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
Receipt is acknowledged of certified copies of papers required by 37 CFR 1.55.
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: S40 (see Figure 1).
The description recites S10 (see line 9 on page 7), S20 (see line 30 on page 7), and S30 (see line 13 on page 8), but the heat-treating step discussed in lines 18-23 on page 8 is not identified by a reference sign.
The drawings are objected to because “MgO (based on w wet process 46) + SiC fiber” should be replaced with “MgO (based on a wet process) + SiC fiber” in Figure 3.
The column header appears to contain a conversion error. The value 46 appearing in the header is the porosity reported in the adjacent column of the same table. Additionally, note the “w”/“a” issue.
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
Applicant is reminded of the proper language and format for an abstract of the disclosure.
The abstract should be in narrative form and generally limited to a single paragraph on a separate sheet within the range of 50 to 150 words in length. The abstract should describe the disclosure sufficiently to assist readers in deciding whether there is a need for consulting the full patent text for details.
The language should be clear and concise and should not repeat information given in the title. It should avoid using phrases which can be implied, such as, “The disclosure concerns,” “The disclosure defined by this invention,” “The disclosure describes,” etc. In addition, the form and legal phraseology often used in patent claims, such as “means” and “said,” should be avoided.
The abstract of the disclosure is objected to because it uses the implied phrase “The present disclosure relates to”. A corrected abstract of the disclosure is required and must be presented on a separate sheet, apart from any other text. See MPEP § 608.01(b).
The disclosure is objected to because of the following informalities:
In line 11 on page 2, “in the case of power form” should be replaced with “in the case of powder form”.
In line 25 on page 3, “In the step of preparing the ceramic power” should be replaced with “In the step of preparing the ceramic powder”.
In lines 21-23 on page 7, “is dissolved in distilled water synthesize powder using a wet preparation process” should be replaced with “is dissolved in distilled water to synthesize powder using a wet preparation process”.
In lines 27-28 on page 7, “has a powder form in a char state includes organic residues” should be replaced with “has a powder form in a char state including organic residues”.
In line 14 on page 8, “the surficial area of the molded body” should be replaced with “the surface area of the molded body” for consistency with line 8 on page 4 and with claim 10.
Appropriate correction is required.
Claim Objections
Claims 1-14 are objected to because of the following informalities:
In claim 1, the introductory clause “As a molded body that is stable in a heat storage and release cycle by adding ceramic fibers” duplicates the recitation of ceramic fibers in the body of the claim and should be deleted, such that the preamble recites “A thermochemical heat storage molded body comprising:”.
In claim 2, “the ceramic powder mixed with ceramic fibers” should be replaced with “the ceramic powder mixed with the ceramic fibers” for consistency with claim 1.
In claim 3, “the ceramic fiber is” should be replaced with “the ceramic fibers are” for consistency with claim 1.
In claim 3, “a powder of a char state including an organic compound” should be replaced with “a powder in a char state, the char including an organic compound”, to make clear that the organic compound is included in the char rather than being a separate constituent of the powder. See lines 26-28 on page 7 and line 20 on page 8.
In claim 4, the introductory clause “As a method for manufacturing a molded body that is stable in a heat storage and release cycle by adding ceramic fibers” should be deleted, such that the preamble recites “A method for manufacturing a thermochemical heat storage molded body comprising steps of:”.
In claim 4, “pressing and molding a mixed powder” should be replaced with “pressing and molding a mixed powder to form a molded body”, and “manufacturing the manufactured molded body in the form of a porous molded body by high-temperature heat treatment” should be replaced with “manufacturing the thermochemical heat storage molded body in the form of a porous molded body by high-temperature heat treatment of the molded body”. These corrections provide antecedent basis for the molded body that is heat treated and for the recitations of the molded body in claims 10, 12, and 14.
In claim 5, “the ceramic power” should be replaced with “the ceramic powder”.
In claim 6, “the wet process” presupposes that the ceramic powder synthesized by a wet process, rather than the commercially available powder, is the powder prepared in claim 5, but claim 6 does not recite that selection. Claim 6 should expressly recite the selection, for example: “wherein the ceramic powder is the ceramic powder synthesized by the wet process, and the wet process is at least one of a Pechini method, a sol-gel method and a Colloidal process”.
In claim 7, “in the case of the commercially available powder” presupposes that the commercially available powder is the powder prepared in claim 5 without expressly reciting that selection. Claim 7 should expressly recite the selection, for example: “wherein the ceramic powder is the commercially available powder, and in the step of mixing ceramic fibers with the ceramic powder, a pore-forming agent is added to form a porous structure”.
In claim 8, “the ceramic fiber is” should be replaced with “the ceramic fibers are” for consistency with claim 4.
In claim 8, “in the case of the powder synthesized by a wet process, the powder in a char state including an organic compound is mixed with the ceramic fibers” presupposes that the ceramic powder synthesized by a wet process is the powder prepared in claim 5 without expressly reciting that selection, and does not make clear whether the organic compound is included in the char or is a separate constituent of the powder. Claim 8 should be revised, for example: “wherein the ceramic powder is the ceramic powder synthesized by the wet process and is a powder in a char state, the char including an organic compound, and in the step of mixing ceramic fibers with the ceramic powder, the powder in the char state is mixed with the ceramic fibers”.
In claim 9, “the char powder” should be replaced with “the powder in the char state” for consistency with claim 8.
In claim 10, “the thickness thereof is determined according to the amount of the powder” should be replaced with “the thickness thereof is determined according to the amount of the mixed powder” for consistency with claim 4.
In claim 11, “for MgO powder preparation via the Pechini method” presupposes both that the wet process of claim 6 is the Pechini method and that the ceramic powder is the MgO powder rather than the CaO powder, without expressly reciting either selection. Claim 11 should expressly recite the selections, for example: “wherein the ceramic powder is a MgO powder, the wet process is the Pechini method, and preparation of the MgO powder comprises dissolving magnesium nitrate in distilled water, adding citric acid to facilitate synthesis of a solution to which nitrate is added, and using ammonium hydroxide to adjust the pH”. See also the rejection of claim 11 under 35 U.S.C. 112(b) below regarding the recitation “a proper level”.
In claim 12, “the step of manufacturing a porous molded body by heat treating the manufactured molded body at high temperatures” should be replaced with “the step of manufacturing the thermochemical heat storage molded body in the form of a porous molded body by high-temperature heat treatment” for consistency with claim 4.
In claim 12, “organic residues included in char” should be replaced with “organic residues included in the char” for consistency with claim 8.
In claim 13, “the manufactured porous molded body” should be replaced with “the porous molded body” for consistency with claim 4.
In claim 14, “the step of heat treating the manufactured molded body, the manufactured molded body at high temperatures is performed in air at 800 °C to 1300 °C for 2 to 5 hours” is grammatically incomplete. The clause should be revised, for example to recite “the high-temperature heat treatment is performed in air at 800 °C to 1300 °C for 2 to 5 hours”, for consistency with claim 4.
Appropriate correction is required.
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.
Claim 11 is rejected under 35 U.S.C. 112(b) as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor regards as the invention.
The term “a proper level” in claim 11 is a relative term which renders the claim indefinite. The term “a proper level” is not defined by the claim, the specification does not provide a standard for ascertaining the requisite degree, and one of ordinary skill in the art would not be reasonably apprised of the scope of the invention. Specifically, claim 11 recites that “ammonium hydroxide is used to adjust the pH to a proper level” but recites no pH value, no pH range, and no property by reference to which a pH would be proper. The specification repeats the same phrase without further definition. See lines 13-15 on page 4 and lines 24-25 on page 7. The pH to which a citrate-nitrate solution is adjusted in a Pechini synthesis varies with the metal cation, the chelating agent, and the target product, and the art does not recognize a single proper pH for such syntheses. For purposes of examination, claim 11 is interpreted as requiring that ammonium hydroxide is used to adjust the pH of the solution, without limitation as to the resulting pH.
Claim Interpretation
Preamble of claims 1 and 4. The recitation “thermochemical heat storage molded body” is given patentable weight. Thermochemical heat storage is distinguished in the specification from sensible heat storage and latent heat storage as storage by way of a reversible chemical conversion. See lines 22-29 on page 1. Accordingly, the recitation requires that the ceramic powder be capable of storing and releasing heat by a reversible chemical reaction, and a ceramic powder that stores heat only as sensible heat or latent heat does not satisfy claims 1 and 4.
The recitation “molded body” is likewise given patentable weight, as to the structure implied by the term. See MPEP 2113. The term requires that the ceramic powder and the ceramic fibers be consolidated into a coherent body, but claim 1 does not require that any particular molding operation be performed.
The introductory clause “As a molded body that is stable in a heat storage and release cycle by adding ceramic fibers” in claim 1, and the corresponding clause in claim 4, are statements of an intended result and are not given patentable weight. The clauses recite no structure or step beyond the ceramic fibers already recited in the bodies of the claims. Should applicant assert that the clauses are limiting, applicant is advised that “stable” is not defined by the claims and that the specification provides no standard for ascertaining the requisite degree of stability, the only quantification being the conversion rates over ten cycles reported in Figure 6.
“Ceramic powder” in claims 1, 3-5, and 8. The specification describes the ceramic powder as being composed of a MgO powder, a CaO powder, and the like. See lines 9-12 on page 7. Consistent with the ordinary meaning of the term, the recitation is interpreted to require a powder of a ceramic material, that is, a powder of an inorganic, non-metallic material.
The recitation is not interpreted to require that the powder be phase pure or free of other constituents. Claim 3 recites a powder in a char state including an organic compound as one species of the ceramic powder, and the specification describes the powder synthesized by the wet powder preparation process as including organic residues. See lines 25-28 on page 7.
The recitation is not interpreted to encompass a powder of a material that is not itself a ceramic and from which a ceramic is subsequently obtained. Magnesium hydroxide and calcium hydroxide are hydroxides, not oxides, and a powder of magnesium hydroxide or calcium hydroxide is a precursor of a ceramic powder rather than a ceramic powder. Note that the thermochemical heat storage recited in the preambles proceeds by dehydration of a hydroxide to an oxide and rehydration of that oxide, so that the material of the claimed molded body is present as the oxide in the heat-stored state and as the hydroxide in the heat-released state. The recitation is satisfied when the material is in the oxide state, and a molded body that is cycled between the two states is not removed from the recitation by reason of the hydroxide state.
“Ceramic fibers” in claims 1 and 4. These claims recite ceramic fibers without qualification. Consistent with the ordinary meaning of the term, the recitation is interpreted to require a fiber of a ceramic material, that is, a fiber of an inorganic, non-metallic material.
Glass fibers are not interpreted to be ceramic fibers. A glass is an amorphous material characterized by a glass transition, and glass is conventionally distinguished from ceramics both in the art and in commercial practice. E glass fiber and other glass fibers are accordingly outside the recitation.
A fiber of a naturally occurring mineral that has not been converted to a ceramic, such as a fiber of an unfired clay mineral, is not interpreted to be a ceramic fiber.
Refractory ceramic fibers are interpreted to be within the recitation. Fibers of that class, including alumina silicate and other aluminosilicate fibers of the type conventionally designated and sold as ceramic fiber, are within the recitation notwithstanding that such fibers may be substantially vitreous, because they are so designated and understood in the art.
Claim 2. Claim 2 is a product-by-process claim. The claim is directed to the thermochemical heat storage molded body of claim 1, not to a process, and is not limited to the manipulations of the recited steps but only to the structure implied by those steps. See MPEP 2113 and In re Thorpe, 777 F.2d 695 (Fed. Cir. 1985). The structure implied by “subjected to pressure molding and high-temperature heat treatment to form a porous molded body shape” is a consolidated and sintered body having porosity, with the ceramic fibers distributed within the sintered ceramic matrix. Claim 2 recites no numerical limit on porosity.
“High-temperature heat treatment” in claims 2, 4, and 12. The term is not considered to be a relative term that renders the claims indefinite. Heat treatment of a green ceramic body at high temperature is understood in the art to refer to firing at a sintering-range temperature for the ceramic in question, and the specification is consistent with that understanding. See lines 21-23 on page 8. The term is being interpreted accordingly.
“At least one of” in claims 3, 6, 8, and 11. The recitations “at least one of an SiC fiber, an Al2O3 fiber and a ZrO2 fiber”, “at least one of a powder of a char state including an organic compound, a MgO powder, and a CaO powder”, “at least one of a Pechini method, a sol-gel method and a Colloidal process”, and “at least one of a MgO powder and a CaO powder” are interpreted as reciting alternatives, such that each recitation is satisfied by any one member of the recited group. The specification describes and exemplifies single members of each group rather than combinations. See lines 16-31 on page 7, for example.
“Char state including an organic compound” in claims 3, 8, and 12. The specification describes the powder produced by the wet powder preparation process as including organic residues and as having a powder form in a char state. See lines 25-28 on page 7. The specification further describes the organic residues as being included in the char. See line 20 on page 8. Char is understood in the art to be the carbonaceous residue that remains after organic matter is thermally decomposed. Consistent with that meaning and with the description above, the recitation is interpreted to require a ceramic powder that includes char, the char retaining an organic compound.
The recitation is not interpreted to require any particular carbon content or degree of thermal decomposition, or to exclude a powder that has been calcined. The specification identifies no carbon content, no extent of decomposition, and no calcination condition by reference to which the char state begins or ends.
The recitation is not interpreted to require that the organic compound function as a pore-forming agent. Claim 12 separately recites that organic residues included in the char are removed to form pores during the heat treatment, and claims 3 and 8 are not interpreted to include that requirement.
The recitation is not interpreted to be limited as to how the char came to be present in the powder. The recitation is directed to the state of the powder rather than to the history of the powder, and the specification describes no step by which the char is formed. The description of the wet powder preparation process proceeds from dissolving magnesium nitrate in distilled water, adding citric acid, and adjusting the pH directly to the statement that the resulting powder includes organic residues, without reciting any pyrolysis, carbonization, drying, or calcination operation, and without reciting any temperature at which such an operation is performed. See lines 21-28 on page 7. Accordingly, a ceramic powder to which a separately prepared char has been added is within the recitation, provided that the added char retains an organic compound.
The requirement that the powder include char, and that the char retain an organic compound, is nonetheless a limitation of substance. A powder to which an organic material that has not been thermally decomposed has been added is not a powder in a char state, and a powder to which a carbonaceous material retaining no organic compound has been added does not satisfy the further requirement that the char include an organic compound. Of the pore-forming agents identified in the specification, starch is not a residue of thermal decomposition, and carbon black and graphite are not understood to retain an organic compound. See lines 13-15 on page 7.
Claims 7 and 8 remain distinct under this interpretation. Claim 7 is directed to the branch of the process in which the commercially available powder is prepared and requires that a pore-forming agent be added to form a porous structure. Claim 8 is directed to the branch in which the powder synthesized by the wet process is prepared and imposes no pore-forming requirement. See the objections to claims 7 and 8 above.
Claim 3 recites the char-state powder without reference to a wet process. Claim 3 is therefore not limited as to the source of the powder or as to the origin of the char. Claim 8 requires that the char-state powder be the powder synthesized by the wet process, but likewise imposes no requirement as to the origin of the char within that powder.
Selections implied in claims 6, 7, 8, and 11. Claim 5 recites that either a ceramic powder synthesized by a wet process or a commercially available powder is prepared. Claims 6 and 8 each recite limitations applicable only where the ceramic powder synthesized by a wet process is prepared, and claim 7 recites a limitation applicable only where the commercially available powder is prepared, but none of these claims expressly recites which alternative is selected. Claim 11 further recites limitations applicable only where the wet process of claim 6 is the Pechini method and where the ceramic powder is a MgO powder, without expressly reciting either selection.
For purposes of examination, each of these claims is interpreted as expressly reciting the selection that its added limitations presuppose. Claims 6, 8, and 11 are interpreted as requiring that the ceramic powder prepared in claim 5 is the ceramic powder synthesized by a wet process; claim 7 is interpreted as requiring that the ceramic powder prepared in claim 5 is the commercially available powder; and claim 11 is further interpreted as requiring that the wet process is the Pechini method and that the ceramic powder is a MgO powder. See the objections to claims 6, 7, 8, and 11 above.
Claim 10. The recitations that “the surface area of the molded body is determined by the surface area of the mold” and that “the thickness thereof is determined according to the amount of the powder” describe consequences of placing the mixed powder into a mold and pressing it. Beyond the recited placement into a mold and pressing, claim 10 does not require any further step.
Claim Rejections - 35 USC § 102
The following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
Claim 1 is rejected under 35 U.S.C. 102(a)(1) as being anticipated by US 2022/0112421 A1 (“Kai”).
Regarding claim 1, Kai discloses a thermochemical heat storage molded body (a plate-shaped chemical heat storage; see [0057]; the heat storage material utilizing heat storage when magnesium hydroxide is dehydrated and converted to magnesium oxide and heat dissipation when magnesium oxide is hydrated and converted to magnesium hydroxide; see [0030]) comprising:
ceramic powder (magnesium oxide; see [0029], [0030], [0060], and [0061]); and
ceramic fibers mixed with the ceramic powder (4 kg of silica-alumina fibers added to 10 kg of kneaded magnesium hydroxide powder and further kneaded to obtain a paste-like chemical heat storage material composition; see [0057]; see also the alumina silicate fiber of [0037] and [0040]).
In Example 1, water is added to 10 kg of magnesium hydroxide powder and kneaded, 4 kg of silica-alumina fibers are added and the mixture is further kneaded to obtain a paste-like composition having a water content of about 40%, the paste is applied by a rolling machine onto an expanded metal substrate so as to fill a mesh of the metal lath plate, and the resulting article is cut, dried at 120 °C for 2 hours, and cut into pieces of 50×50 mm to obtain a plate-shaped chemical heat storage having a thickness of 0.7 mm, the density of the supported heat storage material composition being 0.95 g/cm3 (see [0057]).
The plate-shaped chemical heat storage of Example 1 is thereafter subjected to a durability test in which one cycle consists of a dehydration treatment and a hydration treatment, the dehydration treatment being carried out in the air at 400 °C (see [0060] and Table 1). The dehydration ratio is calculated assuming that the initial magnesium hydroxide is completely converted to magnesium oxide as 100% (see [0061]), and Example 1 exhibits a dehydration ratio of 96% in the first cycle (see Table 2). The magnesium of the Example 1 body is accordingly present as magnesium oxide, which is a powder of an inorganic, non-metallic material and therefore a ceramic powder. See the Claim Interpretation section above.
Regarding the recitation “molded body”, the body of Example 1 is a coherent plate of the recited thickness and density in which the ceramic powder and the ceramic fibers are consolidated (see [0057]). Kai further discloses that the supporting can be carried out by compacting the powder of the heat storage material composition together with the substrate (see [0043]). As set forth in the Claim Interpretation section above, the recitation requires that the ceramic powder and the ceramic fibers be consolidated into a coherent body but does not require that any particular molding operation be performed. See MPEP 2113.
Regarding the recitation “ceramic fibers”, the silica-alumina fibers of Example 1 are aluminosilicate fibers of the type conventionally designated and sold as ceramic fiber, and are accordingly within the recitation. It is noted that Kai itself recites alumina silicate fiber separately from glass fiber and from E glass fiber (see [0037]).
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.
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.
Claims 2, 4, 5, 10, and 14 are rejected under 35 U.S.C. 103 as being unpatentable over US 2022/0112421 A1 (“Kai”) in view of GB 2,015,984 A (“Imae”).
Regarding claim 4, Kai discloses a method for manufacturing a thermochemical heat storage molded body (a method for producing a plate-shaped chemical heat storage; see [0057] as well as [0030] and [0043]) comprising steps of:
preparing ceramic powder (the chemical heat storage material is at least one selected from the group consisting of magnesium hydroxide or oxide, strontium hydroxide or oxide, barium hydroxide or oxide, calcium hydroxide or oxide, and calcium sulfate; see [0029]; magnesium oxide utilizes heat storage when magnesium hydroxide is dehydrated and converted to magnesium oxide and heat dissipation when magnesium oxide is hydrated; see [0030]);
mixing ceramic fibers with the ceramic powder (the heat storage material composition may comprise reinforcing fibers in addition to the chemical heat storage material; see [0035]; alumina silicate fiber; see [0037] and [0040]; the total amount of the additives is preferably not less than 1% by weight and not more than 40% by weight with respect to the total amount of the chemical heat storage material; see [0041]; see also the kneading of silica-alumina fibers into the magnesium hydroxide powder in Example 1 at [0057]);
pressing and molding a mixed powder to form a molded body (the supporting can be carried out by compacting the powder of the heat storage material composition together with the substrate; see [0043]; see also the tableting of the heat storage powder at a pressure of 700 kg/cm2 for 10 seconds to obtain a pellet-shaped heat storage having a diameter of 13 mm and a thickness of 2.4 mm at [0059]).
Kai does not disclose manufacturing the thermochemical heat storage molded body in the form of a porous molded body by high-temperature heat treatment of the molded body. The only thermal operations disclosed by Kai are drying at 120 °C for 2 hours (see [0057]) and the dehydration treatment carried out in the air at 400 °C during the durability test (see [0060] and Table 1), neither of which is a firing at a sintering-range temperature for magnesium oxide. See the Claim Interpretation section above regarding the recitation “high-temperature heat treatment”.
Imae is directed to a process for producing a porous shaped product, and more particularly to a process for producing a porous sintered product, the process comprising firing a shaped article of a mixture comprising fine ceramic particles and carbon powder at a temperature at which the carbon powder undergoes oxidation and combustion, thereby welding the particles to one another at their contact points and obtaining a sintered product having fine pores formed among the particles at their non-contact points (see lines 5-13 on page 1). Imae teaches that inorganic fibers having a high heat resistance, such as ceramic fibers, can be incorporated in the shaped article to be fired in order to improve the mechanical strength of the resulting shaped product, preferably in an amount of 0.1 to 15% by weight of the shaped article (see lines 53-56 on page 1); that it is preferable to prepare the shaped article by dry compression shaping in order to obtain a low bulk specific gravity (see lines 57-58 on page 1); that the preferable firing temperature is 650 °C to 1,100 °C, a shaped product fired below 650 °C often having too low a mechanical strength and a shaped product fired above 1,100 °C often undergoing shrinkage (see lines 28-32 on page 2); and that the firing is preferably carried out for 0.5 to 3 hours (see id.). Imae further teaches that firing forms a strong sintered mass having a large number of continuous or discontinuous fine pores among the particles (see lines 40-44 on page 2). In Example 14, 72.8 parts by weight of ferrosilicon dust, 24.3 parts by weight of magnesium oxide, and 2.9 parts by weight of ceramic fibers are mixed together and dry-compression shaped, and the resulting shaped article is fired at a temperature of 850 °C for 2 hours (see Example 14 on page 12 and Example 12 on page 11).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have manufactured the molded body of Kai in the form of a porous molded body by high-temperature heat treatment as taught by Imae. Kai teaches that gas such as water vapor should easily penetrate to the inside deep of the heat storage so that the efficiency of the endothermic and exothermic reactions and the amount of heat storage per unit weight are high (see [0014]), and that a filler in which the heat storage material composition becomes porous is preferably used (see [0038]). Kai further teaches that the pellet-shaped heat storage of Comparative Example 1, which contains no reinforcing fiber, was in a state where cracks were generated in the second cycle, cracks were generated in the entire surface of the pellets in the fifth cycle, and magnesium powder was attached to hands when touched (see [0062]). Imae teaches a known technique of compression shaping a mixture of a ceramic powder and ceramic fibers and firing the shaped article to obtain a mechanically strong porous sintered body, and applies that technique to a mixture containing magnesium oxide and ceramic fibers. One of ordinary skill in the art would have recognized that applying that known technique to the ceramic powder and the ceramic fibers of Kai would have yielded the predictable result of a self-supporting porous body of improved mechanical strength into which the working medium penetrates. See MPEP 2143(I)(C).
Regarding claim 2, claim 2 is a product-by-process claim and is not limited to the manipulations of the recited steps, but only to the structure implied by those steps. See MPEP 2113 and In re Thorpe, 777 F.2d 695 (Fed. Cir. 1985). As set forth in the Claim Interpretation section above, the structure implied by “subjected to pressure molding and high-temperature heat treatment to form a porous molded body shape” is a consolidated and sintered body having porosity, with the ceramic fibers distributed within the sintered ceramic matrix, and claim 2 recites no numerical limit on porosity.
Modified Kai discloses a body having that structure, for the reasons set forth in the rejection of claim 4 above. The mixture of the ceramic powder of Kai (see [0029]) and the ceramic fibers of Kai (see [0035], [0037], and [0040]) is compression shaped and fired as taught by Imae, so that the particles are welded to one another at their contact points to form a strong sintered mass having a large number of continuous or discontinuous fine pores among the particles (see lines 40-44 on page 2 of Imae). The fired products reported by Imae have porosities of 82 to 93% (see Examples 1, 3, and 18), and Comparative Example 4, which is the fired product of Example 12 without the subsequent hydrothermal treatment, has a bulk specific gravity of 0.37 g/cm3, a bending strength of 3.0 kg/cm2, and a water absorbency of 81.5%.
Where the claimed product appears to be the same as or only slightly different from a product disclosed by the prior art, although produced by a different process, the burden is on applicant to come forward with evidence establishing a nonobvious difference between the claimed product and the prior art product. See MPEP 2113.
Regarding claim 5, modified Kai discloses that in the step of preparing the ceramic powder, a ceramic powder synthesized by a wet process or a commercially available powder is prepared (magnesium hydroxide powder manufactured by Kishida Chemical Co., Ltd.; see [0059] of Kai; see also the commercially supplied amorphous silica powder and ceramic fibers (Kaowool, Isolite Kogyo) of Example 1 of Imae).
Further, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have obtained the magnesium oxide powder of Kai (see [0029]) from a commercial supplier, magnesium oxide being an ordinary article of commerce, since the selection of a known material based on its suitability for its intended use supports a prima facie determination of obviousness. See MPEP 2144.07.
Regarding claim 10, modified Kai discloses that in the step of pressing and molding a mixed powder, the mixed powder is placed into a mold to be pressed and molded (the resulting mixture was placed in a mold, and press shaped to a shaped article with a bulk specific gravity of about 0.37 g/cm3; see Example 12 of Imae; see also the tableting machine of Kai at [0059], which produces a pellet-shaped heat storage having a diameter of 13 mm and a thickness of 2.4 mm). As set forth in the Claim Interpretation section above, the recitations that the surface area of the molded body is determined by the surface area of the mold and that the thickness thereof is determined according to the amount of the mixed powder describe consequences of placing the mixed powder into a mold and pressing it, and claim 10 does not require any further step.
Regarding claim 14, modified Kai discloses that the high-temperature heat treatment is performed at 800 °C to 1300 °C for 2 to 5 hours (the resulting shaped article was fired at a temperature of 850 °C for 2 hours in a firing furnace; see Examples 12 and 14 of Imae). Imae further teaches that the preferred firing temperature is 650 °C to 1,100 °C and that the firing is preferably carried out for 0.5 to 3 hours (see lines 28-32 on page 2), which ranges overlap the ranges recited in claim 14. Where the claimed ranges overlap or lie inside ranges disclosed by the prior art, a prima facie case of obviousness exists. See MPEP 2144.05(I). Imae further identifies both endpoints of its firing temperature range as result-effective, teaching that a shaped product fired below 650 °C often has too low a mechanical strength and that a shaped product fired above 1,100 °C often undergoes shrinkage, so that the discovery of an optimum or workable firing temperature within the general conditions disclosed by Imae would have been a matter of routine experimentation. See MPEP 2144.05(II)(A).
Although Imae does not expressly state that the firing is performed in air, the firing of Imae is necessarily carried out in an oxygen-containing atmosphere. Imae teaches that the shaped article is fired in an atmosphere having an elevated temperature at which the carbon can undergo oxidation and combustion, and that the inside and the outside of the shaped article are heated in a uniform state by the heat of oxidation and combustion of the carbon powder substantially uniformly distributed in the shaped article (see lines 20-27 on page 2). Imae further teaches that the ferrosilicon dust used as a raw material in Example 14 consists mainly of fine amorphous silica and contains 2 to 3% by weight of carbon (see lines 3-6 on page 3). The oxidation and combustion of that carbon cannot occur in the absence of oxygen, and the firing of Imae is therefore inherently carried out in air or another oxygen-containing atmosphere. See MPEP 2112.
Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over US 2022/0112421 A1 (“Kai”) in view of GB 2,015,984 A (“Imae”), as applied to claim 2 above, and further in view of JP S63-74978 A (“Sasaki 1”) and JP S63-74979 A (“Sasaki 2”).
Regarding claim 3, modified Kai discloses that the ceramic powder is at least one of a powder in a char state including an organic compound, a MgO powder, and a CaO powder (magnesium oxide; see [0029] of Kai).
Modified Kai does not disclose that the ceramic fiber is at least one of an SiC fiber, an Al2O3 fiber and a ZrO2 fiber. The fibers of Kai are alumina silicate fibers (see [0037], [0040], and [0057]) and the fibers of Imae are ceramic fibers of the Kaowool type (see Example 1), and an aluminosilicate is not alumina.
Sasaki 1 is directed to a ceramic composite for firing that is resistant to thermal shock (see the Industrial Application Field section on page 2 of the provided translation), and teaches mixing 5 to 60% by weight of alumina fiber with fine Al2O3 powder, adding an appropriate amount of binder to make a mixture of appropriate viscosity, molding it into an appropriate shape by slip casting, mold pressing, extrusion molding, or suction press molding, and firing the molded body at 1300 to 1700 °C (see the Means for Solving the Problems section on pages 3 and 4). Sasaki 1 teaches that the added alumina fibers act on the matrix to absorb strain energy, with the effect of softening the formation of cracks, so that the strength of the composite is improved (see page 5), and that commercially available alumina fibers can be used (see page 7). Sasaki 1 reports in Example 1 a sintered ceramic composite having a porosity of 42% and a flexural strength 1.5 times that of a monolithic material made solely of alumina (see Example 1 on page 7).
Sasaki 2 is directed to the same ceramic composite for firing and teaches the same process with the species of the reinforcing fiber changed, mixing 20 to 70% by weight of zirconia fiber with the fine Al2O3 powder, adding an appropriate amount of binder, molding the mixture into an appropriate shape by slip casting, die pressing, extrusion molding, or suction press molding, and firing the molded body at 1300 to 1700 °C (see the Means for Solving the Problem section on pages 3 and 4 of the provided translation). Sasaki 2 teaches that the tough zirconia fibers act on the matrix to absorb strain energy and thereby mitigate crack formation, so that the strength of the composite is improved (see page 5).
Sasaki 1 and Sasaki 2 were published on the same day and disclose the same ceramic composite and the same process with only the species of the reinforcing fiber changed, an alumina fiber in the one and a zirconia fiber in the other, each fiber being incorporated into a ceramic powder body that is molded and fired for the purpose of arresting the formation of cracks and improving mechanical strength. These documents establish that an alumina fiber and a zirconia fiber were recognized in the art as interchangeable for that purpose. Modified Kai incorporates an alumina silicate fiber into a ceramic powder body that is molded and fired for that same purpose, the pellet-shaped heat storage of Comparative Example 1 of Kai, which contains no reinforcing fiber, having cracked in the second cycle and having been pulverized by the fifth (see [0062] of Kai). It would therefore have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have substituted an alumina fiber as taught by Sasaki 1, or a zirconia fiber as taught by Sasaki 2, for the alumina silicate fiber of modified Kai, since such a substitution is the simple substitution of one known element for another to obtain predictable results, the substituted components and their functions being known in the art. See MPEP 2143(I)(B) and MPEP 2144.06(II).
Sasaki 1 and Sasaki 2 are analogous art. Each is directed to a fiber-reinforced ceramic body formed from a ceramic powder and a ceramic fiber by molding and firing, and each is reasonably pertinent to the particular problem with which the inventor is involved, namely the arresting of the formation of cracks in a ceramic body subject to dimensional strain. See MPEP 2141.01(a).
Claims 6 and 11 are rejected under 35 U.S.C. 103 as being unpatentable over US 2022/0112421 A1 (“Kai”) in view of GB 2,015,984 A (“Imae”) and further in view of Danks et al., “The evolution of ‘sol-gel’ chemistry as a technique for materials synthesis”, Materials Horizons, Vol. 3 (2016), pages 91-112 (“Danks”).
Regarding claim 6, as set forth in the Claim Interpretation section above, claim 6 is interpreted as requiring that the ceramic powder prepared in claim 5 is the ceramic powder synthesized by a wet process.
Modified Kai does not disclose preparing the ceramic powder by a wet process, or that the wet process is at least one of a Pechini method, a sol-gel method and a Colloidal process. The magnesium hydroxide powder of Kai is obtained from a commercial supplier (see [0059]), and Kai is silent as to how the magnesium oxide of [0029] is obtained.
Danks is a review of sol-gel chemistry as a technique for materials synthesis, and teaches that the term sol-gel covers the synthesis of solid materials such as metal oxides from solution-state precursors, including metal alkoxides, metal ion-chelate complexes, and organic polymer gels containing metal species (see page 91). Danks teaches that many inorganic materials can be prepared by mixing powder reactants and heating, but that the drawbacks of that approach center primarily on the inhomogeneity of the starting materials, complete conversion being limited by mass transport, so that areas of unreacted starting material remain where reactant diffusion is blocked (see page 91, section 1). Danks describes the Pechini method, in which a metal salt is dissolved in water with citric acid and ethylene glycol to form a homogeneous precursor solution containing metal-citrate chelate complexes, the solution is heated to initiate polyesterification between the citrate and the ethylene glycol to form an extended covalent network, and the material is thereafter heated in a furnace to combust the organic matrix and form the ceramic product (see page 99, section 4.1), and teaches that many authors have employed the Pechini method to synthesize metal oxides by combining metal salts with ethylene glycol and citric acid and treating the resulting resin in a furnace in air (see page 99, section 4.2).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have prepared the magnesium oxide powder of Kai (see [0029]) by the Pechini method taught by Danks. Danks teaches that preparing a metal oxide from solution-state precursors by the Pechini method avoids the inhomogeneity and the incomplete conversion that attend the mixing and heating of powder reactants (see page 91). One of ordinary skill in the art would have recognized that preparing the magnesium oxide of Kai by that known technique would have yielded the predictable result of a more homogeneous oxide powder of controlled morphology and particle size. See MPEP 2143(I)(D) and MPEP 2144.07.
Regarding claim 11, modified Kai discloses that the ceramic powder is at least one of a MgO powder and a CaO powder (magnesium oxide; see [0029] of Kai), and, as set forth in the rejection of claim 6 above, that the wet process is the Pechini method.
Danks further teaches that in a typical Pechini synthesis a metal salt is dissolved in water with citric acid (see page 99, section 4.1); that where metal nitrates are used in the initial mixture it is possible to generate foams through release of nitrous oxides during the reaction (see page 100, section 4.2); that the binding of citrate to metal ions depends on the pH of the solution, low pH resulting in protonation of the citrate and high pH risking precipitation of metal hydroxides, so that the control of pH is very important in controlling homogeneity in the gel and particle size in the final product; and that many examples of the Pechini method report optimizing the pH in the initial metal-citrate solution using ammonia, ammonium hydroxide or other bases (see page 99, section 4.2).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have selected magnesium nitrate as the metal salt dissolved in water in preparing the magnesium oxide powder of modified Kai by the Pechini method, and to have used ammonium hydroxide to adjust the pH of the resulting solution. Kai teaches that a filler in which the heat storage material composition becomes porous is preferably used (see [0038]) and that gas such as water vapor should easily penetrate to the inside deep of the heat storage (see [0014]), and Danks teaches that the use of a metal nitrate in the initial mixture makes it possible to generate foams through release of nitrous oxides during the reaction. Danks further teaches that the control of the pH of the initial metal-citrate solution governs the homogeneity of the gel and the particle size of the final product, and identifies ammonium hydroxide as a base reported for that purpose in the Pechini method. One of ordinary skill in the art would have recognized that these known measures would have yielded the predictable results of a more porous oxide product and of control over the homogeneity of the gel and the particle size of the resulting magnesium oxide powder. See MPEP 2143(I)(E) and MPEP 2143(I)(G).
As set forth in the rejection of claim 11 under 35 U.S.C. 112(b) above, the recitation “a proper level” is indefinite, and for purposes of applying prior art claim 11 is interpreted as requiring that ammonium hydroxide is used to adjust the pH of the solution, without limitation as to the resulting pH. See MPEP 2173.06.
Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over US 2022/0112421 A1 (“Kai”) in view of GB 2,015,984 A (“Imae”), as applied to claim 5 above, and further in view of US 2018/0072934 A1 (“Kono”).
Regarding claim 7, as set forth in the Claim Interpretation section above, claim 7 is interpreted as requiring that the ceramic powder prepared in claim 5 is the commercially available powder, which modified Kai discloses for the reasons set forth in the rejection of claim 5 above.
Modified Kai further discloses that a pore-forming agent is added in the step of mixing ceramic fibers with the ceramic powder (92 parts by weight of amorphous silica powder, 5 parts by weight of ceramic fibers, and 3 parts by weight of carbon black were dry-compression shaped; see Example 1 of Imae; it is desirable that 2 to 3% by weight of carbon powder, or an equivalent amount of the precursor, be present in the mixture; see lines 48-52 on page 1 of Imae), the fired product of that example having a porosity of 93% (see Example 1).
Modified Kai does not characterize the carbon black as a pore-forming agent added to form a porous structure.
Kono is directed to a composition for forming a chemical heat storage material (see [0001]) in which a Group-2 element compound stores heat on dehydration and releases heat on hydration (see [0028]). Kono teaches that the composition may comprise at least one of a substance consisting of carbon and a hydrocarbon, whereby more numerous pores are formed inside or on the chemical heat storage material, and thereby it is possible to stabilize the shape of the chemical heat storage material, carbon black, graphite, and carbon nanofiber being exemplified as the substance consisting of carbon and paraffin, olefins, and cycloalkanes being exemplified as the hydrocarbon (see [0056]). Kono further teaches that in the calcination step the resin and the substance consisting of carbon or hydrocarbon are gasified and removed from the chemical heat storage material, and that the chemical heat storage material has fine pores formed by the removal of the resin and the substance consisting of carbon or hydrocarbon (see [0061]). The calcination is carried out at a temperature from 200 to 1,200 °C, more preferably from 300 to 1,000 °C (see [0062]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have added carbon black to the mixed powder of modified Kai as a pore-forming agent in order to form a porous structure. Kai teaches that gas such as water vapor should easily penetrate to the inside deep of the heat storage so that the efficiency of the endothermic and exothermic reactions and the amount of heat storage per unit weight are high (see [0014]), and that a filler in which the heat storage material composition becomes porous is preferably used (see [0038]). Kai further teaches that the pellet-shaped heat storage of Comparative Example 1 was in a state where cracks were generated in the second cycle and cracks were generated in the entire surface of the pellets in the fifth cycle (see [0062]). Kono teaches that adding a substance consisting of carbon, such as carbon black, to a chemical heat storage material of the same type forms more numerous pores upon removal of that substance during calcination, and thereby stabilizes the shape of the chemical heat storage material. One of ordinary skill in the art would have recognized that applying that known technique to the mixed powder of modified Kai would have yielded the predictable result of a porous molded body of stabilized shape. See MPEP 2143(I)(C).
Allowable Subject Matter
Claims 8, 9, 12, and 13 are objected to as being dependent upon a rejected base claim, but would be allowable if rewritten in independent form including all of the limitations of the base claim and any intervening claims.
The following is a statement of reasons for the indication of allowable subject matter:
Claim 8 requires that the ceramic powder prepared in the step of preparing ceramic powder is the ceramic powder synthesized by a wet process, that the ceramic powder is a powder in a char state with the char including an organic compound, and that the powder in the char state is the powder mixed with the ceramic fibers. As set forth in the Claim Interpretation section above, that recitation requires a ceramic powder that includes char, that is, the carbonaceous residue that remains after organic matter is thermally decomposed, the char retaining an organic compound. The requirement that the char retain an organic compound is a limitation of substance. A powder to which an organic material that has not been thermally decomposed has been added is not a powder in a char state, and a powder to which a carbonaceous material retaining no organic compound has been added does not satisfy the further requirement that the char include an organic compound.
The prior art of record does not disclose or suggest mixing a ceramic powder in that state with ceramic fibers and pressing and molding the resulting mixture.
The closest prior art is JP 2009-256518 A (“Wakayama”), which discloses a powdered chemical heat storage material brought into contact with a non-volatile organic material and fired in an inert atmosphere so as to form a carbide structure on the surface of the powder, the carbide structure having a cage-like structure with numerous pores preferably of 0.2 µm or less (see [0025] of the provided translation). The firing is carried out in a gas that does not readily undergo chemical reactions, such as helium, neon, argon, or nitrogen, at a holding temperature of 500 to 2000 °C and a holding time of 0.5 to 100 hours, and the resulting material may be molded by extrusion molding or compression molding (see [0045] and [0046]). In Example 1, calcium hydroxide and sucrose in a mass ratio of 90 to 10 are mixed with water and fired in a nitrogen atmosphere at a holding temperature of 1000 °C for a holding time of 2 hours (see [0052]-[0054]), the resulting material exhibiting a reaction rate of 87% in the first cycle and 84% in the tenth cycle (see [0055]).
Wakayama does not reach claim 8. The organic material of Wakayama is fired to completion, at 1000 °C for 2 hours in nitrogen in the worked example, so as to convert it to a carbide structure. A carbonaceous residue so produced does not retain an organic compound, and the powder that is thereafter molded is accordingly not a powder in a char state including an organic compound.
The remaining prior art of record treats the organic constituent of the molding mixture as a material to be removed rather than retained. Imae fires the shaped article at a temperature at which the carbon undergoes oxidation and combustion (see lines 20-27 on page 2 of the provided translation). Kono teaches that in the calcination step the resin and the substance consisting of carbon or hydrocarbon are gasified and removed from the chemical heat storage material, and that the chemical heat storage material has fine pores formed by that removal (see [0061]). JP 2009-256517 A obtains its pores by mixing a clay mineral with a combustible granular material and firing the mixture so that the combustible granular material burns away (see [0013] and [0016] of the provided translation). None of these references teaches or suggests carrying an organic compound into the mixing and molding steps within the ceramic powder itself, and one of ordinary skill in the art would have had no reason to do so.
Claims 9 and 12 contain allowable subject matter based on their dependency from claim 8, and claim 13 contains allowable subject matter based on its dependency from claim 12.
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure:
CN 108546093 A disclose alumina short fibers accounting for 1% to 3% of the mass of the ceramic powder in a fused magnesium oxide ceramic (see [0025]).
CN 108439959 A discloses zirconium dioxide short fibers accounting for 0.5% to 1% of the ceramic powder mass, together with basic magnesium sulfate whiskers, in a fused magnesium oxide ceramic (see [0023]).
JP 2641149 B2 discloses long fibers of the same material as the ceramic raw material powder, 100 µm or more in length, dispersed in an alumina or zirconia raw material powder in an amount of 3 to 20% by weight, the mixture being molded and sintered to obtain thermal shock resistance (see [0006]).
CN 112279637 A discloses activated alumina powder, light magnesium carbonate powder, and alumina chopped fibers in a mass ratio of 25-50 : 60-40 : 10-15, the fibers having a diameter of 3-5 µm and a length of less than 1 mm, the formed blank being held at 1250-1350 °C for 2 to 5 hours to give an apparent porosity of 80-90% (see [0009], [0011], [0017], [0019], and [0021]).
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/John J DeRusso/Primary Examiner, Art Unit 1744
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