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 .
Election/Restrictions
Applicant's election with traverse of Group I in the reply filed on December 18, 2025, is acknowledged. The traversal is on the grounds that there is no serious burden. This is not found persuasive because the groups are classified in different areas, examination of different statutory classes of invention require different considerations, and the claims have different scope because of the different purity levels claimed.
The requirement is still deemed proper and is therefore made FINAL.
Claim Rejections - 35 USC § 112
The following is a quotation of the first paragraph of 35 U.S.C. 112(a):
(a) IN GENERAL.—The specification shall contain a written description of the invention, and of the manner and process of making and using it, in such full, clear, concise, and exact terms as to enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and use the same, and shall set forth the best mode contemplated by the inventor or joint inventor of carrying out the invention.
The following is a quotation of the first paragraph of pre-AIA 35 U.S.C. 112:
The specification shall contain a written description of the invention, and of the manner and process of making and using it, in such full, clear, concise, and exact terms as to enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and use the same, and shall set forth the best mode contemplated by the inventor of carrying out his invention.
Claims 1-33 and 37 are rejected under 35 U.S.C. 112(a) or 35 U.S.C. 112 (pre-AIA ), first paragraph, as failing to comply with the enablement requirement. The claims contain subject matter which was not described in the specification in such a way as to enable one skilled in the art to which it pertains, or with which it is most nearly connected, to make and/or use the invention.
The specification indicates “that certain impurities within the high purity DMAC material must be controlled to not exceed their respective upper concentration limits” [0038], or that the impurities “are maintained at or below” a particular limit [0043]. However, the specification does not provide guidance on how one is to make such a high purity (99.9% or “semiconductor grade”) DMAC. The specification fails to describe specific steps to achieve the purity. At most, the specification describes techniques at a high level of generalization at paragraph 53 (see excerpt provided below).
…By way of non-limiting example, low grade DMAC may undergo rectification, distillation, freeze-pump-thaw, adsorption, or a combination thereof to achieve an impurity profile with the upper concentration limits as mentioned hereinabove. In this manner, the low grade DMAC material is converted to a suitable semiconductor grade DMAC material.
[00053]
This description of steps that may be taken to provide the cited purity is a list of examples and is “non-limiting” as to the particular steps that must be performed to achieve the cited purity. A person of ordinary skill in the art would require undue experimentation to make and use the invention as claimed, for the reasons described below.
There are many factors to be considered when determining whether there is sufficient evidence to support a determination that a disclosure does not satisfy the enablement requirement and whether any necessary experimentation is "undue." These factors include, but are not limited to:
(A) The breadth of the claims;
(B) The nature of the invention;
(C) The state of the prior art;
(D) The level of one of ordinary skill;
(E) The level of predictability in the art;
(F) The amount of direction provided by the inventor;
(G) The existence of working examples; and
(H) The quantity of experimentation needed to make or use the invention based on the content of the disclosure.
In re Wands, 858 F.2d 731, 737, 8 USPQ2d 1400, 1404 (Fed. Cir. 1988)
The broadest reasonable interpretation of claims 1-33 and 37 covers a DMAC at 99.9 mol% purity and the cited impurities collectively at less than 0.1 mol%. The specification does not provide direction on how to purify a composition to achieve the cited purity level. At the time of filing, the following determinations are made with respect to the Wands factors.
(A) The breadth of the claims
The claims are narrow as to the purity level cited, that of 99.9 mol% purity.
(B) The nature of the invention
The nature of the invention is described in the brief “Summary of the Invention.” 37 CFR 1.73, MPEP 608.01(d). The instant specification describes the Summary of the Invention beginning at paragraph 9 and essentially mirrors the claim language of the independent claims. Accordingly, the nature of the invention is a DMAC at 99.9 mol% purity and the cited impurities collectively at less than 0.1 mol%.
(C) The state of the prior art
A search of the prior art reveals that a representative patent of the state of the prior art is Harkonen et al (US 2004/0208994 A1), which is directed to atomic layer deposition with DMAC at 99% purity, available from Crompton [0055]. Applicant cited Eidt (US 4,116,992), which is directed to a process of manufacturing DMAC at 99% purity by reacting starting materials and collecting distillate (Example 4). Takahashi et al (US 2011/0021800 A1) discloses a method with various distillation and zinc treatment steps to obtain dialkylaluminum chloride, especially diethylaluminum chloride with Zn at 10 ppm or less (Fgi.1, Table 1). McBriarty (US 2025/0226213 A1) discloses ALE with DMAC [0082], [0089] but fails to disclose the purity level of the DMAC.
(D) The level of one of ordinary skill
The level of one of ordinary skill in the art is a person having training and/or experience in the preparation of organometallic compounds. Such a person would be familiar with the techniques discussed in the specification of rectification, distillation, freeze-pump-thaw, and adsorption.
(E) The level of predictability in the art
The chemical field by its nature is unpredictable, however the techniques of rectification, distillation, freeze-pump-thaw, adsorption are known and therefore to some degree predictable in what they achieve. However, the ultimate level of purity by using these techniques is unpredictable as to the purity level achieved, and experimentation is required to determine a combination of techniques to achieve a desired purity level.
(F) The amount of direction provided by the inventor
The inventor provides example techniques of rectification, distillation, freeze-pump-thaw, adsorption [00053]. However, the list is non-limiting and no explanation is provided about how to choose among the techniques to obtain the cited purity level.
(G) The existence of working examples
The specification has no working examples.
(H) The quantity of experimentation needed to make or use the invention based on the content of the disclosure.
While prior art Eidt provides some guidance as to the amount of experimentation to obtain close to the desired purity, several experiments would have be conducted to pick and choose from the cited techniques, available starting materials, and available parameters for each step of the purification method to obtain the desired product.
Based on a consideration of all of the above Wands factors, while a high level of purity is known and the level of skill is high, obtaining an even higher level of purity in the final product in an unpredictable field without any direction by the specification and only a recitation of techniques at a high level of generalization favors that a person having ordinary skill in the art would need to conduct undue experimentation to make and use the invention as recited in claims 1-33 and 37.
For the reasons described above, claims 1-33 and 37 are rejected under 35 USC 112 (a) as failing to comply with the enablement requirement.
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.
Claims 1-24, 26-28, 33 and 37 are 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.
In claims 1-13, 24 the term “high purity” is defined in the specification to mean “99.9 mol% or higher for ALE applications and 99% or higher for ion implant applications” [0010]. Claims 1, 13 and 24 cite “about 99.9%,” which renders the claim unclear because “about” can mean different values to different people. Is 99.8% about 99.9%? How close to 99.9% must the value be in order to be “about 99.9%”? The term “about” may be simply deleted to overcome this rejection. Please note that because of the open “comprising” language, impurities other than those cited may be present in the composition.
In claims 1, 14 and 24, the term “high precision” is a relative term. The term 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. The specification defines “high precision etchant” as “atomic removal of materials from features, structures or devices characterized as having relatively high aspect ratios, where aspect ratio is the ratio of the height to depth of the feature, structure, or device.” [0033]. However, the term “high precision” is defined by another relative term “high aspect ratio.” It is unclear what value of aspect ratio is encompassed by this definition, and therefore the metes and bounds of the claim are indefinite. The term may be simply deleted.
In claims 1, 14 and 21, the recitation “high purity DMAC composition maintained under storage conditions in liquid phase that is in substantial equilibrium with a high purity, vapor phase” renders the claim indefinite. Maintaining under storage conditions is a method limitation, while the claim is directed to a composition. It is unclear how this recitation further limits the composition.
In claims 1 and 24, the recitation that “total moles in the vapor phase excludes an optional blanket gas that may occupy said vapor phase” renders the claim indefinite. It is unclear how a blanket gas limits the composition.
In claims 1 and 24, the recitation of gaseous impurities (i) through (viii) is unclear. The word “and” is missing from before “(viii) alkyl-aluminum compounds…” Claim 14 includes the word “and.” Therefore, for purposes of the rejection, claim 1 is treated as reciting “and” requiring that all of the gaseous impurities (i)-(viii) are present because each impurity is present “in an amount greater than 0 mol%.” Claim 24 does not clearly cite Markush group language, but for purposes of the rejection is treated as citing “comprising at least one member selected from the group consisting of” and also citing “and” such that claim 24 requires at least one member be selected from the group.
In claim 13, the limitation “adapted to maintain said purity level of about 99.9 mol% or greater and remain chemically stable at ambient temperature without undergoing decomposition under said storage conditions” appears to be a method limitation. It is unclear how this limitation further limits the composition, which the claims define by purity levels.
In claims 14-22, the term “high purity” is not defined in the base claim, claim 14, however the specification defines it as “99.9 mol% or higher for ALE applications and 99% or higher for ion implant applications” [0010]. The composition is not limited to the intended use of either ALE or ion implant applications, and therefore it is unclear what the purity level is in claim 14.
In claim 23, it is unclear how the limitations related to “transport, storage and use” further limits the claim. A composition is defined by its structure, not by how it is transported, stored and used.
In claims 23 and 24, it is unclear how “predetermined headspace excludes an optional blanket gas” and “total moles in the vapor phase excludes an optional blanket gas” further limits the claim. It is unclear how a blanket gas limits the composition.
In claim 24, it is unclear how the limitation including the canister and that the composition is “maintained in the substantially sealed and passivated canister under storage conditions” further limits the claim. A composition is defined by its structure, not by how it is maintained or stored. It is unclear how “a headspace of a predetermined volume” further limits the claim. A composition is defined by its structure, not by a headspace of a certain volume.
In claim 25, the listing of impurities recites two nested Markush groups, without clearly using Markush group language. Please ensure that this is intended.
In claims 26-27, it is unclear how limitations regarding etch selectivity further limit the base claim. A composition is defined by its structure, not by how it is used.
In claim 28, it is unclear how the limitation regarding storage conditions further limits the composition. A composition is defined by its structure, not by how it is stored.
In claim 33, it is unclear how a limitation about maintaining the composition in a canister further limits the base claim. A composition is defined by its structure, not by how it is maintained.
Claim 37 fails to have clear Markush group language and the use of “and” in the listing of impurities at lines 3-6, and therefore claim 37 is indefinite as to the impurities required. Applicant is encouraged to use proper Markush group language in all of the claims describing the impurities.
Claims 2-12 fail to cure the indefiniteness of their base claims, and are therefore also rejected.
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
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 1-33 and 37 are rejected under 35 U.S.C. 103 as being unpatentable over Harkonen et al (US 2004/0208994 A1) in view of Shenai-Khatkhate et al (US 2007/0117994 A1).
Harkonen teaches that in methods of atomic layer deposition (“ALD”), a step including dimethylaluminum chloride (“DMAC”) provided at 99% purity [0055] is a useful composition. Atomic layer deposition is a technique closely related to atomic layer etching in that steps are repeated in a cyclical manner to achieve atomic layer processing.
Shenai-Khatkhate teaches that in methods of ALD, ultrapure metalorganic compounds should be used [0002]. Shenai-Khatkhate is thus a general teaching that materials should be purified to a high degree to obtain the best results.
It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to further purify the composition of Harkonen to obtain the cited DMAC in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the pure composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. Ex parte Gray 10 USPQ 2d 1922, 1926 (BPAI 1989); Ex parte Steelmand 140 USPQ 189, 190; In re King 43 USPQ 400 (CCPA 1939); In re Merz 38 USPQ 143 (CCPA 1938); In re Ridgeway 25 USPQ 202 (CCPA 1935); Ex parte Windhaus 15 USPQ 45 (PO BdPatApp 1931). See also MPEP 2144.04 VII (Purifying an Old Product).
Secondary considerations such as unexpected results or long felt need may rebut a prima facie case based on purity. Ex parte Stern 13 USPQ 2d 1379, 1381 (BPAI 1989); In re Kratz 201 USPQ 71 (CCPA 1979); In re Bergstrom 166 USPQ 256 (CCPA 1970); In re Irani 166 USPQ 24 (CCPA 1970); In re Cofer 148 USPQ 268 (CCPA 1966); In re Doyle 140 USPQ 421 (CCPA 1964); In re Williams 80 USPQ 150 (CCPA 1948). Here, the record fails to show unexpected results or long felt need. The specification describes higher selectivity levels of etching particular materials [00039], [00057], but only discusses these at a high level of generality without working examples or evidence of unexpected results.
In claim 1, lines 2-3, the limitation, “suitable for use as a high precision, atomic layer etchant (ALE) in a semiconductor fabrication process” is a statement of intended use and given little patentable weight. The composition of modified Harkonen is capable of being used as an atomic layer etchant as cited.
In claim 1, lines 4-5, the phrase “maintained under storage conditions in a liquid phase that is in substantial equilibrium with a high purity, vapor phase” is a statement of intended use that is given little patentable weight. The composition of modified Harkonen is capable of being maintained as cited.
In claim 1, lines 7-9, the phrase “wherein the total moles in the vapor phase excludes an optional blanket gas that may occupy said vapor phase” is treated as citing that the total moles in the vapor phase is limited to the moles in the vapor phase. The limitation of the blanket gas is given little patentable weight because the blanket gas is not included in the DMAC composition. For purposes of the rejection, the DMAC composition includes the DMAC and any impurities that may be present.
The limitations about the impurities are also obvious because if the purity is 99.9 mol%, then impurities are present in the balance of the composition, which is 0.1 mol%.
As to claims 2-12, for the same reasons as cited in claim 1, it would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to provide the cited level of impurities in the modified composition of Harkonen in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the pure composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. MPEP 2144.04 VII (Purifying an Old Product).
As to claim 13, the limitation about maintaining purity is treated as a statement of intended used. The composition of modified Harkonen is capable of being adapted to maintain purity as cited.
As to claim 14, see the rejection of claim 1. It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to provide a high purity DMAC composition with the cited levels of impurities in the composition of Harkonen in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. MPEP 2144.04 VII (Purifying an Old Product).
In claim 14, lines 2-3, the limitation, “suitable for use as a high precision, atomic layer etchant (ALE) in a semiconductor fabrication process” is a statement of intended use and given little patentable weight. The composition of modified Harkonen is capable of being used as an atomic layer etchant as cited.
As to claims 15-20, for the same reasons as cited in claim 14, it would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to provide the cited level of impurities in the modified composition of Harkonen in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. MPEP 2144.04 VII (Purifying an Old Product).
As to claim 21, see the rejection of claim 1. The modified composition of Harkonen is capable of being used as an atomic layer etchant as cited because it is used in ALD (Fig. 1), which like ALE, provides the DMAC composition to a surface to be treated followed by purging [0055]. The limitation about etch selectivity and the limitation regarding a process that uses HF followed by DMAC are method limitations that are treated as limitations of intended use of the composition and are given little patentable weight. The composition is expected to have the same properties of selectivity and process results because if the composition is physically the same, it must have the same properties. MPEP 2112.01 II.
As to claim 22, see the rejection of claim 21. The composition of modified Harkonen is capable of the cited etching. Method limitations are treated as intended use and are given little patentable weight in composition claims.
As to claim 23, see the rejection of claim 1. It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to further purify the DMAC as cited by Harkonen to obtain the cited semiconductor grade DMAC in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. See also MPEP 2144.04 VII (Purifying an Old Product).
As to the limitation about storage in a sealed and passivated canister comprising a liquid phase in equilibrium with a vapor phase at the cited purity during transport, storage and use, this limitation is expected to be inherent in the teachings of Harkonen, which already teaches to use the DMAC material in an atomic layer process, which requires storage and use of a high purity material in order to effectively conduct the process. It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to use a hermetically sealed and passivated canister as cited with the modified material of Harkonen in order to maintain a pure material that is ready for atomic layer processing.
As to claim 24, see the rejection of claim 1. It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to further purify the DMAC as cited by Harkonen to obtain the cited DMAC composition in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. See also MPEP 2144.04 VII (Purifying an Old Product).
The limitation in lines 1-3 “for use as …process” is treated as a statement of intended use and given little patentable weight. The modified composition of Harkonen is capable of being used as the cited etchant.
In claim 24, line 4, the limitation about the canister is treated as a statement of intended use, and given little patentable weight. The modified composition of Harkonen is capable of being used as cited.
In claim 24, lines 5-7, the limitation about maintaining in a canister is treated as a statement of intended use, and is given little patentable weight. The modified composition of Harkonen is capable of being used as cited.
In claim 24, lines 10-11, the limitation about an optional blanket gas is treated as a statement of intended use, and is given little patentable weight. The modified composition of Harkonen is capable of being used as cited.
In claim 24, lines 13-14, the limitation about occupying a headspace is a statement of intended use, and is given little patentable weight. The modified composition of Harkonen is capable of being used as cited.
The claim 24 limitations about the impurities are also obvious because if the purity is 99.9 mol%, then impurities are present in the balance of the composition, which is 0.1 mol%.
As to claim 25, see the rejection of claim 1. It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to further purify the DMAC as cited by Harkonen to obtain the cited semiconductor grade DMAC in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. See also MPEP 2144.04 VII (Purifying an Old Product).
The claim 25 limitations about the impurities are also obvious because if the purity is 99.9 mol%, then impurities are present in the balance of the composition, which is 0.1 mol%.
As to claims 26-27, the modified composition of Harkonen is capable of exhibiting the cited selectivity. The limitations about etch selectivity and species x and y are treated as a limitations of intended use of the composition and are given little patentable weight. The modified composition of Harkonen is expected to have the cited properties because if the composition is physically the same, it must have the same properties. MPEP 2112.01 II.
As to claim 28, the limitation about storage conditions is treated as a limitation of intended use, and is given little patentable weight. The modified composition of Harkonen is capable of being stored as cited.
As to claims 29-32, the limitations about the impurities are also obvious because if the purity is 99.9 mol%, then impurities are present in the balance of the composition, which is 0.1 mol%.
As to claim 33, the limitation about maintaining in a canister is treated as a statement of intended use, and is given little patentable weight.
As to claim 37, see the rejection of claim 1. It would have been obvious to one with ordinary skill in the art before the effective filing date of the claimed invention to further purify the DMAC as cited by Harkonen to obtain the cited DMAC composition in order to optimize the concentration for the best and highest purity because Shenai-Khatkhate teaches that ultrapure materials are desirable, and the composition is expected to give better results with less contamination of the final product. In addition, the courts have held that a product that differs from prior art only in purity is obvious except when the pure product possesses unexpected properties not possessed by the impure one. See also MPEP 2144.04 VII (Purifying an Old Product). The limitations about the impurities are also obvious because if the purity is 99.9 mol%, then impurities are present in the balance of the composition, which is 0.1 mol%.
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure. Takahashi et al (US 2011/0021800 A1) discloses a method with various distillation and zinc treatment steps to obtain dialkylaluminum chloride, especially diethylaluminum chloride with Zn at 10 ppm or less (Fgi.1, Table 1). McBriarty (US 2025/0226213 A1) discloses ALE with DMAC [0082], [0089] but fails to disclose the purity level of the DMAC. Shin et al (US 2024/0030038 A1, [0038]), Routzahn et al (US 2025/0154658 A1, ALE of hafnia with DMAC [0032]), Fischer et al (US 2023/0326761 A1, HF followed by DMAC [0120]), Zandi et al (US 2021/0242031 A1, Fig. 6) are cited to show methods of atomic layer etching, but also fail to disclose the purity of DMAC.
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/ANITA K ALANKO/Patent Examiner, Art Unit 1713