CN1872692A - Preparation method of hydration-resistant easily-dispersible aluminum nitride powder - Google Patents
Preparation method of hydration-resistant easily-dispersible aluminum nitride powder Download PDFInfo
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- CN1872692A CN1872692A CN 200610085434 CN200610085434A CN1872692A CN 1872692 A CN1872692 A CN 1872692A CN 200610085434 CN200610085434 CN 200610085434 CN 200610085434 A CN200610085434 A CN 200610085434A CN 1872692 A CN1872692 A CN 1872692A
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a method for improving hydration resistance of aluminum nitride powder, which utilizes a surface adsorption technology to treat the surface of the aluminum nitride powder, prevents the aluminum nitride powder from being hydrolyzed in a humid environment and improves the hydration resistance of the powder. Firstly, stirring aluminum nitride powder and organic carboxylic acid in an organic solution to enable the surface of the aluminum nitride powder to adsorb a layer of organic carboxylic acid, then adding a nonionic surfactant, stirring and heating in a water bath at 60-80 ℃ for several hours, washing with an ethanol solution for multiple times, and drying the washed aluminum nitride powder at 80-100 ℃. The method has simple operation and outstanding hydration resistance, and well solves the problem that the aluminum nitride is very easy to hydrolyze in a humid environment.
Description
Technical field
The present invention relates to a kind of method that improves the anti-hydratability of aluminium nitride powder, under the prerequisite that does not influence the original performance of aluminium nitride powder, can effectively prevent the hydrolysis of aluminium nitride powder, can in the aqueous solution, prepare the aluminium nitride slurry again, belong to material type ceramic technology field.
Background technology
(theoretical value of monocrystalline is 320W/m.k to aluminium nitride because of it has high thermal conductivity, actual value still can reach 100～280W/m.k, be equivalent to 5～10 times of aluminum oxide), high strength, high volume specific resistance, high dielectric voltage withstand, low-dielectric loss, good characteristics such as thermal expansivity and silicon coupling have become present most promising high heat-conducting ceramic electric substrate of new generation and packaged material.Therefore, to the development of aluminium nitride ceramics, will give electronic technology field, especially development of integrated circuits is brought revolutionary impact.Yet aluminium nitride powder and water have very high reactive behavior, the environment of humidity very easily with water in hydroxyl form aluminium hydroxide, form alumina layer on the aluminium nitride powder surface, the aluminium nitride lattice dissolves in a large amount of oxygen, reduces its thermal conductivity; Aluminium nitride powder is at the wet environment facile hydrolysis, solvent adopts organic solvents such as benzene, dimethylbenzene more in the aluminium nitride blank preparation technics, yet organic solvent such as benzene, dimethylbenzene has toxicity, and environment is caused disadvantageous effect, has limited the application and the popularization of aluminium nitride ceramic.So improve the anti-hydratability of powder, prepare can be in the aqueous solution finely dispersed aluminium nitride powder, the application of promoting aluminium nitride ceramic is had very significant meaning.
At present, to the existing correlative study of aluminium nitride powder hydration resistance, Shanghai Communications University turns round and look at bright unit etc. in " preventing the method for hydrolysis of aluminium nitride " (patent publication No.: propose CN1686946A) to utilize tetraethoxysilane solution to carry out immersion treatment, improve the powder hydration resistance; Chung, Shyan-Lung etc. are in " Surfacetreatment method for preparing water-resistant aluminum nitride powder " (Application No.: 20030118501) propose to use oleic acid, Resins, epoxy, surface-modifying agents such as polyurethane resin etc. are handled aluminium nitride powder, improve its hydration resistance, but existing achievement in research, the powder hydration resistance is not outstanding, and in water, easily reunite through the powder that anti-aquation is handled, can't effectively disperse, and obviously reduce at whipping process powder hydration resistance in the aqueous solution.
Summary of the invention
Technical problem to be solved by this invention is: for the powder hydration resistance in the high temperature wet environment that overcomes above-mentioned technology existence is not given prominence to; Easily reunite in water through the powder that anti-aquation is handled, high shear rate stirs the external parcel layer of destructible powder in the batch mixing process, make powder and water generation hydrolysis reaction, reduce the shortcomings such as nitrogen content of powder, propose a kind of novel method that improves the anti-hydratability of aluminium nitride powder.
Technical scheme of the present invention is: the present invention utilizes surface adsorption technology, at first make organic hydrophobic compound be adsorbed on the aluminium nitride powder surface, thereby the prevention water molecules contacts with aln surface, but because organic hydrophobic compound and water do not dissolve each other, therefore wrap up one deck nonionic surface active agent again at modifying powder surface, both improved the powder hydration resistance, make powder well to soak into again with water, then treated aluminium nitride powder is repeatedly cleaned with ethanolic soln, 80～100 ℃ of oven dry, promptly obtain the outstanding aluminium nitride powder of anti-hydratability.
Concrete technical scheme of the present invention is: the easy dispersive PREPARATION OF ALUMINUM NITRIDE POWDER of anti-aquation method, and its concrete steps are as follows:
It is benchmark that A handles the aluminium nitride powder gross weight with the anti-aquation of being prepared, take by weighing the weight percentage that accounts for above-mentioned total amount and be 85%～90% aluminium nitride powder and organic hydrophobic compound of 5%～12%, and adding organic solvent, the add-on of solvent is a benchmark with the weight of aluminium nitride powder, it is 1～3ml that every gram powder adds solvent, stir, be uniformly dispersed, leave standstill then;
It is benchmark that B handles the aluminium nitride powder gross weight with the anti-aquation of being prepared, and adds the weight percentage that accounts for total amount and be 3～5% nonionic surface active agent in said mixture, the stirring in water bath heating;
C filters mixture, and the aluminium nitride powder that filters out cleans with organic solvent;
Aluminium nitride powder after D will clean is dried, and obtains the aluminium nitride powder of anti-aquation.
Wherein said organic hydrophobic compound is hard ester acid, hexanodioic acid etc., preferred stearic acid; Nonionic surface active agent is the Brij92 type, ethoxylation methyl glucoside stearate type, tween 80 type (polyoxyethylenesorbitan sorbitan monooleate), polysorbas20 type (polyoxyethylene sorbitan mono laurate fat), preferred tween 80 type; Organic solvent is the easy evapourizing type solvent of low temperature, is preferably ethanol, acetone or ether.
Stirred in the steps A 2～4 hours, left standstill 1～2 hour.Adopt planetary mills to be uniformly dispersed in the steps A, rotating speed 188r/min, the time is 2～4 hours, or ultrasonic dispersing is even, and ultrasound intensity is 300～1500W, and ultrasonic time is 5～60min.Add the thermal recovery ultra thermostat among the step B, 60～80 ℃ of constant temperature, churning time 3～5 hours.Generally clean 2 ~ 4 times among the step C with organic solvent.Vacuum drying oven is adopted in oven dry among the step D, and storing temperature is 80～100 ℃, and storing time is 2～5 hours.
The prepared aluminium nitride powder water repelling property of this invention is given prominence to, by Fig. 1,2 (A: starting powder as can be known, B: the powder that anti-aquation is handled), the pH value that aluminium nitride powder that anti-aquation is handled and water prepare solution does not significantly improve with the variation of temperature and time, obvious hydrolysis does not take place in aluminium nitride powder, has stronger hydration resistance; By Fig. 3,4 as can be known, and powder can fully disperse in the aqueous solution, prepares the aluminium nitride slurry of good stability.
Beneficial effect:
1, the prepared aluminium nitride powder water repelling property of the present invention is given prominence to, powder keeps the stable hydrolysis reaction that do not take place in wet environment below 60 ℃, have good anti-hydratability, can effectively solve the difficulty that aluminium nitride powder brings in storage, transportation and follow-up technological process;
2, this technological operation is simple, and production cost is low;
3, the prepared aluminium nitride powder of the present invention can well soak into water, the nitrogen content of powder remains unchanged substantially in water medium high shear rate whipping process, its performance index are shown in table 1,2, the aluminium nitride powder of handling through anti-aquation can prepare slurry with water, prepares aluminium nitride ceramic by moulding process.
Table 1 is depicted as starting powder and anti-aquation and handles the changing conditions nitrogen content of powder soaks 48h in water after.As seen from table, the powder that the anti-aquation of process is handled soaks 48h in water after, its powder nitrogen content remains unchanged substantially,
Table 1 powder soaks the nitrogen content behind the 48h in water
| Test powders | Starting powder | Soak 48h in the starting powder water | Anti-aquation is handled powder | Anti-aquation is handled in the powder water and is soaked 48h |
| Nitrogen content (%) | 33.43％ | 3.25％ | 32.10％ | 31.91％％ |
Table 2 is depicted as nitrogen content that anti-aquation the handles powder changing conditions with milling time in water.As seen from table, the nitrogen content of powder in water of handling through anti-aquation under the grinding condition of long-time high shear rate remains unchanged substantially, and powder has stronger stability.
Table 2 milling time antagonism aquation is handled the nitrogen content influence of powder
| Milling time (h) | 1 | 2 | 3 | 4 |
| Anti-aquation is handled the nitrogen content (%) of powder | 31.89％ | 32.01％ | 31.84％ | 30.38％ |
Description of drawings:
Fig. 1 is powder pH value variation diagram, wherein A under different time: starting powder, B: the powder that anti-aquation is handled.
Fig. 2 is powder pH value variation diagram under differing temps.
Fig. 3 is the slurry shearing stress of different solid volume fractions and the relation curve of shearing rate.
Fig. 4 is the slurry shearing viscosity of different solid volume fractions and the relation curve of shearing rate.
Embodiment:
Further describe technical scheme of the present invention below by embodiment.
Embodiment 1:
1) 85g aluminium nitride powder and the hard ester acid soak of 10g in the 100ml ethanolic soln, and ceaselessly stirred 4 hours, left standstill then 1～2 hour;
2) in said mixture, add the 5g tween 80, in 60 ℃ of stirring in water bath heating 5 hours;
3) mixture is filtered, the aluminium nitride powder that filters out cleans for 3 times with ethanolic soln;
4) 80 ℃ of oven dry of the aluminium nitride powder after will cleaning 5h promptly obtains the exsertile aluminum nitride powder of hydration resistance.
Embodiment 2:
1) 90g aluminium nitride powder and 5g hexanodioic acid are immersed in the 200ml acetone soln, and ceaselessly stirred 3 hours, left standstill then 2 hours;
2) in said mixture, add 5g Brij92 type, in 80 ℃ of stirring in water bath heating 3 hours;
3) mixture is filtered, the aluminium nitride powder that filters out cleans for 4 times with acetone soln;
4) 100 ℃ of oven dry of the aluminium nitride powder after will cleaning 2h promptly obtains the exsertile aluminum nitride powder of hydration resistance.
Embodiment 3:
1) 85g aluminium nitride powder and the hard ester acid soak of 12g in the 200ml diethyl ether solution, and ceaselessly stirred 4 hours, left standstill then 2 hours;
2) in said mixture, add 3g ethoxylation methyl glucoside stearate, in 70 ℃ of stirring in water bath heating 3 hours;
3) mixture is filtered, the aluminium nitride powder that filters out cleans for 4 times with diethyl ether solution;
4) aluminium nitride powder after will cleaning dries by the fire in 4h for 80 ℃, promptly obtains the exsertile aluminum nitride powder of hydration resistance.
Embodiment 4:
1) 90 aluminium nitride powders and 5g hexanodioic acid are immersed in the 250ml ethanolic soln, and ceaselessly stirred 4 hours, left standstill then 2 hours;
2) in said mixture, add the 5g polysorbas20, in 70 ℃ of stirring in water bath heating 3 hours;
3) mixture is filtered, the aluminium nitride powder that filters out cleans for 4 times with ethanolic soln;
4) 100 ℃ of oven dry of the aluminium nitride powder after will cleaning 3h promptly obtains the exsertile aluminum nitride powder of hydration resistance.
Claims (9)
1, the easy dispersive PREPARATION OF ALUMINUM NITRIDE POWDER of anti-aquation method, its concrete steps are as follows:
A. handling the aluminium nitride powder gross weight with the anti-aquation of being prepared is benchmark, take by weighing the weight percentage that accounts for above-mentioned total amount and be 85%～90% aluminium nitride powder and organic hydrophobic compound of 5%～12%, and adding organic solvent, the add-on of solvent is a benchmark with the weight of aluminium nitride powder, it is 1～3ml that every gram powder adds solvent, stir, be uniformly dispersed, leave standstill then;
B. handling the aluminium nitride powder gross weight with the anti-aquation of being prepared is benchmark, adds the weight percentage that accounts for total amount and be 3～5% nonionic surface active agent in said mixture, the stirring in water bath heating;
C. mixture is filtered, the aluminium nitride powder that filters out cleans with organic solvent;
D. the aluminium nitride powder after will cleaning is dried, and obtains the aluminium nitride powder of anti-aquation.
2, method according to claim 1 is characterized in that organic hydrophobic compound is hard ester acid or hexanodioic acid; Nonionic surface active agent is Brij92 type, ethoxylation methyl glucoside stearate, tween 80 type or polysorbas20 type.
3, method according to claim 1 is characterized in that organic hydrophobic compound is a stearic acid; Nonionic surface active agent is the tween 80 type.
4, method according to claim 1 is characterized in that the organic solvent described in steps A, the C is the easy evapourizing type solvent of low temperature.
5, method according to claim 4 is characterized in that the easy evapourizing type solvent of described low temperature is ethanol, acetone or ether.
6, method according to claim 1 is characterized in that stirring in the steps A 2～4 hours, left standstill 1～2 hour.
7, method according to claim 1 is characterized in that adopting in the steps A planetary mills to be uniformly dispersed, rotating speed 188r/min, and the time is 2～4 hours; Or ultrasonic dispersing is even, and ultrasound intensity is 300～1500W, and ultrasonic time is 5～60min.
8, method according to claim 1 is characterized in that adding among the step B 60～80 ℃ of thermal recovery ultra thermostat constant temperature, churning time 3～5 hours.
9, method according to claim 1 is characterized in that vacuum drying oven is adopted in oven dry among the step D, and storing temperature is 80～100 ℃, and storing time is 2～5 hours.
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