DETAILED ACTION
Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claim(s) 1, 2 and 10 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zagumennyi et al (US 2014/0291580) in view of Blahuta et al (US 2016/0252631), Wu et al (CN 106011998A), an English computer translation (CT) is provided, and Chou (US 2017/0088977).
Zagumennyi et al teaches a method of growing a boule of LYSO:Ce:Ca scintillation crystal, comprising the steps of: providing an iridium crucible; loading the iridium crucible with the following compounds and relative amounts on a weight percent basis: Lu2O3 (85.99 wt. %)+ Y2O3 (0.91 wt. %)+ CeO2 (0.05 wt. %)+CaO (0.01 wt. %)+ SiO2 (13.03 wt. %) ([0209]-[0211]); heating the loaded and iridium crucible to yield a melt; placing a seed crystal into the melt and growing an unfinished crystalline boule ([0209] teaches CZ growth in an iridium crucible, which clearly suggest forming a melt and pulling a seed from the melt); annealing the unfinished crystalline samples sliced from the boule at a temperature of at least about 1450° C in an atmosphere of at least about 95% Ar and less than about 5% CO on a weight percent basis to yield the boule of LYSO:Ce:Ca scintillation crystal ([0150], [0239], [0241] teaches annealing at 1400-1500°C in 100% Ar for about 12-72 hrs). Overlapping ranges are prima facie obvious (MPEP 2144.05). It is noted that pressuring with at least 95% Ar and less than 5% CO would include 100% Ar. Zagumennyi et al also teaches (Lu2-w-x+2yAwCexSi1-y)1-zMezJjOq(1) where A is at least one element selected from the group consisting of Sc, Y, Gd, and Lu; Me is at least one element selected from the group consisting of Li, Na, K, Cu, Ag, Mg, Ca, Zn, Sr, Cd, B, Al, Ga, V, Cr, Mn, Fe, Co, Ni, Ti, Ge, Zr, Sn, Hf, La, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb, and Lu; J is at least one element selected from the group consisting of N, F, P, S, and Cl; q is a value between 4.9 f.u. and 5.024 f.u., w is a value between near 0 f.u. and 1 f.u., x is a value between 3.times.10.sup.-4 f.u. and 0.02 f.u., y is a value between 0.003 f.u. and 0.024 f.u., and z is a value between near 0 f.u. and 0.001 f.u, and a specific example of Ce0.0014Lu1.977Y0.037 Ca0.001Si0.992O5.007 which clearly suggests A is Y, Me is Ca and j=0.
Zagumennyi et al teaches a crystal composition example having similar composition of reactant. Zagumennyi et al teaches annealed Ce:Ca:LYSO detectors ([0160]). However, Zagumennyi et al does not explicitly teach Lu2O3 at about 84 to 87 parts, Y2O3 at about 0.1 to 3 parts, SiO2 at about 11.5 to 15 parts, CaCO3 at about 0.01 to 0.03 parts, and CeO2 at about 0.08 to 0.1 parts.
In a method of growing doped scintillation crystals, Blahuta et al teaches a melt may be formed from a combination of Lu2O3, Y2O3, CeO2 and CaO ([0012]). Blahuta et al also teaches doping with a Group 2 element (Me), such as Ca, and forming a LYSO:Ce, Me crystal using a Czochralski or other growth technique, wherein the starting materials include Lu2O3, Y2O3, CeO2 and MeCO3, wherein Me is a Group 2 element ([0023]-[0036]), which clearly suggests CaO and CaCO3 are suitable starting materials for Ca, and equivalents for doping.
It would have been obvious to one of ordinary skill in the art at the time of filing to modify Zagumennyi et al loading with the claimed amounts of raw materials, as taught by Zagumennyi et al, to produce a crystal with a desired composition and properties. Changes in concentration are prima facie obvious (MPEP 2144.05) and by using a CaCO3 starting material, as taught by Blahuta et al, because the selection of a known material based on its suitability for its intended purpose is prima facie obvious (MPEP 2144.07) and substituting equivalents known for the same purpose is prima facie obvious (MPEP 2144.06 II).
The combination of Zagumennyi et al and Blahuta et al does not explicitly teach applying a vacuum and pressurizing the loaded crucible.
Wu et al teaches a Czochralski crystal growth of Ce:LYSO comprising a crucible disposed inside a furnace chamber; growth material is put into an Ir crucible, heating and melting the material, evacuating air from the furnace (applying vacuum), introducing an inert gas of Ar or Ar mixed with 0.01-50% of CO2 (CT [0015]-[0065]); filling the furnace with protective gas to 1.01x105 Pa to 1.2x105 Pa (~1-1.18 atm), which clearly suggests pressurizing the loaded crucible; installing a seed crystal and adjusting a pulling and rotating mechanism to grow a crystal; (CT [0015]-[0065]). It is noted that pressuring with at least 95% Ar and less than 5% CO would include 100% Ar and 0% CO, or 99% Ar, 0.01 CO2 and 0% CO. Overlapping ranges are prima facie obvious (MPEP 2144.05).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al and Blahuta et al to pressurizing the loaded crucible, as taught by Wu et al, because pressure is a result effective variable, and pressurizing the crucible is known in the art to be desirable for LYSO crystal growth.
The combination of Zagumennyi et al, Blahuta et al and Wu et al teaches annealing samples of the boule in 100% Ar at 1400-1600°C for 12-72 hrs (Zagumennyi [0239]-[0241]) . The combination of Zagumennyi et al, Blahuta et al and Wu et al does not explicitly teach annealing the unfinished boule.
In a method of making a double doped scintillation crystal, Chou teaches a single crystal of lutetium yttrium oxyorthosilicate (LYSO) doped with Ce and Ca grown by a Cz method; and thermal annealing the double doped single crystal by heating to a temperature of 1400-1600°C for 50-200 hrs ([0019]-[0027]), which clearly suggests annealing the unfinished boule. Chou teaches annealing achieves a low producing cost, a high yield, less crystal fragmentations, high luminescence intensity and a short decaying time ([0045]). Chou teaches a double doped crystal composed Cax + Cey:Lu2-x-y-zY2SiO5, where x is more than 0.000001 to less than 0.005, y is more than 0.001 to less than 0.1 and z is more than 0.1 to less than 1.898 ([0025]-[0030]).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al and Wu et al by annealing the unfinished boule, as taught by Chou, to increase yield, luminescence intensity and decrease crystal fragmentations.
Referring to claim 2, as discussed above, the combination of Zagumennyi et al, Blahuta et al, Wu et al and Chou teaches a similar composition (Zagumennyi [0067]-[0085]; Chou [0025]-[0030]), and changes in concentration of reactants to form a desired composition. Therefore, it would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al and Chou to load the crucible with claimed amounts of materials to form a desired composition.
Referring to claim 10, the combination of Zagumennyi et al, Blahuta et al, Wu et al and Chou does not explicitly teach the claimed ratio. However, this ratio would be expected because the combination of Zagumennyi et al, Blahuta et al, Wu et al and Chou teaches the method of claim 1, which applicant teaches is used to obtain the claimed ratio; therefore, a similar method would be expected to produce a similar result.
Claim(s) 3 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zagumennyi et al (US 2014/0291580) in view of Blahuta et al (US 2016/0252631), Wu et al (CN 106011998A), an English computer translation (CT) is provided, and Chou (US 2017/0088977), as applied to claim 1, 2 and 10 above, and further in view of Wang et al (US 2021/0381122).
The combination of Zagumennyi et al, Blahuta et al, Wu et al and Chou teaches all of the limitations of claim 3, as discussed above, except the reactants are each about 99.999% pure.
In a method of making scintillation crystals, Wang et al teaches growing doped lutetium yttrium oxyorthosilicate (LYSO) and to make the grown crystal meet the requirements, the purity of the reactants for growing the crystal may be greater than 99% and more preferably, the purity of the reactants may be greater than 99.999% ([0028]-[0033]).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al and Chou by providing reactant each about 99.999% pure, as taught by Wang et al, to produce a higher purity crystal. It is noted that the mere purity of a product, by itself, does not render the product nonobvious (MPEP 2144.04 VII).
Claim(s) 4 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zagumennyi et al (US 2014/0291580) in view of Blahuta et al (US 2016/0252631), Wu et al (CN 106011998A), an English computer translation (CT) is provided, Chou (US 2017/0088977) and Wang et al (US 2021/0381122), as applied to claim 1-3 above, and further in view of Zhou et al (CN 104294365 A), an English computer translation (CT2) is provided.
The combination of Zagumennyi et al, Blahuta et al, Wu et al , Chou and Wang et al teaches all of the limitations of claim 4, as discussed above, except the combination of Zagumennyi et al, Blahuta et al, Wu et al , Chou and Wang et al does not explicitly teach a vacuum of about 1 Pa or less is applied before the steps of pressurizing or heating. Wu et al teaches a Czochralski crystal growth of Ce:LYSO comprising a crucible disposed inside a furnace chamber; growth material is put into an Ir crucible, heating and melting the material, evacuating air from the furnace (applying vacuum), introducing an inert gas of Ar or Ar mixed with 0.01-50% of CO2 (Wu CT [0015]-[0065]), however does not explicitly teach the vacuum pressure.
In a method of cerium-doped yttrium lutetium silicate scintillation crystal growth, Zhou et al teaches loading reactant in a crucible, placing a crucible in a vacuum furnace and evacuate until the pressure inside is < 10 Pa, then filling with protective gas to a pressure of 20-100 kPa and then melting the reactants (CT2 [0011]-[0020]). Overlapping ranges are prima facie obvious (MPEP 2144.05). Zhou et al teaches evacuating the furnace to a pressure ≤10 Pa before heating for the growth of LYSO:Ce scintillation crystals using a molybdenum crucible is similar to the process of growing LYSO:Ce scintillation crystals using an iridium crucible to purify the crucible (CT2 [0028]).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al , Chou and Wang et al by applying a vacuum of about 1 Pa or less is applied before the steps of pressurizing or heating, as taught by Zhou et al, to purify the crucible and remove impurities from the atmosphere prior to melting and growth.
Claim(s) 5-8 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zagumennyi et al (US 2014/0291580) in view of Blahuta et al (US 2016/0252631), Wu et al (CN 106011998A), an English computer translation (CT) is provided, Chou (US 2017/0088977), Wang et al (US 2021/0381122) and Zhou et al (CN 104294365 A), an English computer translation (CT2) is provided, as applied to claim 1-4 above, and further in view of Kamada et al (US 2017/0044433).
The combination of Zagumennyi et al, Blahuta et al, Wu et al , Chou, Wang et al and Zhou et al teaches all of the limitations of claim 5, as discussed above, except the pressuring is with a gas mixture consisting essentially of about 99.75% Ar and 0.25% CO.
In a method of growing a crystal, Kamada et al teaches a scintillator crystal CexRE3-xM5+yO12+3y/2 (where 0.0001≦x≦0.3, 0≦y≦0.5 or 0≦y≦−0.5, M is one type or two or more types selected from Al, Lu, Ga, and Sc, and RE is one type or two or more types selected from La, Pr, Gd, Tb, Yb, Y, and Lu; and the crystal growth is preferably performed under an inert gas (e.g., Ar) atmosphere, or mixed gas of an inert gas (e.g., Ar) and a carbon monoxide gas may be used; and when a mixed gas is used, an oxygen partial pressure is not limited to 2%, and a mixed gas with any percentage of mixture ranging from 0% to 100% may also be used ([0018]-[0035]). Overlapping ranges are prima facie obvious (MPEP 2144.05).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al , Chou, Wang et al and Zhou et al by using a gas mixture consisting essentially of about 99.75% Ar and 0.25% CO, as taught by Kamada et al, because the selection of a known material based on its suitability for its intended purpose is prima facie obvious (MPEP 2144.07) and a mixed gas of Ar and CO is known to be suitable for scintillator crystal growth.
Referring to claim 6, the combination of Zagumennyi et al, Blahuta et al, Wu et al, Chou, Wang et al, Zhou et al and Kamada et al teaches filling the furnace with protective gas to 1.01x105 Pa to 1.2x105 Pa (~1-1.18 atm) (Wu CT [0015]-[0065]). Overlapping ranges are prima facie obvious (MPEP 2144.05).
Referring to claim 7-8, the combination of Zagumennyi et al, Blahuta et al, Wu et al, Chou, Wang et al, Zhou et al and Kamada et al teaches a single crystal of lutetium yttrium oxyorthosilicate (LYSO) doped with Ce and Ca grown by a Cz method; and thermal annealing the double doped single crystal by heating to a temperature of 1400-1600°C for 12-72 hrs (Chou [0019]-[0027]; Zagumennyi ([0150], [0239], [0241] teaches annealing at 1400-1500°C in 100% Ar for about 12-72 hrs). Overlapping ranges are prima facie obvious (MPEP 2144.05). Furthermore, It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al, Chou, Wang et al, Zhou et al and Kamada et al by optimizing the annealing time to obtain the claimed period by conducting routine experimentation of a result effective variable to improve crystal properties.
Claim(s) 9 is/are rejected under 35 U.S.C. 103 as being unpatentable over Zagumennyi et al (US 2014/0291580) in view of Wu et al (CN 106011998A), an English computer translation (CT) is provided, Blahuta et al (US 2016/0252631), and Chou (US 2017/0088977), as applied to claim 1 above, and further in view of Wu (CN 106087037A), an English computer translation (CT2) is provided, and Yokota et al (US 2025/0341023).
The combination of Zagumennyi et al, Blahuta et al, Wu et al, and Chou teaches all of the limitations of claim 9, as discussed above, except the iridium crucible is surround by and in direct contact with a deoxidized zirconia insulation material.
In a crystal pulling growing furnace, Wu teaches an alumina insulation cylinder 1, zirconia brick insulation cylinder 2 in direct contact with an iridium crucible 3, and a zirconia crucible support 4, wherein the (Fig 1; CT2 [0088]-[0096]). Wu teaches the insulation structure reduces energy consumption and cost while ensuring the high temperature and temperature gradient required for pulling growth (CT2 [0008]).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al, and Chou by providing an iridium crucible is surround by and in direct contact with a zirconia insulation material, as taught by Wu, to reduces energy consumption and cost while ensuring the high temperature and temperature gradient required for pulling growth.
The combination of Zagumennyi et al, Blahuta et al, Wu et al, Chou and Wu teaches a zirconia insulation, and does not explicitly teach deoxidized zirconia.
In a crystal growth apparatus, Yakota et al teaches a crucible together with a deoxidized zirconia heat insulating material in an inert atmosphere and unidirectionally solidifying a raw material melt contained in the crucible (CT [0040]-[0047]).
It would have been obvious to one of ordinary skill in the art at the time of filing to modify the combination of Zagumennyi et al, Blahuta et al, Wu et al, Chou and Wu by using a deoxidized zirconia insulation material, as taught by Yakota et al, because the selection of a known material based on its suitability for its intended purpose is prima facie obvious (MPEP 2144.07).
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure.
Chou (US 2011/0204240) teaches Ca atoms are doped for charge compensation with Ce+4 to form Ce+3 and electrovalence of Ce is uniformly distributed in scintillating crystal with greater electrical degree generated; photon yield is increased by non-radiative energy transfer ([0005]-[0015]).
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MATTHEW J. SONG
Examiner
Art Unit 1714
/MATTHEW J SONG/ Primary Examiner, Art Unit 1714
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