CN107140994B - A kind of hot pressed sintering preparation process improving ceramic material consistency - Google Patents
A kind of hot pressed sintering preparation process improving ceramic material consistency Download PDFInfo
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- CN107140994B CN107140994B CN201710344144.2A CN201710344144A CN107140994B CN 107140994 B CN107140994 B CN 107140994B CN 201710344144 A CN201710344144 A CN 201710344144A CN 107140994 B CN107140994 B CN 107140994B
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The present invention relates to ceramic material hot pressed sintering fabricating technology field, especially a kind of hot pressed sintering preparation process for improving ceramic material consistency.Its preparation process is that the ceramic powder that will be pre-sintered is packed into graphite sleeve mold, high-strength graphite lower lock block is installed in its underpart, top is installed by high-strength graphite seaming chuck, high-strength graphite powder is placed respectively as isolated material in the ceramic powder and seaming chuck, lower lock block contact position of pre-sintering, is put into hot-pressed sintering furnace and is sintered according to sintering process.Its operation processing is simple, and the preparation of high-strength graphite powder is convenient, economic and environment-friendly.It is greatly improved and improves using the sintered density and uniformity of the ceramic cutting tool material of hot-pressing sintering technique preparation, therefore the hardness of material is also significantly improved.The present disclosure additionally applies for the exploitation of the structural members such as wear-resistant ceramic, high-hardness ceramic preparations, have very big application potential in the fields such as cutter material and aerospace.
Description
One, technical field
The present invention relates to ceramic material hot pressed sintering fabricating technology field, especially a kind of raising ceramic material is fine and close
The hot pressed sintering preparation process of degree.
Two, background technique
Hot pressed sintering is a kind of ceramic material commonly preparation process, due to supplementing sintering using pressure is longitudinally applied to and driving
Power, therefore the densification of ceramics can be realized in shorter sintering time, and obtain the block body ceramic material of preferable consistency.
Therefore, for ceramic material (such as SiC, Si containing covalent bond hard-to-sinter3N4、TiB2), hot pressed sintering is currently used effective
Preparation process.
For hot pressed sintering mold materials, still upper lower lock block is all used with ultra-fine either big sleeve mold
The high-strength graphite of kernel structure, high-purity and high graphitization degree, compact structure, surface smoothness are high, in addition resist under high temperature
Oxidisability, conduction, thermally conductive, compression strength is all higher, can repeatedly use, therefore is most common hot pressed sintering mould
Has material.Current hot-pressing sintering technique is all according to graphite block, soft graphite paper, ceramic material powder, soft before die-filling sintering
The assemble sequence of graphite paper and graphite block is sequentially loaded into graphite jig, is then added using hot-pressed sintering furnace to ceramic material
Pressure sintering.Wherein above and below powder the soft graphite paper of two sides be used as isolated material, effect is the ceramic material and stone that will be sintered
Black briquetting is kept apart, and is avoided ceramics sample from being sticked on mold in high-temperature sintering process and is caused demoulding difficult, also avoids therefore
Influence repeatedly using for high-strength graphite block.
Although hot pressed sintering can effectively improve the consistency of material, for the hard-to-sinters material such as Whisker-Reinforced Ceramics
Material needs higher temperature and pressure that it can just be made to obtain higher consistency, and tradition heat using current sintering process
The use of soft graphite paper, which will lead to, in pressure sintering process there is sintering structure non-uniform phenomenon, i.e. sample outer edge is obvious to center
Organized layering, and the consistency of the ceramic material at graphite jig is higher than the consistency of its internal material.It is this not
Uniformity and low consistency cause material hardness reduction and material property it is unstable.And the pottery as cutting element
Its material hardness of porcelain cutter has critical influence to its wear resistance, it is therefore necessary to find novel sintered preparation process solution
Certainly tissue odds and the problem of low density, so that it is guaranteed that sintex can have the performances such as reliable and stable high rigidity to refer to
Mark is required with meeting cutting.
Three, summary of the invention
The purpose of the present invention, is to overcome that sintering structure existing for traditional ceramics cutter material preparation process is uneven, causes
Density is not high thus the lower defect of mechanical property especially hardness, provides a kind of hot pressed sintering for improving ceramic material consistency
Preparation process.
Basic conception of the invention is that the isolated material of poor air permeability used by by changing hot pressed sintering in the process is soft
Graphite paper is replaced with high-strength graphite powder, to improve the uniform of ceramic material powder internal gas discharge during the sintering process
Property, and then prepare the higher ceramic cutting tool material of consistency.
The ceramic powder of pre-sintering is packed into graphite cannula by a kind of hot pressed sintering preparation process for improving ceramic material consistency
In cylinder mould tool, high-strength graphite lower lock block is installed in its underpart, high-strength graphite seaming chuck is installed on top, in the ceramic powder of pre-sintering
Isolated material is placed respectively with seaming chuck, lower lock block contact position, is put into hot-pressed sintering furnace and is sintered, the technique of technical solution
Steps are as follows:
(1) preliminary to obtain high-strength graphite powder firstly, by the cutting of high-strength graphite block, crushing；Then 90 are crossed to these graphite powders
Purpose stainless steel sieve is encapsulated spare with obtaining the tiny uniform high-strength graphite powder of granularity；
(2) high-strength graphite lower lock block is fitted into graphite sleeve mold, fixes graphite lower lock block in the position of mold bottom
It sets, prevents loose phenomenon；
(3) according to the size of graphite lower lock block and agglomerated material contact area, according to the thickness range of graphite powder after compacting
Isolated material high-strength graphite powder is weighed for the quality of 0.5~1.5mm, puts it into graphite sleeve mold, is uniformly distributed it
In the upper surface of graphite lower lock block, and compacting pressing processing is carried out to it with pressure head；
(4) the ceramic material powder that pre-sintering is weighed according to the dosage that ceramic material preparation needs, puts it by step
(3) it is placed on the isolated material high-strength graphite powder upper surface in graphite sleeve mold, carries out precompressed pressing processing to it with pressure head,
The range of precompression is 5~8MPa；
(5) isolated material high-strength graphite is weighed according to the quality that the thickness range of graphite powder after compacting is 0.5~1.5mm
Powder is put it into graphite sleeve mold, it is made to be evenly distributed on the upper of the pre-sintered ceramic material powder placed by step (4)
Surface, and compacting pressing processing is carried out to it；
(6) high-strength graphite seaming chuck is put into the isolated material high-strength graphite placed in graphite sleeve mold by step (5)
Above powder, pressurize when to be sintered to powder body material；
(7) graphite jig for installing material according to above-mentioned steps is put into hot-pressed sintering furnace, selects suitable agglomerant
Skill parameter is sintered.
High-strength graphite powder phosphorus content of the present invention is 99.999%.
Invention mechanism: finding in the chronic study procedure for preparing ceramic material, close to graphite sleeve mold after sintering
The consistency of ceramic material at barrel is higher than consistency elsewhere.By XRD material phase analysis, graphite cannula cylinder mould is eliminated
A possibility that tool material and ceramic powder material react.Found by many experiments, used by conventional thermocompression technique every
The exclusion of pre-sintered ceramic powder body material upper and lower surface gas is hindered from material softer graphite paper, and then affects ceramics after sintering
The consistency of material.By improving the smoothness of pre-sintered ceramic powder each surface layer exhaust during hot pressed sintering, using saturating
The good isolated material of gas can significantly improve the consistency of agglomerated material.
Isolated material graphite powder used by preparation process of the invention is high-strength graphite powder, is different from AR grades (analysis is pure)
Flaky graphite powder；After the completion of sintering, high-strength graphite powder still is able to keep being sintered the powdered of preceding good air permeability well
State.It is convenient that it is prepared, and operation processing is simple, is easy to remove from sintered ceramic material surfaces, and can use breakage not
With high-strength graphite block prepare high-strength graphite powder, it is economic and environment-friendly.By doing XRD material phase analysis to sintered ceramic material,
It was found that there is no variations for the component of material, it was demonstrated that the stability of such sintering process method.It is burnt using the novel hot pressing
The ceramic cutting tool material of knot technique preparation can improve its sintered density and uniformity well, therefore the hardness of material also obtains
It is significant to improve.The present disclosure additionally applies for the exploitation of the structural members such as wear-resistant ceramic, high-hardness ceramic preparation, in cutter material and
The fields such as aerospace have very big application potential.
Four, Detailed description of the invention
Fig. 1 is hot pressed sintering preparation process schematic diagram of the present invention；
Fig. 2 is that conventional thermocompression is sintered preparation process schematic diagram；
Fig. 3 is the XRD spectrum of the ceramic material polished surface of hot pressed sintering preparation process of the present invention preparation, in which:
A is Al2O3/SiCwThe XRD diagram of/TiC ceramic material；
B is Al2O3/SiCwThe XRD diagram of ceramic material；
Fig. 4 is that the relative density of the ceramic material of the ceramic material prepared with present invention process and traditional handicraft preparation compares
Figure；
Fig. 5 is that the Vickers hardness of the ceramic material of the ceramic material prepared with present invention process and traditional handicraft preparation compares
Figure.
Appended drawing reference:
1, graphite sleeve mold 2, high-strength graphite seaming chuck 3, the ceramic powder 4 being pre-sintered, high-strength graphite lower lock block
5A-1, isolated material-high-strength graphite powder 5A-2, isolated material-high-strength graphite powder 5B-1, isolated material-flexible graphite paper
5B-2, isolated material-flexible graphite paper
Five, specific embodiment:
In conjunction with attached drawing detailed description of the present invention specific implementation process, as shown in Figure 1:
(1) preliminary to obtain high-strength graphite powder firstly, by high-strength graphite block or the cutting of waste and old high-strength graphite mold, crushing；
Then the stainless steel for crossing 90 mesh to these graphite powders sieves, and to obtain the tiny uniform high-strength graphite powder of granularity, encapsulation is stand-by；
(2) use internal diameter forGraphite sleeve mold 1, be by corresponding internal diameterHigh-strength graphite lower lock block 4 is packed into
In graphite sleeve mold 1, graphite lower lock block 4 is fixed in the position of mold bottom, prevents loose phenomenon；
(3) the isolated material high-strength graphite powder 5A-2 that quality is 1g is weighed, puts it into graphite sleeve mold 1, makes it
It is evenly distributed on the upper surface of graphite lower lock block 4, compacting pressing processing is then carried out to it using pressure head；
(4) by component ratio listed in embodiment parameter subordinate list, the ceramic material powder 3 of pre-sintering is weighed, is put
Enter the upper surface isolated material high-strength graphite powder 5A-2 being placed in graphite sleeve mold 1 by step (3), it is carried out with pressure head
Precompressed pressing processing, the range of precompression are 5~8MPa；
(5) the isolated material high-strength graphite powder that quality is 1g is weighed, the pottery being pre-sintered in graphite sleeve mold 1 is put it into
The upper surface of ceramic material powder 3 makes it be evenly distributed on the upper surface for the pre-sintered ceramic material powder placed by step (4), and
Compacting pressing processing is carried out to it；
(6) willHigh-strength graphite seaming chuck 2 to be put into the isolated material placed in graphite sleeve mold 1 by step (5) high
Above strong graphite powder, pressurize when to be sintered to powder body material；
(7) graphite jig for installing material according to above-mentioned steps is put into hot-pressed sintering furnace, selects sintering process parameter
Are as follows: 1700 DEG C of sintering temperature, heat preservation 30min, sintering pressure 30MPa are sintered.
The density of ceramic material is measured using density balance (DH-120, Japan) after sintering, and measuring medium is distillation
Water；Hardness is measured using Vickers (HVS-50, China), and load selects 20kg, and the dwell time selects 15s；In order to
The accuracy for improving measurement measures impression length using Keyemce 3D laser scanning microscope (VK-X200K, Japan),
It measures 6 points to be averaged, obtains corresponding performance parameter in embodiment parameter and implementation result comparison subordinate list.
Embodiment parameter and implementation result compare subordinate list:
The preparation of isolated material high-strength graphite powder used in hot-pressing sintering technique of the invention is convenient, cheap, is easy to
Demoulding.Under identical hot pressed sintering parameter, using the consistency of the ceramic cutting tool material of hot-pressing sintering technique of the present invention preparation
It is greatly improved with hardness, and the decline of other mechanical property parameters will not be caused.It is burnt with what is reported using conventional thermocompression
The material property that knot technique obtains is compared, and hardness improves 20% or so.The present invention is for conventional thermocompression agglomerated material consistency
The solution of problem provides new process, is preparing the wear-resistant ceramic materials sides such as high-compactness, high performance sintex
Face has important application value.
Claims (1)
1. the ceramic powder of pre-sintering is packed into graphite sleeve by a kind of hot pressed sintering preparation process for improving ceramic material consistency
In mold, its underpart install high-strength graphite lower lock block, top install high-strength graphite seaming chuck, pre-sintering ceramic powder with
Seaming chuck, lower lock block contact position place isolated material respectively, are put into hot-pressed sintering furnace and are sintered, it is characterised in that processing step
It is as follows:
(1) firstly, by the cutting of high-strength graphite block, crushing, the preliminary high-strength graphite powder for obtaining phosphorus content and being 99.999%；Then right
The stainless steel sieve that these graphite powders cross 90 mesh is encapsulated spare with obtaining the tiny uniform high-strength graphite powder of granularity；
(2) high-strength graphite lower lock block is fitted into graphite sleeve mold, fixes graphite lower lock block in the position of mold bottom, prevents
Only there is loose phenomenon；
(3) according to the size of graphite lower lock block and agglomerated material contact area, the thickness range according to graphite powder after compacting is 0.5
The quality of~1.5mm weighs isolated material high-strength graphite powder, puts it into graphite sleeve mold, it is made to be evenly distributed on graphite
The upper surface of lower lock block, and compacting pressing processing is carried out to it with pressure head；
(4) the ceramic material powder that pre-sintering is weighed according to the dosage that ceramic material preparation needs, puts it into and is put by step (3)
The isolated material high-strength graphite powder upper surface in graphite sleeve mold is set, carries out precompressed pressing processing, precompressed to it with pressure head
The range of power is 5~8MPa；
(5) isolated material high-strength graphite powder is weighed according to the quality that the thickness range of graphite powder after compacting is 0.5~1.5mm, it will
It is put into graphite sleeve mold, it is made to be evenly distributed on the upper surface for the pre-sintered ceramic material powder placed by step (4),
And compacting pressing processing is carried out to it；
(6) high-strength graphite seaming chuck is put on the isolated material high-strength graphite powder in graphite sleeve mold by step (5) placement
Face pressurizes to powder body material when to be sintered；
(7) graphite jig for installing material according to above-mentioned steps is put into hot-pressed sintering furnace, suitable sintering process is selected to join
Number is sintered.
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| CN110480800B (en) * | 2019-07-22 | 2021-04-16 | 广东新秀新材料股份有限公司 | 3D ceramic thin-wall part and preparation method thereof |
| CN111943701B (en) * | 2020-07-27 | 2022-08-09 | 赛福纳米科技(徐州)有限公司 | Hot-pressing sintering process for improving compactness of ceramic material |
| CN112142484A (en) * | 2020-09-18 | 2020-12-29 | 株洲三达电子制造有限公司 | Preparation method of ceramic for ceramic sensor |
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| CN203061876U (en) * | 2013-02-19 | 2013-07-17 | 成都超纯应用材料有限责任公司 | Hot-press sintering die with inner lining |
| CN203061875U (en) * | 2013-02-19 | 2013-07-17 | 成都超纯应用材料有限责任公司 | Hot-press sintering die with gaskets |
| CN106498205B (en) * | 2016-12-13 | 2018-03-09 | 合肥工业大学 | A kind of manufacture method of the CuCr alloys of large scale high-compactness high uniformity |
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