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 .
Priority
Acknowledgment is made of applicant’s claim for foreign priority under 35 U.S.C. 119 (a)-(d). The certified copy has been filed in parent Application No. JP 2021-091754, filed on May 31, 2021.
Receipt is acknowledged of certified copies of papers required by 37 CFR 1.55.
Information Disclosure Statement
The information disclosure statement filed January 29, 2026 fails to comply with 37 CFR 1.98(a)(2), which requires a legible copy of each cited foreign patent document; each non-patent literature publication or that portion which caused it to be listed; and all other information or that portion which caused it to be listed. It has been placed in the application file, and the information therein has been considered as the foreign references and non-patent literature have been retrieved and subsequently provided by examiner. Please note that any future information disclosure statements filed where foreign references and non-patent literature copies are not provided by the applicant will not be considered.
Drawings
The drawings are objected to as failing to comply with 37 CFR 1.84(p)(5) because they include the following reference character(s) not mentioned in the description: Fig. 2 member 42 is not referenced in the specification. Corrected drawing sheets in compliance with 37 CFR 1.121(d), or amendment to the specification to add the reference character(s) in the description in compliance with 37 CFR 1.121(b) are required in reply to the Office action to avoid abandonment of the application. Any amended replacement drawing sheet should include all of the figures appearing on the immediate prior version of the sheet, even if only one figure is being amended. Each drawing sheet submitted after the filing date of an application must be labeled in the top margin as either “Replacement Sheet” or “New Sheet” pursuant to 37 CFR 1.121(d). If the changes are not accepted by the examiner, the applicant will be notified and informed of any required corrective action in the next Office action. The objection to the drawings will not be held in abeyance.
Specification
The disclosure is objected to because of the following informalities: Paragraph [0144] second to last sentence states “Formula (1Ie)” instead of “(IIe)”. Paragraph [0223] states that Fig. 8 has gray portion corresponding to fluoride particles 2, the white portion corresponding to lanthanum phosphate 4, and the dark gray portion corresponding to silicon dioxide 6. However, these features are depicted in Fig. 7.
Appropriate correction is required.
Claim Interpretation
For the purposes of examination, claim 3 will be interpreted where F is present as follows: 5.5 ≤ s < 6.0 within the chemical formula I (M2[SipAlqMnrFs]). See also rejection of claim 3 under 35 USC 112(b) below.
For the purposes of examination, claims 22 and 23 will be interpreted where the third heat-treated material will be assumed to produce a “third heat-treated material” as opposed to a “second heat-treated material” for reasons described in their claim rejections under 35 USC 112(b) below.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claim 3 is rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention. Claim 3 provides a range of values for the presence of fluorine, “F”, in chemical formula I (M2[SipAlqMnrFs]) which depends on the independent claim 1. Independent claim 1 states F is present in a “range from 5.5 to less than 6.0”, while claim 3 allows for F to be present at a value of 6.0: “5.5 ≤ s ≤ 6.0”. For the purposes of examination, claim 3 will be interpreted where F is present as follows: 5.5 ≤ s < 6.0.
Claim 22 is rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention. Claim 22 For the purposes of examination, the third heat-treated material will be assumed to produce a “third heat-treated material” as opposed to a “second heat-treated material”. Claim 23 is rejected as being dependent on, and failing to cure the deficiencies of, rejected dependent claim 22.
Claim 23 is rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention. Claim 23 For the purposes of examination, the third heat-treated material will be assumed to produce a “third heat-treated material” as opposed to a “second heat-treated material”.
Claim Rejections - 35 USC § 103
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.
Claims 1-3 are rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1).
Regarding claim 1, Nakazawa describes a fluoride phosphor for use in a light-emitting material. The fluoride phosphor has a composition of A2+xMyMnzFn where A is Na and/or K (thus an alkali metal including K), M is Si and Al, -1 ≦ x ≦ 1 and 0.9 ≦ y + z ≦ 1.1 and 0.001 ≦ z ≦ 0.4 and 5 ≦ n ≦ 7. Nakazawa also mentions that preferably 10% mol or less of a constituent element is replaced with Al and Na, thus Al is included in a range of 0 to 0.1. Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Nakazawa is silent on the lattice constant of the phosphor, however this constant is an inherent property of the fluoride phosphor. Therefore, if one of ordinary skill in the art arrives at the fluoride phosphor having a first composition as claimed, then that fluoride phosphor would also have a lattice constant of 0.8138nm or larger. Additionally, it is well known in the art that KSF-based phosphors generally adopt a cubic crystal structure. Therefore, Nakazawa teaches the claimed “A light-emitting material comprising a fluoride phosphor having a first composition comprising: an alkali metal including K; Si; Al; Mn; and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si, Al, and Mn is in a range from 0.9 to 1.1, a number of moles of Al is in a range from greater than 0 to 0.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0, and the fluoride phosphor having, as a crystal structure, a cubic system crystal structure and having a lattice constant of 0.8138 nm or larger”.
Regarding claim 2, Nakazawa describes a fluoride phosphor for use in a light-emitting material. The fluoride phosphor has a composition of A2+xMyMnzFn where A is Na and/or K (thus an alkali metal including K), M is Si and Al, -1 ≦ x ≦ 1 and 0.9 ≦ y + z ≦ 1.1 and 0.001 ≦ z ≦ 0.4 and 5 ≦ n ≦ 7. Nakazawa also mentions that preferably 10% mol or less of a constituent element is replaced with Al and Na, thus Al is included in a range of 0 to 0.1. Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Nakazawa is silent on the absorption peak in an infrared absorption spectrum, however this absorption is an inherent property of the fluoride phosphor. Therefore, if one of ordinary skill in the art arrives at the fluoride phosphor having a first composition as claimed, then that fluoride phosphor would also have that absorption peak of 590 cm-1 to 610 cm-1 in an infrared absorption spectrum. Thus, Nakazawa teaches the claimed “A light-emitting material comprising a fluoride phosphor having a first composition comprising: an alkali metal including K; Si; Al; Mn; and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si, Al, and Mn is in a range from 0.9 to 1.1, a number of moles of Al is in a range from greater than 0 to 0.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0, and in an infrared absorption spectrum, the fluoride phosphor has an absorption peak in a wavenumber range from 590 cm-1 to 610 cm-1”.
Regarding claim 3, Nakazawa teaches the light-emitting material according to claim 1. Furthermore, when including or excluding sodium, the formula of the fluoride phosphor disclosed is A2+xMyMnzFn where A is Na and/or K (thus an alkali metal including K), M is Si and Al, -1 ≦ x ≦ 1 and 0.9 ≦ y + z ≦ 1.1 and 0.001 ≦ z ≦ 0.4 and 5 ≦ n ≦ 7. Nakazawa also mentions that preferably 10% mol or less of a constituent element is replaced with Al and Na, thus Al is included in a range of 0 to 0.1. Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Thus, Nakazawa teaches the claimed “The light-emitting material according to claim 1, wherein the fluoride phosphor has a composition represented by Formula (I): M2[SipAlqMnrFs] (I) where M represents an alkali metal and includes at least K, and p, q, r, and s satisfy 0.9 ≤ p + q + r ≤ 1.1, 0 < q ≤ 0.1, 0 < r ≤ 0.2, and 5.5 ≤ s ≤ 6.0.”.
Claim 1 is rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1) in view of Setlur et al (US PGPub 20160376499).
Regarding claim 1, Nakazawa describes a fluoride phosphor for use in a light-emitting material. The fluoride phosphor has a composition of A2+xMyMnzFn where A is Na and/or K (thus an alkali metal including K), M is Si and Al, -1 ≦ x ≦ 1 and 0.9 ≦ y + z ≦ 1.1 and 0.001 ≦ z ≦ 0.4 and 5 ≦ n ≦ 7. Nakazawa also mentions that preferably 10% mol or less of a constituent element is replaced with Al and Na, thus Al is included in a range of 0 to 0.1. Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Nakazawa is silent on the lattice constant of the phosphor.
Setlur discloses known lattice parameters in Table 1 for phosphors of K2SiF6 and K3AlF6 (8.184 and 8.405 Angstroms, respectively, or 0.8184 and 0.8405 nm). Setlur teaches that a phosphor composition of K2SiF6:Mn can be combined with a fluoride of composition A3[MF6] that has a lower water solubility such as K3AlF6 (paragraph [0024]). Paragraph [0022] discloses that these two compositions have acceptable lattice matching, and that the combination of these phosphors may improve moisture resistivity (paragraph [0021]). It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to combine these compositions due to their similar lattice constants and to improve moisture resistance. It would be expected that combination of these would not lower lattice parameter beyond 0.8184nm. Therefore, Nakazawa and Setlur teach the claimed “A light-emitting material comprising a fluoride phosphor having a first composition comprising: an alkali metal including K; Si; Al; Mn; and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si, Al, and Mn is in a range from 0.9 to 1.1, a number of moles of Al is in a range from greater than 0 to 0.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0, and the fluoride phosphor having, as a crystal structure, a cubic system crystal structure and having a lattice constant of 0.8138 nm or larger”.
Claim 1 is rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1) in view of Al Saghir et al., "Transparency through Structural Disorder: A New Concept for Innovative Transparent Ceramics", Chem. Mater. 2015, 27, 2, 508-514. https://doi.org/10.1021/cm5037106.
Regarding claim 1, Nakazawa describes a fluoride phosphor for use in a light-emitting material. The fluoride phosphor has a composition of A2+xMyMnzFn where A is Na and/or K (thus an alkali metal including K), M is Si and Al, -1 ≦ x ≦ 1 and 0.9 ≦ y + z ≦ 1.1 and 0.001 ≦ z ≦ 0.4 and 5 ≦ n ≦ 7. Nakazawa also mentions that preferably 10% mol or less of a constituent element is replaced with Al and Na, thus Al is included in a range of 0 to 0.1. Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Nakazawa is silent on the lattice constant of the phosphor, however this constant is an inherent property of the fluoride phosphor. Therefore, if one of ordinary skill in the art arrives at the fluoride phosphor having a first composition as claimed, then that fluoride phosphor would also have a lattice constant of 0.8138nm or larger. Additionally, it is well known in the art that KSF-phosphors generally adopt a cubic structure, but they can also form octahedral systems. Furthermore, Nakazawa teaches that their phosphor is for use in a wavelength conversion layer. The wavelength conversion layer may be a resin, glass, or ceramic matrix, and thus obvious to pick a ceramic-based matrix. Al Saghir teaches that transparency in materials such as ceramics is ensured by optical isotropy such as cubic crystal symmetry (see results in Fig. 3). It is well known in the art that transparency would be desired in a wavelength conversion layer for light penetration/emission. Thus, it would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select for cubic crystal structure KSF phosphors thus having optical isotropy within the ceramic matrix enabling better transparency as a light emitting material. Therefore, Nakazawa and Al Saghir teach the claimed “A light-emitting material comprising a fluoride phosphor having a first composition comprising: an alkali metal including K; Si; Al; Mn; and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si, Al, and Mn is in a range from 0.9 to 1.1, a number of moles of Al is in a range from greater than 0 to 0.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0, and the fluoride phosphor having, as a crystal structure, a cubic system crystal structure and having a lattice constant of 0.8138 nm or larger”.
Claims 4-5 is rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1) in view of Liu et al (CN105623656A).
Regarding claim 4, Nakazawa teaches the light-emitting material of claim 1. Nakazawa does not specify a case where the total number of moles of Si, Al and Mn is 1 when the total number of moles of the alkali metal is 2. Liu et al discloses a fluoride particle of similar structure to Nakazawa: A(2-x)Dx [X1-x-yAlxF6]yMn4+, wherein A is selected from Li, Na and K in the any one kind of or more. D is selected from any of Ba, Sr, Ca and Mg in the one kind of or more, X is selected from Si, Ge and Ti in the any one kind of or more, and x is more than or equal to 0.001 and less than or equal to 0.5, y is between 0.001 and 0.3. Furthermore, Liu also uses Al3+ to replace portions of “X” to influence the luminous center of the Mn crystal field, thereby adjusting light color performance and chroma luminance of the fluoride particle. In the embodiment 1 and subsequent examples 2-13, Liu discloses compositions where the alkali and alkaline metals add to 2 and the Si, Al, and Mn molar components sum to 1. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to synthesize the same phosphors without the addition of any alkaline metals with a predicted result of creating a KSAF-based phosphor.
Regarding claim 5, Nakazawa teaches the light-emitting material of claim 1, but specifies that Al is included below 0.1. As explained in the rejection of claim 4, one of ordinary skill in the art can use the teachings of Liu et al to arrive at a KSAF-based phosphor. Liu teaches in examples 1-3, 6-9, and 11 cases where Al is included within the claimed range of 0 to 0.06, and thus obvious to replicate synthesis with a predicted result of synthesizing a phosphor with adjusted light color performance and chroma luminance.
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1) in view of Niimi Tsuneto (JP2018087323A).
Nakazawa teaches the light-emitting material of claim 1 but does not disclose disposing an oxide on a surface of the fluoride phosphor. Tsuneto similarly teaches fluoride particles but discloses addition of a silicon compound to form a film-like material on the surface of the phosphor core. Tsuneto suggests the mass of the silicon compound should be 5-30 parts by mass with respect to 100 parts by mass of the phosphor, thus 5-30%. Tsuneto discloses examples of the silicon compound that include alkoxy silicon compounds. In example 4, Tsuneto uses tetraethoxysilane as the metal alkoxide and mixes it with an aqueous solution (liquid medium). The metal alkoxide through this process described by Tsuneto forms an oxide layer on the fluoride particles as disclosed in the final sentence of example 4. The surface covering improves adhesion between particles and resin in a light emitting device, thus improving durability of the device, since the resin is sensitive to high currents passing through. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to coat the fluoride particles of Nakazawa with an oxide derived from a metal alkoxide as taught by Tsuneto in order to improve adhesion of particles to a resin for use in a light-emitting device, thus improving the device’s durability. Therefore, Nakazawa and Tsuneto teach the claimed “The light-emitting material according to claim 1, further comprising an oxide disposed on at least a portion of a surface of the fluoride phosphor, wherein the oxide contains at least one element selected from the group consisting of Si, Al, Ti, Zr, Sn, and Zn, and a content percentage of the oxide is in a range from 2 mass% to 30 mass% in relation to the light-emitting material”.
Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1) in view of Niimi Tsuneto (JP2018087323A) as applied to claim 6 above, and further in view of Yoshida et al (US PGPub 20180134955).
Nakazawa and Tsuneto teach the light-emitting material of claim 6 but are silent on including a rare earth element. Yoshida similarly teaches KSF-based phosphors of Nakazawa but also discloses in paragraphs [0011] and [0012] that rare-earth phosphates are adhered to the fluorescent material particles (fluoride particles). Yoshida discloses La, Ce, Dy, and Gd can be used in paragraph [0035]. In examples 1-9, Yoshida discloses addition of La to the fluoride particle by using lanthanum phosphate in the mix. In paragraph [0017], Yoshida discloses that “by using the rare-earth phosphate-adhered fluoride fluorescent material particles may reduce the influence of the composition of the fluoride, and allow the resin included in the fluorescent member to sufficiently cure around its interface with the fluorescent material. This causes a better adhesion between the fluorescent material and the resin.” It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to include rare-earth phosphates adhered to the fluoride particles to allow for better adhesion between the fluorescent material and the resin for use in a light-emitting device. Thus, Nakazawa, Tsuneto, and Yoshida teach the claimed “The light-emitting material according to claim 6, wherein a rare earth phosphate containing at least one rare earth element selected from the group consisting of La, Ce, Dy and Gd is disposed on a surface of the fluoride phosphor, and the oxide is disposed on at least a portion of the surface of the fluoride phosphor with the rare earth phosphate interposed therebetween”.
Claim 8 is rejected under 35 U.S.C. 103 as being unpatentable over Nakazawa (WO 2020230742 A1) in view of Yoshida et al (US PGPub 20180134955).
Regarding claim 8, Nakazawa teaches the light-emitting material of claim 1 but is silent on including a rare earth element. Yoshida similarly teaches KSF-based phosphors of Nakazawa but also discloses in paragraphs [0011] and [0012] that rare-earth phosphates are adhered to the fluorescent material particles (fluoride particles). Yoshida discloses La, Ce, Dy, and Gd can be used in paragraph [0035]. In examples 1-9, Yoshida discloses addition of La to the fluoride particle by using lanthanum phosphate in the mix. In paragraph [0017], Yoshida discloses that “by using the rare-earth phosphate-adhered fluoride fluorescent material particles may reduce the influence of the composition of the fluoride, and allow the resin included in the fluorescent member to sufficiently cure around its interface with the fluorescent material. This causes a better adhesion between the fluorescent material and the resin.” It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to include rare-earth phosphates adhered to the fluoride particles to allow for better adhesion between the fluorescent material and the resin for use in a light-emitting device. Thus, Nakazawa and Yoshida teach the claimed “The light-emitting material according to claim 1, further comprising a rare earth phosphate disposed on at least a portion of the surface of the fluoride phosphor, wherein the rare earth phosphate contains at least one rare earth element selected from the group consisting of La, Ce, Dy and Gd.”.
Claim 9 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al (US PGPub 20160376499) in view of Liu et al., “Hydrophobic surface modification toward highly stable K2SiF6:Mn4+ phosphor for white light-emitting diodes”, Ceramics International, Volume 46, Issue 7, 2020, Pages 8811-8818, ISSN 0272-8842, https://doi.org/10.1016/j.ceramint.2019.12.123.
Regarding claim 9, Setlur teaches that a phosphor composition of K2SiF6:Mn can be combined with a fluoride of composition A3[MF6] that has a lower water solubility such as K3AlF6 (paragraph [0024]). Paragraph [0022] discloses that these two compositions have acceptable lattice matching, and that the combination of these phosphors may improve moisture resistivity (paragraph [0021]). In paragraphs [0043-0044] and [0047], Setlur describes combining K2SiF6:Mn and K3AlF6 in a water or oil bath. However, Setlur does not teach a heat treatment of these particles outside of drying at up to 300°C (paragraph [0039]). Liu similarly teaches a modification of previously created KSF-based particles whereby the temperature of modification occurs at 600°C, thus producing a heat-treated material. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to heat treat the mixture at 600°C to predictably produce a modified fluoride phosphor particle. Therefore, Setlur and Liu satisfy the claimed "A method for producing a light-emitting material, the method comprising: preparing first fluoride particles having a second composition comprising an alkali metal including K, Si, Mn, and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si and Mn is in a range from 0.9 to 1.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0; preparing second fluoride particles having a third composition comprising an alkali metal including K, Al, and F such that when a number of moles of Al is 1, a total number of moles of the alkali metal is in a range from 2 to 3, and a number of moles of F is in a range from 5 to 6; and subjecting a mixture of the first fluoride particles and the second fluoride particles to a first heat treatment in an inert gas atmosphere at a temperature in a range from 600ºC to 780ºC to produce a first heat-treated material.".
Claim 10 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al (US PGPub 20160376499) in view of Liu et al as applied to claim 9 above, and further in view of Rong-hui Liu et al (CN105623656A).
Regarding claim 10, Setlur and Liu teach the method for producing a light-emitting material of claim 9. Setlur and Liu et al 2019 do not specify the molar ratios of Si and Mn in regards to when the total number of moles of the alkali metal is 2. Rong-hui Liu teaches K2SiF6:Mn phosphors that can be modified with Al to create a phosphor of formula (see rejections of claims 4-5) A(2-x)Dx [X1-x-yAlxF6]yMn4+, wherein A is selected from Li, Na and K in the any one kind of or more. D is selected from any of Ba, Sr, Ca and Mg in the one kind of or more, X is selected from Si, Ge and Ti in the any one kind of or more, and x is more than or equal to 0.001 and less than or equal to 0.5, y is between 0.001 and 0.3. Furthermore, Liu also uses Al3+ to replace portions of “X” to influence the luminous center of the Mn crystal field, thereby adjusting light color performance and chroma luminance of the fluoride particle. Thus, to make K2SiF6:Mn, x would be = 0: A2[X1-yF6]yMn4+ where y indicates the amount of Mn present. From comparative example 1, Rong-hui teaches that the prepared K2SiF6:Mn is prepared according to K2Si0.85F6:0.15Mn4+. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to provide prepared K2SiF6:Mn as disclosed with a predictable result of synthesizing a heat-treated phosphor particle with improved moisture reactivity. Thus, Setlur, Liu, and Rong-hui Liu teach the claimed “The method for producing a light-emitting material according to claim 9, wherein in the preparing of the first fluoride particles, the total number of moles of Si and Mn in the second composition is 1 when the total number of moles of the alkali metal is 2”.
Claim 11 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al (US PGPub 20160376499) in view of Liu et al., “Hydrophobic surface modification toward highly stable K2SiF6:Mn4+ phosphor for white light-emitting diodes”, Ceramics International, Volume 46, Issue 7, 2020, Pages 8811-8818, ISSN 0272-8842, https://doi.org/10.1016/j.ceramint.2019.12.123 as applied to claim 9 above, and further in view of Niimi Tsuneto (JP2018087323A).
Setlur and Liu teach the method for producing a light-emitting material according to claim 9 but are silent on contacting the first heat-treated material with a first liquid medium. Tsuneto similarly teaches fluoride particles but discloses addition of a silicon compound to form a film-like material on the surface of the phosphor core. In example 4, Tsuneto uses tetraethoxysilane as the metal alkoxide and mixes it with an aqueous solution (liquid medium). The metal alkoxide through this process described by Tsuneto forms an oxide layer on the fluoride particles as disclosed in the final sentence of example 4. The surface covering improves adhesion between particles and resin in a light emitting device, thus improving durability of the device, since the resin is sensitive to high currents passing through. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to contact the heat-treated material with a first liquid medium to coat the heat-treated material with a surface covering to improve adhesion between particles and resin in a light emitting device, thus improving the durability of the device. Therefore, Setlur, Liu and Tsuneto teach the claimed “The method for producing a light-emitting material according to claim 9, further comprising causing the first heat-treated material to contact a first liquid medium”.
Claim 12 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al (US PGPub 20160376499) in view of Liu et al., “Hydrophobic surface modification toward highly stable K2SiF6:Mn4+ phosphor for white light-emitting diodes”, Ceramics International, Volume 46, Issue 7, 2020, Pages 8811-8818, ISSN 0272-8842, https://doi.org/10.1016/j.ceramint.2019.12.123 as applied to claim 9 above, and further in view of Osborne et al., “New red phosphor ceramic K2SiF6:Mn4+,” Optical Materials, Volume 107, 2020, 110140, ISSN 0925-3467, https://doi.org/10.1016/j.optmat.2020.110140.
Setlur and Liu teach the method according to claim 9 but are silent on second heat treatments. Osborne teaches a heat treatment of KSF-based phosphors at 400°C in order to purify the powder or a heat treatment at ~500°C to produce a ceramic from the powder. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to perform a second heat treatment at 400°C to purify the product or treatment at 500°C to produce a ceramic from the first heat-treated material. Thus, Setlur, Liu, and Osborne teach the claimed “The method for producing a light-emitting material according to claim 9, further comprising subjecting the first heat-treated material to a second heat treatment at a temperature in a range from 400ºC to 600ºC to produce a second heat-treated material”.
Claim 13 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al in view of Liu et al and Osborne et al as applied to claim 12 above, and further in view of Niimi Tsuneto (JP2018087323A).
Setlur, Liu and Osborne teach the method of claim 12 but are silent on disposing an oxide to the treated particles. Tsuneto similarly teaches fluoride particles but discloses addition of a silicon compound to form a film-like material on the surface of the phosphor core. In example 4, Tsuneto uses tetraethoxysilane as the metal alkoxide and mixes it with an aqueous solution (liquid medium). The metal alkoxide through this process described by Tsuneto forms an oxide layer on the fluoride particles as disclosed in the final sentence of example 4. The surface covering improves adhesion between particles and resin in a light emitting device, thus improving durability of the device, since the resin is sensitive to high currents passing through. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to dispose the surface of the heat-treated material with an oxide derived from a metal alkoxide to improve adhesion between particles and resin in a light emitting device, thus improving the durability of the device. Therefore, Setlur, Liu, Osborne and Tsuneto teach the claimed “The method for producing a light-emitting material according to claim 12, further comprising causing the second heat-treated material and a metal alkoxide containing at least one element selected from the group consisting of Si, Al, Ti, Zr, Sn, and Zn to come into contact in a liquid medium to thereby dispose an oxide derived from the metal alkoxide on at least a portion of a surface of the fluoride phosphor at an amount in a range from 2 mass% to 30 mass% relative to the light-emitting material.”.
Claim 14 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al in view of Liu et al and Osborne et al as applied to claim 12 above, and further in view of Yoshida et al (US PGPub 20180134955).
Setlur, Liu and Osborne teach the method of claim 12 but are silent on addition of a rare-earth phosphate disposed to the surface. Yoshida similarly teaches KSF-based phosphors of Nakazawa but also discloses in paragraphs [0011] and [0012] that rare-earth phosphates are adhered to the fluorescent material particles (fluoride particles). Yoshida discloses La, Ce, Dy, and Gd can be used in paragraph [0035]. In examples 1-9, Yoshida discloses addition of La to the fluoride particle by using lanthanum phosphate in the mix. In paragraph [0017], Yoshida discloses that “by using the rare-earth phosphate-adhered fluoride fluorescent material particles may reduce the influence of the composition of the fluoride, and allow the resin included in the fluorescent member to sufficiently cure around its interface with the fluorescent material. This causes a better adhesion between the fluorescent material and the resin.” It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to include rare-earth phosphates adhered to the heat-treated material to allow for better adhesion between the material and the resin for use in a light-emitting device. Thus, Setlur, Liu, Osborne, and Yoshida teach the claimed “The method for producing a light-emitting material according to claim 12, further comprising causing the second heat-treated material, rare earth ions including at least one type selected from the group consisting of La, Ce, Dy, and Gd, and phosphate ions to come into contact in a liquid medium to produce a second heat-treated material having a rare earth phosphate disposed on at least a portion of a surface of the second heat-treated material.”.
Claim 15 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al in view of Liu et al, Osborne et al, and Yoshida et al as applied to claim 14 above, and further in view of Niimi Tsuneto (JP2018087323A).
Setlur, Liu, Osborne, and Yoshida teach the method of claim 14. Setlur, Liu and Osborne are silent on disposing an oxide to the surface. Yoshida does teach that fillers can be included within the fluorescent member such as titanium or aluminum oxide (paragraph [0056]) at an amount of 0.01% by mass to 20% by mass relative to the resin but does not specify deriving it from a metal alkoxide. Tsuneto similarly teaches fluoride particles but discloses addition of a silicon compound to form a film-like material on the surface of the phosphor core. In example 4, Tsuneto uses tetraethoxysilane as the metal alkoxide and mixes it with an aqueous solution (liquid medium). The metal alkoxide through this process described by Tsuneto forms an oxide layer on the fluoride particles as disclosed in the final sentence of example 4. The surface covering improves adhesion between particles and resin in a light emitting device, thus improving durability of the device, since the resin is sensitive to high currents passing through. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to dispose the surface of the heat-treated material with an oxide derived from a metal alkoxide to improve adhesion between particles and resin in a light emitting device, thus improving the durability of the device. Therefore, Setlur, Liu, Obsorne, Yoshida, and Tsuneto teach the claimed “The method for producing a light-emitting material according to claim 14, further comprising causing the second heat-treated material on which the rare earth phosphate is disposed and a metal alkoxide containing at least one element selected from the group consisting of Si, Al, Ti, Zr, Sn, and Zn to come into contact in a liquid medium to thereby dispose, at an amount in a range from 2 mass% to 30 mass% in relation to the light-emitting material, an oxide derived from the metal alkoxide on at least a portion of a surface of the second heat-treated material on which the rare earth phosphate is attached.”.
Claims 16-20 are rejected under 35 U.S.C. 103 as being unpatentable over Setlur et al in view of Liu et al as applied to claim 9 above, and further in view of Yoshida et al (CN105462581A).
Regarding claim 16, Setlur and Liu teach the method of claim 9 but are silent on a pressurizing treatment and a heating treatment together with a second liquid medium. Yoshida et al in CN105462581A disclose a pressurizing treatment and a heating treatment of similar KSF-based phosphors to improve durability and dispersibility. This treatment occurs in a liquid medium containing fluoride and preferably an inorganic acid. Therefore, it would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to subject the heat-treated material under a simultaneous pressurizing and heating treatment in a liquid medium to produce another heat-treated material with predictably improved durability and dispersibility. Thus, Setlur, Liu and Yoshida teach the claimed “The method for producing a light-emitting material according to claim 9, further comprising subjecting the first heat-treated material to a pressurizing treatment and a heating treatment together with a second liquid medium to produce a third heat-treated material.”.
Regarding claim 17, Setlur, Liu and Yoshida teach the method of claim 16. Furthermore, Yoshida discloses that this heat treatment occurs at 100°C or more and below 600°C. In example 22, which teaches the heating and pressurizing treatment, Yoshida et al perform heating at 170°C. Thus, Setlur, Liu, and Yoshida teach the claimed “The method for producing a light-emitting material according to claim 16, wherein the heating treatment is carried out at a temperature of 100ºC or higher.”.
Regarding claim 18, Setlur, Liu and Yoshida teach the method of claim 16. Furthermore, Yoshida discloses that this pressurizing treatment occurs at 1.5MPa or more, more preferably 2.5MPa or more, and below 30MPa from durability viewpoints. In example 22, which teaches the heating and pressurizing treatment, Yoshida et al perform the heating of 170°C at a pressure of 2.3MPa. Thus, Setlur, Liu, and Yoshida teach the claimed “The method for producing a light-emitting material according to claim 16, wherein the pressurizing treatment is carried out at 1.6 MPa or higher.”.
Regarding claim 19, Setlur, Liu and Yoshida teach the method of claim 16. Yoshida discloses that the pressuring and heating treatment occurs in a liquid medium such as water, methanol, ethanol, isopropanol and the like. In example 22, Yoshida discloses that the treatment occurs in an aqueous environment. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select water from the list of provided liquid mediums to arrive at the invention as claimed. Thus, Setlur, Liu, and Yoshida satisfy the claimed “The method for producing a light-emitting material according to claim 16, wherein the second liquid medium contains water.”.
Regarding claim 20, Setlur, Liu and Yoshida teach the method of claim 16. Furthermore, Yoshida teaches the environment preferably contains an inorganic acid salt of potassium nitrate containing potassium ions. Yoshida discloses that the liquid medium comprises potassium hydro-fluoride and fluoride salt under “the condition that the concentration can be less than 10 mass % and not more than 25 mass %, preferably less than 15 mass % and not more than 20 mass %”. In example 22, Yoshida adds KHF2 dissolved in HF aqueous solution to the prepared fluoride phosphor. Thus, Setlur, Liu, and Yoshida teach the claimed “The method for producing a light-emitting material according to claim 16, wherein the second liquid medium contains potassium”.
Claim 21 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur in view of Liu et al and Yoshida et al (CN105462581A) as applied to claim 16 above, and further in view of Niimi Tsuneto (JP2018087323A).
Setlur, Liu, and Yoshida teach the method of claim 16 but are silent on addition of an oxide disposed to the surface. Tsuneto similarly teaches fluoride particles but discloses addition of a silicon compound to form a film-like material on the surface of the phosphor core. In example 4, Tsuneto uses tetraethoxysilane as the metal alkoxide and mixes it with an aqueous solution (liquid medium). The metal alkoxide through this process described by Tsuneto forms an oxide layer on the fluoride particles as disclosed in the final sentence of example 4. The surface covering improves adhesion between particles and resin in a light emitting device, thus improving durability of the device, since the resin is sensitive to high currents passing through. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to dispose the surface of the heat-treated material with an oxide derived from a metal alkoxide to improve adhesion between particles and resin in a light emitting device, thus improving the durability of the device. Therefore, Setlur, Liu, Yoshida, and Tsuneto teach the claimed “The method for producing a light-emitting material according to claim 16, further comprising causing the third heat-treated material and a metal alkoxide containing at least one element selected from the group consisting of Si, Al, Ti, Zr, Sn, and Zn to come into contact in a liquid medium to thereby dispose an oxide derived from the metal alkoxide on at least a portion of a surface of the fluoride phosphor at an amount in a range from 2 mass% to 30 mass% relative to the light-emitting material”.
Claim 22 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur in view of Liu et al and Yoshida et al (CN105462581A) as applied to claim 16 above, and further in view of Yoshida et al (US PGPub 20180134955).
Setlur, Liu, and Yoshida (CN document) teach the method of claim 16 but are silent on addition of a rare earth phosphate disposed on a surface of the heat-treated material. In US PGPub 20180134955, Yoshida similarly teaches KSF-based phosphors of Nakazawa but also discloses in paragraphs [0011] and [0012] that rare-earth phosphates are adhered to the fluorescent material particles (fluoride particles). Yoshida discloses La, Ce, Dy, and Gd can be used in paragraph [0035]. In examples 1-9, Yoshida discloses addition of La to the fluoride particle by using lanthanum phosphate in the mix. In paragraph [0017], Yoshida discloses that “by using the rare-earth phosphate-adhered fluoride fluorescent material particles may reduce the influence of the composition of the fluoride, and allow the resin included in the fluorescent member to sufficiently cure around its interface with the fluorescent material. This causes a better adhesion between the fluorescent material and the resin.” It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to include rare-earth phosphates adhered to the heat-treated material to allow for better adhesion between the material and the resin for use in a light-emitting device. Thus, Setlur, Liu, and Yoshida (in both referenced documents) teach the claimed “The method for producing a light-emitting material according to claim 16, further comprising causing the third heat-treated material, rare earth ions including at least one type selected from the group consisting of La, Ce, Dy, and Gd, and phosphate ions to come into contact in a liquid medium to produce a second heat-treated material having a rare earth phosphate disposed on at least a portion of a surface of the second heat-treated material”.
Claim 23 is rejected under 35 U.S.C. 103 as being unpatentable over Setlur in view of Liu et al, Yoshida et al (CN105462581A), and Yoshida et al (US PGPub 20180134955) as applied to claim 22 above, and further in view of Niimi Tsuneto (JP2018087323A).
Setlur, Liu, and Yoshida teach the method of claim 22 but are silent on including a metal alkoxide disposed on the surface. Tsuneto similarly teaches fluoride particles but discloses addition of a silicon compound to form a film-like material on the surface of the phosphor core. In example 4, Tsuneto uses tetraethoxysilane as the metal alkoxide and mixes it with an aqueous solution (liquid medium). The metal alkoxide through this process described by Tsuneto forms an oxide layer on the fluoride particles as disclosed in the final sentence of example 4. The surface covering improves adhesion between particles and resin in a light emitting device, thus improving durability of the device, since the resin is sensitive to high currents passing through. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to dispose the surface of the heat-treated material with an oxide derived from a metal alkoxide to improve adhesion between particles and resin in a light emitting device, thus improving the durability of the device. Therefore, Setlur, Liu, Yoshida (both documents), and Tsuneto teach the claimed “The method for producing a light-emitting material according to claim 22, further comprising causing the third heat-treated material on which the rare earth phosphate is disposed and a metal alkoxide containing at least one element selected from the group consisting of Si, Al, Ti, Zr, Sn, and Zn to come into contact in a liquid medium to thereby dispose, at an amount in a range from 2 mass% to 30 mass% in relation to the light-emitting material, an oxide derived from the metal alkoxide on at least a portion of a surface of the second heat-treated material on which the rare earth phosphate is attached.”.
Double Patenting
The nonstatutory double patenting rejection is based on a judicially created doctrine grounded in public policy (a policy reflected in the statute) so as to prevent the unjustified or improper timewise extension of the “right to exclude” granted by a patent and to prevent possible harassment by multiple assignees. A nonstatutory double patenting rejection is appropriate where the conflicting claims are not identical, but at least one examined application claim is not patentably distinct from the reference claim(s) because the examined application claim is either anticipated by, or would have been obvious over, the reference claim(s). See, e.g., In re Berg, 140 F.3d 1428, 46 USPQ2d 1226 (Fed. Cir. 1998); In re Goodman, 11 F.3d 1046, 29 USPQ2d 2010 (Fed. Cir. 1993); In re Longi, 759 F.2d 887, 225 USPQ 645 (Fed. Cir. 1985); In re Van Ornum, 686 F.2d 937, 214 USPQ 761 (CCPA 1982); In re Vogel, 422 F.2d 438, 164 USPQ 619 (CCPA 1970); In re Thorington, 418 F.2d 528, 163 USPQ 644 (CCPA 1969).
A timely filed terminal disclaimer in compliance with 37 CFR 1.321(c) or 1.321(d) may be used to overcome an actual or provisional rejection based on nonstatutory double patenting provided the reference application or patent either is shown to be commonly owned with the examined application, or claims an invention made as a result of activities undertaken within the scope of a joint research agreement. See MPEP § 717.02 for applications subject to examination under the first inventor to file provisions of the AIA as explained in MPEP § 2159. See MPEP § 2146 et seq. for applications not subject to examination under the first inventor to file provisions of the AIA . A terminal disclaimer must be signed in compliance with 37 CFR 1.321(b).
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Claims 1-3, 5, 9, 11, and 12 provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1, 5, 8, 2, 13, 14, and 17, respectively (see table below, examiner underlined differences in claimed language for ease of comparison between applications), of copending Application No. 18258737 (reference application). Although the claims at issue are not identical, they are not patentably distinct from each other because the main distinction in language arises from claimed ranges for presence of F between the instant application 18565218 and the copending reference application 18258737. The copending application ‘737 allows for F to be present in a range of 5.9 to 6.1 while the instant application allows for F to be present in a range of 5.5 to less than 6.0. However, overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Additionally, examples 1-5 in the copending application ‘737 disclose KSiAlFMn phosphors where F is present in a range below 6.0 and above 5.5 where all other ranges for K, Si, Al, and Mn hold true as claimed. The same holds true for the case of Al presence in claim 5 of the instant ‘218 and claim 2 of the copending case ’737. Thus, it would have been obvious to select from any of these examples to arrive at the instant invention as claimed. This is a provisional nonstatutory double patenting rejection because the patentably indistinct claims have not in fact been patented.
Claim
Instant Application 18565218
Claim
Reference Application 18258737
1
A light-emitting material comprising a fluoride phosphor having a first composition comprising: an alkali metal including K; Si; Al; Mn; and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si, Al, and Mn is in a range from 0.9 to 1.1, a number of moles of Al is in a range from greater than 0 to 0.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0, and the fluoride phosphor having, as a crystal structure, a cubic system crystal structure and having a lattice constant of 0.8138 nm or larger
1
A fluoride phosphor, having a first composition which comprises an alkali metal containing K, Si, Al, Mn, and F, wherein in the first composition, when a total number of moles of the alkali metal is 2: a total number of moles of Si, Al, and Mn is 0.9 or more and 1.1 or less; a number of moles of Al is more than 0 and 0.1 or less; a number of moles of Mn is more than 0 and 0.2 or less; and a number of moles of F is 5.9 or more and 6.1 or less, and the fluoride phosphor has a crystal structure of cubic system, and a lattice constant of not less than 0.8138 nm
Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Additionally, examples 1-5 in the copending application ‘737 disclose KSiAlFMn phosphors where F is present in a range below 6.0 and above 5.5 where all other ranges for K, Si, Al, and Mn hold true as claimed. Thus, it would have been obvious to select from any of these examples to arrive at the instant invention as claimed.
2
A light-emitting material comprising a fluoride phosphor having a first composition comprising: an alkali metal including K; Si; Al; Mn; and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si, Al, and Mn is in a range from 0.9 to 1.1, a number of moles of Al is in a range from greater than 0 to 0.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0, and in an infrared absorption spectrum, the fluoride phosphor has an absorption peak in a wavenumber range from 590 cm-1 to 610 cm-1
5
The fluoride phosphor according to claim 1, whrein the fluoride phosphor has an absorption peak in a wavenumber range of 590 cm-1 to 610 cm-1 in an infrared absorption spectrum
Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed. Additionally, examples 1-5 in the copending application ‘737 disclose KSiAlFMn phosphors where F is present in a range below 6.0 and above 5.5 where all other ranges for K, Si, Al, and Mn hold true as claimed. Thus, it would have been obvious to select from any of these examples to arrive at the instant invention as claimed.
3
The light-emitting material according to claim 1, wherein the fluoride phosphor has a composition represented by Formula (I): M2[SipAlqMnrFs] (I) where M represents an alkali metal and includes at least K, and p, q, r, and s satisfy 0.9 ≤ p + q + r ≤ 1.1, 0 < q ≤ 0.1, 0 < r ≤ 0.2, and 5.5 ≤ s ≤ 6.0.
8
The fluoride phosphor according to claim 1, wherein the fluoride phosphor has a composition represented by the following Formula (I): M2[SipAlqMnrFs] (I) wherein, M represents an alkali metal and contains at least K; and p, q, r, and s satisfy 0.9 ≤ p + q + r ≤ 1.1, 0 < q ≤ 0.1, 0 < r ≤ 0.2, and 5.9 ≤ s ≤ 6.1.
Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed.
5
The light-emitting material according to claim 1, wherein the number of moles of Al in the first composition is in a range from greater than 0 to 0.06
2
The fluoride phosphor according to claim 1, wherein the number of moles of Al in the first composition is more than 0 but 0.03 or less
9
A method for producing a light-emitting material, the method comprising: preparing first fluoride particles having a second composition comprising an alkali metal including K, Si, Mn, and F such that when a total number of moles of the alkali metal is 2, a total number of moles of Si and Mn is in a range from 0.9 to 1.1, a number of moles of Mn is in a range from greater than 0 to 0.2, and a number of moles of F is in a range from 5.5 to less than 6.0; preparing second fluoride particles having a third composition comprising an alkali metal including K, Al, and F such that when a number of moles of Al is 1, a total number of moles of the alkali metal is in a range from 2 to 3, and a number of moles of F is in a range from 5 to 6; and subjecting a mixture of the first fluoride particles and the second fluoride particles to a first heat treatment in an inert gas atmosphere at a temperature in a range from 600ºC to 780ºC to produce a first heat-treated material.
13
A method of producing a fluoride phosphor, the method comprising: providing first fluoride particles having a second composition which comprises an alkali metal containing K, Si, Mn, and F, and in which, when a total number of moles of the alkali metal is 2: a total number of moles of Si and Mn is 0.9 or more and 1.1 or less; a number of moles of Mn is more than 0 and 0.2 or less; and a number of moles of F is 5.9 or more and 6.1 or less; providing second fluoride particles having a third composition which comprises an alkali metal containing K, Al, and F, and in which, when a number of moles of Al is 1: a total number of moles of the alkali metal is 2 or more and 3 or less; and a number of moles of F is 5 or more and 6 or less; and obtaining a first heat-treated product by performing a first heat treatment of a mixture of the first fluoride particles and the second fluoride particles in an inert gas atmosphere at a temperature of 600°C or higher and 780°C or lower.
Overlapping ranges have been held to present a prima facie case of obviousness over the prior art. It would have been prima facie obvious to one of ordinary skill in the art, as of the effective filing date, to select from the overlapping portion of the range to arrive at the invention as claimed.
11
The method for producing a light-emitting material according to claim 9, further comprising causing the first heat-treated material to contact a first liquid medium
14
The method of producing a fluoride phosphor according to claim 13, the method further comprising bringing the first heat-treated product obtained by the first heat treatment into contact with a liquid medium
12
The method for producing a light-emitting material according to claim 9, further comprising subjecting the first heat-treated material to a second heat treatment at a temperature in a range from 400ºC to 600ºC to produce a second heat-treated material
17
The method of producing a fluoride phosphor according to claim 14, the method further comprising, after bringing the first heat-treated product into contact with the liquid medium, obtaining a second heat-treated product by bringing the first heat-treated product into contact with a fluorine-containing substance and performing a second heat treatment at a temperature of 400°C or higher
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure. Lili Liu et al., “A Reverse Strategy to Restore the Moisture-deteriorated Luminescence Properties and Improve the Humidity Resistance of Mn4+-doped Fluoride Phosphors”, Chem. Asian J.2020, 15, 3326 provides a separate heat-treatment step at 100°C or higher, in water, and with potassium to aid protection properties of KSF-based fluorides but does not provide pressurizing details.
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/NWFG/Examiner, Art Unit 1759
/MELVIN C. MAYES/Supervisory Patent Examiner, Art Unit 1759
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