CN106699189A - Aluminum nitride powder for aluminum nitride ceramic substrate and preparation method of aluminum nitride powder - Google Patents

Aluminum nitride powder for aluminum nitride ceramic substrate and preparation method of aluminum nitride powder Download PDF

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Publication number
CN106699189A
CN106699189A CN201611054095.0A CN201611054095A CN106699189A CN 106699189 A CN106699189 A CN 106699189A CN 201611054095 A CN201611054095 A CN 201611054095A CN 106699189 A CN106699189 A CN 106699189A
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aluminum nitride
aluminium nitride
nitride powder
preparation
powder
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CN106699189B (en
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杨志平
刘少鹏
张银霞
赵金鑫
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Hubei Ledphor Optoelectronics Technology Co Ltd
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Hubei Ledphor Optoelectronics Technology Co Ltd
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Abstract

The invention provides aluminum nitride powder for an aluminum nitride ceramic substrate and a preparation method of the aluminum nitride powder. The preparation method of the aluminum nitride powder comprises the following steps: (a) preparing a precursor mixture; (b) performing high temperature synthesis; (c) performing decarburization treatment; and (d) performing surface treatment. The preparation method provided by the invention is simple, low in synthetic temperature, pollution-free, and suitable for large-scale production. The invention also provides the aluminum nitride powder prepared with the method, the prepared aluminum nitride powder is good in water resistance, microelements required in a sintering process of an aluminum nitride substrate are uniformly distributed in the powder, and a more suitable powder particle size range is obtained by adjusting the usage amount of a sintering aid, thereby improving compactness, heat conductivity and shock resistance of the substrate.

Description

A kind of aluminum nitride ceramic substrate aluminium nitride powder and preparation method thereof
Technical field
The present invention relates to materials science field, and in particular to a kind of aluminum nitride ceramic substrate aluminium nitride powder and its Preparation method.
Background technology
With developing rapidly for modern electronic technology, it is desirable to which whole machine is towards miniaturization, lightness, high integration, highly reliable Property direction is developed.Device is more and more complicated simultaneously, substrate size will be caused to increase and integrated level raising again so that substrate dissipation work Rate increases, therefore, it is important problem that the radiating of substrate and the selection of material become.The thermal conductivity ratio oxygen of aluminium nitride ceramics Change aluminium ceramic high 8~10 times, the electric property such as specific insulation, disruptive field intensity, dielectric loss can match in excellence or beauty with aluminium oxide ceramics, and Dielectric constant is low, high mechanical strength, and thermal coefficient of expansion can carry out multilayer wiring close to silicon, and being considered as a new generation has good hair The superior isolation heat dispersion substrate material of exhibition prospect.
At present, the sintering of aluminum nitride ceramic substrate reduces substrate and sinters using sintering aid is added in aluminium nitride powder Required temperature (about 1900 DEG C), while improving the compactness and thermal conductivity of sintered body, the sintering method cost is relatively low and applies Study relatively broad, such as patent document WO97/03031, WO2005/092789.However, due to the mobility of aluminium nitride powder Very poor, the doping of sintering aid generally requires high intensity and prolonged mixing process, or is carried out using some liquid phase schemes Batch mixing, compounding effect is also very limited, and the performance of obtained substrate is also undesirable.Patent document CN201110349484.7 uses liquid , be evenly distributed on the elements such as Al, Y in carbon source by citric acid and ethylene glycol by phase method batch mixing, has obtained that particle diameter is tiny, component is equal Even Y dopen Nano aluminium nitride powders；CN00120742.3 is then that the required metal such as Al and Li, Y is smelt into alloy, then carries out nitrogen Change, obtain the composite nitride aluminium powder body containing sintering aid.Preparation method disclosed in above-mentioned patent document will nitrogenize aluminum sinter base Auxiliary agent needed for plate is just joined when aluminium nitride powder synthesizes, and auxiliary agent is more held compared to being added during sintered base plate Easily it is evenly distributed.Relatively costly however, above-mentioned preparation method is complex, raw material used is more difficult to be sought or is relatively difficult to ensure and deposit, this Outward, used organic reagent easily causes harm to human body and environment, and obtained aluminium nitride powder doped chemical is not enough, The problems such as uneven batch mixing and undesirable obtained substrate performance are still suffered from during preparing substrate.
The content of the invention
It is existing to solve it is an object of the invention to provide a kind of aluminum nitride ceramic substrate aluminium nitride powder and preparation method thereof Aluminium nitride powder is difficult to uniformly with sintering aid batch mixing in having aluminium nitride substrate sintering process, substrate shock resistance, thermal conductivity and cause The problems such as close property is undesirable.
The purpose of the present invention is achieved through the following technical solutions：A kind of aluminum nitride ceramic substrate aluminium nitride powder Preparation method, comprises the following steps：
(a), prepare precursor mixture：It is 20~50nm to weigh the alumina powder, particle diameter that particle diameter is 0.8~1.2 μm Carbon black, the sintering aid that particle diameter is 1~10 μm, each raw material that will be weighed is sufficiently mixed, and prepares the uniform presoma of batch mixing Mixture；
(b), high―temperature nuclei：Precursor mixture is put into sintering furnace, nitrogen is filled with as reaction gas after excluding air Atmosphere, 2~5h of soaking time under the conditions of being 1500~1600 DEG C in temperature, obtains aluminium nitride powder crude product；
(c), carbonization treatment：Aluminium nitride powder crude product is incubated 2-5h in decarbonizing furnace under the conditions of 600~700 DEG C, is removed Remove unnecessary carbon black；
(d), surface treatment：Carried out being dispersed in organic phosphoric acid compound through the aluminium nitride powder crude product after carbonization treatment Surface treatment, that is, obtain aluminum nitride ceramic substrate aluminium nitride powder.
In the preparation method that the present invention is provided, in step (a), be also weighed out when precursor mixture is prepared particle diameter for 1~ 10 μm of additive, described alumina powder, carbon black, sintering aid and additive are sufficiently mixed uniformly, obtain presoma Mixture.
In the preparation method that the present invention is provided, the sintering aid described in step (a) is rare earth metal, alkali metal, alkaline earth gold The group of one or more compounds in category, the halide of Zn, Cu, Cr, Mn, oxide or its corresponding alkali, carbonate Close；It is preferred that sintering aid is the fluoride of Y, Lu, Ce, Zn, Mn, Ca, Ba element or one or more group of oxide Close.
In the preparation method that the present invention is provided, the additive described in step (a) is BN, Si3N4、TiO2、ZrO2、HfO2、 Ga2O3In one or more combination；Preferable additives are BN, Si3N4、TiO2In one or more group Close, be improved significantly using the corresponding substrate shock resistance of aluminium nitride powder obtained in preferable additives.The addition of additive It is carbon black and 2~10wt% of alumina powder total amount.
In the preparation method that the present invention is provided, the carbon black and the weight ratio of alumina powder weighed in step (a) are 0.38 ~0.50：1, sintering aid is 0.5~10wt% of carbon black and alumina powder total amount.
In the preparation method that the present invention is provided, the mixing of each raw material uses wet ball grinding hybrid mode in step (a), will claim The raw material for taking 8~24h of ball milling in absolute ethyl alcohol, then dries under the conditions of 50~80 DEG C, sieving.
In the preparation method that the present invention is provided, sintering furnace described in step (b) is preferably corundum tube furnace.It can be quick Air in powder and stove is removed, reaction is in anoxybiotic state.
The present invention provide preparation method in, organic phosphoric acid compound described in step (d) be hydroxy ethylidene-diphosphate, One or more in di(2-ethylhexyl)phosphate ethamine, phosphate amine salt, wherein hydroxy ethylidene-diphosphate is necessary.Through organic phosphoric acid Aluminium nitride powder has good water resistance after compound is surface-treated.
Present invention also offers a kind of aluminum nitride ceramic substrate aluminium nitride powder, the powder is by above-mentioned preparation method system , it is uniformly distributed in the aluminium nitride powder by the introduced element of sintering aid and additive.
Aluminium nitride powder prepared by the present invention can be used manufacture substrate, and the preparation method for being provided can make sintering nitrogen Trace element needed for changing aluminium base is more uniformly distributed in aluminium nitride powder, improve institute's sintered aluminum nitride substrate shock resistance, Compactness and thermal conductivity.
The present invention is doped with specific sintering aid and additive, in nitrogen atmosphere based on Ultrafine Aluminium Oxide Particle Lower use carbothermic method has synthesized the aluminium nitride powder for being evenly distributed with trace element needed for aluminum nitride ceramic substrate sintering.This Invention is used as sintering and is helped by appropriate mix the element compounds such as rare earth metal, alkali and alkaline earth metal ions one or more Agent, temperature needed for not only reducing reaction, the aluminium nitride powder for having obtained granularity for 2-3.5 μm and being evenly distributed additionally makes Part trace element needed for synthesis substrate is uniformly distributed in the powder；By BN, Si3N4、TiO2Deng the doping of additive, Reduce further synthesis aluminium nitride substrate during crystal defect generation and inhibit its particle too to grow up, make particle More even compact.
Specifically, the present invention has beneficial effect following prominent：
(1) composition of trace element needed for synthesis aluminium nitride substrate is optimized, and these trace elements is advanceed into powder Added during generation, aluminum oxide compares aluminum nitride particle, batch mixing is simpler and more uniform, uniform point of trace element after treatment Cloth simplifies the production technology of corresponding aluminium nitride substrate in aluminium nitride powder.
(2) compound of the element such as selection Y, Lu, Ce, Zn, Mn, Ca, Ba reduces aluminium nitride synthesis as sintering aid Required temperature, and these elements are evenly distributed in aluminium nitride powder, in sintered aluminum nitride substrate, as nucleus, Improve the compactness and thermal conductivity of substrate.
(3) BN, Si are selected3N4、TiO2、ZrO2、HfO2、Ga2O3Deng as additive, the nitrogen for making it be evenly distributed on generation Change in aluminium powder body, the crystal defect of aluminium nitride, control aluminum nitride crystal growth to suitable grain are made up during sintered base plate Degree, makes the anti-seismic performance of institute's sintered base plate more preferably.
Aluminum nitride powder preparation provided by the present invention is simple and easy to apply, low for equipment requirements, pollution-free, low cost, Low-carbon environment-friendly modern production requirement is disclosure satisfy that, is adapted to large-scale industrial production.Prepared aluminium nitride powder, can burn The substrate of excellent performance is born, and as LED illumination heat dispersion substrate or large scale integrated circuit heat dispersion substrate extensive use.
Specific embodiment
The preparation method in the present invention is described in detail with reference to specific embodiment, and obtained aluminium nitride powder is made Aluminium nitride base carries out the evaluation of correlated performance, wherein, fracture toughness is measured using indentation method, and crystal grain D50 is by laser particle size analysis Instrument is measured, and relative density measures the ratio between density and theoretical value for density of solid tester, and thermal conductivity is measured by thermal conductivity factor instrument.
Comparative example 1
By commercially available high purity silicon nitride aluminium and the Y of aluminium nitride total amount 4%wt2O3The ultrasonic disperse 30min under ethanol medium, so Add ball grinder ball milling 10h, ball milling to dry 4h after 80 DEG C afterwards, cross 200 mesh sieves, mixture is pressed into graphite grinding tool after sieving, Pressure as 5MPa is set, grinding tool lays graphite paper with graphite contact scope, and BN releasing agents are coated on graphite paper surface, in nitrogen gas The lower 1800 DEG C of sintering 4h of atmosphere, nitrogen pressure is 9.8MPa, and room temperature is cooled to after the completion of sintering, obtains aluminium nitride base.To aluminium nitride base Correlated performance test is carried out, as a result as shown in table 1.
Embodiment 1
It is 0.45 by commercially available superfine alumina powder and quality of alumina ratio:The carbon black of 1 ratio, sintering aid (Y2O3 3.2wt%, LuF3Ethanol medium ball grinder is put into after 2wt%) weighing well, then ball milling 10h dries 4h for 80 DEG C, cross 200 mesh Sieve, obtains precursor mixture, then puts it into aluminum oxide Noah's ark crucible, load level corundum tube furnace, 1600 DEG C of sintering 4h, Then the powder that will be obtained again is placed in alumina crucible, in carbonization treatment 2h, gained powder under 700 DEG C of air atmospheres of batch-type furnace 200 mesh sieves are crossed, then it is soaked into 2h in hydroxy ethylidene-diphosphate solution, filtered, dried, sieving.Then by gained powder Press-in graphite grinding tool, sets pressure as 5MPa, and grinding tool lays graphite paper with graphite contact scope, and graphite paper surface is coated BN and taken off Mould agent, 1800 DEG C sinter 4h in a nitrogen atmosphere, and nitrogen pressure is 9.8Mpa, and room temperature is cooled to after the completion of sintering, obtains aluminium nitride Base.Correlated performance test is carried out to aluminium nitride base, as a result as shown in table 1.
Embodiment 2-18
Change the species of sintering aid and corresponding amount (being specifically shown in Table 1), other raw materials and method with embodiment 1, to most The aluminium nitride base for sintering into eventually carries out correlated performance test, as a result as shown in table 1.
Table 1：
As shown in Table 1, the appropriate addition of sintering aid provided by the present invention, can effectively improve aluminium nitride powder and be burnt The performance of the aluminium nitride base of knot, its combination property is superior to comparative example 1, alkali or carbonate in sintering aid of the present invention Compound can be converted into corresponding oxide at high temperature, thus can have same effect；Present invention optimizes synthesis aluminium nitride The composition of trace element needed for substrate, the introducing of the respective compound of these elements can promote Al2O3To in AlN transition processes Generation eutectic so that aluminum nitride grain is of moderate size and more uniform in generating process.
Knowable to comparative example 1 and embodiment 15, sintering aid is just added using in aluminium nitride powder synthesis phase, can made final The aluminium nitride substrate performance of sintering is strengthened, and its reason is that aluminium nitride powder production method provided by the present invention mixes Y etc. Enter element and disperse more uniform (mobility of aluminum oxide is far better compared with aluminium nitride) in final aluminium nitride powder, so that During sintered base plate, nucleation process is more uniform, reduces the mistake big crystal grain in final substrate and crosses little crystal grain, makes Hole between crystal grain and crystal grain is reduced, and increased the compactness of substrate, improves the fracture toughness of substrate, therefore, the present invention The preparation method for being provided is more suitable for preparing the aluminium nitride powder for aluminium nitride substrate.
Embodiment 19-28
When precursor mixture is prepared, add the additive (being specifically shown in Table 2) of variety classes and consumption, other raw materials and Method is same as Example 1.Aluminium nitride base to finally sintering into carries out correlated performance test, as a result as shown in table 2.
Table 2：
As shown in Table 2, the appropriate of additive makes obtained aluminium nitride base performance more preferably, and the covalent bond of Al is more with other The complicated combination of covalent bond Element generation, reduces the hole between aluminum nitride grain and crystal grain, improves correspondence aluminium nitride The compactness of base, so as to improve its fracture toughness, wherein BN, Si3N4、TiO2Using effect the most protrude.Additionally, very few Additive using relative without DeGrain, and excessive addition can change the basic property of AlN, do not meet and add Plus the original intention of agent doping.
Embodiment 29-32
Embodiment 29-32 changes the sintering temperature during synthesis aluminium nitride powder in embodiment 19 based on embodiment 19 Degree (being specifically shown in Table 3), other raw materials and method do not change, and the aluminium nitride base to finally sintering into carries out correlated performance test, Result is as shown in table 3.
Table 3：
As known from Table 3, the sintering temperature of preparation method provided by the present invention is relatively low, and temperature is at 1500~1600 DEG C When, aluminium nitride base performance obtained in gained aluminium nitride powder preferably, this be because sintering aid and other raw materials generate eutectic, Make required sintering temperature reduction；Sintering temperature be 1350 DEG C when, due in gained powder also have largely have neither part nor lot in reaction C or The presence of O elements and sintering aid, is difficult to detect, poor effect after being made aluminium nitride base；After temperature is slightly higher, reaction is entered OK, but grain growth is smaller, compactness and fracture toughness and thermal conductivity have larger gap compared with 1600 DEG C, and it is too high to work as temperature When, due to the presence of sintering aid, substantially, excessive crystal grain directly affects properties of product, crystal grain to the particle diameter change trend of crystal grain It is proper between 2-3.5 μm.
Embodiment 33-37
Embodiment 33-37 adjusts the amount of sintering aid based on embodiment 19, it is ensured that sintering aid Y in embodiment 192O3 And LuF3(Y in the case of constant rate2O3：LuF3=1.6：1) total amount (being specifically shown in Table 4) of sintering aid, is changed, other are former The method of material is identical with embodiment 19.Aluminium nitride base to finally sintering into carries out correlated performance test, as a result as shown in table 4.
Table 4：
As shown in Table 4, sintering powder during adulterate very few sintering aid when, it is similar when situation and relatively low sintering temperature Seemingly, aluminum nitride crystal is grown up and is limited, and too small monocrystalline makes aluminium nitride base have substantial amounts of hole, and effect is poor, and excessive burning Knot auxiliary agent can make grain size depart from optimum range so that the thermal conductivity and compactness of aluminium nitride base are greatly lowered, and sintering is helped In 0.5~10wt%, can guarantee that the aluminium nitride base of final sintering has preferably performance for agent.

Claims (10)

1. a kind of preparation method of aluminum nitride ceramic substrate aluminium nitride powder, it is characterized in that, comprise the following steps：
（a）, prepare precursor mixture：Weigh the alumina powder that particle diameter is 0.8~1.2 μm, the charcoal that particle diameter is 20~50 nm Black, particle diameter is 1~10 μm of sintering aid, and each raw material that will be weighed is sufficiently mixed, and prepares the uniform presoma mixing of batch mixing Thing；
（b）, high―temperature nuclei：Precursor mixture is put into sintering furnace, is protected in nitrogen atmosphere, under the conditions of 1500~1600 DEG C Warm 2~5h of time, obtains aluminium nitride powder crude product；
（c）, carbonization treatment：Aluminium nitride powder crude product is incubated 2-5h in decarbonizing furnace under the conditions of 600~700 DEG C, is removed many Remaining carbon black；
（d）, surface treatment：Surface is carried out by being dispersed in organic phosphoric acid compound through the aluminium nitride powder crude product after carbonization treatment Treatment, that is, obtain aluminum nitride ceramic substrate aluminium nitride powder.
2. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 1, it is characterized in that, step （a）In, the additive that particle diameter is 1~10 μm is also weighed out when precursor mixture is prepared, by described alumina powder, charcoal Black, sintering aid and additive are sufficiently mixed uniformly, obtain precursor mixture.
3. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 1 and 2, it is characterized in that, step Suddenly（a）Described sintering aid be rare earth metal, alkali metal, alkaline-earth metal, the halide of Zn, Cu, Cr, Mn, oxide or its The combination of one or more compounds in corresponding alkali, carbonate.
4. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 3, it is characterized in that, step （a）Described sintering aid for Y, Lu, Ce, Zn, Mn, Ca, Ba element fluoride or oxide one or more Combination.
5. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 2, it is characterized in that, step （a）Described additive is BN, Si3N4、TiO2、ZrO2、HfO2、Ga2O3In one or more combination, additive Addition is 2 ~ 10wt% of carbon black and alumina powder total amount.
6. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 5, it is characterized in that, step （a）Described additive is BN, Si3N4、TiO2In one or more combination, the addition of additive for carbon black and 2 ~ 10wt% of alumina powder total amount.
7. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 1 and 2, it is characterized in that, step Suddenly（a）In the weight ratio of the carbon black that weighs and alumina powder be 0.38~0.50：1, sintering aid is carbon black and alumina powder 0.5~10wt% of last total amount.
8. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 1 and 2, it is characterized in that, step Suddenly（a）In each raw material mixing use wet ball grinding hybrid mode, the raw material that will be weighed 8~24h of ball milling in absolute ethyl alcohol, so Dried under the conditions of 50~80 DEG C afterwards, sieving.
9. the preparation method of aluminum nitride ceramic substrate aluminium nitride powder according to claim 1, it is characterized in that, step （d）Described in organic phosphoric acid compound be hydroxy ethylidene-diphosphate, di(2-ethylhexyl)phosphate ethamine, phosphate amine salt in one kind or one kind with On, wherein hydroxy ethylidene-diphosphate is necessary.
10. a kind of aluminum nitride ceramic substrate aluminium nitride powder, it is characterized in that, the powder is by any preparation in claim 1 ~ 9 Method is obtained, and is uniformly distributed in the aluminium nitride powder with the introduced element of additive by sintering aid or sintering aid.
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