for primary calcination, primary grinding, primary drying, secondary calcination, secondary grinding, secondary drying, and sieving and granulating; pressing the obtained powder raw materials into a cylinder, and cold isostatic pressing; and finally sintering for 2 hours to achieve densification to obtain densified LiBaF3 . The preparation method of the LiBaF3 microwave dielectric material of the invention can achieve densification at a relatively low temperature. Under the preparation conditions, the LiBaF3 microwave dielectric ceramics has a relatively low dielectric constant of 13.72, a relatively high quality of 73000GHz and a near-zero resonant frequency temperature coefficient of ‑35.74×10 ‑6 /°C. Meanwhile, the LiBaF3 microwave dielectric ceramics can coexist with Ag at a low temperature, and are a novel microwave dielectric material with considerable application potential.
Description
Technical Field
The invention relates to the fields of microwave communication and low-temperature co-fired ceramic dielectric materials, in particular to a preparation method of LiBaF microwave dielectric ceramics.
Background
The microwave communication technology has extremely important position in the modern information technology, and has wide and deep application in the fields of military, civil communication, satellite communication, aerospace and the like. With the advent of the 5G/6G age, the communication carrier frequency will extend from microwave to millimeter wave region even higher. In such high frequency communications, signal delay has become a primary problem to be solved. The signal delay time is in direct proportion to the square root of the dielectric constant (epsilon r), the propagation speed of a radio signal can be obviously improved by using a material with a lower dielectric constant, the signal loss and crosstalk risk in the signal transmission process can be reduced by using a high-quality factor (Q multiplied by f), the frequency selection characteristic of the material is improved, the temperature coefficient of the near-zero resonant frequency (tau f) shows that the material has better thermal stability and can be more suitable for the application environment of a complex temperature field, in addition, the low-temperature co-fired ceramic technology (LTCC) is considered as an effective method for realizing the miniaturization and circuit integration of a next-generation communication system module, the loss of a circuit is gradually dominant in the communication system along with the increase of the application frequency, the loss of the low-resistivity Ag and Cu electrodes can be obviously reduced in the signal propagation process, and the signal transmission speed is further improved, and therefore, in order to meet the requirements of high-frequency communication technologies such as 5G/6G, novel microwave dielectric materials with the low dielectric constant, the high-quality factor and the near-zero resonant frequency temperature coefficient are provided.
Disclosure of Invention
In order to solve the technical problems, the technical scheme provided by the invention is that the preparation method of LiBaF < 3 > microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder into a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) in a drying box, and performing primary drying to remove absolute ethyl alcohol;
(4) Putting the mixture material prepared in the step (3) into a heating furnace again, and performing secondary calcination to obtain a main phase LiBaF 3;
(5) Using absolute ethyl alcohol as a grinding medium for the mixed material prepared in the step (4), and carrying out secondary grinding on the calcined powder;
(6) Putting the mixed material prepared in the step (5) into a drying box, and performing secondary drying to remove organic matters;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF 3 was polished for subsequent testing.
Compared with the prior art, the preparation method of the LiBaF 3 microwave dielectric material has the advantages that densification (97 percent) can be realized at a lower temperature (625 ℃), under the preparation condition, the LiBaF 3 microwave dielectric ceramic has a lower dielectric constant of 13.72, a higher quality of 73000GHz and a near-zero resonance frequency temperature coefficient of-35.74 multiplied by 10 -6/DEGC, and meanwhile, the LiBaF 3 microwave dielectric ceramic can coexist with Ag at a low temperature (650 ℃), so that the preparation method is a novel microwave dielectric material with great application potential.
Drawings
FIG. 1 shows XRD results of LiBaF 3 powder calcined at 300-700℃in the present invention.
FIG. 2 is an XRD result for LiBaF 3 ceramics prepared at 600-675 ℃ sintering temperature in the present invention.
FIG. 3 is a graph of the densities and relative densities of LiBaF 3 ceramics prepared at different sintering temperatures in accordance with the present invention.
FIG. 4 shows the microwave dielectric properties of LiBaF 3 ceramics prepared under different sintering conditions in accordance with the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention.
Example 1:
A preparation method of LiBaF microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder with purity of 99.99% in a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder, wherein the calcination temperature of the heating furnace is 500 ℃ and the calcination time is 2 hours;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium for 4 hours to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) into a drying oven for primary drying to remove absolute ethyl alcohol, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(4) And (3) putting the mixture material obtained in the step (3) into a heating furnace again for secondary calcination to obtain a main phase LiBaF 3, wherein the calcination temperature is 300 ℃ and the calcination time is 4 hours.
(5) Using absolute ethyl alcohol as a grinding medium to carry out secondary grinding on the calcined powder for 4 hours on the mixed material prepared in the step (4);
(6) Placing the mixed material prepared in the step (5) into a drying oven for secondary drying to remove organic matters, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF 3 was polished for subsequent testing.
Example 2:
A preparation method of LiBaF microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder with purity of 99.99% in a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder, wherein the calcination temperature of the heating furnace is 500 ℃ and the calcination time is 2 hours;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium for 4 hours to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) into a drying oven for primary drying to remove absolute ethyl alcohol, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(4) Placing the mixture material prepared in the step (3) into a heating furnace again for secondary calcination to obtain a main phase LiBaF 3, wherein the calcination temperature is 700 ℃ and the calcination time is 4 hours;
(5) Using absolute ethyl alcohol as a grinding medium to carry out secondary grinding on the calcined powder for 4 hours on the mixed material prepared in the step (4);
(6) Placing the mixed material prepared in the step (5) into a drying oven for secondary drying to remove organic matters, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF was polished for subsequent testing.
Example 3:
A preparation method of LiBaF microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder with purity of 99.99% in a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder, wherein the calcination temperature of the heating furnace is 500 ℃ and the calcination time is 2 hours;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium for 4 hours to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) into a drying oven for primary drying to remove absolute ethyl alcohol, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(4) Placing the mixture material prepared in the step (3) into a heating furnace again for secondary calcination to obtain a main phase LiBaF 3, wherein the calcination temperature is 600 ℃ and the calcination time is 4 hours;
(5) Using absolute ethyl alcohol as a grinding medium to carry out secondary grinding on the calcined powder for 4 hours on the mixed material prepared in the step (4);
(6) Placing the mixed material prepared in the step (5) into a drying oven for secondary drying to remove organic matters, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF 3 was polished for subsequent testing.
Example 4:
A preparation method of LiBaF microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder with purity of 99.99% in a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder, wherein the calcination temperature of the heating furnace is 500 ℃ and the calcination time is 2 hours;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium for 4 hours to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) into a drying oven for primary drying to remove absolute ethyl alcohol, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(4) Placing the mixture material prepared in the step (3) into a heating furnace again for secondary calcination to obtain a main phase LiBaF 3, wherein the calcination temperature is 625 ℃ and the calcination time is 4 hours;
(5) Using absolute ethyl alcohol as a grinding medium to carry out secondary grinding on the calcined powder for 4 hours on the mixed material prepared in the step (4);
(6) Placing the mixed material prepared in the step (5) into a drying oven for secondary drying to remove organic matters, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF 3 was polished for subsequent testing.
Example 5:
A preparation method of LiBaF microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder with purity of 99.99% in a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder, wherein the calcination temperature of the heating furnace is 500 ℃ and the calcination time is 2 hours;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium for 4 hours to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) into a drying oven for primary drying to remove absolute ethyl alcohol, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(4) Placing the mixture material prepared in the step (3) into a heating furnace again for secondary calcination to obtain a main phase LiBaF 3, wherein the calcination temperature is 650 ℃ and the calcination time is 4 hours;
(5) Using absolute ethyl alcohol as a grinding medium to carry out secondary grinding on the calcined powder for 4 hours on the mixed material prepared in the step (4);
(6) Placing the mixed material prepared in the step (5) into a drying oven for secondary drying to remove organic matters, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF 3 was polished for subsequent testing.
Example 6:
A preparation method of LiBaF microwave dielectric ceramic comprises the following steps:
(1) Respectively placing LiF and BaF 2 powder with purity of 99.99% in a heating furnace for primary calcination to remove volatile impurities and water vapor in the powder, wherein the calcination temperature of the heating furnace is 500 ℃ and the calcination time is 2 hours;
(2) Weighing LiF and BaF 2 powder according to a molar ratio of 1:1, and grinding the LiF and BaF 2 powder once by using absolute ethyl alcohol as a grinding medium for 4 hours to ensure uniform mixing;
(3) Placing the uniformly mixed material prepared in the step (2) into a drying oven for primary drying to remove absolute ethyl alcohol, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(4) Placing the mixture material prepared in the step (3) into a heating furnace again for secondary calcination to obtain a main phase LiBaF 3, wherein the calcination temperature is 675 ℃ and the calcination time is 4 hours;
(5) Using absolute ethyl alcohol as a grinding medium to carry out secondary grinding on the calcined powder for 4 hours on the mixed material prepared in the step (4);
(6) Placing the mixed material prepared in the step (5) into a drying oven for secondary drying to remove organic matters, wherein the temperature of the drying oven is 100 ℃ and the drying time is 4 hours;
(7) Sieving and granulating the mixed split body prepared in the step (6) by using a 100-mesh sieve to obtain a powder raw material with relatively uniform particle size;
(8) Pressing the powder raw material prepared in the step (7) into a cylinder with the diameter of 10mm under the pressure of 150MPa, and then performing cold isostatic pressing for 30 seconds under the pressure of 200MPa to obtain a ceramic blank;
(9) Sintering the ceramic prepared in the step (8) for 2 hours in an air atmosphere at 600-675 ℃ to realize densification, so as to obtain densified LiBaF 3;
(10) The densified LiBaF 3 was polished for subsequent testing.
1. Test results
(1) As shown in FIG. 1, FIG. 1 shows XRD results of LiBaF 3 powder calcined at 300-700 ℃, and as the calcination temperature increases, the impurity phase gradually disappears, and only very weak impurity peaks remain at 600 ℃.
As shown in fig. 2, fig. 2 is an XRD result of LiBaF 3 ceramics prepared at 600-675 ℃ sintering temperature, indicating that single phase LiBaF 3 ceramic materials can be obtained in this sintering temperature range.
(2) As shown in fig. 3, fig. 3 shows the densities and relative densities of LiBaF 3 ceramics prepared at different sintering temperatures, and the result shows that the ceramic material has the highest density under the sintering condition of 625 ℃.
(3) As shown in fig. 4, fig. 4 shows the microwave dielectric properties of LiBaF 3 ceramics prepared under different sintering conditions. The dielectric constant, the quality factor and the temperature coefficient of the resonant frequency are respectively 13.72, 73000GHz and-35.7X10 -6/DEGC at 625 ℃. The LiBaF 3 novel ceramic material prepared by the LTCC technology is a promising microwave dielectric material.
Compared with other LTCC technologies at present, the densification temperature (625 ℃) of the LiBaF 3 ceramic is obviously lower than the sintering temperature adopted by most LTCC technologies, the method is more beneficial to reducing production cost and energy consumption, warpage and cracking of a substrate are avoided, dimensional stability is guaranteed, reliability is improved, co-firing with low-melting-point metal good conductors (such as Cu, ag and the like) is achieved, metal wiring and device integration is facilitated, in addition, compared with widely reported microwave dielectric ceramics of vanadate, molybdate and borate systems, the LiBaF ceramic provided by the invention has better comprehensive dielectric performance, for example, the Ba 3Zn(V2O7)2 ceramic prepared at 660 ℃ has a dielectric constant of 10.3, a quality factor of 43400GHz, a resonant frequency temperature coefficient of-46.87 ppm/°, the Li 2Mg2Mo3O12 ceramic prepared at 650 ℃ has a dielectric constant of 9.3, a quality factor of 58583GHz, a resonant frequency temperature coefficient of-51 ppm/°, the Li 6B4O9 ceramic prepared at 640 ℃ has a dielectric constant of 5.9, a quality factor of GHz, a resonant frequency coefficient of-34 ppm/-72 ℃ and a microwave dielectric constant of the ceramic prepared at 640 ℃ can be obtained by a certain method, and the microwave dielectric material has a certain co-existence performance of the microwave system of the microwave dielectric system, which can be obtained by the method.
The invention and its embodiments have been described above with no limitation, and the actual construction is not limited to the embodiments of the invention as shown in the drawings. In summary, if one of ordinary skill in the art is informed by this disclosure, a structural manner and an embodiment similar to the technical solution should not be creatively devised without departing from the gist of the present invention.
Claims (6)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60155530A (en) * | 1984-01-23 | 1985-08-15 | Kobe Steel Ltd | Production of libaf3 |
| CN101343041A (en) * | 2008-08-25 | 2009-01-14 | 天津大学 | Synthesis of three-component fluoride ABF3 at low-temperature |
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| JP2001244188A (en) * | 2000-03-02 | 2001-09-07 | Optron Inc | Vacuum ultraviolet optical member, exposure apparatus and device manufacturing method using the same |
| US6773501B2 (en) * | 2001-08-27 | 2004-08-10 | Corning Incorporated | Method of making a <250 nm wavelength optical fluoride crystal and device |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60155530A (en) * | 1984-01-23 | 1985-08-15 | Kobe Steel Ltd | Production of libaf3 |
| CN101343041A (en) * | 2008-08-25 | 2009-01-14 | 天津大学 | Synthesis of three-component fluoride ABF3 at low-temperature |
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