T 2395/09 () of 25.10.2011

European Case Law Identifier: ECLI:EP:BA:2011:T239509.20111025
Date of decision: 25 October 2011
Case number: T 2395/09
Application number: 03739116.6
IPC class: B22F 3/00
B22F 9/16
Language of proceedings: EN
Distribution: D
Download and more information:
Decision text in EN (PDF, 31.959K)
Documentation of the appeal procedure can be found in the Register
Bibliographic information is available in: EN
Versions: Unpublished
Title of application: Method for fabricating a metallic article without any melting
Applicant name: GENERAL ELECTRIC COMPANY
Opponent name: -
Board: 3.2.03
Headnote: -
Relevant legal provisions:
European Patent Convention Art 54
European Patent Convention Art 56
European Patent Convention Art 83
Keywords: Novelty (yes)
Inventive step (yes)
Remittal for consideration inter alia of Article 83 EPC
Catchwords:

-

Cited decisions:
-
Citing decisions:
-

Summary of Facts and Submissions

I. European patent application EP-A-03 739 116 originates from international application WO-A-03/106081 and concerns a method for making metallic articles based on titanium.

II. The examining division was of the view that the claimed subject-matter of the main and first auxiliary requests lacked novelty (Article 54 EPC) and contained added subject-matter contrary to Article 123(2) EPC; the second auxiliary request was not admitted into the proceedings as it was filed late and also appeared to contravene Article 123(2) EPC. The examining division thus decided to refuse the application.

III. The decision was posted on 14 July 2009. Notice of appeal was filed by the applicant (hereafter the appellant) on 11 September 2009 and the appeal fee was paid on the same day. A statement containing the grounds of appeal was filed on 18 November 2009.

IV. In accordance with Article 15(1) of the Rules of Procedure of the Boards of Appeal (RPBA), the Board issued a preliminary opinion of the case, together with a summons to attend oral proceedings. In response, the appellant filed with the letter of 23 September 2011 two sets of claims as its main and auxiliary requests.

V. Oral proceedings were held on 25 October 2011.

VI. Requests

The appellant requested that the decision under appeal be set aside and that a patent be granted on the basis of the main alternatively the auxiliary request. In the event of the main request not being granted, the appellant requested that the case be remitted to the examining division for further prosecution.

VII. Claims

Claim 1 of the main request reads as follows:

"1. A method for fabricating a metallic article (20) made of metallic constituent elements, comprising the steps of

furnishing a mixture of nonmetallic precursor compounds of the metallic constituent elements;

chemically reducing (48) the mixture of nonmetallic precursor compounds to produce an initial metallic alloy powder material, without melting the initial metallic alloy powder material, such that it is not macroscopically or grossly melted so that it liquefies and loses its shape; and

consolidating (50) the initial metallic alloy powder material to produce a consolidated metallic article (20), without melting the initial metallic alloy powder material and without melting the consolidated metallic article (20), such that it is not macroscopically or grossly melted so that it liquefies and loses its shape;

wherein the step of furnishing the mixture includes the step of furnishing the mixture comprising more titanium than any other metallic element."

Dependent claim 2 concerns a preferred embodiment of the method of claim 1.

VIII. Prior Art

The following documents are of relevance for this decision.

WO-A1-00/76698 (D1) is referred to in the decision of the examining division.

US-A-3 909 247 (D2) is cited in the international search report.

US-A-5 779 761 (D4) and US-A-5 958 106 (D5) are cited in the application.

IX. Submissions of the Party

(a) Article 123(2) EPC

The appellant submits that the amendments made to the claims address the objections raised by the examining division under Article 123(2) EPC.

(b) Novelty

Document D1:

The appellant argued that D1 does not disclose the chemical reduction of a mixture of nonmetallic precursor compounds to produce an alloy powder. In the case of titanium, the precursor compound is a hydride, which is thermally decomposed rather than chemically reduced to form the metallic powder. There is also no clear teaching in D1 that melting of the alloy powder should be avoided. For example, the list of elements at the bottom of page 13 of D1 includes copper, which is said to be reduced below 1350ºC; this indicates that there is no concern as to whether or not an alloy powder containing copper is melted.

Document D2:

There is no disclosure in D2 of the formation of alloys based on titanium; the example given (example 5) only concerns the making of pure titanium metal. The method of D2 involves the reduction of a cyanide complex to a hydride, which is then decomposed to yield metallic powder. Therefore, as in D1, the step of chemically reducing nonmetallic precursor compounds to produce an alloy powder is not disclosed. In addition, the method of D2 starts with a metal cyanide complex of the metals in question, which the appellant sees as being a single precursor compound rather than a mixture of precursor compounds, as required by claim 1. There is also no requirement in D2 that melting should be avoided, and examples in column 5 include magnesium and aluminium, which could melt under the process conditions described in D2.

Documents D4 and D5:

These documents describe similar processes. The claimed process differs principally in that D4/D5 do not disclose a process in which the initial alloy powder is produced without melting. For example the processes of D4/D5 are said to be suitable for making gallium, which has a melting point of about 30ºC and would inevitably melt. There is therefore no preference expressed in these documents as to whether melting does or does not occur.

The appellant also submitted that there is no enabling disclosure in D4/D5 for making an alloy. Although Table 1 provides a list of metal halides that can be used in the process of D4/D5, there is no example of an alloy being made. In particular, there is no indication of how to combine the metal halides and produce an alloy whilst avoiding melting.

At column 5, lines 29 to 32 it is said that the form of metallic material produced is a titanium sponge that requires jackhammering from the collection vessel; this indicates that the resulting material is not a powder, as required by claim 1.

No consolidation step is disclosed for the powder made by the processes of D4/D5, hence the requirement that such a step must take place without melting is also not disclosed.

(c) Inventive Step

The appellant submits that starting from the cited prior art, one of the problems to be addressed is how to produce a titanium-based article having superior ultrasonic inspectability.

The microstructure present in articles made by the claimed process allows defects to be detected more easily and more reliably. It is therefore possible to manufacture larger components more reliably.

Since there is no indication in the prior art of avoiding melting in order to gain these benefits, the method of claim 1 has an inventive step.

Reasons for the Decision

1. The appeal is admissible.

2. Article 123(2) EPC

2.1 Claim 1 of the application as originally filed (WO-A-03/106081) has been amended to define the initial metallic alloy material as being a powder material. In addition, the expression "without melting" is defined further in claim 1 as taking place so that macroscopic or gross melting with liquefying and loss of shape does not occur.

2.2 The examining division argued that the application does not disclose a method in which a metallic alloy powder is obtained by chemically reducing the compound mixture such that it is not macroscopically or grossly melted so that it liquefies and loses its shape. The reason given by the examining division is that the latter feature is only referred to in the context of a consolidated article and not for the metallic alloy powder.

2.3 In the paragraph bridging pages 9 and 10 of the application it is said that on completion of reduction (step 48 in Figure 2 - the reference here to "step 42" appears to be an error), the physical form of the metallic material depends on that of the precursor compounds. Thus starting with precursor powders or vapours leads to metallic material in powder form. The need to avoid melting is emphasised throughout the application, for example at page 2, the last two paragraphs, page 4, first paragraph, page 11, fourth paragraph and page 13, first paragraph. The concept of "without melting" is specified on page 8 (second paragraph) as meaning that the material is not macroscopically or grossly melted so that it liquefies and loses its shape.

The skilled person would thus derive the features of the amendment from the application, and hence the requirements of Article 123(2) EPC are met.

3. Novelty (Article 54 EPC)

3.1 Document D1

3.1.1 Claim 1 relates to the fabrication of articles made from metallic elements of which titanium forms the major part.

3.1.2 D1 describes a process for making metal articles by the conversion of precursor powders that have been formed into the shape of the required article. This occurs either by the reduction of articles made from metal oxide, or by the decomposition of those made from metal hydrides (see page 5, lines 16 to 23).

3.1.3 Articles made from titanium, along with vanadium and zirconium, are only disclosed in D1 as being made from hydride precursors (see page 2, lines 17 to 24; page 12, lines 10 to 16 and claim 14). Such hydride precursors are not converted to the metals by reduction but by heating at a temperature sufficiently high enough to decompose the hydride (page 2, lines 18 to 20).

3.1.4 Since in D1 the precursor powders are formed into an article prior to conversion, and in case of titanium there is no chemical reduction, the claimed step of "chemically reducing a mixture of nonmetallic precursor compounds to produce an initial alloy powder material" is not disclosed, and hence the method of claim 1 is novel with respect to D1.

3.2 Document D2

According to the process disclosed in D2, a metallic cyanide complex is formed which is then reduced by hydrogen. In the case of titanium (see Example V in column 6) the product is a hydrided titanium powder which is further subjected to a vacuum and a high temperature to yield the metal. The product of the reduction step is therefore not a metallic powder but a hydride which, as in the method of D1, requires further processing to produce the metal. Since there is no indication in D2 that an alloy powder containing titanium could be made without the intermediate step of forming a hydride, the claimed method is novel with respect to this document.

3.3 Documents D4 and D5

3.3.1 D4 discloses a process in which vapours of metal halides are reduced to pure metals or alloys. In particular, D4 describes a method in which titanium tetrachloride is used as the precursor compound.

3.3.2 On the basis of column 5, lines 29 to 32 of D4, the appellant argues that the method of D4 does not result in a powder, as it is a batch process resulting in a sponge that requires jackhammering from the sides of the collection vessel. However this is described in D4 in the context of a discussion of the prior art process. The process of D4 is continuous and is said to avoid the problems associated with the known batch process (see column 5, lines 54 to 58). The product of the process of D4 is clearly a powder (see, for example, claims 21, 28 and 30).

3.3.3 The process of D4 involves injecting titanium tetrachloride vapour into a flowing stream of sodium. A reduction reaction takes place which is highly exothermic, resulting in molten reaction products of titanium and sodium chloride. These molten reaction products are quenched in the bulk sodium stream (column 3, lines 49 to 51) and, by varying the process conditions, are maintained below the sintering temperature, ie below the melting point of the produced metal (column 3, lines 61 to 62 and column 4, lines 4 to 6).

3.3.4 D4 also teaches that alloys can be made by providing a suitable mixture of metal halides at the start of the process (column 3, lines 18 to 21; column 6, lines 9 to 13); examples of suitable halides are given in Table 1. The melting point of some of the elements in Table 1 is relatively low (for example, aluminium, antimony and gallium have melting points of about 660ºC, 631ºC and 30ºC respectively). Given that the reduction reaction delivers a substantial amount of heat, the Board agrees with the appellant's submission that there would inevitably be melting of the initial reaction products when producing alloys containing such metals.

3.3.5 The general teaching of D4 is that the titanium produced by the process is in solid form and is maintained well below its sintering temperature. This applies to both the "low temperature" and the "high temperature" embodiments of the process shown in Figures 2 and 3 respectively (see column 4, lines 4 to 6 and column 5, lines 36 to 42).

However, it cannot be said with certainty that in the initial stages of the process of D4 the metal is not melted; in fact the contrary appears to be the case. Since claim 1 requires that an initial metallic alloy powder is produced without melting, this is a novel feature over D4. There is also no disclosure in D4 of a consolidating step, and whilst such a step is inevitable for turning the powder into a useful object, there is no indication that it would be carried out without any significant melting taking place.

The claimed process is thus novel over D4 and also over D5, which discloses a similar process.

4. Inventive Step (Article 56 EPC)

4.1 One of the ways that the method of claim 1 can be put into practice is by vapour-phase reduction, and reference is made in the application to D4 and D5 as providing a fuller description of this approach (see the application, page 3, lines 3 to 5 and page 9, second paragraph). Consequently, the process of D4 (or D5) is a relevant starting point for the assessment of inventive step. The methods of D1 and D2 result in formation of the alloy material via the thermal decomposition of titanium hydride rather than by chemical reduction, hence are further away from the claimed method than the process of D4.

4.2 As set out above in the section concerning novelty, the claimed method differs from that of D4 principally in that the initial metallic alloy powder produced by the chemical reduction is not melted.

4.3 According to page 5 of the application, articles produced by the claimed invention exhibit significantly reduced noise level during ultrasonic inspection; this allows smaller defects to be detected, or larger articles to be reliably fabricated and inspected. Thus, starting from D4, the objective problem to be solved is how to improve the ability to inspect articles made from the powders of D4.

4.4 The solution is to prevent melting both during production of the initial alloy material and during consolidation of the powder.

4.5 The appellant explained that in prior art processes which involves melting, coarse beta grains are formed; on cooling these lead to a coarse alpha-colony structure in the alloy. During ultrasonic inspection, such a structure creates a background noise that limits the ability to detect defects. The conventional approach to this problem is to use metalworking processes to break up the coarse alpha structure.

By avoiding melting, the coarse beta phase is prevented and the microstructure is free from alpha-phase colonies; any beta phase that forms via a solid state transformation is much finer and does not mask the presence of small defects.

4.6 None of the available prior art documents addresses the objective problem, and none suggest the avoidance of melting as a means for improving the ability to detect defects in articles produced by a chemical reduction process. The method of claim 1 of the main request therefore has an inventive step.

5. Articles 83 EPC

5.1 The application makes it clear that the important aspect of the invention is that there is no melting of the metal. For example, on page 2 the summary of the invention states that

"The present invention provides a fabrication approach for metallic articles in which the metal is never melted. Prior art fabrication techniques require melting the metal at some point in the processing".

Claim 1 defines the method as taking place without melting the initial metallic alloy powder and consolidating without melting either the alloy powder or the article.

5.2 Vapour phase reduction is cited as a particularly suitable method for carrying out the invention, and reference is made to the process described in documents D4 and D5 as being appropriate (see page 9 of the application).

As set out above (see points 3.3.3 and 3.3.4) the method of D4 aims to produce titanium in solid form, but the reduction of metal halides to metals is highly exothermic, such that the initial reaction products are molten.

5.3 The appellant suggests that the skilled person would adjust the process parameters accordingly, and although this would require some trials, it would be well within the skill of the average practitioner.

However, the Board notes that in D4 the flow of sodium is controlled to maintain the titanium in a solid phase, but nevertheless the reaction generates so much heat that initial melting of the metal takes place.

Bearing in mind that the invention requires that the metal is never melted, the application provides no explanation as to how melting is prevented in the very early stages of the process when the heat developed by the exothermic reaction is significant. Consequently, it is questionable if the disclosure is sufficiently complete for the skilled person to carry out the invention.

6. Remittal

6.1 The above issue concerning Article 83 EPC arose for the first time during the oral proceedings before the Board, and is of importance in determining whether or not the patent should be granted. In such a case, it is appropriate for the appellant to have the opportunity to be heard before two instances. The Board therefore agrees to the request of the appellant for the case to be remitted to the examining division for further prosecution.

6.2 If it is found that the invention is sufficiently disclosed, then extensive amendment of the description will be required in order to meet the requirements of Article 84 EPC. Attention is also drawn to application EP-A-03 760 334, which is the subject of appeal T 2321/09. This application is also from the appellant and is directed to a similar process as claimed in the present case, hence the issue of double-patenting may arise.

ORDER

For these reasons it is decided that:

1. The decision under appeal is set aside.

2. The case is remitted to the examining division for further prosecution.

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