CN104761915B - A kind of preparation method of wear-resisting polyimides and fluoro-containing copolymer composition - Google Patents
A kind of preparation method of wear-resisting polyimides and fluoro-containing copolymer composition Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of wear-resisting polyimides and fluoro-containing copolymer composition, comprise the following steps：(a) by weight, by 90~98.9 parts of fluoropolymer micro mist, 1~5 part of metal hydroxides, 0.1~5 part of processing aid, at 15~25 DEG C, mixes 0.5~1h, obtains fluoropolymer micro mist premix under 100~300rpm；(b) by weight, by 80~98 parts of polyimides powder, 2~20 parts of the fluoropolymer micro mist premix that step (a) is obtained, at 15~25 DEG C, mixed under 100~300rpm after 0.5~1h, extruded through double screw extruder, granulating and forming, obtain wear-resisting polyimides and fluoro-containing copolymer composition.Present invention process is simple, easily industrialization, and obtained composition coefficient of friction and frictional dissipation rate is low, and composition can be applied to the fields such as military affairs, Aero-Space, precision optical machinery, machinery, electronics, automobile, food medical treatment by processing and forming.
Description
Technical field
The present invention relates to polymeric material field, and in particular to a kind of wear-resisting polyimides and fluoro-containing copolymer composition
Preparation method.
Background technology
Polyimides as special engineering plastics one kind, because it has excellent high temperature resistant, low temperature resistant, high-strength height
Mould, high creep resistant, high dimensionally stable, low thermal coefficient of expansion, high electric insulation, low-k and loss, radiation hardness, corrosion-resistant etc.
Advantage, is widely used in microelectronics industry and aerospace material.Fluoropolymer particularly ptfe micropowder has
There are the performances such as high thermal stability, chemical resistance and self-lubricating, add in polyimide material, prepare wear-resisting polytetrafluoroethylene (PTFE)
Micro mist/polyimides intermingling material, has been widely used for the sliding axle in the fields such as Aero-Space, automobile, machinery, electronic apparatus
Hold, the part such as thrust washer, sealing ring, blade, valve seat, axle bush and wear-resistant pad.
External ptfe micropowder/polyimides intermingling material has GE companies Ultem series, Mitsui companies
Aurum series, the Torlon series of Solvay companies, the Vespel of Dupont companies is serial and Ensinger companies
Tecasint series etc..Domestic Chinese Academy of Sciences's orchidization is studied and also there is correlative study report in Nanjing University of Technology.At present, state
Inside and outside ptfe micropowder/polyimides intermingling material the conventional method for preparing is directly by ptfe micropowder and polyamides Asia
It is mixed with polyimides after the method for amine mixing is made composition or is surface-treated ptfe micropowder using surfactant
Close, composition is made, part is made after processing.The method is intended to change the surface polarity of ptfe micropowder, increase
With the physical compatibility of polyimides, dispersiveness of the ptfe micropowder in matrix resin polyimides, Jin Erjun are improved
The wearability of even increase polyimides intermingling material.However, in intermingling material prepared by above-mentioned conventional method, polytetrafluoroethylene (PTFE)
It is Physical interaction between micro mist and polyimide molecule, in use, ptfe micropowder is easily lost, intermingling material
Crocking resistance is gradually reduced, and the service life of intermingling material is low.
To overcome above-mentioned intermingling material, crocking resistance is gradually reduced in use, causes intermingling material service life
Low the problem of, now it is badly in need of exploring a kind of preparation side of the stable ptfe micropowder/polyimide compositions of crocking resistance
Method.
The content of the invention
The present invention simply, is easily industrialized there is provided a kind of technique in view of the deficiencies of the prior art, obtained composition
Coefficient of friction and frictional dissipation rate are low, the wear-resisting polyimides of long product lifecycle and fluoropolymer combination after processing and forming
The preparation method of thing.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of wear-resisting polyimides and fluorine-containing poly-
The preparation method of polymer composition, comprises the following steps：
(a) by weight, by 90~98.9 parts of fluoropolymer micro mist, 1~5 part of metal hydroxides, processing aid
0.1~5 part, at 15~25 DEG C, 0.5~1h is mixed under 100~300rpm, fluoropolymer micro mist premix is obtained；
(b) by weight, by 80~98 parts of polyimides powder, the fluoropolymer micro mist premix that step (a) is obtained
2~20 parts of material, at 15~25 DEG C, mixes after 0.5~1h under 100~300rpm, is extruded through double screw extruder, granulating and forming,
Obtain wear-resisting polyimides and fluoro-containing copolymer composition.
Described fluoropolymer micro mist is preferably proplast micro mist, tetrafluoroethene and CTFE copolymerization
Thing micro mist, tetrafluoroethene and vinylidene fluoride copolymers micro mist, tetrafluoroethene and hexafluoropropylene copolymer micro mist, tetrafluoroethene with it is complete
Fluoropropyl vinyl ether co-polymer micro mist, tetrafluoroethene and perfluoroethylvinyl ether copolymer micropowders, tetrafluoroethene and perfluor
One kind in methyl vinyl ether copolymer micro mist.
Described fluoropolymer micro mist average grain diameter is preferably 500nm~15 μm, more preferably 2~8 μm.
Described metal hydroxides is preferably Ca (OH)2、Mg(OH)2、Zn(OH)2、Cu(OH)2、Al(OH)3In one kind
Or two kinds of mixture.
Described processing aid is preferably methyl methacrylate/acrylic acid ester copolymer, methyl methacrylate/benzene second
One kind in alkene copolymer, acrylonitrile/styrol copolymer.
The mixing section temperature of described double screw extruder is preferably 250~280 DEG C, and hot melt section temperature is preferably 330~
350 DEG C, compression section temperature is preferably 310~330 DEG C, and die head temperature is preferably 300~320 DEG C.
The present invention is surface-treated and is pre-mixed by fluoropolymer micro mist, with polyimides extrusion mixing, obtained combine
The technique of thing, carries out chemical bond by polyimides and fluoropolymer micro mist molecule and composition is even made.Solve conventional method
In the composition of preparation between fluoropolymer micro mist and polyimide molecule be only Physical interaction, in use, contain
Fluoropolymer micro mist is easily lost, and composition crocking resistance is gradually reduced, and causes the problem of composition service life is low.This preparation
Method technique is simple, easily realizes industrialization, and obtained composition coefficient of friction and frictional dissipation rate is low, and composition passes through shaping
Processing can be applied to the fields such as military affairs, Aero-Space, precision optical machinery, machinery, electronics, automobile, food medical treatment.
At present, fluoropolymer micro mist is typically prepared using cracking process or direct polymerization method, fluorine-containing in the present invention
Polymer micro mist can be using proplast micro mist or tetrafluoroethene and CTFE, vinylidene, hexafluoropropene, complete
A kind of obtained copolymer micropowders in fluoropropyl vinyl ethers, perfluoroethylvinyl ether, perfluoro methyl vinyl ether.It is logical
Cross during direct polymerization method prepares ptfe micropowder, the species of initiator and telogen determines ptfe micropowder
The unit structure of end group, by using different initiator and telogen, the end moieties of ptfe micropowder can for carboxylic acid,
Hydroxyl, sulfonic acid or sulfate group, imine group and hydroxy-acid group that these groups can be formed with the polyimides after open loop
React under certain condition, polyimides connects with the intermolecular generation chemical bond of ptfe micropowder, reduction composition
Coefficient of friction and frictional dissipation, the service life of product after extension composition molding processing.Therefore, it is of the present invention fluorine-containing poly-
Compound micro mist be preferably proplast micro mist, tetrafluoroethene and chlorotrifluoroethylene micro mist, tetrafluoroethene with partially
Fluoride copolymers micro mist, tetrafluoroethene and hexafluoropropylene copolymer micro mist, tetrafluoroethene and perfluoro propyl vinyl ether copolymerization
Thing micro mist, tetrafluoroethene and perfluoroethylvinyl ether copolymer micropowders, tetrafluoroethene and perfluoro methyl vinyl ether copolymer
One kind in micro mist.
The average grain diameter of fluoropolymer micro mist is mixed into the dispersiveness of " sea-island " structure formed during polyimides to it
There is direct relation, the dispersiveness of fluoropolymer micro mist directly influences fluoropolymer micro mist and polyimides blend composition
And its after processing and forming product performance, therefore, the average grain diameter of fluoropolymer micro mist of the present invention is preferably 500nm
~15 μm, more preferably 2~8 μm.
Polyimides water, acid/base exist and certain temperature under, imide group occur open loop, formed imine group or
Hydroxy-acid group, metal hydroxides can resolve into the metal hydroxides of metal oxide and hydrone in a heated condition,
So, it on the one hand can uniformly be scattered in composition, acid imide open loop is distributed in the composition relatively uniform, improve acyl
The probability that the group formed after imine group open loop reacts with fluoropolymer end group；On the other hand inorganic oxide is formed
Thing, increases the wearability and mechanical property of composition, makes up the addition of fluoropolymer micro mist to intermingling material mechanical property
Influence.Metal hydroxides of the present invention is Ca (OH)2、Mg(OH)2、Zn(OH)2、Cu(OH)2、Al(OH)3In one kind
Or two kinds of mixture.
, it is necessary to melt polyimides under certain condition after polyimides is mixed with fluoropolymer micro mist premix,
Polyimides and fluoropolymer, which react, simultaneously needs also exist for certain temperature, according to the rheological property of polyimides and poly-
Acid imide open loop is extruded with temperature needed for fluoropolymer reaction, therefore the present invention through double screw extruder, and comminutor is a granulated into
Type, obtains wear-resisting polyimides and ptfe micropowder composition, and the mixing section temperature of double screw extruder is preferably 250~
280 DEG C, hot melt section temperature is preferably 330~350 DEG C, and compression section temperature is preferably 310~330 DEG C, and die head temperature is preferably 300
~320 DEG C.
Compared with prior art, the present invention has advantages below：
1st, obtained composition coefficient of friction and frictional dissipation rate are low, long product lifecycle, this hair after processing and forming
The open loop of polyimide molecule segment is formed imines and hydroxy-acid group by bright use metal hydroxides, at a certain temperature with poly- four
PVF micro mist carboxylic acids or hydroxyl end groups chemically react, and form chemical bond and connect, improve polyimides and polytetrafluoro
Ethene micro mist be based composition and use thereof in packaging crocking resistance, extend the life-span of product after processing and forming, coefficient of friction below 0.35,
Minimum reachable 0.09, frictional dissipation rate is 7.8 × 10-6mm3/ below Nm, it is minimum up to 2.2 × 10-6mm3/Nm；
2nd, technique is simple, easily realizes industrialization, compared with conventional machining process, further simplify technological process.
Embodiment
The present invention is described in further detail with reference to embodiments, but the present invention is not limited solely to following implementation
Example.
Embodiment 1
(1) average grain diameter 500nm polytetrafluoroethylene (PTFE) homopolymer micro mist 45kg, Ca (OH) is weighed22.5kg, metering system
Sour methyl esters/acrylate copolymer 2.5kg, 0.5h is mixed under 25 DEG C, 100rpm rotating speeds, obtains ptfe micropowder premix
Material；
(2) polyimides powder (GE Ultem1000) 40kg, ptfe micropowder premix made from step (1) are weighed
Expect 10kg, mixed under 20 DEG C, 100rpm rotating speeds after 0.5h, be respectively in mixing section, hot melt section, compression section and die head temperature
Extruded at 250 DEG C, 340 DEG C, 320 DEG C, 300 DEG C through double screw extruder, comminutor granulating and forming obtains composition.
Embodiment 2
(1) polytetrafluoroethylene (PTFE) homopolymer the micro mist 46kg, Mg (OH) of 10 μm of average grain diameter are claimed22kg, methyl methacrylate
Ester/styrol copolymer 2kg, 0.7h is mixed under 20 DEG C, 200rpm rotating speeds, obtains ptfe micropowder premix.
(2) polyimides powder (GE Ultem1000) 41kg is weighed, ptfe micropowder made from step (1) is premixed
Expect 9kg, mixed under 15 DEG C, 200rpm rotating speeds after 0.6h, be respectively 260 in mixing section, hot melt section, compression section and die head temperature
DEG C, 340 DEG C, 320 DEG C, extruded through double screw extruder at 300 DEG C, comminutor granulating and forming obtains composition.
Embodiment 3
(1) polytetrafluoroethylene (PTFE) homopolymer the micro mist 47kg, Zn (OH) of 5 μm of average grain diameter are weighed21.5kg, acrylonitrile/benzene second
Alkene copolymer 1.5kg, 0.6h is mixed under 15 DEG C, 300rpm rotating speeds, obtains ptfe micropowder premix.
(2) polyimides powder (GE Ultem1000) 42.5kg is weighed, ptfe micropowder made from step (1) is pre-
Batch mixing 7.5kg, is mixed after 0.8h under 18 DEG C, 300rpm rotating speeds, in mixing section, hot melt section, compression section and die head temperature difference
To be extruded at 270 DEG C, 340 DEG C, 320 DEG C, 300 DEG C through double screw extruder, comminutor granulating and forming obtains composition.
Embodiment 4
(1) polytetrafluoroethylene (PTFE) homopolymer the micro mist 48kg, Cu (OH) of 8 μm of average grain diameter are weighed21kg, methyl methacrylate
Ester/acrylate copolymer 1kg, 0.8h is mixed under 18 DEG C, 100rpm rotating speeds, obtains ptfe micropowder premix.
(2) polyimides powder (GE Ultem1000) 45kg is weighed, ptfe micropowder made from step (1) is premixed
Expect 5kg, mixed under 20 DEG C, 100rpm rotating speeds after 0.8h, be respectively 280 in mixing section, hot melt section, compression section and die head temperature
DEG C, 340 DEG C, 320 DEG C, extruded through double screw extruder at 300 DEG C, comminutor granulating and forming obtains composition.
Embodiment 5
(1) tetrafluoroethene and chlorotrifluoroethylene micro mist 49kg, Al (OH) of 15 μm of average grain diameter are weighed30.5kg,
Methyl methacrylate/styrol copolymer 0.05kg, 0.9h is mixed under 22 DEG C, 200rpm rotating speeds, obtain tetrafluoroethene and
Chlorotrifluoroethylene micro mist premix.
(2) polyimides powder (GE Ultem1000) 47kg, tetrafluoroethene and trifluoro chloroethene made from step (1) are weighed
Alkene copolymer micro mist premix 3kg, at 22 DEG C, is mixed after 0.9h under 200rpm, in mixing section, hot melt section, compression section and die head
Temperature is respectively to be extruded through double screw extruder at 270 DEG C, 340 DEG C, 320 DEG C, 300 DEG C, and comminutor granulating and forming is combined
Thing.
Embodiment 6
(1) tetrafluoroethene and chlorotrifluoroethylene micro mist 45kg, Ca (OH) of 12 μm of average grain diameter are weighed22.5kg,
Acrylonitrile/styrol copolymer 2.5kg, mixes 0.5h under 25 DEG C, 300rpm rotating speeds, obtains tetrafluoroethene and CTFE
Copolymer micropowders premix.
(2) polyimides powder (GE Ultem1000) 49kg, tetrafluoroethene and trifluoro chloroethene made from step (1) are weighed
Alkene copolymer micro mist premix 1kg, under 25 DEG C, 300rpm rotating speeds mix 0.5h after, mixing section, hot melt section, compression section and
Die head temperature is respectively to be extruded through double screw extruder at 280 DEG C, 345 DEG C, 325 DEG C, 320 DEG C, and comminutor granulating and forming is obtained
Composition.
Embodiment 7
(1) tetrafluoroethene and hexafluoropropylene copolymer micro mist 46kg, Mg (OH) of 2 μm of average grain diameter are weighed21kg, Zn
(OH)21kg, methyl methacrylate/acrylic acid ester copolymer 2kg, mixes 1h under 25 DEG C, 200rpm rotating speeds, obtains tetrafluoro
Ethene and hexafluoropropylene copolymer micro mist premix.
(2) polyimides powder (GE Ultem1000) 40kg, tetrafluoroethene and hexafluoropropene made from step (1) are weighed
Copolymer micropowders premix 10kg, is mixed after 1h under 25 DEG C, 200rpm rotating speeds, in mixing section, hot melt section, compression section and die head
Temperature is respectively to be extruded through double screw extruder at 280 DEG C, 350 DEG C, 330 DEG C, 310 DEG C, and comminutor granulating and forming is combined
Thing.
Embodiment 8
(1) tetrafluoroethene and perfluoro propyl vinyl ether copolymer micropowders 47kg, Cu (OH) of 12 μm of average grain diameter are weighed20.6kg, Al (OH)30.6kg, methyl methacrylate/styrol copolymer 1.8kg is mixed under 25 DEG C, 100rpm rotating speeds
1h, obtains tetrafluoroethene and perfluoro propyl vinyl ether copolymer micropowders premix.
(2) polyimides powder (GE Ultem1000) 42.5kg, tetrafluoroethene and perfluor third made from step (1) are weighed
Base vinyl ether co-polymer micro mist premix 7.5kg, under 25 DEG C, 100rpm rotating speeds mix 1h after, mixing section, hot melt section,
Compression section and die head temperature are respectively to be extruded through double screw extruder at 280 DEG C, 335 DEG C, 315 DEG C, 305 DEG C, comminutor granulation
Shaping, forms composition.
Embodiment 9
(1) tetrafluoroethene and perfluoroethylvinyl ether copolymer micropowders 48kg, Cu (OH) of 8 μm of average grain diameter are weighed20.5kg, Mg (OH)20.5kg, methyl methacrylate/acrylic acid ester copolymer 1kg, are mixed under 25 DEG C, 200rpm rotating speeds
0.5h, obtains tetrafluoroethene and perfluoroethylvinyl ether copolymer micropowders premix.
(2) polyimides powder (GE Ultem1000) 45kg, tetrafluoroethene and perfluoro-ethyl made from step (1) are weighed
Vinyl ether co-polymer micro mist premix 5kg, is mixed after 0.5h under 25 DEG C, 200rpm rotating speeds, in mixing section, hot melt section, pressure
Contracting section and die head temperature are respectively to be extruded through double screw extruder at 280 DEG C, 330 DEG C, 310 DEG C, 300 DEG C, and comminutor is a granulated into
Type, obtains composition.
Embodiment 10
(1) tetrafluoroethene and perfluoro methyl vinyl ether copolymer micropowders 49.45kg, Mg of 3 μm of average grain diameter are weighed
(OH)20.5kg, acrylonitrile/styrol copolymer 0.05kg, 1h is mixed under 25 DEG C, 100rpm rotating speeds, obtain tetrafluoroethene and
Perfluoro methyl vinyl ether copolymer micropowders premix.
(2) polyimides powder (GE Ultem1000) 45kg, tetrafluoroethene and perfluoro-methyl made from step (1) are weighed
Vinyl ether co-polymer micro mist premix 5kg, is mixed after 1h under 25 DEG C, 100rpm rotating speeds, in mixing section, hot melt section, compression
Section and die head temperature are respectively to be extruded through double screw extruder at 280 DEG C, 340 DEG C, 320 DEG C, 300 DEG C, comminutor granulating and forming,
Obtain composition.
Comparative example 1
(1) average grain diameter 500nm polytetrafluoroethylene (PTFE) homopolymer micro mist 45kg, silane coupler KH5602.5kg is weighed,
Methyl methacrylate/acrylic acid ester copolymer 2.5kg, mixes 0.5h under 25 DEG C, 100rpm rotating speeds, obtains polytetrafluoroethylene (PTFE)
Micro mist premix.
(2) polyimides powder (GE Ultem1000) 40kg, ptfe micropowder premix made from step (1) are weighed
Expect 10kg, mixed under 25 DEG C, 100rpm rotating speeds after 0.5h, be respectively in mixing section, hot melt section, compression section and die head temperature
Extruded at 250 DEG C, 340 DEG C, 320,300 DEG C through double screw extruder, comminutor granulating and forming obtains composition.
Comparative example 2
(1) tetrafluoroethene and chlorotrifluoroethylene micro mist 49kg of 15 μm of average grain diameter, methyl methacrylate are weighed
Ester/styrol copolymer 0.05kg, 0.5h is mixed under 25 DEG C, 200rpm rotating speeds, obtains ptfe micropowder premix.
(2) polyimides powder (GE Ultem1000) 47kg is weighed, ptfe micropowder made from step (1) is premixed
Expect 3kg, mixed under 25 DEG C, 200rpm rotating speeds after 0.5h, be respectively 270 in mixing section, hot melt section, compression section and die head temperature
DEG C, 340 DEG C, 320 DEG C, extruded through double screw extruder at 300 DEG C, comminutor granulating and forming obtains composition.
Comparative example 3
(1) tetrafluoroethene and hexafluoropropylene copolymer micro mist 46kg of 2 μm of average grain diameter, silane coupler are weighed
KH5602kg, methyl methacrylate/acrylic acid ester copolymer 2kg, 1h is mixed under 25 DEG C, 200rpm rotating speeds, obtains poly- four
PVF micro mist premix.
(2) polyimides powder (GE Ultem1000) 40kg is weighed, ptfe micropowder made from step (1) is premixed
Expect 10kg, mixed under 25 DEG C, 200rpm rotating speeds after 1h, be respectively 280 in mixing section, hot melt section, compression section and die head temperature
DEG C, 340 DEG C, 320 DEG C, extruded through double screw extruder at 300 DEG C, comminutor granulating and forming obtains composition.
Performance test methods
Frictional behaviour is determined with MPX-2000 types friction wear testing machine by GB3960-83, and specific data see the table below.
Composition frictional behaviour data made from embodiment 1~10 and comparative example 1~3
| Performance | Coefficient of friction | Frictional dissipation rate (× 10-6mm3/N.m) |
| Embodiment 1 | 0.12 | 3 |
| Embodiment 2 | 0.09 | 2.5 |
| Embodiment 3 | 0.22 | 7.8 |
| Embodiment 4 | 0.31 | 6 |
| Embodiment 5 | 0.35 | 7 |
| Embodiment 6 | 0.1 | 2.2 |
| Embodiment 7 | 0.1 | 2.7 |
| Embodiment 8 | 0.21 | 7.1 |
| Embodiment 9 | 0.33 | 7.7 |
| Embodiment 10 | 0.33 | 5 |
| Comparative example 1 | 0.53 | 10 |
| Comparative example 2 | 0.51 | 14.5 |
| Comparative example 3 | 0.53 | 11.5 |
Claims (1)
1. the preparation method of a kind of wear-resisting polyimides and fluoro-containing copolymer composition, comprises the following steps：
(a) by weight, by 90~98.9 parts of fluoropolymer micro mist, 1~5 part of metal hydroxides, processing aid 0.1~
5 parts, at 15~25 DEG C, 0.5~1h is mixed under 100~300rpm, fluoropolymer micro mist premix is obtained；
(b) by weight, by 80~98 parts of polyimides powder, the fluoropolymer micro mist premix 2 that step (a) is obtained~
20 parts, at 15~25 DEG C, mixed under 100~300rpm after 0.5~1h, extruded through double screw extruder, granulating and forming, obtain resistance to
Grind polyimides and fluoro-containing copolymer composition；
It is characterized in that described fluoropolymer micro mist is the proplast micro mist of 2 μm~15 μm of average grain diameter, four
PVF and one kind in chlorotrifluoroethylene micro mist, tetrafluoroethene and hexafluoropropylene copolymer micro mist；Described metal
Hydroxide is Ca (OH)2、Mg(OH)2Or Mg (OH)2With Zn (OH)2Mixture；Described processing aid is methacrylic acid
One kind in methyl esters/acrylate copolymer, methyl methacrylate/styrol copolymer, acrylonitrile/styrol copolymer；
The mixing section temperature of described double screw extruder is 250~280 DEG C, and hot melt section temperature is 330~350 DEG C, compression section temperature
For 310~330 DEG C, die head temperature is 300~320 DEG C.
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| US4433104A (en) * | 1982-03-18 | 1984-02-21 | General Electric Company | Polyetherimide-fluorinated polyolefin blends |
| JPH083041B2 (en) * | 1986-06-30 | 1996-01-17 | 三井東圧化学株式会社 | Polyimide resin composition |
| CN1186827A (en) * | 1996-12-24 | 1998-07-08 | 中国科学院兰州化学物理研究所 | Polyimide self lubricating composite material |
| CN1324789A (en) * | 2001-06-26 | 2001-12-05 | 中国科学院长春应用化学研究所 | Polyimide hydrolyzing recovery process |
| CN1256387C (en) * | 2001-07-26 | 2006-05-17 | 索尔维先进聚合物有限责任公司 | Improved polyamide-imide molding resins and methods for their preparation |
| KR20060113979A (en) * | 2003-12-30 | 2006-11-03 | 제너럴 일렉트릭 캄파니 | Polymer compositions, method of manufacture, and articles formed therefrom |
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