CN104690811A - Hot pressing mold easy to de-mold and method for preparing porous structure ceramic by hot pressing mold - Google Patents

Hot pressing mold easy to de-mold and method for preparing porous structure ceramic by hot pressing mold Download PDF

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Publication number
CN104690811A
CN104690811A CN201510114751.0A CN201510114751A CN104690811A CN 104690811 A CN104690811 A CN 104690811A CN 201510114751 A CN201510114751 A CN 201510114751A CN 104690811 A CN104690811 A CN 104690811A
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CN
China
Prior art keywords
hot pressing
mold
guide pillar
down head
push
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Pending
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CN201510114751.0A
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Chinese (zh)
Inventor
周有福
王坤
王志光
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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Priority to CN201510114751.0A priority Critical patent/CN104690811A/en
Publication of CN104690811A publication Critical patent/CN104690811A/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00Moulds; Cores; Mandrels
    • B28B7/16Moulds for making shaped articles with cavities or holes open to the surface, e.g. with blind holes
    • B28B7/18Moulds for making shaped articles with cavities or holes open to the surface, e.g. with blind holes the holes passing completely through the article
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/02Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
    • B28B3/021Ram heads of special form
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B3/00Producing shaped articles from the material by using presses; Presses specially adapted therefor
    • B28B3/02Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form
    • B28B3/08Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein a ram exerts pressure on the material in a moulding space; Ram heads of special form with two or more rams per mould
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B7/00Moulds; Cores; Mandrels
    • B28B7/28Cores; Mandrels

Abstract

The invention discloses a hot pressing mold. The hot pressing mold comprises an upper pressing head, a combined mold sleeve, a lower pressing head and a guide column, wherein the combined mold sleeve comprises an outer mold and an inner mold. With the adoption of the hot pressing mold, the de-molding is convenient to carry out, and the mold is prevented from cracking and damaging in the de-molding process. Structure ceramic prepared by using the hot pressing mold has high density and good mechanical performance; the obtained large-size porous structure ceramic has the advantages of accurate pore diameter and size. The invention further discloses a method for preparing the porous structure ceramic by the hot pressing mold. The method comprises the following steps: assembling a hydraulic mold; sintering the assembled hot pressing mold for 1-3 hours under the conditions that the pressure is 10Mpa-40Mpa the temperature is 1800-2000 DEG C in a non-active atmosphere; and cooling the sintered hot pressing mold to the room temprature, and de-molding and removing the guide column to obtain the porous structure ceramic.

Description

Easy demoulding hot pressing die and prepare porous structure ceramic method
Technical field
The application belongs to structural ceramics field, in particular to a kind of easy demoulding hot pressing die and prepare the method for porous structure ceramic.
Background technology
Structural ceramics is as carborundum, titanium carbide, zirconium carbide, silicon nitride etc., there is hardness high, the advantages such as high temperature resistant, corrosion-resistant, good mechanical property, especially it can adapt to the working environment in high temperature, intense radiation, therefore has a wide range of applications in nuclear energy.
Silicon carbide ceramics is a kind of structural ceramics of function admirable, and this sentences silicon carbide ceramics is that example launches explanation.Carborundum itself is a kind of intrinsic low neutron activation material.The intensity of carborundum can reach 1000Mpa.Until 1900 DEG C there is not thermal creep.Carborundum has good thermal conductivity, and neutron absorption cross-section is little, can meet the requirement as the structural material stopping fission product in reactor.Prepare structural ceramics at present and have a variety of method, comprising: hot pressed sintering, solid-phase sintering with no pressure, liquid-phase sintering with no pressure, HIP sintering etc.Wherein, pressureless sintering silicon carbide ceramic needs to add boride as sintering aid, boron energy and thermal neutron are dispersed nuclear reaction according to certain reaction cross-section and are produced lithium and helium, thus affect the mechanical performance of whole material, and biscuit can obviously shrink in sintering process, be difficult to the precision ensureing large scale goods and axial aperture.And high temperature insostatic pressing (HIP) is high to equipment requirement, and need wrap up biscuit, be unfavorable for industrial applications, at present also in the laboratory research stage.Hot pressed sintering can prepare the high and silicon carbide ceramics of good mechanical performance of density at lower temperature, and common die, for the preparation of disc-shaped ceramic, is not suitable for preparing complex-shaped, to have internal gutter structural ceramics goods.Easily there is mold sticking simultaneously, cause the demoulding more difficult.
Summary of the invention
According to an aspect of the application, provide a kind of hot pressing die, can prepare aperture, size is accurate, density is high and the big size porous structural ceramics of good mechanical performance, this hot pressing die has the advantage of the easy demoulding.
Described hot pressing die, is characterized in that, comprises seaming chuck, combination die sleeve, push-down head and guide pillar;
Described combination die cover top possesses upper shed and coordinates with described seaming chuck, and described external mold bottom possesses under shed and coordinates with described push-down head;
The one side that described seaming chuck coordinates with described combination die sleeve possesses hole;
The one side that described push-down head coordinates with described combination die sleeve possesses hole;
Described combination die sleeve comprises external mold and internal mold, and described outer mold is for hollow structure, and described inner mold is for hollow structure, and described external mold inwall and described internal mold outer wall fit;
Described guide pillar is arranged in the hollow structure of described internal mold, and described guide pillar two ends insert the hole of described seaming chuck and the hole of described push-down head respectively.
Guide pillar is possessed in hot pressing die described in the application, guide pillar takies the space in mould in advance, mutually separate between guide pillar, ceramic powder is loaded in remaining space between guide pillar, after oversintering, the demoulding, inside the structural ceramics obtained, be inlaid with through guide pillar, guide pillar is removed, can obtain porous structure ceramic, its pore structure, hole dimension, pore size distribution decide by the shape of guide pillar, size and the arrangement in described hot pressing die thereof.By designing the shape of guide pillar, size and arrangement thereof, corresponding porous structure ceramic can be obtained.
The combination die sleeve of hot pressing die described in the application comprises external mold and internal mold, and after sintering, during the demoulding, external mold can be separated with internal mold, is therefore easy to the demoulding, removes the internal mold being coated on structural ceramics outside after the demoulding again.By adopting the combination die sleeve of external mold and internal mold composition, the demoulding can be made more for convenience, and reduce mould and to burst apart in knockout course breaking-up.
Preferably, the one side that described push-down head coordinates with described combination die sleeve possesses projection structure, and described projection structure is inserted and closed the under shed of described combination die sleeve;
The one side that described seaming chuck coordinates with described combination die sleeve possesses lower convexity structure, and described lower convexity structure is inserted and closed the upper shed of described combination die sleeve.
In the application, described push-down head and the size and dimension of described seaming chuck by matching with described combination die sleeve inside, go deep into described combination die sleeve and closely cooperate with described combination die cover, can better seal combination die sleeve inner space, be beneficial to and obtain that shape is complete, the structural ceramic product of surfacing.
Preferably, described hot pressing die, also comprises and is arranged at Upper gasket in described combination die sleeve and lower gasket;
Described Upper gasket contacts with described seaming chuck, and described Upper gasket possesses the hole corresponding with the hole in described seaming chuck;
Described lower gasket contacts with described push-down head, and described lower gasket possesses the hole corresponding with the hole in described push-down head.
Those skilled in the art can select whether to adopt pad, can realize the technique effect of the application when not using pad; Use pad can reduce the requirement on machining accuracy of other associated components, be more conducive to operation simultaneously, seaming chuck and push-down head and ceramic powder can be separated by pad, and close guide pillar and the gap between seaming chuck and push-down head further, and external mold and the gap between seaming chuck and push-down head.The introducing of pad can make the micro-pore face of the structural ceramics prepared more smooth.
Preferably, described guide pillar one end inserts the hole of described Upper gasket and described seaming chuck successively, and the described guide pillar other end inserts the hole of described lower gasket and described push-down head successively.
Preferably, described guide pillar be cylinder and its axis being parallel in the axis of the hollow structure of described internal mold.
Preferably, described guide pillar is no less than 7, and the hole number of described Upper gasket, lower gasket, seaming chuck and push-down head is equal with guide pillar quantity.
Art technology people can the shape of hollow structure of size design internal mold of structural ceramics as required.The hole of the hole structural ceramics as required of seaming chuck and push-down head is designed, and size and the quantity of its guide pillar also determine thus.Further preferably, described guide pillar is 37 and is hexagonal accumulation arrangement in cross section, and the hole number of described Upper gasket, lower gasket, seaming chuck and push-down head is equal with guide pillar quantity.
Further preferably, described guide pillar inserts and closes the hole of described Upper gasket, lower gasket, seaming chuck and push-down head.The diameter of guide pillar determines the aperture of structural ceramics, and therefore those skilled in the art can select the diameter of guide pillar by the aperture needed, and the diameter of conventional guide pillar is: 8 ~ 18mm.The mould of the application can prepare the structural ceramics in the hole of large-size.
As a preferred embodiment of the application, described combination die sleeve is made up of external mold and internal mold.
As a preferred embodiment of the application, the hollow structure of described external mold is cylinder; The profile of described internal mold is the hollow circular cylinder corresponding to the hollow structure of external mold.
The hollow structure of described internal mold is six prisms.
Described lower convexity structure and projection structure are six prisms matched with inner membrance hollow structure.
In the application, the inner wall shape of described external mold and size, match with the outer wall shape and size of described internal mold, is assemblied in by described internal mold in described external mold, namely obtains described combination die sleeve.Described internal mold, according to concrete shape, can be overall, also can be formed by multiple piece piece.The internal mold of multiple piece piece, no longer need to apply larger power during the demoulding structural ceramics is released from mould, and make it be separated with structural ceramics respectively to outside force multiple parts of internal mold simply, the damage of structural ceramics and mould can also be avoided while being therefore easy to the demoulding.
Preferably, the flap internal mold that described internal mold is no less than 2 by quantity forms.
As a preferred embodiment of the application, the hollow structure of described internal mold is six prisms; Described internal mold is made up of 6 flap internal molds.Further preferably, described flap internal mold side is plane, and described plane forms a side in six sides of described six prisms, and the face relative with described plane is the face of cylinder and the cylinder of the hollow structure of radian and radius and described external mold is identical.
Preferably, described external mold is identical with described internal mold length vertically.
Preferably, described seaming chuck possesses fixed structure away from the one side of described combination die sleeve; Described push-down head possesses fixed structure away from the one side of described combination die sleeve.
Those skilled in the art can be beneficial to operation according to actual conditions designed, designed, the described fixed structure of seaming chuck and push-down head of taking, load and unload, and can adopt corresponding described fixed structure according to demoulding equipment.As a preferred version, the described fixed structure structure that to be seaming chuck and push-down head extend from surface away from the one side of described combination die sleeve, is beneficial to handling and makes to coordinate with other equipment.
Preferably, described Upper gasket, lower gasket, seaming chuck, push-down head, internal mold and external mold adopt the graphite material that Shore hardness is greater than 75; Described guide pillar adopts Shore hardness to be not more than the graphite material of 75.
Those skilled in the art can select the material not affecting arbitrarily structural ceramics synthesis to manufacture guide pillar, and because guide pillar needs to obtain corresponding hole by being removed, therefore comparatively suitable scheme is select graphite that hardness is lower as the material of guide pillar.
Further preferably, described Upper gasket, lower gasket, seaming chuck, push-down head, internal mold, flap internal mold, external mold adopt ISO-68 graphite material.
According to another aspect of the application, provide the method adopting described hot pressing die to prepare porous structure ceramic, comprise the steps:
A) described external mold and described internal mold are assembled into combination die sleeve, described push-down head and described combination die cover are assembled together, described lower gasket is put into the upper surface of described push-down head, described guide pillar is passed described lower gasket and inserts in the hole of described push-down head, ceramic powder containing sintering aid is loaded in described hot pressing die, respectively described Upper gasket and seaming chuck are loaded in described combination die sleeve successively, obtain the hot pressing die assembled;
B) by step a) described in the hot pressing die assembled under pressure 10 ~ 40Mpa, temperature 1800 ~ 2000 DEG C, inert atmosphere, sinter 1 ~ 3 hour;
C) by step b) the middle hot pressing die cool to room temperature sintered, de-external mold, obtains the structural ceramics that outside is coated with internal mold, inside is inlaid with guide pillar; Removing internal mold and guide pillar, obtain described porous structure ceramic.
Preferably, step a) pieces together for described flap internal mold is put into external mold successively the combination die sleeve that hollow structure is six prisms, described push-down head and described combination die cover are assembled together, described guide pillar is inserted in the hole of described push-down head, described lower gasket is put into the described push-down head upper surface of described hot pressing die, ceramic powder containing sintering aid is loaded in described hot pressing die, respectively described Upper gasket and seaming chuck are loaded in described combination die sleeve, obtain the hot pressing die assembled.
Preferably, step a) described in containing sintering aid ceramic powder in, the mass percentage of sintering aid is 1 ~ 5%.
Preferably, step a) described in the particle diameter of ceramic powder containing sintering aid be no more than 150 microns.
Preferably, step a) described in containing the ceramic powder of sintering aid, by ceramic powder and sintering aid mixs, grinding, dry, sieve and obtain.
Preferably, step a) described in load in described hot pressing die containing the ceramic powder of sintering aid before, the inner surface first contacted with ceramic powder at hot pressing die applies bn slurry.
Abundant mixed sintering auxiliary agent and ceramic powder, can give full play to sintering aid to the synthesis of structural ceramics and shaping booster action.Grind and sieve while sintering aid and ceramic powder can be made to mix, its granularity is less also more even, is beneficial to and obtains the better more stable structure pottery of performance.Those skilled in the art can select any-mode to grind the mixture of ceramic powder and sintering aid, comparatively easy mode is ball milling, for obtaining better effect, usually adds medium, this medium is selected do not react with system and be beneficial to the material of removal, and comparatively economic medium is ethanol.As a preferred version, described attrition process adopts ball milling method, take ethanol as medium, rotational speed of ball-mill 200 ~ 500rpm, Ball-milling Time 10 ~ 30 hours; Described screening process sieve gets the powder of wherein less than 150 microns.Dry run is removing medium ethanol and/or other volatilizable components.
Preferably, step b) for by step a) described in the hot pressing die assembled under pressure 15 ~ 30Mpa, temperature 1850 ~ 1980 DEG C, inert atmosphere, sinter 1.5 ~ 2.5 hours.Those skilled in the art can select the inert atmosphere do not reacted with ceramic powder and mould arbitrarily to sinter, and comparatively common inert atmosphere is nitrogen, helium, argon gas.Preferably, described inert atmosphere is one or more in nitrogen, helium, argon gas.
Those skilled in the art can adopt distinct methods to remove guide pillar, comparatively the method for economical and convenient is that physics cuts, for the columned guide pillar being embedded in structural ceramics inside, typical method is by rig, adopts the drill bit suitable with guide pillar diameter guide pillar part to be drilled through.As a preferred version, step c) described in remove the process of guide pillar, be drilled through the described guide pillar part be inlaid with in the structural ceramics of guide pillar to realize by rig.
By the hot pressing die of the application, adopt the method preparing porous structure ceramic of the application, can prepare the porous structure ceramic of different hole dimension, pore structure, pore size distribution, simultaneously the easily demoulding, porous structure ceramic product's dimensional precision is high, avoids aft-loaded airfoil.
The beneficial effect that the application can produce at least comprises:
1) demoulding more for convenience, reduces mould and to burst apart in knockout course breaking-up.
2) the high and good mechanical performance of the structural ceramics density prepared.
3) aperture, accurate in size big size porous structural ceramics can be prepared.
Accompanying drawing explanation
Fig. 1 is the cross-sectional schematic in a kind of embodiment of the application's hot pressing die.
Fig. 2 is seaming chuck elevational schematic view (a) in a kind of embodiment of the application's hot pressing die and schematic side view (b).
Fig. 3 is push-down head schematic side view (a) in a kind of embodiment of the application's hot pressing die and schematic top plan view (b).
Fig. 4 is guide pillar schematic side view (a) in a kind of embodiment of the application's hot pressing die and schematic top plan view (b).
Fig. 5 is flap internal mold schematic side view (a) in a kind of embodiment of the application's hot pressing die and schematic top plan view (b).
Fig. 6 is the combination die sleeve schematic top plan view in a kind of embodiment of the application's hot pressing die.
Mark in accompanying drawing is specific as follows:
10-seaming chuck; 12-combines die sleeve; 120-flap internal mold; 122-external mold; 14-push-down head; 16-guide pillar; 18-Upper gasket; 19-lower gasket.
Detailed description of the invention
Below by embodiment in detail the application is described in detail, but the application is not limited to these embodiments.
If no special instructions, raw material in embodiment is all bought by commercial sources, wherein seaming chuck, flap internal mold, external mold, push-down head, Upper gasket and lower gasket all adopt to buy and process from the ISO-68 graphite material of Japanese Japan (TOYO) company, and guide pillar employing is the SMF650 high purity graphite of 68.6MPa purchased from Shanghai Ying Mei graphite product Co., Ltd compression strength.
do as detailed below to the hot pressing die of the application by reference to the accompanying drawings:
Fig. 1 is the cross-sectional schematic in the application in a kind of embodiment of hot pressing die.As shown in Figure 1, the hot pressing die 1 for the preparation of big size porous structural ceramics comprises: seaming chuck 10, combination die sleeve 12, push-down head 14, guide pillar 16, Upper gasket 18 and lower gasket 19.Wherein combine die sleeve 12 and comprise flap internal mold 120 and external mold 122.
External mold 122 inwall of first being fitted by flap internal mold 120 in use pieces together, and obtains combining die sleeve, and as shown in Figure 6, the hollow space of combination die sleeve is six prisms.Wherein external mold 122 is hollow circular cylinder, and its hollow structure is cylinder.Internal mold is put together by six flap internal molds 120.Internal mold is hollow circular cylinder, and its hollow structure is six prisms.The outer surface of internal mold and the inner surface of external mold are fitted.The schematic side view of flap internal mold 120 and schematic top plan view are as shown in Figure 5.
Please continue to refer to Fig. 1, the combination die sleeve that split is good is bolted together with push-down head 14 again.The insertion combination lower convexity structure of die sleeve 12 inside of seaming chuck 10 and push-down head 14 and the profile of projection structure are also six prisms, as shown in Figure 2, the schematic side view of push-down head 14 and schematic top plan view are as shown in Figure 3 for the elevational schematic view of seaming chuck and schematic side view.Please continue to refer to Fig. 1, place lower gasket 19 on the surface of push-down head 14 afterwards, then guide pillar 16 is inserted in each hole of push-down head 14 through lower gasket 19.Guide pillar 16 is cylinder, and the schematic side view of guide pillar 16 and schematic top plan view are as shown in Figure 4.Please continue to refer to Fig. 1, at mould inner surface uniform application bn slurry (consisting of the ethanol emulsion of boron nitride) thin layer, the mixed powder of ceramic powder and sintering aid is loaded again from top, Upper gasket 18 and seaming chuck 10 are successively put into mould, and guide pillar 16 inserts in the hole of seaming chuck 10 through Upper gasket 18.Namely hot pressing die described in the present embodiment is assembled complete.
Embodiment 1
utilize above-mentioned hot pressing die to prepare porous six prism silicon carbide ceramics, concrete steps are as follows:
(1) hybrid silicon carbide powder and sintering aid: purity be 99%, granularity is add the aluminium powder that percentage by weight is 3%, purity is 99.95%, granularity is 1 ~ 2 μm in the carborundum powder of 3 μm, mixed powder is loaded in polyurethane ball-milling pot, add absolute ethyl alcohol, in planetary ball mill, with rotating speed 300rpm ball milling 20h.
(2) dry, sieve: vacuum drying chamber put into by the powder that ball milling is good, vacuum drying 5h at 60 DEG C.Again dried mixed powder is sieved on 100 object screen clothes, get the powder by screen cloth.
(3) dress powder: the powder above by screen cloth is loaded inner surface and evenly scribbles in the above-mentioned hot pressing die of bn slurry thin layer, constantly beat outside mould in charging process, closely knit to make mixed powder in mould be evenly distributed, put into Upper gasket 18 and seaming chuck 10 after installing powder again.
(4) sintering: the graphite jig installing powder is put into hot-pressed sintering furnace, and in argon atmosphere, pressure is 30MPa, sinters 2h at temperature 1920 DEG C.
(5) the demoulding: after the temperature in sintering furnace drops to room temperature, mould is together taken out together with the pottery sintered, carry out the demoulding on a hydraulic press with demoulding rod and stripper sleeve.First thick and heavy external mold is separated during the demoulding, then flap internal mold is separated with burned pottery.
(6) subsequent treatment: to the six prism silicon carbide ceramics obtained, use drilling machine removing guide pillar 16, obtain porous six prism silicon carbide ceramics.
Embodiment 2
Hot pressing die used is identical with embodiment 1.
utilize above-mentioned hot pressing die to prepare porous six prism silicon carbide ceramics, concrete steps are as follows:
(1) hybrid silicon carbide powder and sintering aid: at the aluminium powder that purity is 99%, granularity be that to add percentage by weight in the carborundum powder of 3 μm be 1% purity is 99.95%, granularity is 1 ~ 2 μm, mixed powder is loaded in polyurethane ball-milling pot, add absolute ethyl alcohol, in planetary ball mill, with rotating speed 300rpm ball milling 20h.
(2) dry, sieve: vacuum drying chamber put into by the powder that ball milling is good, vacuum drying 5h at 60 DEG C.Again dried mixed powder is sieved on 100 object screen clothes, get the powder by screen cloth.
(3) dress powder: the powder above by screen cloth is loaded inner surface and evenly scribbles in the above-mentioned hot pressing die of bn slurry thin layer, constantly beat outside mould in charging process, closely knit to make mixed powder in mould be evenly distributed, put into Upper gasket 18 and seaming chuck 10 after installing powder again.
(4) sintering: the graphite jig installing powder is put into hot-pressed sintering furnace, and in argon atmosphere, pressure is 20MPa, sinters 2h at temperature 1950 DEG C.
(5) the demoulding: after the temperature in sintering furnace drops to room temperature, mould is together taken out together with the pottery sintered, carry out the demoulding on a hydraulic press with demoulding rod and stripper sleeve.First external mold is separated during the demoulding, then flap internal mold is separated with burned pottery.
(6) subsequent treatment: to the six prism silicon carbide ceramics obtained, use drilling machine removing guide pillar 16, obtain porous six prism silicon carbide ceramics.
Embodiment 3
Hot pressing die used is identical with specific embodiment 1.
utilize above-mentioned hot pressing die to prepare porous six prism aluminium nitride ceramics, concrete steps are as follows:
(1) mixed nitride aluminium powder material and sintering aid: purity be 99%, granularity is add the calcirm-fluoride sintering aid that percentage by weight is 5%, purity is 99.5% in the aluminum nitride powder of 1.8 μm, mixed powder is loaded in polyurethane ball-milling pot, add absolute ethyl alcohol, be 300rpm ball milling 20h with rotating speed in planetary ball mill.
(2) dry, sieve: vacuum drying chamber put into by the powder that ball milling is good, vacuum drying 5h at 60 DEG C.Again dried mixed powder is sieved on 100 object screen clothes, get the powder by screen cloth.
(3) dress powder: the powder above by screen cloth is loaded inner surface and evenly scribbles in the above-mentioned hot pressing die of bn slurry thin layer, constantly beat outside mould in charging process, closely knit to make mixed powder in mould be evenly distributed, put into Upper gasket 18 and seaming chuck 10 after installing powder again.
(4) sintering: the graphite jig installing powder is put into hot-pressed sintering furnace, and in nitrogen atmosphere, pressure is 30MPa, sinters 2h at temperature 1800 DEG C.
(5) the demoulding: after the temperature in sintering furnace drops to room temperature, mould is together taken out together with the pottery sintered, carry out the demoulding on a hydraulic press with demoulding rod and stripper sleeve.First thick and heavy external mold is separated during the demoulding, then flap internal mold is separated with burned pottery.
(6) subsequent treatment: to the six prism aluminium nitride ceramics obtained, use drilling machine removing guide pillar 16, obtain porous six prism aluminium nitride ceramics.
The above, only several embodiments of the application, not any type of restriction is done to the application, although the application discloses as above with preferred embodiment, but and be not used to limit the application, any those skilled in the art, not departing from the scope of technical scheme, utilize the technology contents of above-mentioned announcement to make a little variation or modify and be all equal to equivalent case study on implementation, all belong within the scope of technical scheme.

Claims (10)

1. a hot pressing die, is characterized in that, comprises seaming chuck, combination die sleeve, push-down head and guide pillar;
Described combination die cover top possesses upper shed and coordinates with described seaming chuck, and described combination die sleeve bottom possesses under shed and coordinates with described push-down head;
The one side that described seaming chuck coordinates with described combination die sleeve possesses hole;
The one side that described push-down head coordinates with described combination die sleeve possesses hole;
Described combination die sleeve comprises external mold and internal mold; Described outer mold is for hollow structure; Described inner mold is for hollow structure; Described external mold inwall and described internal mold outer wall fit;
Described guide pillar is arranged in the hollow structure of described internal mold, and described guide pillar two ends insert the hole of described seaming chuck and the hole of described push-down head respectively.
2. hot pressing die according to claim 1, is characterized in that, the one side that described push-down head coordinates with described combination die sleeve possesses projection structure, and described projection structure is inserted and closed the under shed of described combination die sleeve;
The one side that described seaming chuck coordinates with described combination die sleeve possesses lower convexity structure, and described lower convexity structure is inserted and closed the upper shed of described combination die sleeve.
3. hot pressing die according to claim 1, is characterized in that, also comprises and is arranged at Upper gasket in described combination die sleeve and lower gasket;
Described Upper gasket contacts with described seaming chuck, and described Upper gasket possesses the hole corresponding with the hole in described seaming chuck;
Described lower gasket contacts with described push-down head, and described lower gasket possesses the hole corresponding with the hole in described push-down head;
Described guide pillar one end inserts the hole of described Upper gasket and described seaming chuck successively, and the described guide pillar other end inserts the hole of described lower gasket and described push-down head successively;
Described guide pillar be cylinder and its axis being parallel in the axis of the hollow structure of described internal mold;
Described guide pillar is no less than 7, and the hole number of described Upper gasket, lower gasket, seaming chuck and push-down head is equal with guide pillar quantity.
4. hot pressing die according to claim 1, is characterized in that, the hollow structure of described external mold is cylinder; The profile of described internal mold is the hollow circular cylinder corresponding to the hollow structure of external mold.
5. hot pressing die according to claim 1, is characterized in that, the flap internal mold that described internal mold is no less than 2 by quantity forms.
6. hot pressing die according to claim 1, is characterized in that, the hollow structure of described internal mold is six prisms; Described internal mold is made up of 6 flap internal molds.
7. hot pressing die according to claim 3, is characterized in that, the graphite material that described Upper gasket, lower gasket, seaming chuck, push-down head, internal mold and external mold adopt Shore hardness to be greater than 75; Described guide pillar adopts Shore hardness to be not more than the graphite material of 75.
8. adopt hot pressing die described in any one of claim 1 to 7 to prepare a method for porous structure ceramic, it is characterized in that, comprise the steps:
A) described external mold and described internal mold are assembled into combination die sleeve, described push-down head and described combination die cover are assembled together, described lower gasket is put into the upper surface of described push-down head, described guide pillar is passed described lower gasket and inserts in the hole of described push-down head, ceramic powder containing sintering aid is loaded in described hot pressing die, respectively described Upper gasket and seaming chuck are loaded in described combination die sleeve successively, obtain the hot pressing die assembled;
B) by step a) described in the hot pressing die assembled under pressure 10 ~ 40Mpa, temperature 1800 ~ 2000 DEG C, inert atmosphere, sinter 1 ~ 3 hour;
C) by step b) the middle hot pressing die cool to room temperature sintered, de-external mold, obtains the structural ceramics that outside is coated with internal mold, inside is inlaid with guide pillar; Removing internal mold and guide pillar, obtain described porous structure ceramic.
9. method according to claim 8, is characterized in that, step a) described in containing sintering aid ceramic powder in, the mass percentage of sintering aid is 1 ~ 5%; The particle diameter of the described ceramic powder containing sintering aid is no more than 150 microns; The described ceramic powder containing sintering aid first applies bn slurry at the hot pressing die inner surface contacted with ceramic powder before loading in described hot pressing die.
10. method according to claim 8, is characterized in that, step b) for by step a) described in the hot pressing die assembled under pressure 15 ~ 30Mpa, temperature 1850 ~ 1980 DEG C, inert atmosphere, sinter 1.5 ~ 2.5 hours; Described inert atmosphere is one or more in nitrogen, helium, argon gas.
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CN110385773A (en) * 2019-08-29 2019-10-29 济源市东方自动化设备有限公司 A kind of ceramic rod cage compacting tool set component
CN110756799A (en) * 2019-11-29 2020-02-07 安徽工业大学 Foamed aluminum foaming precursor mould pressing preparation facilities
WO2022042467A1 (en) * 2020-08-31 2022-03-03 深圳大学 Preparation method for amorphous micro-nano structure, and hot-press forming device

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