US20040164442A1 - Method of producing a multilayer body by coalescence and the multi-layer body produced - Google Patents

Method of producing a multilayer body by coalescence and the multi-layer body produced Download PDF

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Publication number
US20040164442A1
US20040164442A1 US10/343,083 US34308303A US2004164442A1 US 20040164442 A1 US20040164442 A1 US 20040164442A1 US 34308303 A US34308303 A US 34308303A US 2004164442 A1 US2004164442 A1 US 2004164442A1
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compacting
mould
powder
energy
stroke
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Kent Olsson
Jianguo Li
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Individual
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/006—Pressing and sintering powders, granules or fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B29C43/14—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles in several steps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
    • A61L27/44—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having a macromolecular matrix
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B29C43/14—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles in several steps
    • B29C43/146—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles in several steps for making multilayered articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
    • B29C43/16—Forging
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2023/00—Use of polyalkenes or derivatives thereof as moulding material
    • B29K2023/04—Polymers of ethylene
    • B29K2023/06—PE, i.e. polyethylene
    • B29K2023/0658—PE, i.e. polyethylene characterised by its molecular weight
    • B29K2023/0683—UHMWPE, i.e. ultra high molecular weight polyethylene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
    • B29K2033/04—Polymers of esters
    • B29K2033/12—Polymers of methacrylic acid esters, e.g. PMMA, i.e. polymethylmethacrylate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
    • B29K2033/18—Polymers of nitriles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/25—Solid
    • B29K2105/251—Particles, powder or granules
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/753—Medical equipment; Accessories therefor
    • B29L2031/7532—Artificial members, protheses

Definitions

  • the invention concerns a method of producing a multilayer body by coalescence as well as the multilayer body produced by this method.
  • WO-A1-9700751 an impact machine and a method of cutting rods with the machine is described.
  • the document also describes a method of deforming a metal body.
  • the method utilises the machine described in the document and is characterised in that a metallic material either in solid form or in the form of powder such as grains, pellets and the like, is fixed preferably at the end of a mould, holder or the like and that the material is subjected to adiabatic coalescence by a striking unit such as an impact ram, the motion of the ram being effected by a liquid.
  • a striking unit such as an impact ram
  • WO-A1-9700751 shaping of components, such as spheres, is described.
  • a metal powder is supplied to a tool divided in two parts, and the powder is supplied through a connecting tube.
  • the metal powder has preferably been gas-atomized.
  • a rod passing through the connecting tube is subjected to impact from the percussion machine in order to influence the material enclosed in the spherical mould.
  • specifing parameters for how a body is produced according to this method is not shown in any embodiment specifing parameters for how a body is produced according to this method.
  • the compacting according to this document is performed in several steps, e.g. three. These steps are performed very quickly and the three strokes are performed as described below.
  • Stroke 1 an extremely light stroke, which forces out most of the air from the powder and orients the powder particles to ensure that there are no great irregularities.
  • Stroke 2 a stroke with very high energy density and high impact velocity, for local adiabatic coalescence of the powder particles so that they are compressed against each other to extremely high density.
  • the local temperature increase of each particle is dependent on the degree of deformation during the stroke.
  • Stroke 3 a stroke with medium-high energy and with high contact energy for final shaping of the substantially compact material body.
  • the compacted body can thereafter be sintered.
  • SE 9803956-3 a method and a device for deformation of a material body are described. This is substantially a development of the invention described in WO-A1-9700751.
  • the striking unit is brought to the material by such a velocity that at least one rebounding blow of the striking unit is generated, wherein the rebounding blow is counteracted whereby at least one further stroke of the striking unit is generated.
  • the object of the present invention is to achieve a process for efficient production of multilayer products at a low cost.
  • These products may be both medical devices such as medical implants or bone cement in orthopaedic surgery, instruments or diagnostic equipment, or non medical devices such as tools, insulator applications, crucibles, spray nozzles, tubes, cutting edges, jointing rings, ball bearings and engine parts.
  • Another object is to achieve a multilayer product of the described type.
  • multilayer is used here to define a product composed of different parts integrally joined to each other. These parts may be in the form of flat layers or have any other suitable form provided that the form of the different parts fit closely together. One part may have a convex surface fitting around a concave surface on another part. Examples of different multilayer products are shown in FIGS. 2 a - 2 f .
  • the different parts may be made of the same type of material or of different types of material. It is possible to combine a ceramic material with a layer of a polymeric material. It is also possible to have a multilayer product with layers or parts of different polymers.
  • the material to be compressed is for example in the form of powder, pellets, grains and the like and is filled in a mould, pre-compacted and compressed by at least one stroke.
  • the machine to use in the method may be the one described in WO-A1-9700751 and SE 9803956-3.
  • the method according to the invention utilises hydraulics in the percussion machine, which may be the machine utilised in WO-A1-9700751 and SE 9803956-3.
  • the striking unit can be given such movement that, upon impact with the material to be compressed, it emits sufficient energy at sufficient speed for coalescence to be achieved. This coalescence may be adiabatic.
  • a stroke is carried out quickly and for some materials the wave in the material decay in between 5 and 15 milliseconds.
  • the hydraulic use also gives a better sequence control and lower running costs compared to the use of compressed air.
  • a spring-actuated percussion machine will be more complicated to use and will give rise to long setting times and poor flexibility when integrating it with other machines.
  • the method according to the invention will thus be less expensive and easier to carry out.
  • the optimal machine has a large press for pre-compacting and post-compacting and a small striking unit with high speed. Machines according to such a construction are therefore probably more interesting to use. Different machines could also be used, one for the pre-compacting and post-compacting and one for the compression.
  • FIG. 1 shows a cross sectional view of a device for deformation of a material in the form of a powder, pellets, grains and the like
  • FIGS. 2 a - 2 f shows the forming of different types of multilayer products
  • FIGS. 3 - 4 are diagrams showing results obtained in the embodiments described in the examples.
  • the invention concerns a method of producing a multilayer body by coalescence, wherein the method comprises the steps of
  • the pre-compacting mould may be the same as the compression mould, which means that the material does not have to be moved between the step b) and c). It is also possible to use different moulds and move the material between the steps b) and c) from the pre-compacting mould to the compression mould. This could only be done if a body is formed of the material in the pre-compacting step.
  • the first material is only pre-compacted before the insertion of the second material. Thereafter, a second pre-compaction is performed and the multilayer material is struck with at least one stroke to achieve coalescence and form an integral product. It is also possible to insert the further material or materials in powder form before the pre-compaction or the first or start material. All materials will be compacted and struck together in this case.
  • the first and second materials are inserted in powder form beside each other or as layers above each other, whereafter pre-compaction and striking are performed.
  • the first material is pre-compacted and struck to make a coalescent element, whereafter this element is placed in a second mould on top of a powder of the second material or surrounded by the second material.
  • the first element together with the second material are pre-compacted and struck with a coalescing stroke.
  • any step described may refer to a process performed on one layer or element of the multilayer product or on several layers or elements together.
  • the device in FIG. 1 comprises a striking unit 2 .
  • the material in FIG. 1 is in the form of powder, pellets, grains or the like.
  • the device is arranged with a striking unit 3 , which with a powerful impact may achieve an immediate and relatively large deformation of the material body 1 .
  • the invention also refers to compression of a body, which will be described below. In such a case, a solid body 1 , such as a solid homogeneous multilayer body, would be placed in a mould.
  • the striking unit 2 is so arranged, that, under influence of the gravitation force, which acts thereon, it accelerates against the material 1 .
  • the mass m of the striking unit 2 is preferably essentially larger than the mass of the material 1 .
  • the striking unit 2 is allowed to hit the material 1 , and the striking unit 2 emits enough kinetic energy to compress and form the body when striking the material in the compression mould. This causes a local coalescence and thereby a consequent deformation of the material 1 is achieved.
  • the deformation of the material 1 is plastic and consequently permanent. Waves or vibrations are generated in the material 1 in the direction of the impact direction of the striking unit 2 .
  • the pre-compaction is a very important step. This is done in order to drive out air and orient the particles in the material.
  • the pre-compaction step is much slower than the compression step, and therefore it is easier to drive out the air.
  • the compression step which is done very quickly, may not have the same possibility to drive out air. In such case, the air may be enclosed in the produced body, which is a disadvantage.
  • the pre-compaction is performed at a minimum pressure enough to obtain a maximum degree of packing of the particles which results in a maximum contact surface between the particles. This is material dependent and depends on the softness and melting point of the material.
  • the pre-compacting step in the Examples has been performed by compacting with an axial load of about 117680 N. This is done in the pre-compacting mould or the final mould. According to the examples in this description, this has been done in a cylindrical mould, which is a part of the tool, and has a circular cross section with a diameter of 30 mm, and the area of this cross section is about 7 cm 2 . This means that a pressure of about 1.7 ⁇ 10 8 N/m 2 has been used.
  • the material may be pre-compacted with a pressure of at least about 0.25 ⁇ 10 8 N/m 2 , and preferably with a pressure of at least about 0.6 ⁇ 10 8 N/m 2 .
  • the necessary or preferred pre-compaction pressure to be used is material dependent and for a softer multilayer it could be enough to compact at a pressure of about 0.2 ⁇ 10 8 N/m 2 .
  • Other possible values are 1.0 ⁇ 10 8 N/m 2 , 1.5 ⁇ 10 8 N/m 2 .
  • the studies made in this application are made in air and at room temperature. All values obtained in the studies are thus achieved in air and room temperature. It may be possible to use lower pressures if vacuum or heated material is used.
  • the height of the cylinder is 60 mm.
  • a striking area In the claims is referred to a striking area and this area is the area of the circular cross section of the striking unit which acts on the material in the mould.
  • the striking area in this case is the cross section area.
  • the invention further comprises a method of producing a multilayer body by coalescence, wherein the method comprises compressing a solid body of a first or start material (i.e. a body where the target density for specific applications has been achieved) together with at least one further material in the form of powder or in the form of a solid body in a compression mould by at least one stroke, where a striking unit emits enough energy to cause coalescence of the material in the body. Slip planes are activated during a large local temperature increase in the material, whereby the deformation is achieved.
  • the method also comprises deforming the body.
  • the pressing step is very much like cold and hot pressing. The intention is to get a green body from powder. It has turned out to be most beneficial to perform two compactions of the powder. One compaction alone gives about 2-3% lower density than two consecutive compactions of the powder.
  • This step is the preparation of the powder by evacuation of the air and orientation of the powder particles in a beneficial way. The density values of the green body is more or less the same as for normal cold and hot pressuring.
  • the impact step is the actual high-speed step, where a striking unit strikes the powder with a defined area. A material wave starts off in the powder and interparticular melting takes place between the powder particles. Velocity of the striking unit seems to have an important role only during a very short time initially. The mass of the powder and the properties of the material decides the extent of the interparticular melting taking place.
  • the energy retention step aims at keeping the delivered energy inside the solid body produced. It is physically a compaction with at least the same pressure as the pre-compaction of the powder. The result is an increase of the density of the produced body by about 1-2%. It is performed by letting the striking unit stay in place on the solid body after the impact and press with at least the same pressure as at pre-compaction, or release after the impact step. The idea is that more transformations of the powder will take place in the produced body.
  • the compression strokes emit a total energy corresponding to at least 100 Nm in a cylindrical tool having a striking area of 7 cm 2 in air and at room temperature.
  • Other total energy levels may be at least 300, 600, 1000, 1500, 2000, 2500, 3000 and 3500 Nm. Energy levels of at least 10 000, 20 000 Nm may also be used.
  • the energy levels depend on the material used, and in which application the body produced will be used. Different energy levels for one material will give different relative densities of the material body. The higher energy level, the more dense material will be obtained. Different materials will need different energy levels to get the same density. This depends on for example the hardness of the material and the melting point of the material.
  • the compression strokes emit an energy per mass corresponding to at least 5 Nm/g in a cylindrical tool having a striking area of 7 cm 2 in air and at room temperature.
  • Other energies per mass may be at least 20 Nm/g, 50 Nm/g, 100 Nm/g, 150 Nm/g, 200 Nm/g, 250 Nm/g, 350 Nm/g and 450 Nm/g.
  • the energy level needs to be amended and adapted to the form and construction of the mould. If for example, the mould is spherical, another energy level will be needed. A person skilled in the art will be able to test what energy level is needed with a special form, with the help and direction of the values given above.
  • the energy level depends on what the body will be used for, i.e. which relative density is desired, the geometry of the mould and the properties of the material.
  • the striking unit must emit enough kinetic energy to form a body when striking the material inserted in the compression mould. With a higher velocity of the stroke, more vibrations, increased friction between particles,. increased local heat, and increased interparticular melting of the material will be achieved. The bigger the stroke area is, the more vibrations are achieved. There is a limit where more energy will be delivered to the tool than to the material. Therefore, there is also an optimum for the height of the material.
  • the porosity of the material and the surface is also affected by the method. If a porous surface or body is desired, the material should not be compressed as much as if a less porous surface or body is desired.
  • the individual strokes affect material orientation, driving out air, pre-moulding, coalescence, tool filling and final calibration. It has been noted that the back and forth going waves travels essentially in the stroke direction of the striking unit, i. e. from the surface of the material body which is hit by the striking unit to the surface which is placed against the bottom of the mould and then back.
  • a solid body is a body where the target density for specific applications has been achieved.
  • the striking unit preferably has a velocity of at least 0.1 m/s or at least 1.5 m/s during the stroke in order to give the impact the required energy level. Much lower velocities may be used than according to the technique in the prior art. The velocity depends on the weight of the striking unit and what energy is desired. The total energy level in the compression step is at least about 100 to 4000 Nm. But much higher energy levels may be used. By total energy is meant the energy level for all strokes added together.
  • the striking unit makes at least one stroke or a number of consecutive strokes. The interval between the strokes according to the Examples was 0.4 and 0.8 seconds. For example at least two strikes may be used. According to the Examples one stroke has shown promising results. These Examples were performed in air and at room temperature. If for example vacuum and heat or some other improving treating is used, perhaps even lower energies may be used to obtain good relative densities.
  • the multilayer product may be compressed to a relative density of 60%, preferably 65%. More preferred relative densities are also 70% and 75%. Other preferred densities are 80 and 85%. Densities of at least 90 and up to 100% are especially preferred. However, other relative densities are also possible. If a green body is to be produced, it may be enough with a relative density of about 40-60%. Load bearing implants need a relative density of 90 to 100% and in some biomaterials it is good with some porosity. If a porosity of at most 5% is obtained and this is sufficient for the use, no further post-processing is necessary. This may be the choice for certain applications. If a relative density of less than 95% is obtained, and this is not enough, the process need to continue with further processing such as sintering. Several manufacturing steps have even in this case been cut compared to conventional manufacturing methods.
  • the method also comprises pre-compacting the material at least twice. It has been shown that this could be advantageous in order to get a high relative density compared to strokes used with the same total energy and only one pre-compacting.
  • Two compactions may give about 1-5% higher density than one compacting depending on the material used. The increase may be even higher for some materials.
  • pre-compacting twice the compacting steps are performed with a small interval between, such as about 5 seconds. About the same pressure may be used in the second pre-compacting.
  • the method may also comprise a step of compacting the material at least once after the compression step. This has also been shown to give very good results.
  • the post-compacting should be carried out at at least the same pressure as the pre-compacting pressure, i.e. 0,25 ⁇ 10 8 N/m 2 . Other possible values are 1.0 ⁇ 10 8 N/m 2 .
  • Higher post-compacting pressures may also be desired, such as a pressure which is twice the pressure of the pre-compacting pressure.
  • the pre-compacting pressure should be at least about 0.25 ⁇ 10 8 N/m 2 and this would be the lowest possible post-compacting pressure for hydroxyapatite.
  • the pre-compacting value has to be tested out for every material.
  • a post-compacting effects the sample differently than a pre-compacting.
  • the transmitted energy which increases the local temperature between the powder particles from the stroke, is conserved for a longer time and can effect the sample to consolidate for a longer period after the stroke.
  • the energy is kept inside the solid body produced. Probably the “lifetime” for the material wave in the sample increases and it can affect the sample for a longer period and more particles can melt together.
  • the after compaction or post-compaction is performed by letting the striking unit stay in place on the solid body after the impact and press with at least the same pressure as at pre-compacting, i.e. at least about 0.25 ⁇ 10 8 N/m 2 hydroxyapatite. More transformations of the powder will take place in the produced body.
  • the powder could be pre-heated to e.g. ⁇ 200-300° C. or higher depending on what material type to pre-heat.
  • the powder could be pre-heated to a temperature which is close to the melting temperature of the material. Suitable ways of pre-heating may be used, such as normal heating of the powder in an oven.
  • vacuum or inert gas could be used. This would have the effect that air is not enclosed in the material to the same extent during the process.
  • the body may according to another embodiment of the invention be heated and/or sintered any time after compression or post-compacting.
  • a post-heating is used to relax the bindings in the material (obtained by increased binding strain).
  • a lower sintering temperature may be used owing to the fact that the compacted body has a higher density than compacts obtained by other types of powder compression. This is an advantage as a higher temperature may cause decomposition or transformation of the constituting material.
  • the produced body may also be post-processed in some other way, such as by HIP (Hot Isostatic Pressing).
  • the body produced may be a green body and the method may also comprise a further step of sintering the green body.
  • the green body of the invention gives a coherent integral body even without use of any additives.
  • the green body may be stored and handled and also worked, for instance polished or cut. It may also be possible to use the green body as a finished product, without any intervening sintering. This is the case when the body is a bone implant or replacement where the implant is to be resorbed in the bone.
  • the materials for the multilayer product could be homogenously mixed with additives. Predrying of the granulate could also be used to decrease the water content of the raw material. Some multilayers do not absorb humidity, while other multilayers easily absorb humidity which can disturb the processing of the material, and decrease the homogeneity of the worked material because a high humidity rate can raise steam bubbles in the material.
  • the multilayer materials may be chosen from the group comprising a metallic, polymeric or ceramic materials such as stainless steel, aluminium alloy, titanium, UHMWPE, PMMA, PEEK, rubber, alumina, zirconia, silicon carbide, hydroxyapatite or silicon nitride.
  • the multilayer may comprise a composite material containing reinforcements fibres or powders from the group comprising carbon, metals, glass or ceramics such as alumina, silica, silicon nitride, zirconia, silicon carbide.
  • the compression strokes need to emit a total energy corresponding to at least 100 Nm in a cylindrical tool having a striking area of 7 cm 2 for multilayer products or layers.
  • the compression strokes need to emit an energy per mass corresponding to at least 5 Nm/g in a cylindrical tool having a striking area of 7 cm 2 for multilayer products.
  • the first or second material may comprise a lubricant and/or a sintering aid.
  • a lubricant may be useful to mix with the material. Sometimes the material needs a lubricant in the mould, in order to easily remove the body. In certain cases this could be a choice if a lubricant is used in the material, since this also makes it easier to remove the body from the mould.
  • a lubricant cools, takes up space and lubricates the material particles. This is both negative and positive.
  • Interior lubrication is good, because the particles will then slip in place more easily and thereby compact the body to a higher degree. It is good for pure compaction. Interior lubrication decreases the friction between the particles, thereby emitting less energy, and the result is less inter-particular melting. It is not good for compression to achieve a high density, and the lubricant must be removed for example with sintering.
  • Exterior lubrication increases the amount of energy delivered to the material and thereby indirectly diminishes the load on the tool. The result is more vibrations in the material, increased energy and a greater degree of inter-particular melting. Less material sticks to the mould and the body is easier to extrude. It is good for both compaction and compression.
  • a lubricant is Acrawax C, but other conventional lubricants may be used. If the material will be used in a medical body, the lubricant need to be medically acceptable, or it should be removed in some way during the process.
  • Polishing and cleaning of the tool may be avoided if the tool is lubricated and if the powder is preheated.
  • a sintering aid may also be included in the material.
  • the sintering aid may be useful in a later processing step, such as a sintering step. However, the sintering aid is in some cases not so useful during the method embodiment, which does not include a sintering step.
  • the sintering aid may be yttrium oxide, alumina or magnesia or some other conventional sintering aid. It should, as the lubricant, also be medically acceptable or removed, if used in a medical body.
  • a lubricant in some cases, it may be useful to use both a lubricant and a sintering aid. This depends on the process used, the material used and the intended use of the body which is produced.
  • a lubricant in the mould in order to remove the body easily. It is also possible to use a coating in the mould.
  • the coating may be made of for example TiNAl or Balinit Hardlube. If the tool has an optimal coating no material will stick to the tool parts and consume part of the delivered energy, which increase the energy delivered to the powder. No time-consuming lubricating would be necessary in cases where it is difficult to remove the formed body.
  • a very dense material and depending on the material, a hard material will be achieved, when the multilayer material is produced by coalescence.
  • the surface of the material will be very smooth, which is important in several applications.
  • strokes may be executed continually or various intervals may be inserted between the strokes, thereby offering wide variation with regard to the strokes.
  • one to about six strokes may be used.
  • the energy level could be the same for all strokes, the energy could be increasing or decreasing.
  • Stroke series may start with at least two strokes with the same level and the last stroke has the double energy. The opposite could also be used.
  • the highest density is often obtained by delivering a total energy with one stroke. If the total energy instead is delivered by several strokes a lower relative density may be obtained, but the tool is saved. A multi-stroke can therefore be used for applications where a maximum relative density is not necessary.
  • the impulse, with which the striking unit hits the material body decreases for each stroke in a series of strokes.
  • the difference is large between the first and second stroke. It will also be easier to achieve a second stroke with smaller impulse than the first impulse during such a short period (preferably approximately 1 ms), for example by an effective reduction of the rebounding blow. It is however possible to apply a larger impulse than the first or preceding stroke, if required.
  • a multilayer body produced by the method of the invention may be used in medical devices such as medical implants or bone cement in orthopaedic surgery, instruments or diagnostic equipment.
  • medical implants may be for examples skeletal or tooth prostheses.
  • the material is medically acceptable.
  • Such materials are for example suitable multilayer products containing an element or layer of hydroxyapatite or zirconia.
  • a material to be used in implants needs to be biocompatible and haemocoinpatible as well as mechanically durable, such as hydroxyapatite and zirconia or other suitable multilayer materials.
  • the body produced by the process of the present invention may also be a non medical product such as cutting tools, insulator applications, crucibles, spray nozzles, tubes, cutting edges, jointing rings, ball bearings and engine parts.
  • Alumina is a good electrical insulator and has at the same time an acceptable thermal conductivity and is therefore used for producing substrates where electrical components are mounted, insulation for ignition plugs and insulation in the high-tension areas.
  • Alumina is also a common material type in orthopaedic implants, e.g. femoral-head in hip prostheses. Hydroxyapatite is one of the most important biomaterials extensively used in orthopaedic surgery.
  • zirconia is cutting tools, components for adiabatic engines and it is also a common material type in orthopaedic implants, e.g. femoral-head in hip prostheses.
  • the invention thus has a big application area for producing products according to the invention.
  • a hard, smooth and dense surface is achieved on the body formed. This is an important feature of the body.
  • a hard surface gives the body excellent mechanical properties such as high abrasion resistance and scratch resistance.
  • the smooth and dense surface makes the material resistant to for example corrosion.
  • a coating may also be manufactured according to the method of the invention.
  • a coating may for example be formed on a surface of an element or of a multilayer product.
  • the element When manufacturing a coated element, the element is placed in the mould and may be fixed therein in a conventional way.
  • the coating material is inserted in the mould around the element to be coated, by for example gas-atomizing, and thereafter the coating is formed by coalescence.
  • the element to be coated may be any material formed according to this application, or it may be any conventionally formed element. Such a coating may be very advantageous, since the coating can give the element specific properties.
  • a coating may also be applied on a body produced in accordance with the invention in a conventional way, such as by dip coating and spray coating.
  • the invention also concerns the product obtained by the methods described above.
  • the method according to the invention has several advantages compared to pressing.
  • Pressing methods comprise a first step of forming a green body from a powder containing sinterinc, aids. This green body will be sintered in a second step, wherein the sintering aids are burned out or may be burned out in a further step.
  • the pressing methods also require a final working of the body produced, since the surface need to be mechanically worked. According to the method of the invention, it is possible to produce the body in one step or two steps and no mechanical working of the surface of the body is needed.
  • a further advantage is that the method of the invention may be used on powder carrying a charge repelling the particles without treating the powder to neutralize the charge.
  • the process may be performed independent of the electrical charges or surface tensions of the powder particles. However, this does not exclude a possible use of a further powder or additive carrying an opposite charge.
  • By the use of the present method it is possible to control the surface tension of the body produced. In some instances a low surface tension may be desired, such as for a wearing surface requiring a liquid film, in other instances a high surface tension is desired.
  • Silicone nitride was a pure freeze granulated powder. Hydroxyapatite and alumina was not pre-processed at all. The metal and polymer powder was initially dry-mixed for 10 minutes to obtain a homogeneous particle size distribution in the powder.
  • a multilayer has many applications areas e.g. implants.
  • the weight specified in the test specification of each constituent of the multilayer was divided by the number of layers in the multilayer. This means that the impact energy to obtain a visibility index for the weight specified in the test specification also has to be divided by the number of layers. If a horizontal layer consisted of two vertical layers then the material with the lowest hardness has to be consider when choosing impact energies. A polymer was never processed like material 1 as a single horizontal layer.
  • the multilayer impact stroke will be performed with machine pre-compacting and the maximum allowable impact energy for material 2 and 3 respectively. Depending if the multilayer has two or three horizontal layers.
  • ⁇ multilayer m total /(m a / ⁇ a +m b / ⁇ b +m c /r d +m c / ⁇ d +.m c / ⁇ d )
  • Table 1 shows the different powders used in this study.
  • TABLE 1 Silicone Properties nitride Hydroxyapatite Alumina Co-28Cr-6Mo Titanium PMMA UHMWPE Particle size ⁇ 0.5 ⁇ 1 ⁇ 0.5 ⁇ 150 ⁇ 150 ⁇ 600 (micron) Particle — ⁇ 1 0.3-0.5 2% > 150 ⁇ 5% ⁇ 250 distribution balance ⁇ 150 5% 25-355 (micron) 10% 355-500 45% 500-710 35% ⁇ 710 Particle Cubic Irregular irregular Irregular Irregular Irregular morphology Powder Granulated Wet chemistry Grinding Water atomised Hydrided ex-reacted production precipitation Crystal structure 98% alfa Apatite alfa 85% alpha phase, HCP amorphous 2% beta 15% carbides (hexagonal) Theoretical 3.18 3.15 3.98 8.5 4.5 1.19 density (g/cm 3 ) Apparent density 0.38 0.6 0.5-0.8 3.4
  • FIG. 2 a shows the look of a two horizontal layer. The different material combinations used are specified in table 2.
  • Alumina and silicone nitride has not been successfully compressed as a single material and the same result was obtained in the multilayer compressing series.
  • the ceramic material felled apart and could not bind to the added material 2 .
  • Co-28Cr-6Mo has also been complicated to solidified as a single material. It was compressed together with PMMA and UHMWPE. Some solid samples were obtained with UHMWPE when Co-28Cr-6Mo was struck to a solid material body first. No fine samples for the Co-28Cr-6Mo/PMMA two-layer were obtained. TABLE 2 Number of Material 1 Material 2 samples Hydroxyapatite UHMWPE 2 Hydroxyapatite Titanium 6 Alumina UHMWPE 8 Titanium PMMA 7 Titanium UHMWPE 5 Co-28Cr-6Mo PMMA 8 Co-28Cr-6Mo UHMWPE 9 Silicone nitride Titanium 5 Silicone nitride UHMWPE 5
  • FIG. 2 b shows the look of a three horizontal layer. The different material combinations used are specified in table 3.
  • Table 3 shows the different material combinations tested in three horizontal layers. TABLE 3 Number of Material 1 Material 2 Material 3 samples Hydroxyapatite Titanium UHMWPE 28 Silicone nitride Titanium UHMWPE 28
  • FIG. 2 c shows the look of a multilayer with one horizontal layer and two vertical layers. The different material combinations used are specified in table 4.
  • FIG. 4 shows the look of a two horizontal layer. The different material combinations used are specified in table 5.
  • FIG. 2 e shows the look of a two horizontal layer. The different material combinations used are specified in table 6.
  • FIG. 2 f shows the look of a two horizontal layer.
  • the different material combinations used are specified in table 7.
  • the second layer containing two vertical layers was twisted 180 degrees to obtain a cross in the centre of the multilayer.
  • Hydroxyapatite obtained finest samples when it was compacted together with titanium by first only hand compact or pre-compact with the machine the first two vertical layers and then strike the two other vertical layers. No solid samples were obtained compressing hydroxyapatite compressed together with UHMWPE. The hydroxyapatite felled apart and the polymer did not phase change. TABLE 8 Number of Material 1 Material 2 samples Titanium UHMWPE 3 Titanium Hydroxyapatite 5 Hydroxyapatite UHMWPE 5
  • the ideal could be to strike one material and then add a thin layer of powder which only is pre-compacted and the add the third layer which is completely solidified. The material in the centre can then bind the two solid layers together.
  • Post-processing for a multilayer is complicated, because of the different material properties between the components.
  • a polymer can for example not be sintered and the sintering parameters between different metals or between a metal and a ceramic material are very different.
  • One solution could be to compress one layer and then remove the material and sinter the sample. After the sintering is the material placed in the tool and next sample or powder is added and compressed. This compressing process can also compress or deform solid samples which means that all layers in a multilayer could be compressed and sintered and then compressed to one solid material body.
  • the ss 316L powder was prepared by dry mixing for 10 minutes to obtain a homogeneous particle size distribution.
  • the rubber powder was not prepared partly due to that the particles would glue together and partly that the particle size was homogeneous.
  • Second sample a pre-compacting was performed and third sample a stroke at the lowest impact energy possible (150 Nm).
  • the last (fifth) sample was stricken by half the maximum impact energy of the earlier test with pure ss 316L.
  • the forth sample was stricken by an impact energy in between the impact energy of the third and the fifth sample.
  • Visibility index 1 corresponds to a powder sample
  • visibility index 2 corresponds to a brittle sample
  • visibility index 3 corresponds to a solid sample.
  • the theoretical density was taken from the manufacturers. Out of that a theoretical density has been calculated that corresponds to this certain mix between 50% rubber and 50% ss 316L.
  • the relative density is obtained by taking the obtained density for each sample divided by the theoretical density.
  • the dimensions of the manufactured sample in these tests is a disc with a diameter of ⁇ 30.0 mm and a height between 5-10 mm. The height depends on the obtained relative density. If a relative density of 100% should be obtained the thickness is 5.00 mm for ss 316L rubber. That is the reason to the half weight of each material type.
  • Powder properties are given in Table 9 and test results in Table 10. TABLE 9 Properties Rubber ss316L 1. Particle size (micron) ⁇ 496 ⁇ 2. Particle distribution 99.8 wt % ⁇ 1.0 mm 0.0% > 150 mic 42.7% ⁇ 115 mic 3. Particle morphology Irregular Irregular 4. Powder production Polymerised thereafter Water atom grinding to powder 5. Type of material Elastomer I 6. Theoretical density 0.99 7.90 gc 7. Apparent density — 2.64 gc 8. Melt temperature (° C.) Not applicable I 9. Sintering — 1315 temperature (° C.) 10. Hardness 40 shore A 160-190 HV
  • FIGS. 3 and 4 show relative density as a function of impact energy per mass and of total impact energy. The following described phenomena could be seen for all curves.
  • the two first samples where the first material type is either hand compacted or pre-compacted by the machine, render a higher relative density than the third sample, where the first material type is stricken with the lowest impact energy.
  • the impact energy of the first stroke increases the relative density increases and ends up at a higher relative density than the two first samples.
  • the maximum relative density, 98.4%, is obtained when the first stroke is struck with the highest impact energy.
  • ss 316L has a melting temperature of 1427° C. Even though it is quite high the ss 316L part of the samples got dense. The local increase of temperature among the particles, due to transmitted energy, makes the particles to soften, deform and the surface of the particles to melt. This inter-particular melting enables the particles to re-solidify together and dense material can be obtained.
  • the ss 316L powder is softer than e.g. CoCrMo.
  • the hardness of ss 316L is ⁇ 160-190 HV and CoCrMo ⁇ 460-830 HV.
  • the softer a material is the more soften and deformed the particles get. That enables the particles to get well soften, deformed and compressed before the inter particular melting occurs.
  • a pre-treating process to increase the relative density of the ss 316L could be to pre-heat either only the powder or both powder and the tool.
  • the material could possibly be heated to ⁇ 250° C. in in air without any reactions of the powder occur.
  • the hardness of materials affect the results.
  • the hardness of rubber is lower comparing with e.g. PMMA.
  • PMMA required a higher amount of transformed impact energy compared with rubber to obtain a sample with visibility index 2 .
  • the softer a material is the more soften and deformed the particles get, which easily has occurred with the rubber particles. That enables the particles to get softened, deformed and compressed before the inter-particular melting occurs.
  • the particles could still be determined in the sample. Therefore should probably a post-processing follows.
  • the rubber normally processes as a thermoplastic polymer where vulcanising follows. The vulcanising renders a high elastic material, elastomer, due to that the material gets cross-linked.
  • the particle size distribution should probably be wide. When different particle sizes are used small particles could fill up the empty space between big particles. Thus there are particle surfaces that are in contact with other particles everywhere in the sample. That increases the possibility to succeed in inter-particular melting (e.g. small particles' surfaces against big particles' surfaces).
  • Rubber is an amorphous polymer.
  • the sample is already room tempered when it is released from the mould. That means that the cooling process is much faster than other manufacturing processes. Due to this fast cooling process this manufacturing process could perhaps suit amorphous polymer production better than crystalline polymer production.
  • the structure of crystalline polymers is in the form of lamellas and amorphous polymers' structure is not a well organised structure. To obtain this organised structure of crystalline polymers the cooling time could probably need more time than for amorphous polymers. This cooling process could possibly effect the structure and material properties of the rubber. Therefore is there an importance of investigating the microstructure and the material properties.
  • the invention concerns a new method which comprises both pre-compacting and in some cases post-compacting and there between at least one stroke on the material.
  • the new method has proved to give very good results and is an improved process over the prior art.

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WO2024127646A1 (fr) * 2022-12-16 2024-06-20 クラレノリタケデンタル株式会社 Procédé de fabrication de corps moulé en oxyde-céramique
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CN102472349A (zh) * 2009-12-28 2012-05-23 中岛医疗有限公司 冲击吸收结构体及其制造方法
CN102653120A (zh) * 2011-03-02 2012-09-05 株式会社普利司通 隔震塞的制造方法、隔震塞以及隔震塞的制造装置
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