EP0755427B1 - Lubricated metal workpiece and method - Google Patents
Lubricated metal workpiece and method Download PDFInfo
- Publication number
- EP0755427B1 EP0755427B1 EP95915241A EP95915241A EP0755427B1 EP 0755427 B1 EP0755427 B1 EP 0755427B1 EP 95915241 A EP95915241 A EP 95915241A EP 95915241 A EP95915241 A EP 95915241A EP 0755427 B1 EP0755427 B1 EP 0755427B1
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- European Patent Office
- Prior art keywords
- lubricant
- metal
- range
- lubricated
- components
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
- C10M105/38—Esters of polyhydroxy compounds
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/04—Hydroxy compounds
- C10M129/06—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
- C10M129/08—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least 2 hydroxy groups
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- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
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- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
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- C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
- C10M129/40—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms monocarboxylic
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- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
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Definitions
- This invention relates to lubricated metal workpieces, particularly of steel and aluminium, used in the production of press-formed components, and in particular to a method of using such workpieces to make structures of shaped components.
- the press-formed components may be secured together to form the structure by mechanical means, e.g. by rivets or spot-welds, either in addition to or instead of adhesive bonding.
- a lubricant for use in such a technique needs to fulfil several requirements:
- the lubricants of EPA 227360 are designed to be useful, not only for the technique described above, but also for other forming and shaping operations performed on a variety of metals.
- EPA 227360 provides a lubricating composition for press forming consisting of a lubricant dissolved or dispersed in a volatile liquid medium, wherein the lubricant comprises at least one ester of a polyhydric alcohol having two or three hydroxyl groups of which one or two are esterified with a long chain carboxylic acid and has a melting point above ambient temperature but low enough to permit removal from a metal surface by an aqueous alkaline cleaner.
- EPA 227360 mentions that mixtures of esters may be used and may be advantageous; and that the lubricant may contain a minor proportion up to 50% of one or more other lubricating compounds such as long-chain carboxylic acids.
- the lubricants exemplified are: diethylene glycol monostearate in solution in xylene; and diethylene glycol distearate in solution in xylene.
- lubricants described in EPA 227360 are generally successful at meeting requirements c) and d), they are sometimes less successful at meeting requirements a) and b). It is surprisingly found that lubricants of this kind are ineffective, so far as aluminium forming operations are concerned, at temperatures above their liquidus. For good aluminium lubricating properties, in ester lubricants of this kind, it appears necessary that some component be present in the solid state, so that the lubricant is solid or at least mushy or viscous, at the forming temperature which may be as high as 35°C or 40°C or even higher.
- EPA 276 568 refers to a metal forming lubricant composition comprising partial ester of polyhydric alcohols and ammonium salt of a long chain monocarboxylic acid and discloses a specific composition consisting of ethylene glycol monostearate and stearic acid. The lubricant is applied to the metal in form of an emulsion.
- JP-A-62127237 discloses according to the abstract that an aliphatic diester (e.g. ethylene glycol dilaurate) when used for metal forming reduces the sliding friction, prevents irregular coating or release during handling and crack formation.
- the ester is used as the sole lubricant.
- the invention provides lubricant which consists essentially of (in wt %) ethylene glycol dilaurate 50 - 85 ethylene glycol monolaurate 10 - 30 stearic acid up to 20 other glycol, ester and carboxylic acid species up to 20 as determined by analysis,
- the invention provides lubricated metal wherein a surface of the metal carries a film of the lubricant as defined.
- the present invention provides a method of making a structure of shaped aluminium components starting from lubricated aluminium metal sheet as defined, comprising the steps:
- Hardness of the lubricant is measured by a technique whereby a block of the uncoated lubricant is equilibrated at a given temperature and is penetrated by a steel needle.
- the test procedure used essentially involves driving a pointed 12 mm diameter needle into the lubricant at a speed of 20 mm/minute, achieved with the use of materials testing machine such as an Instron, and recording the load as a function of the needle penetration into the lubricant. Separate tests are conducted at various temperatures to derive the full curves. The hardness value quoted is then found as the slope of the graph of penetration load versus penetration distance.
- lubricant films of this invention have specified hardness values at temperatures within the range 15 - 40°C, in the case of particularly preferred lubricants, within the range 15 - 45°C.
- the lubricant film is too hard, it is likely to be brittle and have poor frictional characteristics during forming e.g. press-forming. If the lubricant film is too soft, then again the lubricating characteristics are inferior.
- the lubricant film has a hardness in the range 0.1 - 5 N/mm at all temperatures within the range specified at which forming e.g. press-forming is likely to take place in different parts of the world. It is surprising that the hardness of the lubricant film has useful predictive value for its lubricating characteristics.
- the major component of the lubricant film is ethylene glycol di-laurate (EGDL).
- EGDL ethylene glycol di-laurate
- the full ester or esters may be used optionally in admixture with a minor amount of stearic acid.
- This optional minor component is present in an amount of most usually 5 - 20%, by weight on the weight of the mixture.
- the full ester is used in admixture with a minor amount of ethylene glycol monolaurate (EGML).
- EGML ethylene glycol monolaurate
- Lubricant composition can drift during storage, resulting in a somewhat different composition on the lubricated metal surface, and these figures refer to the lubricant when freshly made.
- Proportions herein are determined by analysis e.g. by standard techniques involving gas chromatography, mass spectrometry and IR spectrometry; they do not necessarily correspond closely to manufacturers' stated proportions in commercially available materials.
- Suitable lubricants may be achieved in one or both of two ways. The first is by blending two or more components together. The second is by using purer material.
- Full esters and partial esters such as EGDL and EGML can have impurities arising from two main sources:-
- the lubricating characteristics of the lubricant film on lubricated metal according to this invention fall off at both excessively high and excessively low temperature.
- This frictional coefficient is preferably below about 0.1 at all temperatures within the range of interest, that is to say 15°C up to 30°C or 35°C or 40°C or 45°C.
- the hardness of the lubricant film at any temperature is predictive of its frictional coefficient.
- the lubricant may need to be compatible with subsequently applied adhesive.
- the esters described herein are compatible as a result of being either absorbed or displaced by subsequently applied adhesive without grossly impairing the adhesive bond strength obtainable.
- resinous lubricants and metal soap lubricants are generally not adhesive compatible in this sense.
- the lubricant has a melting point above ambient temperature, preferably of at least 30°C, more preferably at least 40°C. This ensures that the lubricant is present as a solid film on the metal substrate, which avoids problems with smearing and blocking during coiling, decoiling, slitting and cutting.
- the use of such a lubricant avoids contamination of the metal surface with a possible adhesive-incompatible oil or contaminant and prevents local build up of lubricant to an undesirably thick layer.
- the lubricant melts at a temperature low enough to permit its removal from a metal surface by an aqueous alkaline cleaner, such as is used in automotive production lines to prepare metal parts for painting.
- the highest practicable temperature for aqueous alkaline cleaners in such circumstances is about 70°C.
- Lubricants melting below 70°C and preferably below 65°C can thus be removed by aqueous alkaline cleaners.
- Lubricants melting above 70°C may or may not be removable depending on whether they have chemical groups, e.g. hydroxyl groups, which can react with the alkali to assist removal from the metal surface.
- a commercially available wax having a melting point of 85°C and an acid number of 135 to 155 by DIN 53402 was found not to be removable by aqueous alkaline cleaners.
- a lubricant is deemed removable by aqueous alkaline cleaners if it can be removed by treatment for 2 minutes at 70°C with a 15% by weight aqueous solution of Ridolene 160 (a silicate-based proprietary cleaner marketed by I.C.I. plc.)
- a further aspect of this invention involves applying the lubricant to the metal in the absence of any volatile solvent or diluent. This avoids the need to evaporate volatile liquid from the lubricant film, and avoids the need to include any surface active agent in the lubricant. It is found that the molten lubricants have satisfactory viscosity for spraying or for application by roller coat. To ensure rapid solidification of the lubricant film, the metal may be pre-cooled. To ensure good adhesion of a uniform film, the metal may be pre-heated.
- the lubricant may be dissolved in a volatile solvent for application to the metal. Indeed, very thin films can only be applied from solution. The use of solution permits control of lubricant film thickness to within less than 0.5 g/m 2 .
- the lubricant may be applied to steel or other metals, but is likely to be principally used on aluminium, which term is used to cover the pure metal and alloys in which Al is the major component.
- a metal surface may carry a strongly-bonded inorganic and/or organic pretreatment or primer layer, on the top of which the lubricant is present.
- Such non-metallic layers are well known, and may be provided for example as chemical conversion coatings or deposited coatings of the no-rinse type, based on chromium, titanium or zirconium; or may be an anodic oxide layer (on Al or Ti) or a siloxane layer.
- the metal may be in sheet form.
- the rate of application of lubricant will depend on the intended use, but may typically be in the range of 0.1 - 10 g/m 2 , e.g. 0.25 - 8 g/m 2 , particularly 1 - 4 g/m 2 , for aluminium coil to be formed into adhesively bonded structures.
- a purpose built strip-draw rig was designed and constructed with reference to ASTM 4173-82 for testing sheet metal forming lubricants.
- the apparatus is shown in Figures 1 and 2.
- the die set shown in Figure 1 was designed to simulate material flowing between pressurised binder surfaces containing a draw bead arrangement.
- the die set of Figure 2 was designed to simulate flow between parallel binder surfaces so as to allow conventional frictional values to be obtained.
- one die 10 of each tool set is mounted on a load cell 12.
- the other die 14 of the tool set is mounted on a hydraulic cylinder 16.
- Flat strips 18, hydraulically pressurised between the two dies, can then be pulled through a particular tool set while the clamp load is measured.
- the draw load is also measured using a second load cell 20 mounted between a testing machine gripping jaw 22 and a cross head 24.
- the strip draw rig is designed to be mounted on either a press simulator or a standard tensile testing frame, depending on the variables under investigation.
- Lubricated strips of material 50 mm wide, were placed between the two faces of the flat tool set of Figure 2 and hydraulically pressurised to a particular load. The strips were then drawn through the die set of Figure 1 for a distance of approximately 250 mm, the draw and clamp forces being recorded as a function of time/displacement of the drawn strip. Results presented in the form of a graph (draw force/2) versus clamp load have a slope equal to the conventional friction coefficient.
- a lubricant formulation according to the invention had the composition, in wt%:-
- lubricant 1 The identity of the components was determined by standard gas chromatography/mass spectrometry techniques. This formulation is hereinafter called lubricant 1.
- Another lubricant formulation according to the invention had the composition, in wt%:-
- lubricant 3 The identity of these components also was determined by standard gas chromatography/mass spectrometry techniques. The formulation is hereinafter called lubricant 3.
- Lubricant 2 contains commercially available EGML 90% and stearic acid 10%. This lubricant falls outside the scope of the present invention, and is included for comparison purposes only.
- Lubricants 1, 2 and 3 were applied by spraying on to aluminium alloy sheets which had been preheated to 50°C. By this means, uniform films could be applied at controlled thickness. The hardness of the lubricants was measured (by the method described above) and the results are recorded in Figure 3.
- Lubricants 1 and 2 were further tested in the strip draw rig illustrated in Figures 1 and 2. In each case, tests were performed at different temperatures in the range 0 - 50°C; and at five different rates of lubricant application ranging from 1 - 6 g/m 2 . The results of these tests are shown in Figure 4 (for lubricant 2) and Figure 6 (for lubricant 1 batch 2, see below).
- Lubricants 1 and 3 from Example 1 were evaluated.
- Lubricant 2 from Example 1 was used for comparative purposes.
- the procedure for lubricant application consisted of pre-heating a reservoir of the new lubricant to 70°C, and applying this onto sheets using air-assisted airless spray nozzles. Lubricant was applied to sheets which were held at both room temperature (20°C), and preheated to 60°C. These sheets were then placed in stacks. In the case of the pre-heated material, the sheets were placed in a stack when the lubricant had solidified.
- the standard test method for adhesive compatibility is to assemble standard lap shear joints with a 10 mm overlap, using lubricated 1.6 mm pretreated coupons and a standard adhesive. A string of six such joints are then exposed to combined stress/humidity testing under a constant load. The time to failure of the first three joints in a set of six joints is then noted. Individual lap shear joints are also exposed to salt spray for given periods of time, and then tested for static strength retention.
- Tests were carried out on joints manufactured with the lubricant 1 on their surfaces prior to bonding. Two lubricant weight levels were evaluated, namely 2.0 g/m 2 and 5.5 g/m 2 .
- the Wax Penetration Test was used to determine the softening response as a function of temperature.
- the test procedure used essentially involves driving a pointed 12 mm diameter needle into the lubricant at a speed of 20 mm/minute, achieved with the use of materials testing machine such as an Instron, and recording the load as a function of the needle penetration into the lubricant. Separate tests are conducted at various temperatures to derive the full curves. The hardness value quoted is then found as the slope of the graph of penetration load versus penetration distance.
- Lubricated sheets were produced with 3 g/m 2 of different lubricants via the pre-heated blank route, as indicated in section 2.1. These sheets were guillotined into strips 50 mm wide and then drawn through the strip draw rig, using the described procedure, to allow friction values to be determined at temperatures of 10, 20, 30, 40 and 50°C.
- Sheets of AA5754-0 were pressed with 3 g/m 2 of both lubricants 1 and 2 to allow the comparative performance to be assessed.
- lubricated stacks were produced by applying the lubricant to pre-heated blanks, as described in section 2.1.
- pretreated strips of aluminium were lubricated with lubricant 2 (3.4 g/m 2 ) and lubricant 1 (3.8 g/m 2 ), and given the following treatment:
- Table 1 The results of stress-humidity and salt spray testing on joints produced with lubricant 1 on their surfaces are presented in Table 1. This Table shows a good strength retention after 20 weeks salt spray, and a testing duration in excess of 100 days during stress/humidity with a 5 MPa applied stress.
- Lubricant 2 is shown for comparison. The hardness was relatively low at all temperatures.
- Table 2 shows the comparative performance of the lubricants 1, 2 and 3 over the measured temperature range for a given lubricant weight of 3 g/m 2 . These figures show an improved performance of the lubricant 1 batch 1 at temperatures of 30, 40 and 50°C. They also indicate a similar performance at 20°C.
- Salt spray data after 20 weeks exposure shows excellent strength retention at both lubricant weight levels, out-performing the lubricant 2.
Abstract
Description
- The metal surface is pre-treated to provide a strongly bonded layer thereon which acts as a base for subsequently applied adhesive.
- A lubricant is applied to the treated metal coil. The coil may then be stored or transported, with the lubricant serving to protect the treated metal surface, and is cut up into pieces ready for press-forming.
- The pieces of metal sheet are press-formed into components of desired shape. This and subsequent operations are all performed on an automobile production line.
- Adhesive is applied to selected areas of the shaped components, without first removing the lubricant.
- The components are assembled into the shape of the desired structure, and may be spot welded or otherwise fixed to hold the structure together until the adhesive is cured.
- The adhesive is cured at elevated temperature.
- The metal surfaces of the structure are subjected to an aqueous alkaline cleaner which removes the lubricant.
- The structure is painted.
ethylene glycol dilaurate | 50 - 85 |
ethylene glycol monolaurate | 10 - 30 |
stearic acid | up to 20 |
other glycol, ester and carboxylic acid species | up to 20 |
- forming pieces of the sheet into components,
- bringing the components together in the shape of the desired structure,
- and securing the components together by mechanical and/or adhesive means.
- Figure 1 is a schematic view of a strip-draw apparatus used for testing lubricated metal;
- Figure 2 is a perspective view of a modified strip-draw apparatus;
- Figure 3 is a graph of hardness against temperature for several lubricants.
- Figures 4 and 6 are Bar Charts showing
frictional coefficients of two lubricants at different
temperatures and different rates of application.
Figure 4 is for
lubricant 2. Figure 6 is forlubricant 1. - Figure 5 is a bar chart showing lubricant residues after different bakes followed by cleaning.
Stress/Humidity and Salt Spray Data for the | ||||||
Lubricant Weight g/m2 | Stress/Humidity Days to Failure | Salt Spray Results (MPa) | ||||
3 | 4 | 5 | 0 | 8 | 20 wks | |
2.0 | 190+ | 190+ | 190+ | 27.8 | 25.5 (92%) | 25.1 (90%) |
5.5 | 190+ | 190+ | 137 | 28.4 | 25.2 (89%) | 23.6 (83%) |
Friction Value at temperature ° | |||||
Lubricant | |||||
10° | 20° | 30° | 40° | 50° | |
1 | 0.017 | 0.012 | 0.046 | 0.069 | |
2 | 0.020 | 0.036 | 0.096 | 0.107 | |
3 | 0.092 | 0.020 | 0.043 | nd | nd |
nd - not determined |
Effect of Lubricant on Press Formability | |||
Lubricant | Coat Weight (g/m2) | Square Pan Depth mm | |
2 | 3.0 | 59.1 | 51.5 |
1 | 3.0 | 74.3 | 52.0 |
Claims (11)
- Lubricant which consists essentially of (in wt %)
ethylene glycol dilaurate 50 - 85 ethylene glycol monolaurate 10 - 30 stearic acid up to 20
as determined by analysis,
which lubricant has a hardness in the range 0.1 - 10 N/mm at all temperatures in the range 15 - 35°C. - Lubricant as claimed in claim 1, wherein the lubricant has a hardness in the range 0.1-5 N/mm at all temperatures within the range specified.
- Lubricant as claimed in claim 1 or claim 2, wherein the lubricant has a hardness within the range specified at all temperatures in the range 15 - 40°C.
- Lubricant as claimed in any one of claims 1 to 3, wherein the stearic acid content is 5-20% by weight.
- Lubricated metal, wherein a surface of the metal carries a film of the lubricant of any one of claims 1 to 4.
- Lubricated metal as claimed in claim 5, wherein the metal is sheet.
- Lubricated metal as claimed in claim 5 or claim 6, wherein the metal is aluminium.
- Lubricated metal as claimed in claim 7, wherein the aluminium carries a strongly-bonded - artificial inorganic surface layer on top of which the film of lubricant is present.
- A method of making a structure of shaped aluminium components starting from lubricated aluminium metal sheet according to any one of claims 6 to 8, comprising the steps:forming pieces of the sheet into components,bringing the components together in the shape of the desired structure,and securing the components together by mechanical and/or adhesive means.
- A method as claimed in claim 9, comprising the steps:forming pieces of the sheet into components,applying adhesive to the components,bringing the components together in the shape of the desired structure, andcuring the adhesive.
- A method as claimed in claim 9 or claim 10, comprising the additional steps of subjecting the structure to the action of an aqueous alkaline cleaner, and thereafter painting the structure.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP94302557 | 1994-04-12 | ||
AT94302/55 | 1994-04-12 | ||
PCT/GB1995/000829 WO1995027767A1 (en) | 1994-04-12 | 1995-04-12 | Lubricated metal workpiece and method |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0755427A1 EP0755427A1 (en) | 1997-01-29 |
EP0755427B1 true EP0755427B1 (en) | 1998-07-29 |
Family
ID=8217644
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP95915241A Expired - Lifetime EP0755427B1 (en) | 1994-04-12 | 1995-04-12 | Lubricated metal workpiece and method |
Country Status (12)
Country | Link |
---|---|
EP (1) | EP0755427B1 (en) |
JP (1) | JPH09511542A (en) |
KR (1) | KR100388008B1 (en) |
CN (1) | CN1044003C (en) |
AT (1) | ATE169055T1 (en) |
AU (1) | AU682599B2 (en) |
BR (1) | BR9507319A (en) |
CA (1) | CA2186848A1 (en) |
DE (1) | DE69503773T2 (en) |
ES (1) | ES2120742T3 (en) |
MX (1) | MX9604675A (en) |
WO (1) | WO1995027767A1 (en) |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1644871B2 (en) * | 1964-05-08 | 1973-03-08 | Dynamit Nobel Ag, 5210 Troisdorf | LUBRICANT |
JPS62127237A (en) * | 1985-11-28 | 1987-06-09 | 日本製箔株式会社 | Metallic sheet metal for molding |
GB8530146D0 (en) * | 1985-12-06 | 1986-01-15 | Alcan Int Ltd | Lubricating composition |
DE3626376C1 (en) * | 1986-08-04 | 1987-04-30 | Hans Schur | Adhesive oil and its use for chainsaw chains and for construction formwork |
GB8630971D0 (en) * | 1986-12-29 | 1987-02-04 | Alcan Int Ltd | Lubricant emulsion |
CN1004143B (en) * | 1987-06-06 | 1989-05-10 | 河北省体育科学研究所 | Water-solid two-phase motion drag reducer |
US4950415A (en) * | 1989-11-17 | 1990-08-21 | Nalco Chemical Company | Water washable dry film lubricants |
-
1995
- 1995-04-12 ES ES95915241T patent/ES2120742T3/en not_active Expired - Lifetime
- 1995-04-12 AT AT95915241T patent/ATE169055T1/en not_active IP Right Cessation
- 1995-04-12 JP JP7526188A patent/JPH09511542A/en not_active Ceased
- 1995-04-12 KR KR1019960705697A patent/KR100388008B1/en not_active IP Right Cessation
- 1995-04-12 DE DE69503773T patent/DE69503773T2/en not_active Expired - Lifetime
- 1995-04-12 EP EP95915241A patent/EP0755427B1/en not_active Expired - Lifetime
- 1995-04-12 CA CA002186848A patent/CA2186848A1/en not_active Abandoned
- 1995-04-12 BR BR9507319A patent/BR9507319A/en not_active IP Right Cessation
- 1995-04-12 AU AU22185/95A patent/AU682599B2/en not_active Ceased
- 1995-04-12 MX MX9604675A patent/MX9604675A/en not_active IP Right Cessation
- 1995-04-12 CN CN95193350A patent/CN1044003C/en not_active Expired - Fee Related
- 1995-04-12 WO PCT/GB1995/000829 patent/WO1995027767A1/en active IP Right Grant
Also Published As
Publication number | Publication date |
---|---|
DE69503773D1 (en) | 1998-09-03 |
KR970702352A (en) | 1997-05-13 |
EP0755427A1 (en) | 1997-01-29 |
CN1149311A (en) | 1997-05-07 |
BR9507319A (en) | 1997-09-30 |
CN1044003C (en) | 1999-07-07 |
AU2218595A (en) | 1995-10-30 |
JPH09511542A (en) | 1997-11-18 |
WO1995027767A1 (en) | 1995-10-19 |
KR100388008B1 (en) | 2003-10-22 |
AU682599B2 (en) | 1997-10-09 |
DE69503773T2 (en) | 1999-02-04 |
CA2186848A1 (en) | 1995-10-19 |
MX9604675A (en) | 1997-12-31 |
ATE169055T1 (en) | 1998-08-15 |
ES2120742T3 (en) | 1998-11-01 |
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