CN110317065A - A kind of forming method of cross-section aluminium nitride product - Google Patents
A kind of forming method of cross-section aluminium nitride product Download PDFInfo
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- CN110317065A CN110317065A CN201910483500.8A CN201910483500A CN110317065A CN 110317065 A CN110317065 A CN 110317065A CN 201910483500 A CN201910483500 A CN 201910483500A CN 110317065 A CN110317065 A CN 110317065A
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Abstract
The present invention proposes a kind of forming method of cross-section aluminium nitride product, including being granulated, it is dry-mixed, wet mixing, molding, the step of dumping, the method of the present invention is by aluminum nitride powder, binder, after solvent mixes, use vacuum pugging equipment pugging, improve uniformity of mixture, it reuses screw extrusion or squeeze equipment is continuously shaped, not only production process is few, high production efficiency, and the biscuit intensity after drying is big, be conducive to following process, the method of the present invention is by aluminum nitride powder, binder, after solvent mixes, use vacuum pugging equipment pugging, improve uniformity of mixture, it reuses screw extrusion or squeeze equipment is continuously shaped, not only production process is few, high production efficiency, and the biscuit intensity after drying is big, be conducive to following process.
Description
Technical field
The present invention relates to aluminium nitride preparation technical field more particularly to a kind of forming methods of cross-section aluminium nitride product.
Background technique
Aluminium nitride ceramics is widely used in military and space because it possesses good heating conduction, as new function material
The every field such as technology communication, computer, instrument and meter industry, electronic equipment, automobile, daily electrical home appliance, office automation.Nitridation
Aluminium ceramic product includes the products of different shapes such as substrate, dry-pressing part, shaped piece, and different products has different forming methods,
After general longer cross-section ceramic product is using the big blocky biscuit of dry-pressing formed method molding, then machine after dumping, sintering
Processing obtains product, and low efficiency, waste of material is big, at high cost.
The forming method of aluminium nitride ceramics product mainly has dry-pressing formed, isostatic pressing, the tape casting molding and is injected into
4 kinds of type etc..
Dry-pressing formed is that will be added through the pretreated AlN powder such as surfactant-modified into metal die, is slowly applied
Plus-pressure becomes fine and close blank forming technique.Advantage be it is easy to operate, process procedure is few, high-efficient, the disadvantage is that not
The green body of complex geometric shapes can be suppressed.
Isostatic pressing is the improved method of traditional dry pressing, AlN powder is placed in high-pressure bottle, not using liquid
Powder is placed in the molding die of elastic material manufacture, from different sides the characteristic of pressure conduction by compressibility and liquid
It is uniformly pressed to powder compact is treated, the method for being pressurizeed and being made blank forming to mold with liquid.Its advantage is that green body
Consistency it is higher, even density can be with near-net-shape, the disadvantage is that molding equipment is expensive, and demoulds difficult, limit
It is applied to large-scale industrial production.
Doctor-blade casting process be by AlN powder and dispersing agent, solvent, binder and plasticizer after mixing, obtain AlN stream
Prolong slurry, using green band is obtained after casting machine curtain coating after degassing, cuts, obtains biscuit after lamination.Its advantage is that can be continuous
Operation, high production efficiency, the degree of automation height etc., the disadvantage is that slurry is high to aluminium nitride powder requirement, during biscuit dumping
Easily there is bending deformation phenomenon, and this method is only used for the production of flaky material.
Injection moulding: dispersing agent, solvent, binder and plasticizer is added after mixing in AlN powder, formation has
Viscoplastic feeding is injected feeding in mould cavity using injection (mo(u)lding) machine, condensation molding obtains element in a heated state
Base.Its advantage is that consistency is high, Density Distribution is uniform, can be used for complicated form blank forming, and formed precision is high, is not necessarily to the later period
Machining, the disadvantage is that easily there is the defects of shorting, overlap, weld mark, air pocket.
CN201210428467 patent in the prior art, be using aluminium nitride powder as base stock, with ethyl alcohol, propyl alcohol,
Or mixtures thereof butanol etc. are used as organic solvent, form premixed liquid with epoxy resin and dispersing agent, and mixing and ball milling forms slurry,
Curing agent is added after vacuum outgas to stir evenly, then by process flows such as moulding by casting, solidification, demoulding, dryings, forms tool
There are the special-shaped ceramics green compact of larger intensity.This method is due to moulding by casting to be used, and not only complex procedures, production efficiency are low, and
And biscuit intensity is low, and breakage is easy in subsequent production, forms waste product.
CN201080054835 patent is mixed using two different aluminium nitride powders and AlN- pellet, it is desirable that is preferably provided with
Organic coating and have sufficiently high yttria levels, when be added water go to dissolve water-soluble binder when, aluminium nitride will not be sent out
Unboiled water solution, this has higher requirement to raw material, and satisfactory aln raw material realizes production domesticization not yet, can only import price
Higher raw material, this improves cost of material, is unfavorable for the popularization and application of product.
The sectional area of usual cross-section ceramic product is equal, and length is longer, be greater than or much larger than section length or width,
After this kind of product obtains biscuit using dry-pressing formed, isostatic pressing, semi-finished product ceramics are obtained after dumping, sintering, then carry out machine
Processing obtains product.These methods are suitable for the product that sectional area is larger, length is short, if the production that sectional area is smaller, length is big
Just not only production efficiency is very low with these methods for product, but also yield rate is low, at high cost.
Summary of the invention
It is necessary to propose a kind of forming method of cross-section aluminium nitride product.
A kind of forming method of cross-section aluminium nitride product, comprising the following steps:
It is granulated: aluminium nitride is mixed with yttrium oxide, the weight ratio that the yttrium oxide accounts for aluminium nitride is 2-6%, and mist projection granulating is formed
Aluminium nitride pelletizing；
It is dry-mixed: pelletizing is mixed with dispersing agent, plasticiser according to weight ratio for 72-84:0.5-1.5:0.5-1.5；
Wet mixing: binder is added into dry blend, after mixing, adds 5-10 parts of castor oil, is uniformly mixed, is obtained
The weight ratio of aluminium nitride pug, binder additional amount and pelletizing additional amount is 10-15:72-84；
Molding: pugging is carried out to the aluminium nitride creme using vacuum deairing machine, keeps pug mixing more uniform, pug is placed in
In extrusion equipment, to carry out extruding conveying to pug, extrusion die is set in the outlet of extrusion equipment, to squeeze pug
Molding, obtains prismatic rodlike or tubulose biscuit；
Above-mentioned biscuit is put into draft glue discharging furnace and carries out dumping, removes organic component, is sintered, is caused in sintering furnace high temperature later
Close cross-section aluminium nitride ceramics product.
After the method for the present invention mixes aluminum nitride powder, binder, solvent, using vacuum pugging equipment pugging, mixing is improved
The uniformity of object, reuses screw extrusion or squeeze equipment is continuously shaped, and not only production process is few, high production efficiency, and
And the biscuit intensity after drying is big, is conducive to following process.
After this method uses domestic aln raw material, addition yttrium oxide, organic solvent, dispersing agent to mix, mist projection granulating
For powder granule D50For the pelletizing of 20-80 μ m, do not have to carry out water-proofing treatment to aluminium nitride powder, cost of material is low, has
Conducive to reduction production cost.
Detailed description of the invention
Fig. 1,2 be two kinds of extrusion dies structural schematic diagram.
In figure: extrusion equipment 10, extrusion die 20.
Specific embodiment
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, common for this field
For technical staff, without creative efforts, it is also possible to obtain other drawings based on these drawings.
The embodiment of the invention provides a kind of forming methods of cross-section aluminium nitride product, comprising the following steps:
It is granulated: aluminium nitride is mixed with yttrium oxide, the weight ratio that the yttrium oxide accounts for aluminium nitride is 2-6%, and mist projection granulating is formed
Aluminium nitride pelletizing；For example, yttrium oxide account for aluminium nitride weight ratio can for 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%,
5.5%、6%。
It is dry-mixed: pelletizing is mixed with dispersing agent, plasticiser according to weight ratio for 72-84:0.5-1.5:0.5-1.5；Point
Weight ratio shared by powder be 0.5 part or 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts, 1.1 parts, 1.2 parts, 1.3 parts, 1.4 parts,
1.5 parts etc..
Weight ratio shared by plasticiser be 0.5 part or 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1.0 parts, 1.1 parts, 1.2 parts,
1.3 parts, 1.4 parts, 1.5 parts etc..
Wet mixing: binder is added into dry blend, after mixing, adds 5-10 parts of castor oil, is uniformly mixed,
Obtain aluminium nitride pug, the weight ratio of binder additional amount and pelletizing additional amount is 10-15:72-84；Weight shared by binder
Than being 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts etc..Weight ratio shared by castor oil is 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10
Part etc..
Molding: pugging is carried out to the aluminium nitride creme using vacuum deairing machine, keeps pug mixing more uniform, by pug
It is placed in extrusion equipment 10, to carry out extruding conveying to pug, extrusion die 20 is set in the outlet of extrusion equipment, to pug
It carries out extrusion forming and obtains prismatic rodlike or tubulose biscuit；Wherein, the extrusion equipment is spiral squeezing equipment or hydraulic
Extrusion equipment.
Above-mentioned biscuit is put into draft glue discharging furnace and carries out dumping, removes organic component, is sintered, obtains in sintering furnace high temperature later
To fine and close cross-section aluminium nitride ceramics product.
Further, the partial size of the aluminium nitride is 20-100 μm, D50It is 60 ± 10 μm, the partial size D of yttrium oxide50For 0.5-2
μm。
Further, the dispersing agent is fish oil.
Further, the plasticiser is polyethylene glycol.
Further, the binder is PVB solution, and the PVB solution is that PVB is dissolved in absolute alcohol to be formed,
The mass ratio of PVB and absolute alcohol is 1:4 ~ 1:8.PVB is polyvinyl butyral.
Further, ageing mixture step, the ageing mixture step are as follows: set the aluminium nitride pug are set also after wet mixing step
1-4h is kept in hermetic bag.
Wherein, ageing mixture step is the blank tentatively stirred, and sealing storage certain time has under the conditions of 25 ± 2 DEG C of temperature
Conducive to the problem that bonding agent is not uniform enough, pug stickiness is poor is alleviated in pug, to improve the uniformity and plasticity of pug.
It further, further include ageing mixture step in " molding " step, the ageing mixture step is will be after vacuum deairing machine pugging
Aluminium nitride creme be placed in hermetic bag and keep 24-48h.
Further, the extrusion die is the conical rigid mold that arrival end internal diameter is big, outlet section internal diameter is small, the outlet
The internal diameter of section is arranged according to the diameter of section of the cross-section aluminium nitride product.For example, slightly larger than cross-section aluminium nitride product
Diameter of section, about 0.5mm-2mm or so.
Further, the extrusion die is the hollow centrum of hollow centrum or built-in core bar.Referring to Fig. 1,2.
Below by way of three embodiments using the method for the present invention are enumerated, wherein the unit of the parts by weight referred to can be
kg。
Embodiment 1: in parts by weight, by 79 parts of aluminium nitride pelletizings (that is, by weight ratio be 2 parts of yttrium oxides and
100 parts of aluminum nitride powders are mixed to get aluminium nitride pelletizing), 1.5 parts of dispersing agent fish oil and 1.5 parts of plasticiser polyethylene glycol are done
Mixed 3h, is then added 12 parts of binder PVB solution, mixes 2h, adds 6 parts of castor oil, and mixing 2h after mixing evenly, takes out mud
Material packs, and vacuum pugging after ageing mixture 2h refills bag ageing mixture for 24 hours.Outer diameter φ 24mm is assembled in screw extruder, internal diameter φ 16mm's
Mold.The pug for completing ageing mixture is taken out, forms hollow tubulose aluminium nitride biscuit on screw extruder, when molding, every 50cm was cut
Disconnected biscuit is primary, obtains outer diameter φ 24mm, the tubulose biscuit of internal diameter φ 16mm, length 50cm.By biscuit 600 DEG C in draft glue discharging furnace
Dumping is carried out, organic principle is removed, obtains dry aluminium nitride tubulose biscuit, then be put into graphite sintering furnace in nitrogen protection gas
Lower 1810 DEG C of atmosphere are sintered, and obtain tubulose aluminium nitride ceramics.
Embodiment 2: in parts by weight, by 75 parts of aluminium nitride pelletizings (that is, by weight ratio be 3 parts of yttrium oxides and
100 parts of aluminum nitride powders are mixed to get aluminium nitride pelletizing), 1 part of dispersing agent fish oil and 1 part of plasticiser polyethylene glycol carry out it is dry-mixed
Then 15 parts of binder PVB solution are added in 3h, mix 3h, add 8 parts of castor oil, and mixing 3h after mixing evenly, takes out pug
It packs, vacuum pugging after ageing mixture 2h refills bag ageing mixture for 24 hours.Outer diameter φ 12mm, the mould of internal diameter φ 6mm are assembled in screw extruder
Tool.The pug for completing ageing mixture is taken out, forms hollow tubulose aluminium nitride biscuit on screw extruder, the every 10cm cutting of when molding
Biscuit is primary, obtains outer diameter φ 12mm, the tubulose biscuit of internal diameter φ 6mm, length 10cm.By biscuit in draft glue discharging furnace 600 DEG C into
Row dumping removes organic principle, obtains dry aluminium nitride tubulose biscuit, then be put into graphite sintering furnace
It is sintered for 1810 DEG C under nitrogen protection atmosphere, obtains tubulose aluminium nitride ceramics.
Embodiment 3: in parts by weight, by 73 parts of aluminium nitride pelletizings (that is, by weight ratio be 5 parts of yttrium oxides and
100 parts of aluminum nitride powders are mixed to get aluminium nitride pelletizing), 1 part of dispersing agent fish oil and 1 part of plasticiser polyethylene glycol carry out it is dry-mixed
Then 15 parts of binder PVB solution are added in 3h, mix 2h, add 10 parts of castor oil, and mixing 2h after mixing evenly, takes out mud
Material packs, and vacuum pugging after ageing mixture 2h refills bag ageing mixture for 24 hours.In the mold of screw extruder assembly φ 16mm.It takes out and completes to be stranded
The pug of material, the rodlike aluminium nitride biscuit of shaping solid on screw extruder, when molding, every 30cm cutting biscuit was primary, obtained
The rodlike biscuit of φ 16mm, length 30cm.By biscuit, 600 DEG C of progress dumpings, removing organic principle obtain drying in draft glue discharging furnace
The rodlike biscuit of aluminium nitride, then be put into graphite sintering furnace and be sintered for 1810 DEG C under nitrogen protection atmosphere, obtain rodlike nitrogen
Change aluminium ceramics.
Performance detection is carried out to the product of three embodiment productions below, obtains following table:
Upper table is as it can be seen that the potsherd produced using the method for the present invention, and undeformed, roundness tolerance is very small, and density is also above standard
It is required that.As it can be seen that the outer dimension for the aluminium nitride product that the reasonable cooperation production of each ingredient and its component obtains in through the invention,
Circularity degree, density are superior to parameter in the prior art.
In addition, according to the execution standard of the industry, it is strong using the thermal conductivity and bending resistance of above three embodiments of the invention
Degree is superior to normal data.As shown in the table.
| Execution standard | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Thermal conductivity (W/m.K) | ≥170 | 175 | 174 | 172 |
| Bending strength (MPa) | > 300 | 355 | 317 | 378 |
Module or unit in the device of that embodiment of the invention can be combined, divided and deleted according to actual needs.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and wants according to right of the present invention
Made equivalent variations is sought, is still belonged to the scope covered by the invention.
Claims (9)
1. a kind of forming method of cross-section aluminium nitride product, it is characterised in that the following steps are included:
It is granulated: aluminium nitride is mixed with yttrium oxide, the weight ratio that the yttrium oxide accounts for aluminium nitride is 2-6%, and mist projection granulating is formed
Aluminium nitride pelletizing；
It is dry-mixed: pelletizing is mixed with dispersing agent, plasticiser according to weight ratio for 72-84:0.5-1.5:0.5-1.5；
Wet mixing: binder is added into dry blend, after mixing, adds 5-10 parts of castor oil, is uniformly mixed, is obtained
The weight ratio of aluminium nitride pug, binder additional amount and pelletizing additional amount is 10-15:72-84；
Molding: pugging is carried out to the aluminium nitride creme using vacuum deairing machine, keeps pug mixing more uniform, pug is placed in
In extrusion equipment, to carry out extruding conveying to pug, extrusion die is set in the outlet of extrusion equipment, to squeeze pug
Molding, obtains prismatic rodlike or tubulose biscuit；
Above-mentioned biscuit is put into draft glue discharging furnace and carries out dumping, removes organic component, is sintered, is caused in sintering furnace high temperature later
Close cross-section aluminium nitride ceramics product.
2. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: the partial size of the aluminium nitride
It is 20-100 μm, D50It is 60 ± 10 μm, the partial size D of yttrium oxide50It is 0.5-2 μm.
3. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: the dispersing agent is fish
Oil.
4. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: the plasticiser is poly- second
Glycol.
5. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: the binder is PVB
Solution, the PVB solution are that PVB is dissolved in absolute alcohol to be formed, and the mass ratio of PVB and absolute alcohol is 1:4 ~ 1:8.
6. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: also after wet mixing step
Ageing mixture step, the ageing mixture step are as follows: the aluminium nitride pug is placed in hermetic bag and keeps 1-4h are set.
7. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: in " molding " step,
It further include ageing mixture step, the ageing mixture step is that the aluminium nitride creme after vacuum deairing machine pugging is placed in hermetic bag to keep
24-48h。
8. the forming method of cross-section aluminium nitride product as described in claim 1, it is characterised in that: the extrusion die be into
The conical rigid mold that mouth end internal diameter is big, outlet section internal diameter is small, the internal diameter of the outlet section are produced according to the cross-section aluminium nitride
The diameter of section of product is arranged.
9. the forming method of cross-section aluminium nitride product as claimed in claim 8, it is characterised in that: the extrusion die is sky
Heart centrum or the hollow centrum of built-in core bar.
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| CN105461306A (en) * | 2015-11-16 | 2016-04-06 | 石婷 | High-strength silicon carbide ceramic pipe and manufacturing method thereof |
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| CN101560104A (en) * | 2009-05-12 | 2009-10-21 | 宁波欧翔精细陶瓷技术有限公司 | Preparation method for silicon carbide ceramic tube or rod |
| WO2012064512A1 (en) * | 2010-11-08 | 2012-05-18 | Dow Global Technologies Llc | Composition for extrusion-molded bodies comprising a methyl cellulose |
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