CN105408100A - Compression molding apparatus and method for manufacturing compression molded article - Google Patents

Compression molding apparatus and method for manufacturing compression molded article Download PDF

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Publication number
CN105408100A
CN105408100A CN201580001415.3A CN201580001415A CN105408100A CN 105408100 A CN105408100 A CN 105408100A CN 201580001415 A CN201580001415 A CN 201580001415A CN 105408100 A CN105408100 A CN 105408100A
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CN
China
Prior art keywords
drift
pressurized plane
compressed
compression molding
hole
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Pending
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CN201580001415.3A
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Chinese (zh)
Inventor
重久大麿
福田雅彦
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Idemitsu Kosan Co Ltd
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Idemitsu Kosan Co Ltd
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Publication of CN105408100A publication Critical patent/CN105408100A/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C33/00Moulds or cores; Details thereof or accessories therefor
    • B29C33/38Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/006Pressing and sintering powders, granules or fibres
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32Component parts, details or accessories; Auxiliary operations
    • B29C43/36Moulds for making articles of definite length, i.e. discrete articles
    • B29C43/361Moulds for making articles of definite length, i.e. discrete articles with pressing members independently movable of the parts for opening or closing the mould, e.g. movable pistons
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B30PRESSES
    • B30BPRESSES IN GENERAL
    • B30B11/00Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses
    • B30B11/02Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space
    • B30B11/022Presses specially adapted for forming shaped articles from material in particulate or plastic state, e.g. briquetting presses, tabletting presses using a ram exerting pressure on the material in a moulding space whereby the material is subjected to vibrations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B30PRESSES
    • B30BPRESSES IN GENERAL
    • B30B15/00Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/0005Details of, or accessories for, presses; Auxiliary measures in connection with pressing for briquetting presses
    • B30B15/0017Deairing means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B30PRESSES
    • B30BPRESSES IN GENERAL
    • B30B15/00Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/02Dies; Inserts therefor; Mounting thereof; Moulds
    • B30B15/022Moulds for compacting material in powder, granular of pasta form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B30PRESSES
    • B30BPRESSES IN GENERAL
    • B30B15/00Details of, or accessories for, presses; Auxiliary measures in connection with pressing
    • B30B15/06Platens or press rams
    • B30B15/065Press rams
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C43/00Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
    • B29C43/32Component parts, details or accessories; Auxiliary operations
    • B29C43/36Moulds for making articles of definite length, i.e. discrete articles
    • B29C43/361Moulds for making articles of definite length, i.e. discrete articles with pressing members independently movable of the parts for opening or closing the mould, e.g. movable pistons
    • B29C2043/3615Forming elements, e.g. mandrels or rams or stampers or pistons or plungers or punching devices
    • B29C2043/3628Forming elements, e.g. mandrels or rams or stampers or pistons or plungers or punching devices moving inside a barrel or container like sleeve

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)
  • Press-Shaping Or Shaping Using Conveyers (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)

Abstract

The invention provides a compression molding device, which comprises: a compression molding die having a through-hole, wherein a contact angle of water on an inner circumferential surface of the through-hole is 80 degrees or more; and a 1 st punch and a 2 nd punch each provided with a pressing surface for pressing the powder material by being inserted from different through-hole inlets of the through-holes, and a contact angle of water of the pressing surface is 80 degrees or more.

Description

Compression molding apparatus and be compressed into the manufacture method of body
Technical field
The present invention relates to compression molding apparatus and be compressed into the manufacture method of body.
Background technology
In the past, powder filler material in the working chamber of compression molding die is adopted and the method carried out compressing with drift and be shaped.
In addition, in recent years, have studied the method for the dusty material of the middle organic materials used such as electronic equipment being carried out compression molding.The organic layer arranged between the pair of electrodes of such organic electronic material element is formed by heating in vacuum evaporation usually.This is because, the organic element material added in vapor deposition source is generally Powdered, if but Powdered, then produce that charging efficiency is low, treatability poor, the powder problem of dispersing in addition.
Prior art document
Patent document
Patent document 1: KR published patent 10-2009-0097318 publication
Summary of the invention
Invent problem to be solved
The object of this invention is to provide and material can be suppressed after the compression molding of dusty material from the compression molding apparatus that formed body is partly peeled off or powder disperses from formed body surface and the manufacture method that is compressed into body.
For solving the scheme of problem
According to a mode of the present invention, provide a kind of compression molding apparatus, it possesses compression molding die and the 1st drift and the 2nd drift,
Described compression molding die has through hole and the contact angle of the water of the inner peripheral surface of described through hole is more than 80 degree,
Described 1st drift and the 2nd drift are respectively arranged with pressurized plane,
Described pressurized plane is used for inserting from the through hole entrance different from each other of described through hole respectively and pressurizeing to dusty material,
And the contact angle of the water of described pressurized plane is more than 80 degree.
In addition, according to another way of the present invention, a kind of compression molding apparatus is provided, it possess there is through hole compression molding die, be provided with the 1st drift of the 1st pressurized plane of the organic material contact be configured in described through hole and be provided with the 2nd drift with the 2nd pressurized plane of the organic material contact be configured in described through hole, the contact angle of the water of at least one in the inner peripheral surface of described 1st pressurized plane, described 2nd pressurized plane and described through hole is more than 80 degree.
In addition, according to another way of the present invention, there is provided a kind of manufacture method being compressed into body, it has following operation: by from be arranged at compression molding die through hole side insert the 1st drift the 1st pressurized plane towards described through hole inside and by the 1st drift insert operation;
The operation of powder filler material in described through hole;
By from be arranged at described compression molding die described through hole opposite side insert the 2nd drift the 2nd pressurized plane towards described through hole inside and by the 2nd drift insert, make the 1st pressurized plane of itself and described 1st drift facing, thus the operation of described 2nd pressurized plane forming shaped room by the inner peripheral surface of described through hole, described 1st pressurized plane of described 1st drift and described 2nd drift; With
The operation between described 1st pressurized plane and described 2nd pressurized plane, described dusty material compressed,
The contact angle of the water of described 1st pressurized plane, described 2nd pressurized plane and described inner peripheral surface is more than 80 degree.
According to compression molding apparatus of the present invention and the manufacture method being compressed into body, after the compression molding of dusty material, material can be suppressed partly to peel off from formed body or powder disperses from formed body surface.
Accompanying drawing explanation
Fig. 1 is the schematic partial cross-sectional view of the formation of the compression molding apparatus represented described in an embodiment.
Fig. 2 A is the figure that the manufacture method being compressed into body implemented the compression molding apparatus used described in above-mentioned embodiment is described.
Fig. 2 B is the figure that the manufacture method being compressed into body implemented the compression molding apparatus used described in above-mentioned embodiment is described.
Fig. 2 C is the figure that the manufacture method being compressed into body implemented the compression molding apparatus used described in above-mentioned embodiment is described.
Fig. 2 D is the figure that the manufacture method being compressed into body implemented the compression molding apparatus used described in above-mentioned embodiment is described.
Fig. 2 E is the figure that the manufacture method being compressed into body implemented the compression molding apparatus used described in above-mentioned embodiment is described.
Fig. 3 A is the figure be described the manufacture method being compressed into body different from the manufacture method being compressed into body illustrated in Fig. 2 A ~ Fig. 2 E.
Fig. 3 B is the figure be described the manufacture method being compressed into body different from the manufacture method being compressed into body illustrated in Fig. 2 A ~ Fig. 2 E.
Fig. 3 C is the figure be described the manufacture method being compressed into body different from the manufacture method being compressed into body illustrated in Fig. 2 A ~ Fig. 2 E.
Fig. 4 is the chart being compressed into the relation of the molding hardness of body and the particle diameter of dusty material represented described in embodiment.
Fig. 5 is the chart being compressed into the relation of the molding hardness of body and the bulk density of dusty material represented described in embodiment.
Detailed description of the invention
< first embodiment >
(1) formation of compression molding apparatus
The schematic diagram of the compression molding apparatus 1 shown in Fig. 1 described in present embodiment.
The 2nd drift 4 that compression molding apparatus 1 possesses compression molding die 2, the 1st drift 3 and relatively arranges with the 1st drift 3.Compression molding apparatus 1 possesses basal part 10 further, is set up in upper frame 12 that 2 guide pillars 11 on basal part 10 are connected with the upper end of guide pillar 11 parallel to each other, between basal part 10 and upper frame 12 by the lower movable plate 13, middle part movable platen 14 and the upper movable plate 15 that support.As shown in Figure 1, lower movable plate 13, middle part movable platen 14 and upper movable plate 15 are arranged parallel to each other successively from basal part 10 side.In addition, lower movable plate 13, middle part movable platen 14 and upper movable plate 15 are according to arranging along the mode of guide pillar 11 separately movement in the vertical direction.In addition, lower movable plate 13, middle part movable platen 14 and upper movable plate 15 are formed according to the mode can carrying out movement by the vapour-pressure type driving mechanisms such as fluid pressure type driving mechanism, cylinder such as not shown hydraulic cylinder or the mechanical drive mechanism such as cam or crank mechanism.
Compression molding die 2 is installed on the substantially central portion of middle part movable platen 14 in removable mode.Compression molding die 2 has the through hole 21 of up/down perforation as shown in Figure 1.In this through hole 21, insert the 1st drift 3 and the 2nd drift 4, form the working chamber 22 being used for powder filler material in the inside of compression molding die 2.Working chamber 22 is in the to be formed shape being compressed into body.The shape of working chamber 22, the shape being namely compressed into body can be cylindric or oval column, and cross section can be polygon or the ellipses such as semicircle, fan-shaped, triangle, quadrangle.In addition, to be compressed into body can be solid also can be hollow body.
The dusty material be filled in working chamber 22 compresses from opposite directions pressurization by the 1st drift 3 and the 2nd drift 4.1st drift 3 is fixed on the upper surface of lower movable plate 13.1st drift 3 is according to be moved along the vertical direction by lower movable plate 13 thus the mode moved axially along through hole 21 is formed.1st drift 3 inserts from another through hole entrance 21b of through hole 21.2nd drift 4 is fixed on the lower surface of upper movable plate 15.2nd drift 4 is according to be moved along the vertical direction by upper movable plate 15 thus the mode moved axially along through hole 21 is formed.2nd drift 4 inserts from a through hole entrance 21a of through hole 21.1st drift 3 and the 2nd drift 4 are preferably slightly smaller than through hole 21 ground and are formed.Preferably form gap in the side of the 1st inserted drift 3 and between the side of the 2nd drift 4 and the inner peripheral surface 21c of through hole 21, the gas degassed from the dusty material in working chamber 22 is discharged by this gap.
In the 1st drift 3 and the respective end of the 2nd drift 4, be provided with the 1st pressurized plane 31 and the 2nd pressurized plane 41 that dusty material is pressurizeed.In present embodiment, the 1st pressurized plane 31 of the 1st drift 3 and the 2nd pressurized plane 41 of the 2nd drift 4 are smooth face.By the inner peripheral surface 21c forming shaped room 22 of the through hole 21 of the 1st pressurized plane 31 of the 1st drift 3, the 2nd pressurized plane 41 of the 2nd drift 4 and compression molding die 2.By under the state that is filled with dusty material in working chamber 22, carry out pressurizeing from above-below direction with the 1st drift 3 and the 2nd drift 4 and obtain being compressed into body.
The contact angle of the water of the inner peripheral surface 21c of the through hole 21 of the 1st pressurized plane 31 of the 1st drift 3, the 2nd pressurized plane 41 of the 2nd drift 4 and compression molding die 2 is more than 80 degree.The contact angle of water is set to and drips water droplet on each, the tangent line that the surface at the edge of water droplet is drawn and this face angulation.Therefore, this angle is the scope of 0 ° to 180 °.In addition, the contact angle of the water of the 1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c is preferably more than 80 degree and less than 120 degree, is more preferably more than 80 degree and less than 100 degree.In addition, the contact angle of the water of the inner peripheral surface 21c of so-called 1st pressurized plane 31 of the 1st drift 3, the 2nd pressurized plane 41 of the 2nd drift 4 and through hole 21,1st pressurized plane 31, the 2nd pressurized plane 41, inner peripheral surface 21c do not form film, for the contact angle of the water of the 1st pressurized plane 31, the 2nd pressurized plane 41, inner peripheral surface 21c, each is formed with film, it is the contact angle of the water on the surface of this film.
In present embodiment, the 1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c form nitride film, the contact angle of the water of these nitride faces is more than 80 degree.The contact angle of the water of these nitride faces is preferably more than 80 degree and less than 120 degree, is more preferably more than 80 degree and less than 100 degree.As above-mentioned nitride film, be preferably made up of the nitride be selected from TiAlN, titanium carbonitride, chromium nitride, titanium nitride, titanium silicon nitride and TiAlN silicon.Nitride film can be formed by physical vapour deposition (PVD) (PhysicalVaporDeposition, PVD) method or chemical vapour deposition (CVD) (ChemicalVaporDeposition, CVD) method etc.In present embodiment, above-mentioned nitride film is made up of the TiAlN by physical vaporous deposition film forming.Before the formation of nitride film, preferably by the clean surface of the 1st drift 3, the 2nd drift 4 and compression molding die 2.As purifying process, include, for example out surface grinding process, dipping and the ultrasonic washing process carried out in organic solvent etc., the bombardment processing etc. that utilizes argon ion etc., also these process combinations can be implemented.
In addition, in present embodiment, the center line average roughness Ra of the 1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c is preferably less than 0.5 μm, is more preferably less than 0.1 μm.If center line average roughness Ra is less than 0.5 μm, then after compression molding, dusty material becomes and is difficult to attachment on these faces, is inhibited from the stripping being compressed into body.In addition, the center line average roughness Ra of the inner peripheral surface 21c of so-called 1st pressurized plane 31 of the 1st drift 3, the 2nd pressurized plane 41 of the 2nd drift 4 and through hole 21,1st pressurized plane 31, the 2nd pressurized plane 41, inner peripheral surface 21c do not form film, for the center line average roughness Ra of the 1st pressurized plane 31, the 2nd pressurized plane 41, inner peripheral surface 21c, each is formed with film, be the center line average roughness Ra on the surface of this film.
Compression molding apparatus 1 preferably has the degas module from working chamber 22 interior Exhaust Gas, and at least one in preferred compressed shaping dies 2, the 1st drift 3 and the 2nd drift 4 has degas module.In present embodiment, the 1st drift 3 has the not shown vibrating device as degas module.The 1st drift 3 is inserted by the through hole entrance 21b from through hole 21, in the recess formed by the inner peripheral surface 21c of through hole 21 and the 1st pressurized plane 31 of the 1st drift 3 after powder filler material, utilize this vibrating device that the 1st drift 3 is vibrated, carry out degassed and outside to working chamber 22 is discharged from the dusty material of occupied state.
(2) manufacture method of body is compressed into
Then, the manufacture method being compressed into body of the dusty material implemented using compression molding apparatus 1 is described.
In Fig. 2 A ~ Fig. 2 E, to be compressed into body manufacture method each operation in the compression molding die 2 of compression molding apparatus 1, the 1st drift 3 and the 2nd drift 4 record, other formation is omitted.Use compression molding apparatus 1 and the manufacture method being compressed into body of present embodiment implemented is powder filler material, and with the method formed along the plus-pressure of single shaft.
First, as shown in Figure 2 A, by internally insertion the 1st drift 3 of the 1st pressurized plane 31 towards through hole 21.Now, the position that the 1st pressurized plane 31 arrives the prescribed depth size in through hole 21 is inserted into.This depth dimensions sets according to the gauge etc. being compressed into body.
Then, as shown in Figure 2 B, the inside powder filler material P of through hole 21 of bottom surface is being formed by the 1st pressurized plane 31.After powder filler material P, utilize above-mentioned vibrating device that the 1st drift 3 is vibrated, carry out degassed process.
Then, as that shown in fig. 2 c, by internally insertion 2nd drift 4 of the 2nd pressurized plane 41 towards through hole 21, make it relative with the 1st pressurized plane 31 of the 1st drift 3, thus by the inner peripheral surface 21c of through hole 21, the 1st pressurized plane 31 and the 2nd pressurized plane 41 forming shaped room 22.
Then, compressed by dusty material P between the 1st pressurized plane 31 and the 2nd pressurized plane 41, being shaped thus is compressed into body Q.In present embodiment, list the example that two pressure modes of moving simultaneously and dusty material P is carried out pressurize from both sides with the 1st drift 3 and the 2nd drift 4 carry out and be described, but be not limited to which.
Compression pressure is preferably more than 11MPa.In addition, the surface temperature of the 2nd pressurized plane 41 of the inner peripheral surface 21c of compression molding die 2, the 1st pressurized plane 31 of the 1st drift 3 and the 2nd drift 4 is preferably more than 10 DEG C.
Then, as shown in Figure 2 D, sandwich the state being compressed into body Q between the 1st pressurized plane 31 and the 2nd pressurized plane 41 of the 2nd drift 4 of the 1st drift 3 under, make the 1st drift 3 and the 2nd drift 4 increase mobile, body Q will be compressed into and extract from through hole 21.The rising of the 1st drift 3 and the 2nd drift 4 is moved and is preferably stopped in the position that the 1st pressurized plane 31 of the 1st drift 3 is consistent with the upper surface of compression molding die 2.1st drift 3 and the 2nd drift 4 preferably can not be risen mobile by the mode discharged quickly according to acting on the stress being compressed into body Q with low velocity.
Then, as shown in Figure 2 E, make the 2nd drift 4 increase mobile, will the upper surface open of body Q be compressed into.Afterwards, the body Q that is compressed into be placed on the 1st pressurized plane 31 is taken out.Preferred use so operates obtain be compressed into body Q to implement the manufacture method of organic EL element by organic EL element Material compression.
The dusty material P of present embodiment is organic EL element material, does not have the shaping additive such as mixed adhesive or lubricant.As long as the material used in organic EL element material organic EL element, just be not particularly limited, the electron transporting material etc. used in the hole transport ability material used in such as hole transmission layer, the main material used in luminescent layer, dopant material, electron transfer layer can be listed.In addition, organic EL element material also can be the mixing of multiple organic EL element material and form.
The average grain diameter D50 (median particle diameter) of the dusty material P of present embodiment is preferably less.The average grain diameter D50 of dusty material P more diminishes, and more can improve the hardness being compressed into body.The average grain diameter D50 of dusty material P is preferably less than 70 μm, is more preferably less than 45 μm, more preferably less than 30 μm.In the domain size distribution of dusty material P, the difference of preferred maximum particle diameter and minimum particle diameter is little.
In addition, the average grain diameter D50 of dusty material P meets above-mentioned preferred scope is suitable in the present embodiment.
(3) effect of present embodiment
In the compression molding apparatus 1 described in present embodiment, the working chamber 22 of powder filler material P is formed by the inner peripheral surface 21c of the through hole 21 of the 1st pressurized plane 31 of the 1st drift 3, the 2nd pressurized plane 41 of the 2nd drift 4 and compression molding die 2.1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c form nitride film, and the contact angle of water is more than 80 degree.Like this, in the compression molding apparatus 1 of present embodiment, pressurized compression under the state that dusty material P encloses at the bread by the contact angle of water being more than 80 degree.Consequently, after can suppressing compression molding, material partly to be peeled off or powder disperses from formed body surface from being compressed into body Q.On the other hand, if the 1st pressurized plane 31, the contact angle of the water of the 2nd pressurized plane 41 and inner peripheral surface 21c is lower than 80 degree, then material increases from the amount peeled off with being compressed into body segments or powder disperses from formed body surface, the weight being compressed into body after shaping reduces more than 10%, and weight reduces significantly.
In present embodiment, after powder filler material P, above-mentioned vibrating device is utilized to make the 1st drift 3 vibration carry out degassed process, the gas removing that can will contain in fill dusty material P.In addition, in present embodiment, be more than 11MPa by the compression pressure between the 1st pressurized plane 31 and the 2nd pressurized plane 41 during compressing powder material P.Consequently, the particle of dusty material P is filled each other more densely, and after can suppressing compression molding, material partly to be peeled off or powder disperses from formed body surface from being compressed into body Q.
In present embodiment, as dusty material, the organic EL element material listed not containing shaping additive is that example is illustrated.After shaping to be peeling etc. be compressed into body because its hardness is insufficient, produce and be compressed into the crackle of body etc. and be difficult to hold its weight exactly, the raising of the productivity ratio of organic EL element cannot be sought.On the other hand, the compress moulding method of compression molding apparatus 1 described according to the present embodiment and use compression molding apparatus 1, even if not containing shaping additive, material also can be suppressed partly to peel off or powder disperses from formed body surface from being compressed into body Q.Therefore, it is possible to reduce the number of times being compressed into body to vapor deposition source supply, the raising of the productivity ratio of organic EL element can be sought.
In addition, owing to being formed with nitride film on the 1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c, so the wearability in these faces can be improved.
< second embodiment >
In the explanation of the second embodiment, same symbol or title etc. marked to the inscape identical with the first embodiment and explanation omitted or simplifies.In addition, in the second embodiment, the material identical with the material illustrated in the first embodiment or compound can be used.
In the first embodiment, the 1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c are formed with nitride film, on the other hand, in this second embodiment, be formed three layers of stacked film formed in different.
In present embodiment, the inner peripheral surface 21c of the compression molding die 2 of compression molding apparatus 1, the 1st drift 3 and the 2nd drift 4, the 1st pressurized plane 31 and the 2nd pressurized plane 41 separately on form stacked film, the contact angle of the water of the face on its most top layer is more than 80 degree.In the present embodiment, the contact angle of water is also preferably more than 80 degree and less than 120 degree, is more preferably more than 80 degree less than 110 degree.
The stacked film of present embodiment is 3 layers of stacked film formed.Specifically, in the 1st pressurized plane 31, the 2nd pressurized plane 41 and inner peripheral surface 21c side, first the nitride film illustrated in above-mentioned first embodiment is formed, activation process is implemented to the surface of nitride film and forms active layer, and then form the fluorinated nitride layer containing fluorine carbon based compound on this active layer.
By carrying out the activation process for the formation of active layer, the dirt be attached on nitride film surface is decomposed and purifying, the active layer with molecular link chalaza is formed on nitride film surface, this molecular link chalaza adsorbs hydroxyl, reacts with the reactive group of fluorine carbon based compound and become easy bonding.
As activation process, be not particularly limited, as physical method, Corona discharge Treatment, plasma treatment, Ultraviolet radiation process, flame treatment etc. can be listed, as chemical method, the process, oxidizer treatment, ozone treatment etc. of flooding in the solution of at least one in acid and alkali can be listed.In these activation process, Corona discharge Treatment, plasma treatment, Ultraviolet radiation process, ozone treatment are owing to can prevent the damage on nitride film surface, so preferably, plasma treatment and the Ultraviolet radiation process efficiency being carried out activating in nitride film surface is high and preferred further.
Being formed in the fluorinated nitride layer on active layer, containing fluorine carbon based compound.Fluorine carbon based compound is by the chain position formed with fluorocarbons and formed with the reactive group of other material bondings.As the method forming fluorinated nitride layer, can list and such as the releasing agent containing fluorine carbon based compound is applied on active layer, and carry out the method for heat drying.
As fluorine carbon based compound, such as perfluoroalkyl silanes class, silane compound class etc. containing holo-fluorine polyester can be listed.
As perfluoroalkyl silanes class, following formula (1) or the compound represented by formula (2) can be listed.
CF 3(CF 2) nCH 2CH 2Si(OMe) m...(1)
CF 3(CF 2) nCH 2CH 2Si(OR) m...(2)
Wherein, in above-mentioned formula (1), n be 1,3,5 or 7, m be 2 or 3, Me be methyl or ethyl.
In addition, in above-mentioned formula (2), n be 1,3,5 or 7, m be 2 or 3, R be halogens.
As the object lesson of the compound represented by above-mentioned formula (1) or formula (2), CF can be listed 3(CF 2) 5cH 2cH 2si (OCH 3) 3(such as, the TSL8257 of MomentivePerformanceMaterialsInc.), CF 3(CF 2) 7cH 2cH 2si (OCH 3) 3(such as, the TSL8233 of MomentivePerformanceMaterialsInc.), CF 3(CF 2) 7cH 2cH 2si (OCH 3) 2(such as, the TSL8231 of MomentivePerformanceMaterialsInc. or the KBM7803 of SHIN-ETSU HANTOTAI's chemical industry), CF 3(CF 2) 7cH 2cH 2si (OC 2h 5) 3(such as, the AY43-158E of DowCorningTorayCo., Ltd.) etc.
Perfluoropolyether-modified amino silane, perfluoropolyether-modified polysilazane etc. are had in silane compound class containing holo-fluorine polyester.Specifically, KY-164, DAIKININDUSTRIES of such as SHIN-ETSU HANTOTAI's chemical industry can be listed, the Optool series etc. of ltd..
According to the present embodiment, except the effect brought by above-mentioned first embodiment, effect as following is also played.
By the contact angle of the most top layer of stacked film and the water on fluorinated nitride layer surface is set to more than 80 degree, if dusty material is carried out compression molding with the inner peripheral surface 21c of the through hole 21 of the 2nd pressurized plane 41 of the 1st pressurized plane 31 of the 1st drift 3 being formed with this stacked film, the 2nd drift 4 and compression molding die 2, then can to improve after suppressing compression molding material further from being compressed into the effect that body Q partly peels off or powder disperses from formed body surface.
< variation >
In addition, the present invention is not limited to above-mentioned embodiment, in the scope can reaching object of the present invention, also comprises distortion etc. shown below.
As long as the contact angle of the water of at least one in the inner peripheral surface of the 1st pressurized plane, above-mentioned 2nd pressurized plane and above-mentioned through hole is more than 80 degree, then also can adopt other method.In addition, as long as be more than 80 degree with the contact angle of the water in the face of organic material contact, then other method can also be adopted.Such as, at the inner peripheral surface of the 1st pressurized plane, above-mentioned 2nd pressurized plane, above-mentioned through hole or with on the face of organic material contact, the compound film of other kinds can be formed, also can implement chemical surface treatment or milled processed to adjust contact angle.
In addition, the formation of stacked film is not limited to the example that illustrates in above-mentioned embodiment.The layer different with active layer can be clamped between nitride film from fluorinated nitride layer, also the formation of active layer can be omitted thus make the direct stacked film formed by the bilayer that nitride film and fluoride are folded layer by layer and obtained.In addition the layer being arranged on the most surface of stacked film is also not limited to the layer containing fluorine carbon based compound, as long as the contact angle of water reaches the layer of more than 80 degree.
The degas module arranged in compression molding apparatus 1 is not limited to vibrating device, such as, also can be ultrasonic generator, knocking device, vacuum degasser.As degas module, as long as the dusty material can filled from working chamber 22 carries out degassed.In addition, degas module is not limited to be arranged on the situation in the 1st drift 3, also can be arranged in the 2nd drift 4 or compression molding die 2.
Also taper WEDM can be implemented to the through hole entrance 21a of the through hole 21 of compression molding die 2.The mode that this taper WEDM expands from the inside of through hole 21 towards through hole entrance 21a according to aperture is implemented.In this taper WEDM part, also the contact angle of preferred water is set to more than 80 degree, such as, be preferably formed nitride film as described above.In addition, also taper WEDM can be implemented to through hole entrance 21b.
In addition, be not limited to from compression molding die 2 method for pulling out the method that illustrates above-mentioned embodiment by being compressed into body Q.
Such as, as shown in Figure 3A, compression molding die 2 is made to decline mobile.As shown in Figure 3 B, the decline of compression molding die 2 is moved and is preferably stopped in the position that the upper surface of compression molding die 2 is consistent with the 1st pressurized plane 31 of the 1st drift 3.Compression molding die 2 preferably can not be declined mobile by the mode discharged quickly according to acting on the stress being compressed into body Q with low velocity.Then, as shown in Figure 3 C, make the 2nd drift 4 increase mobile, will the upper surface open of body Q be compressed into.Afterwards, the body Q that is compressed into be placed on the 1st pressurized plane 31 is taken out.
Compress moulding method is not limited to the method illustrated in above-mentioned embodiment.Such as also can carry out compression molding by floating die mode.In floating die mode, pressurize with the 2nd drift 4, between the inner peripheral surface 21c and dusty material of the through hole 21 of compression molding die 2, frictional force increases gradually, and be greater than the support force of compression molding die 2 if become, then compression molding die 2 declines together with middle part movable platen 14.Now, the 1st drift 3 becomes and relatively rises.Afterwards, make the 2nd drift 4 increase, body will be compressed into and take out.According to such floating die mode, the density adjustment be compressed on the thickness direction of body can be carried out.In addition, the list pressure mode etc. that extraction mode, only the 2nd drift 4 decline can be adopted.When adopting these modes, be set to more than 80 degree by the contact angle of the water of the inner peripheral surface 21c of the through hole 21 by the 1st pressurized plane 31 of the 1st drift 3, the 2nd pressurized plane 41 of the 2nd drift 4 and compression molding die 2, after also can suppressing compression molding, material partly to be peeled off or powder disperses from formed body surface from being compressed into body Q.
Embodiment
Below, embodiment is described, but the present invention is not by the restriction of these embodiments.
(embodiment 1)
By the compression molding apparatus 1 described in above-mentioned embodiment, be 20.71 μm by average grain diameter D50, bulk density is that the dusty material of 0.33g/ml carries out compression molding.Measure the molding hardness being compressed into body described in embodiment 1.The characteristic of dusty material shown in table 1 and molding hardness.In addition, average grain diameter D50 is median particle diameter.Median particle diameter is that the particle diameter measured in the laser diffraction and scattering formula grain size analysis MT3300II of Nikkiso Company Limited is expressed as cumulative distribution, is measured by this cumulative distribution.
Bulk density uses the apparent specific gravity (gd) of cylinder well Physicochemical apparatus Co., Ltd. to measure meter JIS-K-5101 and measures.
The molding hardness being compressed into body installs IMADACO. on the vertical hand-operated measurement support SVH-1000N of IMADACO., LTD., and the popular digital force gauge DS2-50N of LTD. measures.
(embodiment 2)
Use the dusty material that average grain diameter D50 is 41.15 μm, bulk density is 0.44g/ml, in addition, make similarly to Example 1 and be compressed into body, measure molding hardness.Show the result in table 1.
(embodiment 3)
Use the dusty material that average grain diameter D50 is 65.27 μm, bulk density is 0.44g/ml, in addition, make similarly to Example 1 and be compressed into body, measure molding hardness.Show the result in table 1.
(comparative example 1)
Use the dusty material that average grain diameter D50 is 92.81 μm, bulk density is 0.74g/ml, in addition, make similarly to Example 1 and be compressed into body, measure molding hardness.Show the result in table 1.
By shown in Figure 4 for the chart being compressed into the relation of the molding hardness of body and the particle diameter of dusty material represented described in embodiment and comparative example, will represent that the chart being compressed into the relation of the molding hardness of body and the bulk density of dusty material is shown in Figure 5.
In addition, in table 1, Fig. 4 and Fig. 5, molding hardness represents with normalized value.That is, in the present embodiment, by the measured value normalization divided by the measured value of the molding hardness of comparative example 1 respectively of the molding hardness of embodiment 1 ~ 3 and comparative example 1.
[table 1]
As the result as shown in table 1 and Fig. 4, the average grain diameter of dusty material is less, and molding hardness becomes higher.
In addition, as the result as shown in table 1 and Fig. 5, the bulk density of dusty material is less, and molding hardness becomes higher.
(being compressed into the release property of body)
The inner peripheral surface of the pressurized plane of the 1st drift of compression molding apparatus, the pressurized plane of the 2nd drift and the through hole of compression molding die is formed the fluorinated nitride layer containing fluorine carbon based compound.The contact angle of the water of the fluorinated nitride layer in the compression molding apparatus of embodiment 4 ~ 7 and comparative example 2 ~ 3 is adjusted to the value shown in table 2 respectively.This compression molding apparatus is used to carry out compression molding to dusty material.By the outward appearance being compressed into body after the visual confirmation demoulding.The confirmation result of outward appearance is shown in Table 2.In table 2, " B " represents that material is to peel off with being compressed into body segments or powder disperses from compression molding surface, and " A " represents and do not produce such stripping or disperse.
[table 2]
If the contact angle of the water in the known face contacted with dusty material is more than 80 degree, then the release property being compressed into body is excellent.The contact angle of known water also can be larger, more than 80 degree, also can obtain good release property in the scope of less than 100 degree.
Symbol description
1... compression molding apparatus, 2... compression molding die, 21... through hole, 21a, 21b... through hole entrance, 21c... inner peripheral surface, 22... working chamber, 3... the 1st drift, 31... the 1st pressurized plane, 4... the 2nd drift, 41... the 2nd pressurized plane, P... dusty material, Q... are compressed into body.

Claims (20)

1. a compression molding apparatus, it possesses compression molding die and the 1st drift and the 2nd drift,
Described compression molding die has through hole and the contact angle of the water of the inner peripheral surface of described through hole is more than 80 degree,
Described 1st drift and the 2nd drift are respectively arranged with pressurized plane,
Described pressurized plane is used for inserting from the through hole entrance different from each other of described through hole respectively and pressurizeing to dusty material,
And the contact angle of the water of described pressurized plane is more than 80 degree.
2. a compression molding apparatus, it possess there is through hole compression molding die, be provided with the 1st drift of the 1st pressurized plane of the organic material contact be configured in described through hole and be provided with the 2nd drift with the 2nd pressurized plane of the organic material contact be configured in described through hole, the contact angle of the water of at least one in the inner peripheral surface of described 1st pressurized plane, described 2nd pressurized plane and described through hole is more than 80 degree.
3. according to compression molding apparatus according to claim 1 or claim 2, wherein, described contact angle is more than 80 degree and less than 120 degree.
4. according to compression molding apparatus according to claim 1 or claim 2, wherein, described contact angle is more than 80 degree and less than 100 degree.
5. the compression molding apparatus according to any one of claim 1 to claim 4, wherein, the inner peripheral surface of described through hole and the center line average roughness Ra of described pressurized plane are less than 0.5 μm.
6. according to claim 1 to the compression molding apparatus according to any one of claim 5, wherein, be formed with nitride film at the inner peripheral surface of described through hole and described pressurized plane.
7. compression molding apparatus according to claim 6, wherein, described nitride film is made up of the nitride be selected from TiAlN, titanium carbonitride, chromium nitride, titanium nitride, titanium silicon nitride and TiAlN silicon.
8. compression molding apparatus according to claim 7, wherein, described nitride film is made up of TiAlN.
9. the compression molding apparatus according to any one of claim 6 to claim 8, wherein, the fluorinated nitride layer containing fluorine carbon based compound is formed on described nitride film.
10. the compression molding apparatus according to any one of claim 1 to claim 9, wherein, at least one in described compression molding die, described 1st drift and described 2nd drift has from the described inner peripheral surface by described through hole, the degas module of the interior Exhaust Gas of working chamber that formed with the described pressurized plane of described 1st drift and described 2nd drift.
11. 1 kinds of manufacture methods being compressed into body, it has following operation: the 1st pressurized plane of the 1st drift inserted the side from the through hole being arranged at compression molding die is the operation inserted by the 1st drift towards the inside of described through hole;
The operation of powder filler material in described through hole;
By from be arranged at described compression molding die described through hole opposite side insert the 2nd drift the 2nd pressurized plane towards described through hole inside and by the 2nd drift insert, make the 1st pressurized plane of itself and described 1st drift facing, thus the operation of described 2nd pressurized plane forming shaped room by the inner peripheral surface of described through hole, described 1st pressurized plane of described 1st drift and described 2nd drift; With
The operation between described 1st pressurized plane and described 2nd pressurized plane, described dusty material compressed,
The contact angle of the water of described 1st pressurized plane, described 2nd pressurized plane and described inner peripheral surface is more than 80 degree.
12. manufacture methods being compressed into body according to claim 11, wherein, described contact angle is more than 80 degree and less than 120 degree.
13. manufacture methods being compressed into body according to claim 11, wherein, described contact angle is more than 80 degree and less than 100 degree.
14. manufacture methods being compressed into body according to any one of claim 11 to claim 13, wherein, before carrying out the operation compressed, have the degassed treatment process of described dusty material between described 1st pressurized plane and described 2nd pressurized plane.
15. manufacture methods being compressed into body according to any one of claim 11 to claim 14, wherein, between described 1st pressurized plane and described 2nd pressurized plane, the compression pressure carried out in the operation compressed is more than 11MPa.
16. manufacture methods being compressed into body according to any one of claim 11 to claim 15, wherein, there is following operation: between described 1st pressurized plane and described 2nd pressurized plane, described dusty material compressed and under the state being compressed into body formed, make described 1st drift and described 2nd drift move and be extracted from described through hole by the described body that is compressed into clipping.
17. manufacture methods being compressed into body according to any one of claim 11 to claim 15, wherein, there is following operation: between described 1st pressurized plane and described 2nd pressurized plane, described dusty material compressed and under the state being compressed into body formed, make described compression molding die move and be extracted from described through hole by the described body that is compressed into clipping.
18. manufacture methods being compressed into body according to any one of claim 11 to claim 17, wherein, not containing shaping additive in described dusty material.
19. manufacture methods being compressed into body according to any one of claim 11 to claim 18, wherein, described dusty material is organic electroluminescent element material.
20. manufacture methods being compressed into body according to claim 19, wherein, described dusty material is that multiple organic electroluminescent element material mixes.
CN201580001415.3A 2014-03-31 2015-03-19 Compression molding apparatus and method for manufacturing compression molded article Pending CN105408100A (en)

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