CN107399973A - The technique that a kind of direct nitridation method prepares aluminium nitride powder - Google Patents
The technique that a kind of direct nitridation method prepares aluminium nitride powder Download PDFInfo
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- CN107399973A CN107399973A CN201610336622.0A CN201610336622A CN107399973A CN 107399973 A CN107399973 A CN 107399973A CN 201610336622 A CN201610336622 A CN 201610336622A CN 107399973 A CN107399973 A CN 107399973A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
Abstract
A kind of direct nitridation method prepares the technique of aluminium nitride powder, belongs to the preparing technical field of non-oxide ceramic powder material.Concretely comprise the following steps：1st, after high-purity Al powder, additive, diluent being weighed by certain proportioning, it is put into together with absolute ethyl alcohol in ball grinder, 3~20h of ball milling.2nd, the compound after ball milling is dried in 50~80 DEG C of environment.3rd, raw material is placed in crucible, be put into sintering furnace, nitridation reaction is carried out with high pure nitrogen at 800~1200 DEG C of temperature.4th, powder is heat-treated to improve pattern after nitridation reaction terminates.The aluminium nitride powder color that the technique obtains is uniformly, well-crystallized, pattern be good, high conversion rate, suitable for industrialized production.
Description
Technical field
The invention belongs to the preparing technical field of non-oxide ceramic powder material, and in particular to a kind of direct nitridation method prepares the technology of aluminium nitride powder.
Background technology
Aluminium nitride is a kind of covalent key compound of hexagonal wurtzite structure, belongs to hexagonal crystal system, and decomposition temperature is 2480 DEG C at ambient pressure.The special lattice structure of aluminium nitride makes it have high thermal conductivity, low thermal coefficient of expansion, high mechanical strength, excellent insulating property, high temperature resistant, corrosion-resistant, dielectric loss is small, many excellent performances such as nontoxic.With developing rapidly for microelectric technique, microelectronic product develops towards directions such as Highgrade integration, wiring miniaturizations, and this heat dissipation problem to electronic integrated circuit substrate, heat dissipation element, electronic package material etc. requires more and more higher.Aluminium nitride has been substituted aluminum oxide and beryllium oxide and has been turned into the preferred material of current super large-scale integration substrate due to the excellent properties of itself.And the crucible of the Metal Melting such as founding pure iron, aluminium, copper, silver, lead and the ideal material of casting die.
The method for industrially preparing aluminium nitride powder at present mainly has aluminium powder direct nitridation method, carbothermic method, self-propagating high-temperature synthesis.The aluminium nitride powder that carbothermic method obtains is close to spherical, but its particle diameter is generally large, is sub-micron or so.Later stage may increase oxygen impurities content except carbon process, and this thermal conductivity to later stage ceramics is unfavorable.In addition, this method synthesis temperature is high（1600~1800 DEG C）, the cost for preparing aluminium nitride powder is higher.Self-propagating synthesis technology is spontaneously carried out come maintenance reaction using reaction heat, although reaction speed is fast, energy consumption is low, technique is simple, the cycle is short, reaction speed is too fast, ignition temperature is too high and exist the problems such as thermograde is excessive make process difficulty or ease control.And aluminium powder direct nitridation method reaction temperature is low（800~1200 DEG C）, cost of material is low, technique is simple, process is easy to control, suitable for industrialized production.The good aluminium nitride powder of well-crystallized, pattern is obtained using direct nitridation method herein.
The content of the invention
The present invention provides the technology that a kind of direct nitridation method prepares aluminium nitride powder, and the aluminium nitride powder color that the technique obtains is uniformly, well-crystallized, pattern be good, high conversion rate, suitable for industrialized production.The technical solution adopted in the present invention is：
（1）After high-purity Al powder, additive, diluent are weighed by certain proportioning, it is put into together with absolute ethyl alcohol in ball grinder, 3~20h of ball milling；
（2）Compound after ball milling is dried in 50~80 DEG C of environment；
（3）Raw material is placed in crucible, is put into sintering furnace, nitridation reaction is carried out with high pure nitrogen at 800~1200 DEG C of temperature；
（4）Nitridation reaction is heat-treated to improve pattern after terminating to powder.
Step（1）Described in the particle diameter of high-purity Al powder be not more than 30 μm, the mass ratio of high-purity Al powder and additive is 1：（0.1~0.9）, diluent accounts for 0~70wt% of Al powder.
Step（1）Described in additive be NH4Cl、NH4The mixture of and KCl in F a kind of, diluent are AlN powder, wherein KCl and NH4Cl（Or NH4F）Mass ratio be 1:（2~15）.
Step（4）Described in heat treatment temperature be 1400~1650 DEG C, soaking time is 1~5h.
The obtained aluminium nitride powder well-crystallized of preparation method of the present invention, pattern are good, and cost of material is relatively low, with short production cycle, suitable for industrialized production.Played an important role in application aspects such as electronic package material, ic substrate, crucible die materials.
Brief description of the drawings
Fig. 1 is the XRD for the aluminium nitride powder being prepared using the technique of the present invention.
Fig. 2 is the SEM figures for the aluminium nitride powder being prepared using the technique of the present invention.
Embodiment
Below in conjunction with case study on implementation, the present invention is described further, but is not limited solely to embodiment.
Embodiment
1
By high-purity Al powder, NH4100g, 41.5g, 8.5g are put into ball grinder respectively by Cl, KCl, add absolute ethyl alcohol ball milling 5h.Mixed slurry is put into corundum crucible in drying box after 60 DEG C of drying, 1450 DEG C of heat treatment 3h are warming up to after being incubated 2h at 850 DEG C.The loose block of aluminium nitride is obtained after cooling, mills to obtain aluminium nitride powder.Heating-insulation-heat treatment whole process is always ensured that nitrogen atmosphere, and gas displacement is suitably carried out before nitridation reaction, to ensure that ammonia of generation etc. does not influence the purity of nitrogen.
Embodiment
2
By high-purity Al powder, NH4Cl, KCl are weighed by 100g, 22g, 3g quality, add AlN powder 25g.The ball milling 6h in ball grinder, ball-milling medium are absolute ethyl alcohol.It is placed in after 70 DEG C of dryings in crucible, 950 DEG C of insulation 1h is warming up in multifunctional sintering furnace, is to slowly warm up to 1600 DEG C of insulation 2h immediately, pattern, the aluminium nitride powder of well-crystallized is prepared.Whole process is always nitrogen atmosphere.
Embodiment
3
By high-purity Al powder, NH4F, KCl is put into ball grinder by 100g, 54g, 6g, adds absolute ethyl alcohol ball milling 10h.It is put into after mixed slurry is dried in drying box in corundum crucible, 1500 DEG C of heat treatment 1h is warming up to after being incubated 2h at 1000 DEG C.Furnace cooling simultaneously mills to obtain aluminium nitride powder.
Claims (5)
1. the technique that a kind of direct nitridation method prepares aluminium nitride powder, it is characterised in that comprise the following steps：
（1）After high-purity Al powder, additive, diluent are weighed by certain proportioning, it is put into together with absolute ethyl alcohol in ball grinder, 3~20h of ball milling；
（2）Compound after ball milling is dried in 50~80 DEG C of environment；
（3）Raw material is placed in crucible, is put into sintering furnace, nitridation reaction is carried out with high pure nitrogen at 800~1200 DEG C of temperature；
（4）Nitridation reaction is heat-treated to improve pattern after terminating to powder.
2. the technique for preparing aluminium nitride powder according to a kind of direct nitridation method described in claim 1, it is characterised in that step（1）Described in the particle diameter of high-purity Al powder be not more than 30 μm, the mass ratio of high-purity Al powder and additive is 1：（0.1~0.9）, diluent accounts for 0~70wt% of Al powder.
3. the technique for preparing aluminium nitride powder according to a kind of direct nitridation method described in claim 1, it is characterised in that step（1）Described in additive be NH4Cl、NH4The mixture of and KCl in F a kind of, diluent are AlN powder.
4. the technique for preparing aluminium nitride powder according to a kind of direct nitridation method described in claim 3, it is characterised in that described KCl and NH4Cl（Or NH4F）Mass ratio be 1:（2~15）.
5. the technique for preparing aluminium nitride powder according to a kind of direct nitridation method described in claim 1, it is characterised in that step（4）Described in heat treatment temperature be 1400~1650 DEG C, soaking time is 1~5h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107698264A (en) * | 2016-08-09 | 2018-02-16 | 河北高富氮化硅材料有限公司 | A kind of preparation method of modified alpha-phase silicon nitride powder |
| CN110577198A (en) * | 2018-06-11 | 2019-12-17 | 河北高富氮化硅材料有限公司 | Method for removing crushed small particles in aluminum nitride powder |
| CN115010100A (en) * | 2022-06-21 | 2022-09-06 | 西安交通大学 | Flaky aluminum nitride powder and preparation method thereof |
-
2016
- 2016-05-20 CN CN201610336622.0A patent/CN107399973A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107698264A (en) * | 2016-08-09 | 2018-02-16 | 河北高富氮化硅材料有限公司 | A kind of preparation method of modified alpha-phase silicon nitride powder |
| CN110577198A (en) * | 2018-06-11 | 2019-12-17 | 河北高富氮化硅材料有限公司 | Method for removing crushed small particles in aluminum nitride powder |
| CN115010100A (en) * | 2022-06-21 | 2022-09-06 | 西安交通大学 | Flaky aluminum nitride powder and preparation method thereof |
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Application publication date: 20171128 |