CH707572B1 - Binder, useful in injection molding composition, which is useful for making metal/ceramic part for watch industry, comprises polymeric base containing copolymers of ethylene and methacrylic/acrylic acid, wax mixture and surfactant - Google Patents

Binder, useful in injection molding composition, which is useful for making metal/ceramic part for watch industry, comprises polymeric base containing copolymers of ethylene and methacrylic/acrylic acid, wax mixture and surfactant Download PDF

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Publication number
CH707572B1
CH707572B1 CH01258/13A CH12582013A CH707572B1 CH 707572 B1 CH707572 B1 CH 707572B1 CH 01258/13 A CH01258/13 A CH 01258/13A CH 12582013 A CH12582013 A CH 12582013A CH 707572 B1 CH707572 B1 CH 707572B1
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binder
ethylene
mixture
powder
copolymers
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CH01258/13A
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French (fr)
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Damien Cartier
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Comadur Sa
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    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
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    • B22F1/0059Metallic powders mixed with a lubricating or binding agent or organic material
    • B22F1/0077Mixtures obtained by warm mixing
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER
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    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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Abstract

Binder comprises 35-54 vol.% of a polymeric base, 40-55 vol.% of a wax mixture, and 10 vol.% of a surfactant. The polymeric base contains copolymers of ethylene and methacrylic or acrylic acid, copolymers of ethylene and vinyl acetate, or copolymers of ethylene comprising maleic anhydride or mixture of these copolymers, as well as polyethylene, polypropylene and acrylic resin. An independent claim is included for an injection molding composition, preferably feedstock, comprising 76-96 wt.% of an inorganic powder, and 4-24 wt.% of the binder.

Description

The invention relates to a binder composition for injection molding and an injection molding composition (feedstock) for the manufacture of metal or ceramic shaped parts.

In the manufacture of hard materials for jewelery and the watch industry, or for technical applications such as medical, electronics, telephony, tooling, cutting cutting inserts, the In the consumer goods industry, particularly with regard to hard materials generally referred to generically as inorganic "ceramics", powder metallurgy techniques are used. The term "ceramic" will be referred to herein as the inorganic synthesis material obtained, whatever the nature of this material, sapphire, ruby, artificial diamond, sapphire crystal, ceramic, micro-magnet, metal, alloy, or other.

The basic raw materials are of different types, in general, and comprise at least on the one hand ceramic powder and on the other hand organic binders, such as resins or plastics or the like that allow the injection and good performance of the component made with the mixture of all the raw materials. Other additives may be incorporated into the mixture. These raw materials can also be of different textures: solid, powdery, liquid, or pasty. The mixture can furthermore change its structure during its preparation, in particular, and without limitation, when complementary components of a resin undergo a polymerization reaction.

The overall process for manufacturing an inorganic ceramic component comprises at least the following steps: preparation of raw materials; mixture (s) of raw materials, or / and premix two to two (or more) if necessary; homogenization; granulation; pressing, especially in a molding chamber, a quantity of powder or granules feedstock resulting from mixing and granulation, for producing a component blank. This pressing can be carried out by injection, under pressure, in particular in a screw injector comprising means for heating this quantity of powder or feedstock granules resulting from kneading and granulation; quenching debinding for the combustion and / or dissolution of certain components of the mixture; heat treatment of the blank at the debinding end, for the sintering giving its final coherence to the finished component. This heat treatment causes a dimensional shrinkage, which makes it possible to obtain a component in finished dimensions; appearance finishing treatment of the component.

The invention is more particularly to provide a binder for optimized injection molding composition facilitating mixing in metallurgy powders for obtaining ceramics or metals, so as to obtain a very reproducible quality of production, with a controlled withdrawal coefficient.

Already known, for example US Pat. No. 5,145,900, thermoplastic materials (feedstock) for the manufacture of ceramic moldings which contain a sinterable inorganic powder and a polymeric organic binder, the latter consisting essentially of a mixture of polyoxymethylene and copolymers of polyoxymethylene and polyoxolanes.

These feedstocks have however revealed numerous drawbacks, such as insufficient fluidity in injection molding, and resistance problems of shaped mold parts that have cracks and lamination, especially when the shape of the parts is complex. ; they are also responsible for environmental problems due to the need to use aggressive products, such as nitric acid, especially for the final elimination of the organic phase. In addition, the use of water in this process of removing the organic binder is problematic in the case where the feedstocks contain metal materials that are likely to be oxidized.

Accordingly, the object of the present invention is to provide a binder for molding composition which obviates the aforementioned drawbacks, and more particularly which aims to improve the homogeneity and fluidity of the feedstock to allow the manufacture of metal parts or ceramics of more complex shapes, to reduce the cycle time in production, to increase the mechanical strength of the green and loosening bodies to the constraints of production (handling and various operations of recovery), and finally which removes the need to use products environmentally friendly for removal of the organic binder, replacing them with non-polluting solvents that can be removed by simple heat treatment.

For this purpose, the subject of the invention is a binder for an injection molding composition comprising: From 35 to 54% vol. a polymeric base, 40 to 55% vol. a mixture of waxes, - and about 10% vol. a surfactant, wherein the polymeric base contains copolymers of ethylene and methacrylic or acrylic acid, or copolymers of ethylene and vinyl acetate, or copolymers of ethylene comprising a maleic anhydride or a mixture of these copolymers, as well as only polyethylene, polypropylene and acrylic resin.

Preferably, the binder of the invention comprises from 2 to 7% by volume. of one of said copolymers or mixtures thereof, about 25% vol. of polyethylene, from 2 to 15% vol. polypropylene and 6 to 15 vol. of acrylic resin.

According to a preferred embodiment, the copolymer of ethylene and methacrylic acid or acrylic contains from 3 to 10% by weight. of methacrylic or acrylic comonomer, the copolymer of ethylene and vinyl acetate contains from 7 to 18 wt%. of vinyl acetate comonomer, and the ethylene-anhydride copolymer is a random (random) copolymer of ethylene and maleic anhydride having a melting point of 100 to 110 ° C or a copolymer of polyethylene HD and a modified anhydride having a melting point of 130 to 134 ° C.

Preferably, the acrylic resin has a molecular weight of between 50,000 and 220,000 and a viscosity of 0.21 to 0.83, and is selected from the group consisting of isobutyl methacrylate, methyl methacrylate and methacrylate polymers. ethyl and N-butyl, and methacrylate copolymers of isobutyl and N-butyl and methacrylates of methyl and N-butyl or a mixture of these polymers and / or copolymers.

Advantageously, the wax is a carnauba wax or a paraffin wax, or a palm oil, or a mixture of these elements.

According to another preferred feature, the surfactant is a NN-ethylene-bis (stearamide) or a mixture of stearic and palmitic acids (stearin), or a mixture of these elements.

The invention also relates to an injection molding composition (feedstock) for the manufacture of metal or ceramic shaped parts comprising 76 to 96 wt%. inorganic powder and 4 to 24 wt%. binder comprising: From 35 to 54% vol. a polymeric base, 40 to 55% vol. a mixture of waxes, - and about 10% vol. a surfactant, wherein the polymeric base contains copolymers of ethylene and methacrylic or acrylic acid, or copolymers of ethylene and vinyl acetate, or copolymers of ethylene comprising a maleic anhydride or a mixture of these copolymers, as well as only polyethylene, polypropylene and acrylic resin.

According to one particular characteristic, the inorganic powder of the injection molding composition may be chosen from the group consisting of an oxide, nitride, carbide or metal powder, or a mixture of these said powders and of the inorganic powder is preferably chosen from the group comprising an alumina powder, a zirconium oxide powder, a chromium carbide powder, a titanium carbide powder or a tungsten carbide powder, a tungsten powder, metal or silicon nitride, a stainless steel powder, a titanium metal powder or a mixture of these powders.

According to preferred embodiments of the injection molding composition, the latter contains, in% by weight: <tb> • <SEP> 76 to 88% of alumina and 12 to 24% of binder according to the invention as defined above, or <tb> • <SEP> 76 to 88% alumina and 0.1 to 0.6% magnesium oxide and 12 to 24% binder of the invention, or <tb> • <SEP> 58 to 86.5% zirconium oxide and 3.9 to 4.6% yttrium oxide and 0.18 to 18.5% alumina and 9 to 22% binder of the invention, or <tb> • <SEP> 61.5 to 84% of zirconium oxide and 3.9 to 4.6% of yttrium oxide and 0.2 to 9% of alumina and 2 to 5.5% of inorganic pigments from a list comprising iron oxide, cobalt oxide, chromium oxide, titanium oxide, manganese oxide, zinc oxide or a mixture of said oxides and at 22% of binder of the invention, or <tb> • <SEP> of 88 to 91% of chromium or titanium carbide, and 9 to 12% of the binder of the invention, or <tb> • <SEP> from 93 to 96% of tungsten carbide or metal tungsten and from 4 to 7% of the binder of the invention, or <tb> • <SEP> 78 to 85% silicon nitride and 15 to 22% binder of the invention.

The present invention will now be illustrated in more detail by the following non-limiting examples.

Example 1

The polymeric portion of the binder is mixed with a black zirconium oxide powder (St. Gobain Zir Black type) at a temperature of about 150 ° C to form a premix. To this premix are added the waxes and the surfactant, and the temperature is again increased to about 180 ° C to form a kind of homogeneous paste, which is then cooled and granulated until solidification, and then kept to form the feedstock can be used in the manufacture of a piece of injection molding according to a known technique.

In this example, 17.2 kg of the zirconia powder (86% by weight) and 2.8 kg of the binder (approximately 14% by weight) having the following volume composition: 24% polyethylene HD 10% polypropylene 4% copolymer of ethylene and methacrylic acid (6.5% by weight of methacrylic acid, for example of the "Nucrel (TM)" type from DuPont) 10% of an isobutyl methacrylate polymer resin having a molecular weight of 195,000 (for example of the "Elvacite (TM) 2045" type from Lucite International) 1% of a copolymer resin of isobutyl methacrylate and N-butyl having a molecular weight of 165,000 (for example of the type "Elvacite (TM) 2046" from Lucite International) 11% Carnauba wax 31% of a paraffin wax (for example of the type "Carisma 54 T (TM)" of Alpha Wax BV) 6% N, N-ethylene bis-stearamide 3% of a mixture of stearic and palmitic acids (for example of the Stearin Dubois type).

Example 2

The same type of feedstock as in Example 1 above is prepared by replacing the black zirconium oxide with white zirconium oxide, and using slightly different values of the various components of the binder, more particularly: 26% polyethylene HD 10% polypropylene 4% copolymer of ethylene and methacrylic acid 11% of the resin "Elvacite 2045" 1% of resin "Elvacite 2046" 11% Carnauba wax 29% of paraffin wax 8% of the bis-stearamide of N, N-ethylene

Example 3

Still with the same components of the organic binder, with slightly different volume proportions, other feedstocks can be prepared with various ceramic or metal powders, more particularly alumina, with removal index of 1.19 or 1 , (Translucent), chromium carbide or titanium carbide, tungsten carbide (of different grades) and metallic tungsten, according to the following Table.

[0023] <img class = "EMIRef" id = "319275196-ib0002" />

Claims (10)

  1. A binder for an injection molding composition comprising: From 35 to 54% vol. a polymeric base, 40 to 55% vol. a mixture of waxes, - and about 10% vol. a surfactant, wherein the polymeric base contains copolymers of ethylene and methacrylic or acrylic acid, or copolymers of ethylene and vinyl acetate, or copolymers of ethylene comprising a maleic anhydride or a mixture of these copolymers, as well as only polyethylene, polypropylene and acrylic resin.
  2. 2. Binder according to claim 1 comprising from 2 to 7% vol. of one of said copolymers or mixtures thereof, about 25% vol. of polyethylene, from 2 to 15% vol. polypropylene and 6 to 15 vol. of acrylic resin.
  3. A binder according to claim 1 or claim 2 wherein the copolymer of ethylene and methacrylic or acrylic acid contains from 3 to 10 wt%. of methacrylic or acrylic comonomer, the copolymer of ethylene and vinyl acetate contains from 7 to 18 wt%. of vinyl acetate comonomer, and the ethylene-anhydride copolymer is a random, random copolymer of ethylene and maleic anhydride having a melting point of 100 to 110 ° C or a copolymer of polyethylene HD and a modified anhydride having a melting point of 130 to 134 ° C.
  4. 4. Binder according to one of the preceding claims, wherein the acrylic resin has a molecular weight between 50 000 and 220 000 and a viscosity of 0.21 to 0.83, and is selected from isobutyl methacrylate polymers, methyl, ethyl and N-butyl, and methacrylate copolymers of isobutyl and N-butyl and methyl and N-butyl methacrylates or a mixture of these polymers and / or copolymers.
  5. Binder according to one of the preceding claims, wherein the wax mixture comprises a carnauba wax or a paraffin wax or a palm oil or a mixture of these elements.
  6. Binder according to one of the preceding claims, wherein the surfactant is an NN-ethylene-bis (stearamide), or a mixture of stearic and palmitic acids, stearin, or a mixture of these elements.
  7. 7. Injection molding composition, feedstock, for the manufacture of metal or ceramic shaped parts comprising 76 to 96 wt%. inorganic powder and 4 to 24 wt%. binder according to one of claims 1 to 6.
  8. The molding composition of claim 7, wherein the inorganic powder is selected from the group consisting of oxide, nitride, carbide, metal powder, or a mixture thereof.
  9. The molding composition of claim 8, wherein the inorganic powder is selected from the group consisting of alumina powder, zirconium oxide powder, chromium carbide powder, titanium carbide powder, or a tungsten carbide powder, a metal tungsten powder or a silicon nitride powder, a stainless steel powder, a titanium metal powder, or a mixture of these powders.
  10. 10. Molding composition according to claim 8 or 9, which contains in% by weight: - 76 to 88% of alumina and 12 to 24% of binder, Or 76 to 88% of alumina and 0.1 to 0.6% of magnesium oxide and 12 to 24% of binder, Or 58 to 86.5% of zirconium oxide and 3.9 to 4.6% of yttrium oxide and 0.18 to 18.5% of alumina and 9 to 22% of binder, Either 61.5 to 84% of zirconium oxide and 3.9 to 4.6% of yttrium oxide and 0.2 to 9% of alumina and 2 to 5.5% of inorganic pigments from a list comprising iron oxide, cobalt oxide, chromium oxide, titanium oxide, manganese oxide, zinc oxide or a mixture of said oxides and 9 to 22% of binder , From 88 to 91% of chromium or titanium carbide and from 9 to 12% of binder, From 93 to 96% of tungsten carbide or of metallic tungsten and from 4 to 7% of binder, Or 78 to 85% of silicon nitride and 15 to 22% of binder.
CH01258/13A 2013-07-15 2013-07-15 Binder, useful in injection molding composition, which is useful for making metal/ceramic part for watch industry, comprises polymeric base containing copolymers of ethylene and methacrylic/acrylic acid, wax mixture and surfactant CH707572B1 (en)

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CH01258/13A CH707572B1 (en) 2013-07-15 2013-07-15 Binder, useful in injection molding composition, which is useful for making metal/ceramic part for watch industry, comprises polymeric base containing copolymers of ethylene and methacrylic/acrylic acid, wax mixture and surfactant

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3332897A1 (en) 2016-12-08 2018-06-13 The Swatch Group Research and Development Ltd Binder for injection-moulding composition
EP3563950A1 (en) * 2018-05-04 2019-11-06 Comadur S.A. Binder for injection-moulding composition

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3332897A1 (en) 2016-12-08 2018-06-13 The Swatch Group Research and Development Ltd Binder for injection-moulding composition
EP3563950A1 (en) * 2018-05-04 2019-11-06 Comadur S.A. Binder for injection-moulding composition

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