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T. 26, 1995 Mary(Bos)Z Formula 1 (51) Int US00568.4813A United States Patent (19) 11 Patent Number: 5,684.813 Keszler 45 Date of Patent: Nov. 4, 1997 54 POLYBORATES USEFUL FOR OPTICAL "New Nonlinear Optical Crystal Cesium Lithium Borate.” FREQUENCY CONVERSION Proceeding of Advanced Solid-State lasers Conference, Memphis, Tennessee, Jan. 30-Feb. 2, 1995 (Paper WD3), 75) Inventor: Douglas A. Keszler, Corvallis, Oreg. Sasaki, et al., 5 pp. 73) Assignee: The State of Oregon Acting By and Primary Examiner-Leon Scott, Jr. Through the Oregon State Board of Attorney, Agent, or Firm-Klarquist Sparkman Campbell Higher Education on Behalf of Leigh & Whinston, LLP Oregon State University, Corvallis, Oreg. 57 ABSTRACT Nonlinear optical materials are described which satisfy 21 Appl. No.: 548,458 Formula 1 22 Filled: Oct. 26, 1995 Mary(BOs)Z Formula 1 (51) int. Cl. BO1S 3/10 whereinM and Maremono- or divalent metalions, Xvaries 52 U.S. Cl. ............................... 372/21; 372/22; 117/13; from about 0.1 to about 1.9, Yvaries from about 1.9 to about 359/328; 359/330 0.1, and Z is 2 or 3. Currently, the best nonlinear optical 581 Field of Search ................................. 372/21, 22, 39, materials also satisfy Formula 2 372/41;359/328,330, 117/13 MMOBOs)K+Y Formula 2 56 References Cited wherein M and Mare monovalent metalions independently U.S. PATENT DOCUMENTS selected from the group consisting of Group LA metals, X 3,934,154 1/1976 Cook, Jr. ................................ 359,328 varies from 0.1 to about 1.9, and wherein Y varies from 5,144,630 9/1992 Lin ............................................ 372/21 about 1.9 to about 0.1. The best results are achieved when 5,191587 3/1993 Hanson et al. ............................ 372/21 compounds satisfying Formula 2 have X=Y=1, and the 5,381,754 1/1995 Wu et al. ................................. 372/21 metal ions are independently selected from the group con 5,390,211 2/1995 Clark et al. ............................... 372/21 sisting of lithium, sodium, potassium, rubidium, cesium and francium. One example, without limitation, of a compound OTHER PUBLICATIONS that satisfies Formulas 1 and 2 is CsI iBO, The disclosure "New Nonlinear Optical Crystal: Cesium Lithium Borate,” also describes compositions that include the described non Yusuke Mori, et al., Appl. Phys. Lett. 67(13), Sep. 25, 1995, linear optical materials, methods for making such nonlinear pp. 1818-1820. optical materials, and devices which include the nonlinear "Caesium Lithium Borate: A New Nonlinear Optical Crys optical materials. tal.' Takatomo Sasaki, et al., Acta Crystallographica, Sec tion C, 1995, pp. 2222-2224. 32 Claims, 2 Drawing Sheets G. (3) &R - NYC YGY(3 GPGPVG)AGREY (3) 3.SSES (SSEYs9 G3SS 26SV S 523 3: lé e G3 NG Ss (2 (3. s (3) 1.3:G 2O3) r 5/ t. (3.2 SSNSSaSNSS 23SC) 2e333'N,a. 2S2) S. SaS2S25GO U.S. Patent Nov. 4, 1997 Sheet 1 of 2 5,684.813 FIG. 1 Q $36,636- S Q & SPS-SSMG) 3) GsNa2SšYASS23S-G)7 S; s SYS S2S25; ) QSS3 S&Ex8 S 22 i 33 SS 1.33SNS 4 (2 S t (NGSE 2&s;%S2312 ASN e 37-SN N 2 G a aer633-77SS7533 63233. 5,684.813 1 2 POLYBORATES USEFUL FOR OPTICAL powered lasers; (4) excessive absorption and light scattering FREQUENCY CONVERSION of incident light; and (5) too costly and time consuming for commercial production. These and other deficiencies are ACKNOWLEDGMENT OF GOVERNMENT discussed in Chemistry of Materials, 1:492-508 (1989). SUPPORT SUMMARY OF THE INVENTION This invention was developed with funds from the National Science Foundation, grant numbers DMR-8814432 The present invention concerns nonlinear optical materi and DMR-9221372. The United States Government may als according to Formula 1 have rights to this invention. 10 MM(BOs): Formula 1 FIELD OF THE INVENTION wherein MandM are mono- or divalent metalions, Xvaries This invention concerns nonlinear optical materials and from about 0.1 to about 1.9, Yvaries from about 1.9 to about devices employing such materials. 0.1, and Z is 2 or 3. Mono- and divalent metal ions M and 15 M'suitable for forming compounds satisfying Formula 1 can BACKGROUND OF THE INVENTION be independently selected from the group consisting of Nonlinear optical (NLO) materials are unusual in that Group LA and IIA metals. The best results are achieved by their optical properties are affected by light. For instance, independently selecting MandM' from the group consisting light polarizes certain materials. If the polarization is linear, of cesium, lithium, barium, sodium and strontium. Examples then light emitted by the material has the same frequency as 20 of nonlinear optical materials satisfying Formula 1 include, the absorbed light. NLO materials are polarized in a non without limitation, CsI i(BOs), Sri(BOs), BaNa linear manner. As a result, the frequency of the light emitted (BO) and Balli(BO). by a nonlinear optical material is some value times the Best examples of currently known nonlinear optical com frequency of the light incident on the material. pounds according to this invention also satisfy Formula 2 Laser technology is one field that has prompted the 25 MMOBOs):r Formula 2 development of new NLO materials. Known NLO materials generally are suitable only for those applications for which wherein M and Mare monovalent metalions independently they were particularly designed. As a result, new NLO selected from the group consisting of Group A metals, X materials continually must be developed having properties varies from 0.1 to about 1.9, and wherein Y varies from 30 about 1.9 to about 0.1. The best results are achieved when selected for a particular application. compounds satisfying Formula 2 have X=Y=1. The Furthermore, most known NLO materials have incongru monovalent metalions generally are independently selected ent melting points. This means that as the compounds melt, from the group consisting of lithium, sodium and cesium, the solid compound cannot coexist with the liquid of the and the best results are achieved using monovalent metal same composition. The practical result is that the solid-to 35 ions independently selected from the group consisting of liquid phase transformation does not occur at a specific lithium and cesium. One example, without limitation, of a temperature for the entire material. Instead, the solid-to compound that satisfies Formula 1 is CsILi(BO). liquid transformation occurs over a temperature range. This The nonlinear optical materials of the present invention melting property makes it difficult to process known NLO can be combined with other materials to form useful materials on a commercial scale because a flux agent must compositions, as long as the other materials do not unduly be added to the pure material to enable the production of compromise the nonlinear optical features. For instance, the single crystals. This leads either to the inclusion of defects nonlinear optical materials may be mixed with inert mate that limit the performance of the material, or requires very rials to form composites which still exhibit nonlinear optical long crystal growth times. properties. Thus, new NLO materials having congruent melting 45 Methods for making nonlinear optical materials that sat points are particularly desirable. These material may be isfy both Formulas 1 and 2 also are described. One embodi grown from a stoichiometric melt, thereby limiting defects ment comprises forming a mixture comprising from about and decreasing growth times. Moreover, with congruently 10 to about 20 mole percent of a source of M, from about 10 melting materials it generally is possible to adjust the melt to about 20 mole percent of a source of M', and from about composition slightly of stoichiometry to further improve 50 60 to about 80 mole percent of boron oxide. The mixture is crystal-growth characteristics. heated to a temperature and for a period of time sufficient to Boric crystals are a particular class of NLO materials form the NLO material. For instance, the step of heating may having properties suitable for ultraviolet, nonlinear optic comprise heating the mixture to a first temperature of at least applications. Examples of known boric-crystal NLO mate 825 K, and generally greater than about 850 K. The mixture rials include LiBOs and B-Bab.O. These compounds are 55 is then cooled. The cooled mixture is comminuted (ground known to generate UV light by frequency mixing of to a fine powder, such as by grinding with a mortar and Nd:YAG laser outputs. See Chin et al.'s J. Opt. Soc. Am, pestle), and then heated to a second temperature of at least 6:616 (1989), and Chin et al.'s Sci. Sin, 579 (1984). Boric 900 K, generally greater than about 1000 K. If M is Cs, then crystals also have been used in patented devices. For the source of M generally is cesium carbonate. If M is Li, instance, Chuangtian et al.'s U.S. Pat. No. 4,863,283 then the source of M' generally is lithium nitrate. describes an NLO device that uses a single crystal of The present invention also concerns devices which some LIBOs. how use or require nonlinear optical materials for operation. In summary, known NLO compounds are limited to An example, without limitation, of such a device is an particular applications, and most suffer from one or more of optical parametric oscillator (OPO). An OPO uses NLO the following undesirable properties: (1) incongruous melt 65 materials to produce widely tunable coherent light. Optical ing; (2) excessive energy requirements for inducing NLO devices of the present invention comprise a light source, effects; (3) excessive material damage by exposure to high such as a laser, optically coupled to nonlinear optical mate 5,684.813 3 4 rials that satisfy Formula 1, Formula 2 or both.
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