CN103990791A - Powder mixture - Google Patents
Powder mixture Download PDFInfo
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- CN103990791A CN103990791A CN201410054903.8A CN201410054903A CN103990791A CN 103990791 A CN103990791 A CN 103990791A CN 201410054903 A CN201410054903 A CN 201410054903A CN 103990791 A CN103990791 A CN 103990791A
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- iron
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- electronegative
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/004—Filling molds with powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F2003/023—Lubricant mixed with the metal powder
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
A powder mixture of the present invention is characterized in that it comprises: an iron powder or an iron-based alloy powder, wherein a graphite powder is adhered to a surface of the iron powder or the iron-based alloy powder by a binding agent containing a polyolefin wax; and a negatively-charged powder to be mixed with the iron powder or the iron-based alloy powder, and consisting of an iron powder and/or an iron-based alloy powder treated for negatively charging. This enables keeping the good adhering property of a graphite powder in a mixed powder and high flowability as a mixture of the raw material powder.
Description
Technical field
The present invention relates to a kind of mixture of powders, is the mixture of powders particularly using as material powder in compression moulding in powder metallurgic method.In more detail, the present invention relates to a kind of mixture of powders that suppresses the segregation of the powder in mixed-powder and the mobility excellence of mixed-powder.
Background technology
As shown in Figure 4, the manufacture of the sintered mechanical part carrying out according to powder metallurgic method is to have filled after material powder in the inner chamber that the nib 11 by by mould 10 and low punch 20 form, with low punch 20 and upper punch 30 by material powder compression molding, be made into body (so-called compression moulding), the formed body obtaining heated in sintering furnace and sintering.Such compression moulding is except can be by the moulding of sintered mechanical part near-net-shape ground, as long as and the pressing mold of producing once, just can produce in large quantities identical shaped goods, have advantages of cheap for manufacturing cost.Thus, be used in various fields.
The material powder of using in compression moulding is to select main material powder according to the desired characteristic of its target mechanical part, adds therein, mixes auxiliary material powder and adjust.For example, in structure, use in mechanical part, material powder is that to take iron powder or iron(-)base powder be main material powder, add, admixed graphite powder and add as required the auxiliary material powder of copper powders, nickel by powder, a small amount of iron(-)base powder different from main material powder composition etc., meanwhile, the shaping lubricant that adds zinc stearate etc. is adjusted.In addition, in above-mentioned raw materials powder, also with good grounds need to take the machinability of improving mechanical part be object, and the magnesium silicate of usining is the situation that machinability powder is used as above-mentioned auxiliary material powder of improving of mineral dust, sulfide powder etc.
But material powder is to be generally stored in loading hopper 40, is situated between and by flexible pipe 50, by gravity fall, is transported to the feeder 60 of bottom surface opened.When this feeder 60 moves and is positioned on the cavity being formed by nib 11 and low punch 20 on mould 10, from the bottom surface of the opening of feeder 60, material powder is filled into cavity.Therefore, because material powder will keep fillibility smoothly and suppress the inequality of loading, so require to have high fluidity.
As mentioned above, because material powder is that interpolation, admixed graphite powder and auxiliary material powder are as required modulated in main material powder, therefore, material powder is to consist of size, shape, the different powder of proportion.If powdered graphite, auxiliary material powder generation segregation, form and can produce inequality, size can change, and it is large that the unstability of the characteristics such as intensity becomes, and is the reason that causes substandard products.Therefore, require not occur the segregation of powdered graphite and auxiliary material powder.Particularly, because powdered graphite is compared to the iron powder of main material powder or the proportion of iron(-)base powder is little, when the powder landing causing is filled in the interior generation of loading hopper 40, the little powdered graphite of proportion is easily kicked up, and therefore, very expectation prevents the segregation of powdered graphite.
About such segregation problem, there are various motions, as prevented segregation (patent documentation 1 etc.) by the melting of shaping lubricant being made powdered graphite and auxiliary material powder stick together at main material powder surface, and for example add adhesive ingredients and make powdered graphite and auxiliary material powder stick together the various motions that prevent segregation (patent documentation 2 etc.) etc. at main material powder surface.
Prior art document
Patent documentation
Patent documentation 1: Unexamined Patent 01-219101 communique
Patent documentation 2: Unexamined Patent 02-217403 communique
Summary of the invention
In above-mentioned various motions, some situations are that the auxiliary material powder of powdered graphite and copper powders, nickel by powder etc. is insufficient sticking together of main material powder surface, even if some situations are that ink powder end and auxiliary material powder are abundant sticking together of main material powder surface, but the mobility of material powder declines.For this reason, seeking powdered graphite and auxiliary material powder sticking together fully and the high powder used in metallurgy material powder of mobility of material powder at main material powder surface.Under such background, the present invention take that the mixture of powders of the powder characteristics excellence that can suppress the segregation of powdered graphite and mobility etc. is provided is object.
In order to solve above-mentioned problem, the present inventor studies repeatedly, has found that the tackness of the powder that obtains is as follows good.
(1) first, when powdered graphite and auxiliary material powder are sticked together main material powder, to simultaneously stir adhesive (polyolefin wax) and main material powder, more than one side is warming up to the fusing point of polyolefin wax, with melting the surface of the coated main material powder of polyolefin wax.
(2) next, when adding and stirring powdered graphite and auxiliary material powder, be cooled to below the fusing point of polyolefin wax, by polyolefin wax, powdered graphite and auxiliary material powder sticked together on the surface of main material powder, obtain powder.
But, by above-mentioned melting mixing method, make powdered graphite and auxiliary material powder be attached to the mobility variation of the surperficial material powder of main material powder.The present inventor is studied the reason of this mobility variation, has obtained following discovery.
That is: as shown in model utility in Fig. 3, when being uniformly mixed, on a part of powder, the surperficial part generation adhesive (Knot drug) 4 of main material powder 1, powdered graphite 2 and auxiliary material powder 3 is peeled off, and is difficult to become main material powder 1 by the completely coated state of adhesive 4.In addition, as shown in Figure 4, material powder is via flexible pipe 50 and feeder 60, to be filled into cavity from loading hopper 40, but during this, material powder limit be in contact with one another friction limit mobile in, its part is that limit and the inwall of loading hopper 40, the inwall contact friction limit of the inner surface of flexible pipe and feeder are transported.
Fig. 2 shows the charged state (each symbol is identical with Fig. 3) that friction when the time comes causes.The polyolefin wax containing in adhesive 4 is easy electronegative material, and is the material with insulating properties, therefore, the friction when transporting, surface becomes electronegative.In addition, the copper powders of using as auxiliary material powder is also easy electronegative material, and by thering is the polyolefin wax of insulating properties and iron powder or iron(-)base powder, with the state of insulation, bond, the friction when transporting, making to be exposed to surperficial copper powders surface becomes electronegative.
On the other hand, as the iron powder of main material powder or iron(-)base powder, be the easy material of positively charged by friction, the friction when transporting, the surface of exposing becomes positively charged.As shown in Figure 2 (a) shows, in the iron powder of this positively charged or the exposed portions serve of iron(-)base powder, aggegation can be thought with the mutual electric attraction in surperficial, the electronegative copper powders of electronegative polyolefin wax surface of other powder, and its result causes mobility variation.
Therefore, the present inventor considers as shown in Fig. 2 (b), if add the electronegative powder 5 with high negative electricity, the electronegative powder with high negative electricity can optionally attracted to the iron powder of positively charged or the exposed division of iron(-)base powder, can prevent from attracting other powder and prevent aggegation, simultaneously, can be by not being attracted the electronegative powder with high negative electricity and each powder repulsive force that electricity repels being mutually left, the mobility of material powder is further improved, obtain experiment effect, thereby completed the present invention.
The mixture of powders of the present invention obtaining according to above-mentioned discovery is characterised in that, with the adhesive that contains polyolefin wax, powdered graphite is sticked together in surperficial iron powder or iron(-)base powder, sneaking into (add, mix) by the iron powder through electronegative processing and/or the electronegative powder that iron(-)base powder forms.
In addition, be further characterized in that, in the situation that mixture of powders comprises auxiliary material powder, with the adhesive that contains polyolefin wax, powdered graphite and auxiliary material powder are attached in surperficial iron powder or iron(-)base powder, are sneaking into (add, mix) at least one electronegative powder forming in the iron powder, iron(-)base powder and the auxiliary material powder that are selected from through electronegative processing.
The preferred configuration of each mixture of powders of the present invention is above: said polyolefins is that wax is at least one being selected from Tissuemat E and polypropylene wax.
In addition, the preferred configuration of each mixture of powders of the present invention is: above-mentioned electronegative processing is by being selected from least one the coated processing carried out in alkyl silane, dimethylsilane, octyl group silane, methacrylic acid silane (methacrylsilane), fluoro alkyl-silane and HMDS.In addition, preferred configuration is: the maximum particle diameter of above-mentioned electronegative powder is 1～15 μ m, and with respect to 100 mass parts iron powder or iron(-)base powders, the addition of above-mentioned electronegative powder is 0.02～0.5 mass parts.
In addition, in the situation that each mixture of powders of the present invention comprises auxiliary material powder, the form that this auxiliary material powder is sticked together on iron powder or iron(-)base powder surface together with powdered graphite by adhesive of take is preferred configuration, but can be also part or all form containing as free powder of this auxiliary material powder.In addition, in the situation that each mixture of powders of the present invention comprises shaping lubricant powder, take that to contain this shaping lubricant powder be preferred configuration as free powder.
In the present invention, be to use the adhesive of the polyolefin wax that contains tackness excellence to make powdered graphite stick together the mixture of powders at main material powder surface, therefore, can conscientiously suppress the segregation of the powdered graphite in mixture of powders.Meanwhile, by add electronegative powder in mixed-powder, can suppress polyolefin wax because of the charged aggegation causing, obtain high fluidity.
The Topic relative connection of recording in No. 2013-28703, the Patent of the application's announcement and on February 18th, 2013 application, at this, these disclosure are continued to use by reference.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that shows an example of mixture of powders of the present invention.
Fig. 2 is the schematic diagram that shows the electriferous state of mixture of powders, and Fig. 2 (a) only has by adhesive 4 to make powdered graphite 2 and auxiliary material powder 3 stick together the situation at the surperficial powder of main material powder 1.Fig. 2 (b) is for to make powdered graphite 2 and auxiliary material powder 3 stick together the situation of having added electronegative powder in the surperficial powder of main material powder 1 by adhesive 4.
Fig. 3 is the schematic diagram that shows the state of the powder forming according to melting mixing method.
Fig. 4 is the figure that shows the summary of the building mortion in the forming process of carrying out according to compression moulding.
Symbol description:
1-main material powder; 2-powdered graphite; 3-auxiliary material powder; 4-adhesive; 5-electronegative powder; 6-shaping lubricant powder; 10-mould; 11-nib; 20-low punch; 30-upper punch; 40-loading hopper; 50-flexible pipe; 60-feeder.
The specific embodiment
In the present invention, owing to having used the adhesive by the polyolefin wax that contains tackness excellence to make powdered graphite stick together the mixture of powders at main material powder surface, therefore, can conscientiously suppress the segregation of the powdered graphite in mixture of powders.Meanwhile, by add electronegative powder in mixed-powder, can suppress, because of the charged aggegation causing of polyolefin wax, to obtain high fluidity.
In the present invention, as polyolefin wax, or as electronegative processing clad material, be all to use general material, be therefore easy to implement.In addition, in the present invention, as illustrated in table 1, table 3, conscientiously obtained effect and the high fluidity of above-mentioned inhibition segregation.
And then, in the present invention, in the form that comprises auxiliary material powder, it can be also its all or part of mode of sticking together surperficial mode at main material powder, the mode that contains remainder as free powder and containing whole auxiliary material powder as free powder together with powdered graphite.In addition, in the present invention, in the form that contains the lubricated powder that is shaped, be the mode that contains the lubricated powder of this shaping as free powder.
In the present invention, electronegative powder will be blended in main material powder, iron powder and/or iron(-)base powder through electronegative processing, consist of.In the form that comprises auxiliary material powder, also can be that a part for above-mentioned auxiliary material powder is carried out to electronegative processing, replace iron powder and/or iron(-)base powder through electronegative processing, electronegative powder is the mode comprising through the auxiliary material powder of electronegative processing, can also be except the iron powder and/or iron(-)base powder of the electronegative processing of above-mentioned process, electronegative powder also contains the mode through the auxiliary material powder of above-mentioned electronegative processing.
These are clearly confirmed the details of above-mentioned each invention.
Below, the present invention is described in detail.
Below, after preferred forms of the present invention is described, by exemplifying the clear and definite practicality of embodiment.The schematic diagram of Fig. 1 shows an example of the structure of mixture of powders of the present invention.In the figure, mixture of powders comprises: the main material powder 1 consisting of iron powder or iron(-)base powder, powdered graphite 2, the auxiliary material powder 3 consisting of copper powders, shaping lubricant powder 6, electronegative powder 5 and adhesive 4.
Powdered graphite 2 and auxiliary material powder 3 stick together the surface at main material powder 1 by the adhesive 4 that comprises polyolefin wax.In addition, electronegative powder 5 and shaping lubricant 6 are not bonded on main material powder 1, but exist as free powder.
At this, as the first requirement characteristic of adhesive 4, must from be transported to shaping stage during, maintain powdered graphite sticking together main material powder surface.For this reason, as this adhesive, not only to there is high adhesion, and the intensity of the vibration importantly will there is resistance to transporting time etc.For example, the adhesive of patent documentation 1 (lubricant) is fragility, even if can make powdered graphite a period of time stick together at main material powder surface, but vibration owing to transporting etc. are easy to peel off, and therefore can not suppress the segregation of powdered graphite.In the present invention, the adhesion of the polyolefin wax using as adhesive is high, and has extensibility to a certain degree, the intensity of the vibration when having abundant tolerance and transporting etc.
As second of adhesive, require characteristic, due to when sintered shaped body, adhesive can decompose at an easy rate when sintering heats, and must be therefore that sintered body is not had to influential adhesive completely.In addition, because being to make it disappear like this, therefore, requirement is cheap as far as possible adhesive.In this, in the present invention, the polyolefin wax using as adhesive, for example, can learn from Tissuemat E, polypropylene wax, it is relatively simple for structure and inexpensive, can decompose at an easy rate disappearance because of heating again, can not affect sintered body completely.
As the 3rd of adhesive, require characteristic, must have and can make powdered graphite stick together at an easy rate the character at main material powder surface.About this point, the fusing point of polyolefin wax is low, can make at an easy rate its melting, therefore, can carry out melting mixing at low temperatures and make powdered graphite stick together the surface at main material powder.
The polyolefin wax using as adhesive, its molecular weight more tackness and intensity more increases.From this viewpoint, preferable weight-average molecular weight Mw is more than 1000 polyolefin wax.On the other hand, because the larger fusing point of molecular weight and decomposition temperature more rise, therefore preferably using weight average molecular weight Mw is the polyolefin wax below 400000.Thus, preferably (weight average molecular weight Mw is preferably 1000～40000 degree to the Tissuemat E in use polyolefin wax, 1000～10000 degree more preferably), polypropylene wax (weight average molecular weight Mw is preferably 1000～40000 degree, more preferably 10000～35000 degree) etc.If mix to use weight average molecular weight different Tissuemat E of more than two kinds and polypropylene wax separately, the decomposition of adhesive during sintering can not occur quickly, can periodically carry out, and be therefore preferred.
The polyolefin wax with above-mentioned weight average molecular weight can be used commercially available prod, also can use the product obtaining by the suitable modulation of any manufacture method.
Preferred adhesive consists of polyolefin wax.
The polyolefin wax using as adhesive must disappear when sintering, does not affect the characteristic of sintered body, and therefore, use amount is for can make powdered graphite fully stick together the surperficial amount at the iron powder as main material powder or iron(-)base powder.For example, if used in a large number because adhesive proportion is little, the quantitative change of the adhesive comprising in formed body is many, thus, can make formed body density decline, and the formability of material powder is declined.Therefore, the use amount of adhesive should be adjusted according to the addition of powdered graphite, preferably, with respect to the addition of the powdered graphite of 100 mass parts, uses 10～80 mass parts adhesives.
In addition, in the situation that auxiliary material powder is sticked together on main material powder together with powdered graphite, preferably with respect to 100 mass parts, be attached to powdered graphite and the auxiliary material powder on main material powder, use 10～80 mass parts adhesives.
Preferably, with respect to the iron powder as main material powder or the iron(-)base powder of 100 mass parts, the addition of powdered graphite is 0.1～2.5 mass parts.In the situation that mixture of powders of the present invention is used on structure member, preferably, with respect to the iron powder as main material powder or the iron(-)base powder of 100 mass parts, the addition of powdered graphite is 0.1～1.2 mass parts.
Preferred polyolefm is the state that wax becomes completely coated main material powder surface, but it is more difficult to become such state, can become the state that the part surface of main material powder exposes.In the present invention, main material powder is to use iron powder or iron(-)base powder, therefore, can become the state that the part surface of iron powder or iron(-)base powder exposes.
Like this by polyolefin wax clad surface, make the friction owing to transporting of powder that powdered graphite sticks together, the mantle friction of polyolefin wax is charged and electronegative.In addition, because the insulating properties of polyolefin wax is high, so polyolefin wax surface just becomes electronegative state.On the other hand, friction when transporting of the iron powder of exposing on a part of surface or iron(-)base powder and therefore positively charged, applies electrical affinity to electronegative polyolefin wax cladding powder around.
In order to prevent this polyolefin wax cladding powder electric attraction each other, in the present invention, add electronegative powder as free powder.Because electronegative powder is the free powder of not adhered, therefore, in the iron powder of positively charged or the exposed portions serve of iron(-)base powder, electronegative powder is covered the exposed portions serve of iron powder or iron(-)base powder by electric attraction.Thus, absorption has the powder surface integral body being coated by polyolefin wax of electronegative powder to become negative electrical charge, can prevent the powder that is coated by polyolefin wax electric attraction each other.
And then, by electric attraction, to the remaining electronegative powder of the exposed portions serve of iron powder or iron(-)base powder, with respect to surface integral, do not become the powder being coated by polyolefin wax of negative electrical charge, be subject to electric mutual expelling force, the mobility of mixture of powders is improved.
In addition, can be by the complete coated iron powder of polyolefin wax or iron(-)base powder surface in the situation that, can there is not the above-mentioned powder being coated by polyolefin wax electric attraction each other, even if but in this case, if add electronegative powder, due to the effect of electric mutual expelling force between electronegative powder and the powder that is coated by polyolefin wax, therefore, can access the effect that the mobility of mixture of powders is improved.
Because electronegative powder performance is attracted, to the effect of the exposed portions serve of iron powder or iron(-)base powder, therefore, use the electronegative powder having than the larger negative electrical charge of negative electrical charge of the polyolefin wax of frictional electrification energetically.Wherein, because alkyl silane, dialkyl silane, methacrylic acid silane, haloalkyl silane and six alkyl disilazanes have, be with high elecrtonegativity, therefore, preferably use wherein at least one is coated on to surperficial powder.
As the alkyl in above-claimed cpd, preferably exemplify the alkyl of carbon number 1～10, more preferably exemplified by methyl, ethyl, propyl group, butyl, amyl group, hexyl, octyl group etc.
As alkyl silane, be not particularly limited, but exemplified by methyl silane, ethylsilane, propyl silane, butyl silane, amyl group silane, hexyl silane, octyl group silane etc.
As dialkyl silane, be not particularly limited, but exemplify dimethylsilane, diethylsilane, dipropyl silane etc.
As methacrylic acid silane, be not particularly limited, but exemplify organic silane compound having acryloxy or methacryloxy etc.
As haloalkyl silane, be not particularly limited, but exemplify methyl fluoride silane, difluoromethyl silane, chloromethyl silane, fluorine chloromethyl silane, fluoro ethyl silane etc.
As six alkyl disilazanes, be not particularly limited, but enumerate HMDS, hexaethyl disilazine etc.
Dimethylsilane, octyl group silane, methacrylic acid silane, fluoro alkyl-silane and HMDS are with high elecrtonegativity owing to having, preferably surface is used as electronegative powder by least one coated powder wherein, particularly preferably by octyl group silane, the coated powder of HMDS.
In the electronegative processing that alkyl silane etc. is coated, carry out powder that one side stirs alkyl silane and will carry out electronegative processing and simultaneously be warming up to the mixed processes more than fusing point of alkyl silane etc.By this mixed processes, make melting alkyl silane etc. be covered in the surface that will carry out the powder of electronegative processing, by be cooled to the fusing point of alkyl silane etc. below, on the surface that will carry out the powder of electronegative processing form the cakey overlay film of alkyl silane etc. thereafter.
In addition, the electronegative powder that preferably do not hinder sintering, sintered body is exerted an influence.From this point, consider, the above-mentioned powder that will carry out electronegative processing is at least one in iron powder and iron(-)base powder.Because main material powder is iron powder or iron(-)base powder, therefore, the powder that will carry out electronegative processing that at least one in iron powder and iron(-)base powder forms is easy to and the mutual diffusion bond of main material powder, and can not have a negative impact to the metal structure of sintered body.At this, as the powder that will carry out electronegative processing, if the powder of use and main material powder identical component can not be woven with impact to metal group completely, thereby preferably.
In addition, the more tiny specific area of electronegative powder more increases, and meanwhile, quality diminishes, and the exposed portions serve that is easily main material powder 1 by above-mentioned positively charged iron powder or iron(-)base powder attracts.In addition, if electronegative powder is thick, also likely hinder agglutinating property.
For this reason, the maximum particle diameter of preferred electronegative powder is below 15 μ m.On the other hand, if too small, the electronegative powder adding with the form of powder likely can immerse in the gap of mould and drift etc., and snap gauge easily occurs.Therefore, the minimum grain size of preferred electronegative powder is more than 1 μ m.
The average grain diameter of main material powder (D50) is preferably 50～150 μ m, more preferably 50～120 μ m.Preferably the average grain diameter (D50) of auxiliary material powder is 50～100 μ m, and is less than the average grain diameter of main material powder.The average grain diameter of the primary particle size of powdered graphite (D50) is preferably 1～50 μ m, more preferably 1～10 μ m.
Main material powder, auxiliary material powder and the powdered graphite with above-mentioned particle diameter, can be used commercially available product, also can modulate by the product of being made by any means being screened etc.
In addition, the addition of electronegative powder is preferably 0.02～0.5 mass parts with respect to 100 mass parts iron powder or iron(-)base powder (main material powder).This is because if addition less than 0.02 mass parts of electronegative powder is difficult to conscientiously obtain its effect, in addition, if addition surpasses 0.5 mass parts, the ejection pressure that forms the powder compact after powder can extremely increase.
Auxiliary material powder is the powder with following effect: diffusion in the matrix of the sintered body being formed by main material powder and make the effect of sintered body matrix solution strengthening, forming compound makes the matrix strengthening of sintered body improve the effect of the intensity of sintered body, in the matrix of the sintered body being formed by main material powder, diffusion improves the effect of the characteristics such as hardenability of sintered body matrix, make sintering have activity carry out acceleration of sintering and improve sintered body intensity effect and be dispersed in the wear-resistant that improves sintered body in sintered body, the effect of the characteristics such as the machinability of sintered body.
In addition, in the situation that using iron powder or iron(-)base powder as main material powder, as auxiliary material powder, can use that the iron(-)base powder (in this case, being the composition a small amount of iron(-)base powder different from main material powder) of copper alloy powder such as powdered graphite, copper powders and signal bronze powder etc., nickel by powder, molybdenum powder, ferrophosphor(us) powder etc., various hard phase form powder, magnesium silicate is mineral dust, calcirm-fluoride powder, sulfide powder etc.With respect to 100 mass parts main material powder, use below 30 mass parts, preferably use below 20 mass parts, more preferably the auxiliary material powder below 10 mass parts.
Such auxiliary material powder is preferably same with powdered graphite, and the auxiliary material powder 3 as Fig. 1, sticks together the surface at the iron powder as main material powder or iron(-)base powder.Particularly using as illustrative magnesium silicate is mineral dust, calcirm-fluoride powder, a part of sulfide powder, proportion is than becoming in the situation of the auxiliary material powder that the iron powder of main material powder or iron(-)base powder are little, and use in powder that particle diameter the is little situation as auxiliary material powder, with the same easily generation of powdered graphite segregation, therefore, preferably auxiliary material powder is sticked together to the surface at the iron powder as main material powder or iron(-)base powder together with powdered graphite.
On the other hand, in the situation that use proportion to approach the metal dust of iron powder or iron(-)base powder and have the to a certain degree auxiliary material powder of size, owing to being difficult for occurring segregation, the form of therefore paying free powder is also harmless.In this case, owing to not needing to stick together auxiliary material powder, can reduce thus the amount of the polyolefin wax of this part.
Therefore, auxiliary material powder consists of various powders, in the situation that a part is easy segregation powder, if only a part of auxiliary material powder that segregation easily occurs is sticked together to the surface at iron powder or iron(-)base powder, using the auxiliary material powder of the remainder of difficult generation segregation as free powder, can make the amount of polyolefin wax is only necessary amount, is therefore preferred.
In the situation that as above using auxiliary material powder, also can replace as the iron powder of electronegative powder use and at least one in iron(-)base powder, use the auxiliary material powder of the electronegative processing of process as electronegative powder, or except the iron powder used as electronegative powder and at least one in iron(-)base powder, also use auxiliary material powder through electronegative processing as electronegative powder.This is because using auxiliary material powder as electronegative powder use in the situation that, be also easy to and the mutual diffusion bond of main material powder, and can not have a negative impact to the metal structure of sintered body.
Polyolefin wax is normally used as shaping lubricant, but in mixture of powders of the present invention, polyolefin wax is used as binding agent, therefore, lower as the function of shaping lubricant.For this reason, in the situation that used the metal pattern lubricating method (external lubrication method) that the lubricant of the wall coating powder of metal pattern or liquid is formed, can former state use.On the other hand, in the situation that used, the wall coating powder of metal pattern or the lubricant of liquid are not formed, preferably use shaping lubricant powder is mixed to provide with material powder sneak into lubricating method (internal lubrication).
As shaping lubricant powder, can use the shaping lubricant powder in the past using.For example, can use the slaine etc. of higher fatty acids of higher fatty acids, zinc stearate and the lithium stearate etc. of stearic acid etc.If shaping lubricant powder is added by melting, lubrication property declines, and therefore preferably as free powder, provides.In addition, the addition of shaping lubricant powder, as carried out, with respect to 100 mass parts main material powder, is the degree of 0.1～1.5 mass parts in the past.
Shaping lubricant powder is as long as used the common product using in powder metallurgy to be just not particularly limited.
Above-mentioned mixture of powders can for example be manufactured as follows.That is: as manufacture method, the method through following operation: be situated between and by powdered graphite or by powdered graphite and auxiliary material powder, stick together the surperficial operation at iron powder or iron(-)base powder by the adhesive that contains polyolefin wax, and, by by adding through the iron powder of electronegative processing and/or electronegative powder that iron(-)base powder forms and being mixed into the operation in the material powder being obtained by above-mentioned operation.
In detail, first, carry out one side and stir using the adhesive that contains polyolefin wax with as the iron powder of main material powder or the mixture of iron(-)base powder, one side is warming up to the mixed processes for the first time more than fusing point of polyolefin wax.By this mixed processes for the first time, at the melt surface of iron powder or iron(-)base powder polyolefin wax be coated on the surface of iron powder or iron(-)base powder.
Next, carry out under the condition more than the fusing point of polyolefin wax, adding the mixed processes for the second time of powdered graphite stirring in the mixture of powders by mixed processes obtains for the first time.By this mixed processes for the second time, powdered graphite be attached to coated iron powder or iron(-)base powder surperficial melting polyolefin wax.Under this state, as long as carry out coolingly to become the temperature below the fusing point of polyolefin wax, can obtain making powdered graphite stick together the surperficial mixture of powders at iron powder or iron(-)base powder by adhesive.After mixed processes for the first time, once also can become after mixture of powders cooling, mixed processes is for the second time carried out in heating more separately, if but consider the cooling bothersome and power consumption of heating again, preferably after mixed processes for the first time, do not carry out cooling but continue to add powdered graphite and carry out mixed processes for the second time.
After mixed processes for the second time, carry out the mixed processes for the third time that adds electronegative powder at the temperature below the fusing point of polyolefin wax and mix in the mixture of powders obtaining.So, by carrying out mixed processes for the third time at the temperature below the fusing point at polyolefin wax, electronegative powder can be provided as free powder.Also can be in the cooling procedure after mixed processes for the second time, the stage of the temperature below the fusing point that becomes polyolefin wax starts mixed processes for the third time, can also, after by the mixture of powders cool to room temperature by mixed processes obtains for the second time, add at ambient temperature electronegative powder and mix.In the situation that adding shaping lubricant powder, by adding and mix in mixed processes for the third time at this, the lubricant powder that can make to be shaped provides as free powder.
In the situation that mixture of powders comprises auxiliary material powder, if adding and mix auxiliary material powder in mixed processes for the second time, can make auxiliary material powder stick together the surface at iron powder or iron(-)base powder.In addition, if adding and mix auxiliary material powder in mixed processes for the third time, can make auxiliary material powder provide as free powder.
Embodiment
The first embodiment
Prepare iron powder (100 orders, 75 μ m), cathode copper powder (200 orders average grain diameter (D50):, 45 μ m), powdered graphite (325 orders average grain diameter (D50):, average grain diameter (D50): 10 μ m) and as the zinc stearate powder of shaping lubricant powder, and prepared the polyolefin wax (Tissuemat E) that weight average molecular weight Mw is 8000.In addition, as electronegative powder, prepared surface by the coated iron powder of alkyl silane (octyl group silane) and the surperficial iron powder (maximum particle diameter is 5 μ m) being coated by HMDS.
With respect to 100 mass parts iron powder, add the polyolefin wax of 0.5 mass parts, drop in Henschel mixer, in mixer, one side heating one side is mixed, be warming up to 130 ℃ of fusing point (110 ℃) higher than polyolefin wax, carried out by melting the mixed processes for the first time on polyolefin wax coated iron powder surface.Then, under the state of polyolefin wax melting, with respect to 100 mass parts iron powder, 1.5 mass parts copper powders and 1.0 mass parts powdered graphites are added in mixture and mixed respectively, by the polyolefin wax of melting, make copper powders and powdered graphite fully be attached to iron powder, and it is disperseed in heterogeneity, thereby carry out mixed processes for the second time.Thereafter, one side stirs one side and is cooled to room temperature, obtains mixture for the second time.This for the second time mixture be that to take the polyolefin wax of 0.5 mass parts be adhesive, 1.5 mass parts copper powders and 1.0 mass parts powdered graphites are sticked together with respect to 100 mass parts iron powder.With respect to the 100 mass parts powdered graphites that add, the addition of polyolefin wax is 50 mass parts.
In the mixture for the second time obtaining, in the ratio shown in table 1, add electronegative powder (adding proportion is the mass parts with respect to 100 mass parts iron powder), simultaneously, add 0.8 mass parts shaping lubricant powder, by V-Mixer, mixed, made the mixture of powders of specimen coding 01～17.In addition, in order comparing, with respect to 100 mass parts iron powder, to add 1.5 mass parts copper powders, 1.0 mass parts powdered graphites and 0.8 mass parts shaping lubricant powder, by V-Mixer, to be mixed, made the mixture of powders of specimen coding 18.
About these mixture of powders, measured adhesion amount, fluidity and the ejection pressure (ejection pressure MPa) of powdered graphite.
Wherein, adhesive rate is first to not adding the mixture of powders (specimen coding 01) of electronegative powder, and the high-frequency induction furnace burning-infrared absorption of stipulating in the G1211 by JIS standard is carried out carbon content analysis and measured carbon amount.This carbon amount is to comprise can not stick together and the carbon amount (the carbon amount that adds up to the carbon component of powdered graphite and wax) of the mixture of powders sample integral body of free powdered graphite.Then, for each mixture of powders sample, the impact of free powdered graphite etc. and the free electronegative powder causing for fear of not sticking together, mixed-powder is sieved with 100 orders and 200 object sieves, extraction has been passed through 100 object sieves but not by the powder (powder of particle diameter 75～150 μ m) of 200 mesh sieve, to this powder, the high-frequency induction furnace burning-infrared absorption of stipulating in the G1211 by JIS standard is carried out carbon content analysis and has been measured carbon amount.This carbon amount is to be situated between by wax, to be attached to the carbon amount (the carbon amount that adds up to the carbon component of powdered graphite and wax) of the powdered graphite in iron powder.The adhesive rate of powdered graphite is by the carbon amount of the mixture of powders sample integral body of the free powdered graphite that comprises such mensuration and the carbon amount of the graphite powder that is attached to iron powder by wax of being situated between, and tries to achieve the ratio with respect to the carbon amount carbon amount of the mixture of powders sample integral body that comprises free powdered graphite, that be situated between the powdered graphite that is attached to iron powder by wax.
The mensuration of the fluidity of mixture of powders is to carry out according to the slump test method of stipulating in the Z2502 of JIS standard.
As got off, try to achieve ejection pressure: the die assembly that is become the fixing floating die mode of low punch by spring supporting mould, the die assembly of the structure of load cell has been combined in use on the compression plate of low punch, by the pull-up universal testing machine of A Musi, the cylindric formed body of diameter 11.3mm, high 10mm is formed with the pressure of 700MPa, the load of mensuration during from the metal pattern demoulding, then remove by the outer circumferential area of formed body.These values are presented in table 1 in the lump.
Table 1
Table 1 has been investigated the impact of the addition of electronegative powder, specimen coding 01～09th, has been used the example by the situation of the iron powder of alkyl silane (octyl group silane) clad surface, and specimen coding 01,10～17th has been used the example by the situation of the iron powder of HMDS clad surface.
The specimen coding 18 of table 1 is the example of mixture of powders of not using the common simple mixing of polyolefin wax, but by 100 object sieves, do not passing through in the powder (powder of particle diameter 75～150 μ m) of 200 object sieves the low value that the adhesive rate of powdered graphite is 30%.In addition, this 30% powdered graphite be to be embedded in the powdered graphite existing in the depression etc. of erose iron powder.On the other hand, the mixture of powders sample of specimen coding 01 is to make powdered graphite be attached to iron powder surface by polyolefin wax, and the adhesive rate of powdered graphite is shown as 97% high adhesive rate.But with respect to the mixture of powders of the common simple mixing of specimen coding 18, the fluidity of the mixture of powders sample of specimen coding 01 declines.
At the mixture of powders that makes powdered graphite be attached to such iron powder surface by polyolefin wax, close the middle mixture of powders sample (specimen coding 02 and 10) that has added the electronegative powder of 0.02 mass parts, the mobility of its mixture of powders improves, compare with the mixture of powders of the simple mixing of specimen coding 18, fluidity is little.In addition, along with the increase of the addition of electronegative powder, the mobility of mixture of powders further improves, and fluidity further diminishes.But electronegative powder surpasses 0.3 mass parts, even if add in mixture of powders, also fails to confirm the raising of the mobility on this.
From above-mentioned situation, can confirm, by using polyolefin wax to make powdered graphite be attached to the surface of iron powder, can improve significantly the adhesive rate of powdered graphite, mobility declines, the decline of this mobility can be by being that more than 0.02 mass parts electronegative powder is improved make powdered graphite add in being attached to the mixture of powders on iron powder surface with respect to 100 mass parts iron powder with polyolefin wax, in this case, mobility is higher than the mixture of powders of common simple mixing.
In addition, also can confirm, the effect of above electronegative powder, even if in the situation of any that has used coated alkyl silane iron powder and coated HMDS iron powder as electronegative powder, also there is same effect, can confirm so long as electronegative powder just can obtain same effect.
In addition, by polyolefin wax, make powdered graphite be attached to the mixture of powders (specimen coding 01) on iron powder surface and compare with the mixture of powders (specimen coding 18) using wax as the common simple mixing of lubricant performance function, ejection pressure is reduced to about 7 one-tenth.If make powdered graphite add electronegative powder in being attached to the mixture of powders on iron powder surface by polyolefin wax, ejection pressure increases.In addition, can confirm that ejection pressure is along with the addition of electronegative powder increases and the tendency that increases, the addition of electronegative powder is about 8 one-tenth of the ejection pressure of mixture of powders of the sample (specimen coding 08 and 16) of the 0.5 mass parts mixture of powders (specimen coding 18) that is reduced to common simple mixing.If the addition of electronegative powder surpasses 0.5 mass parts (specimen coding 17), ejection pressure is reduced to about 9 one-tenth of mixture of powders (specimen coding 18) of common simple mixing.By above situation, can be learnt, to the addition that makes powdered graphite be attached to the electronegative powder adding in the mixture of powders on iron powder surface by polyolefin wax, be preferably below 0.5 mass parts.
The second embodiment
When the second embodiment is the iron powder of stating in the use the first embodiment, copper powders, powdered graphite, shaping lubricant powder, as electronegative powder, use by the coated iron powder of alkyl silane (octyl group silane), polyolefin wax changes to the wax (Tissuemat E) of the weight average molecular weight Mw of table 2, in addition, same with the first embodiment, made the mixture of powders of specimen coding 19～29.For the mixture of powders obtaining, adhesive rate, fluidity and ejection pressure have been measured equally with the first embodiment.These results are presented in table 2 in the lump.
Table 2
| Specimen coding | The weight average molecular weight of polyolefin wax | Adhesive rate (%) | Fluidity (second) | Ejection pressure (MPa) |
| 19 | 500 | 94 | 34 | 12.2 |
| 20 | 1000 | 95 | 30 | 12.8 |
| 21 | 3000 | 95 | 29 | 12.9 |
| 22 | 5000 | 97 | 28 | 13.0 |
| 05 | 8000 | 97 | 27 | 13.3 |
| 23 | 10000 | 97 | 25 | 13.6 |
| 24 | 15000 | 97 | 25 | 14.7 |
| 25 | 20000 | 97 | 25 | 16.2 |
| 26 | 25000 | 97 | 25 | 16.5 |
| 27 | 30000 | 97 | 25 | 17.0 |
| 28 | 35000 | 97 | 25 | 17.0 |
| 29 | 40000 | 97 | 25 | 17.6 |
| 18 | — | 30 | 34 | 18.1 |
From table 2, learn, weight average molecular weight not based on polyolefin wax, by polyolefin wax, make powdered graphite be attached to the mixture of powders on iron powder surface and compare with the mixture of powders of common simple mixing (specimen coding 18), show the high adhesive rate of powdered graphite.
In addition, it is softer owing to being coated on the wax on iron powder surface that the weight average molecular weight of polyolefin wax is 500 mixture of powders sample (specimen coding 19), adhesive rate is lower thus, and the mixture of powders of fluidity and common simple mixing (specimen coding 18) is equal extent.On the other hand, the weight average molecular weight at polyolefin wax is that in more than 1000 mixture of powders samples (specimen coding 05,20～29), the wax that is coated on iron powder surface is harder than the mixture of powders sample of specimen coding 19.Thus, adhesive rate improves, and mobility improves than the mixture of powders of common simple mixing (specimen coding 18).Learning thus, is more than 1000 polyolefin wax if use weight average molecular weight, and not only the adhesive rate of powdered graphite can improve but also mobility also can improve, and is desirable.
On the other hand, along with the weight average molecular weight Mw increase of polyolefin wax, ejection pressure shows the tendency increasing.Just, the ejection pressure of the mixture of powders sample that the weight average molecular weight Mw of polyolefin wax is 40000 (specimen coding 29) is still than the low value of the mixture of powders of common simple mixing (specimen coding 18).But can think, if the weight average molecular weight Mw of polyolefin wax surpasses 40000, ejection pressure can be increased to part mixture of powders (specimen coding 18) equal extent with common simple mixing.Therefore,, if consider ejection pressure, preferably use the weight average molecular weight Mw of the polyolefin wax below 40000.
The 3rd embodiment
The 3rd embodiment is in the iron powder of using the first embodiment, copper powders, powdered graphite, shaping lubricant powder, as electronegative powder, use by the coated copper powders of alkyl silane (octyl group silane) (maximum particle diameter 5 μ m), make the proportioning shown in table 3, same with the first embodiment, made the mixture of powders of specimen coding 30～37.About the mixture of powders obtaining, adhesive rate, fluidity and ejection pressure have been measured equally with the first embodiment.These results are presented in table 3 in the lump.
Table 3
Table 3 has been investigated and has been used auxiliary material powder as the impact in the situation of electronegative powder, specimen coding 30～37th, and the iron powder of replacement the first embodiment, use is by the example in the situation of the copper powders of alkyl silane (octyl group silane) clad surface.
From table 3, learn, used the mobility that the situation of the mixture of powders sample (specimen coding 30) of the electronegative powder of auxiliary material powder is mixture of powders to improve making powdered graphite add 0.02 mass parts in being attached to the mixture of powders on iron powder surface by polyolefin wax (Tissuemat E), compare with the mixture of powders of the common simple mixing of specimen coding 18, fluidity diminishes.In addition, along with the increase of the addition of electronegative powder, the mobility of mixture of powders further improves, and fluidity further diminishes.Just, even if make electronegative powder surpass 0.3 mass parts, add in mixture of powders, can not confirm the raising higher than this mobility.
In addition, if the electronegative powder that has used auxiliary material powder is added to by polyolefin wax powdered graphite is attached in the mixture of powders on iron powder surface, ejection pressure increases.In addition, can confirm to have the tendency that ejection pressure increases along with the increase of the addition of electronegative powder, the addition of electronegative powder is the degree of 8 one-tenth that the ejection pressure of mixture of powders of the sample (specimen coding 36) of 0.5 mass parts is reduced to the mixture of powders (specimen coding 18) of common simple mixing, if the addition of electronegative powder surpasses 0.5 mass parts (specimen coding 37), ejection pressure is reduced to the degree of 9 one-tenth of the mixture of powders (specimen coding 18) of common simple mixing.
As above can learn, even if the powder through electronegative processing is changed to copper powders (composition of auxiliary material powder) by iron powder (with main material powder identical component), also can obtain same result.
Utilizability in industry
Mixture of powders of the present invention is the mixture of powders that can suppress the segregation of the powder in mixed-powder and the mobility excellence of mixed-powder, because it can sintered mechanical part not occur to manufacture unevenly by compression moulding, be therefore the mixture of powders of the manufacture of suitable various sintered mechanical parts.
Claims (11)
1. a mixture of powders, it is characterized in that, contain: by the adhesive that contains polyolefin wax, make powdered graphite be attached to surperficial iron powder or iron(-)base powder, and sneak in this iron(-)base powder, by through the iron powder of electronegative processing and/or the electronegative powder that iron(-)base powder forms.
2. mixture of powders according to claim 1, is characterized in that,
Described polyolefin wax is at least one being selected from Tissuemat E and polypropylene wax.
3. according to mixture of powders described in claim 1 or 2, it is characterized in that,
Described electronegative being treated to by least one the coated processing carried out being selected from alkyl silane, dialkyl silane, methacrylic acid silane, haloalkyl silane and six alkyl disilazanes.
4. according to the mixture of powders described in any one of claim 1～3, it is characterized in that,
The maximum particle diameter of described electronegative powder is 1～15 μ m.
5. according to the mixture of powders described in any one of claim 1～4, it is characterized in that,
With respect to iron powder or iron(-)base powder described in 100 mass parts, the addition of described electronegative powder is 0.02～0.5 mass parts.
6. according to the mixture of powders described in any one of claim 1～5, it is characterized in that,
Described mixture of powders also comprises auxiliary material powder,
Described auxiliary material powder sticks together the surface at described iron powder or iron(-)base powder by described adhesive together with described powdered graphite.
7. according to the mixture of powders described in any one of claim 1～5, it is characterized in that,
Described mixture of powders also comprises auxiliary material powder,
Described auxiliary material powder is involved as being sticked together at the surperficial powder of described iron powder or iron(-)base powder by described adhesive together with described powdered graphite, is also as free powder and involved.
8. according to the mixture of powders described in any one of claim 1～5, it is characterized in that,
Described mixture of powders also comprises auxiliary material powder,
Described auxiliary material powder is as free powder and involved.
9. according to the mixture of powders described in any one of claim 6～8, it is characterized in that,
A part for described auxiliary material powder is the auxiliary material powder through electronegative processing,
Described electronegative powder consists of the auxiliary material powder of the electronegative processing of described process, to replace iron powder and/or the iron(-)base powder of the electronegative processing of described process.
10. according to the mixture of powders described in any one of claim 6～8, it is characterized in that,
A part for described auxiliary material powder is the auxiliary material powder through electronegative processing,
Except the iron powder and/or iron(-)base powder of the electronegative processing of described process, described electronegative powder also comprises the auxiliary material powder of the electronegative processing of described process.
11. according to the mixture of powders described in any one of claim 1～10, it is characterized in that,
Described mixture of powders also comprises shaping lubricant powder,
Described shaping lubricant powder is as free powder and involved.
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| JP2013028703A JP6171390B2 (en) | 2013-02-18 | 2013-02-18 | Powder mixture |
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| CN110709191A (en) * | 2017-06-16 | 2020-01-17 | 杰富意钢铁株式会社 | Powder mixture for powder metallurgy and method for producing same |
| US11224914B2 (en) | 2017-06-16 | 2022-01-18 | Jfe Steel Corporation | Powder mixture for powder metallurgy and method of manufacturing same |
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| JP6413522B2 (en) * | 2014-09-09 | 2018-10-31 | セイコーエプソン株式会社 | Sheet manufacturing apparatus, sheet manufacturing method, sheet manufactured by these, composite used for these, and container for the same |
| WO2018083821A1 (en) * | 2016-11-01 | 2018-05-11 | 国立大学法人東北大学 | Composite powder, method for producing same, heat-resistant material and method for producing said heat-resistant material |
| KR20240003693A (en) | 2022-06-30 | 2024-01-09 | 스테타시 가부시키가이샤 | Manufacturing method of resin sheets, vinyl chloride leather, and vegan leather |
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Also Published As
| Publication number | Publication date |
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| JP2014156638A (en) | 2014-08-28 |
| US20140230603A1 (en) | 2014-08-21 |
| JP6171390B2 (en) | 2017-08-02 |
| IN2014CH00716A (en) | 2015-04-24 |
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Application publication date: 20140820 |