CN107365155A - A kind of low-temperature sintering adjuvant system of aluminium nitride ceramics - Google Patents
A kind of low-temperature sintering adjuvant system of aluminium nitride ceramics Download PDFInfo
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Abstract
The present invention relates to a kind of low-temperature sintering adjuvant system of aluminium nitride ceramics, the low-temperature sintering adjuvant system includes component A and component B；The component A is TiO2、ZrO2、HfO2At least one of；The component B is V2O5、Nb2O5、Ta2O5At least one of.Sintering aid scheme proposed by the present invention, compared with the scheme of current document report, the densification process of material, simple and reliable process can be realized in the short period of time, and higher thermal conductivity can be obtained.
Description
Technical field
The present invention proposes a kind of sintering temperature for aluminium nitride ceramics sintering temperature height, the problem that sintering time is long, cost is high
The sintering aid system that low, soaking time is short, can effectively realize densification is spent, belongs to the preparation technology and application neck of ceramics
Domain.
Background technology
With the development of modern science and technology, the particularly development of Electronic Encapsulating Technology, the increase of power electronic devices integrated level,
And the application of LED illumination, radiating turn into key issue urgently to be resolved hurrily.If caused heat can not dissipate in time, can
Cause semiconductor chip temperature to rise, cause electronic device performance unstable, or LED junction temperature rises, and causes under luminous efficiency
Drop, the lost of life.Heat dissipation problem has become the key for restricting electronic power parts and great power LED application at present.Conventional
Baseplate material has Al2O3, BeO, SiC and AlN.A12O3Ceramics are current using Ceramic Substrate Material the most ripe, its price
Cheap, resistance to sudden heating and electrical insulation capability are preferable, make and process technology is ripe, thus use is most extensive, accounts for ceramic substrate
The 90% of material.But Al2O3Thermal conductivity there was only 22-28W/mK or so, the radiating requirements of great power LED far can not be met.
The thermal conductivity of carborundum (SiC) ceramics is high, and thermal coefficient of expansion is the most close with Si, but its poor insulativity, and sinters difficult, it is difficult to
Fine and close product is made.Although by adding a small amount of beryllium oxide sintering aid and can obtain height using the method for hot pressed sintering
The SiC substrate (270W/mK) of heat conduction, but its loss is big, and hot pressing cost is high, limits its development and high volume applications.BeO
Ceramics are the best ceramic substrate materials of current heat conductivility, and its synthesis dielectric properties is good, but its thermal conductivity rises with temperature
It can decline to a great extent, BeO toxicity is larger in addition, limits its use, has not allowed BeO to produce in Japan at present, in Europe
Have started to limit the electronic product containing BeO.
AlN ceramic is a kind of novel encapsulated material unanimously being had an optimistic view of by domestic and international expert, and it has excellent electric heating property.
Compared with aluminum oxide, aluminium nitride has high thermal conductivity, is 5~10 times of aluminum oxide, is adapted to high power, high lead and big chi
Very little chip；Its thermal coefficient of expansion matches with silicon, and dielectric constant is relatively low；Material high mechanical strength.AlN ceramic as it is highly thermally conductive,
Highly dense closure material has very big development potentiality, is the important development direction of ceramic packaging material research.It is contemplated that in substrate and
Two big fields are encapsulated, AlN ceramic most substitutes current Al at last2O3With BeO ceramics.
But because aluminium nitride powder cost is higher, sintering is difficult, causes the cost of aluminium nitride chip to remain high, nothing
Method meets LED industry low cost, the application demand of mass.Aluminium nitride powder price domestic at present is relatively low, although oxygen content
It is higher, but can meet LED application demand, it is crucial the problem of be to reduce sintering cost.
Aluminium nitride ceramics is non-oxide ceramicses, and pure aluminium nitride is difficult densified sintering product at high temperature, it usually needs addition is burnt
Tie auxiliary agent.The main function of sintering aid is that the oxidation reactive aluminum with aln surface in sintering process generates answering for low melting point
Oxide is closed, liquid phase is produced and surrounds aluminium nitride powder, reach wetting, stickup, tension, the purpose of surface active, promote base substrate to cause
Densification；Secondly, even in liquid phase is distributed near aluminium nitride crystal boundary and three phase point, is formed oxygen trap, can be captured the oxygen in aluminium nitride,
It is segregated in after cooling at three phase point so that aluminum nitride grain can be in close contact, and reach the mesh for improving aluminium nitride ceramics thermal conductivity
's.The conventional sintering aid of AlN ceramic mainly has Y at present2O3、CaO、Er2O3、Yb2O3、Sm2O3、Dy2O3、Li2O、B2O3、CaF2、
YF3、CaC2Deng or be used in mixed way, the sintering of AlN powders can not only be effectively facilitated, and contribute to carrying for sintered products thermal conductivity
It is high.But usual sintering temperature is 1700-1850 DEG C, soaking time is longer, and sintering cost is very high.And LED development, especially
It is the development in domestic lighting field, it is necessary to constantly reduce cost, reaches the cost water suitable with current fluorescent lamp or incandescent lamp
It is flat, it can introduce to the market.Cost Problems turn into the key factor that limitation aluminium nitride chip is applied in LED field at present.
Low-temperature sintering can effectively reduce sintering cost, be one of domestic and international focus of attention.There is lot of documents report
Road.Conventional sintering aid system has Y2O3With CaO or Y2O3, CaO, Li2O, other rare earth oxides can also be used such as
Dy2O3Substitute Y2O3, with CaF2Substitute CaO, with Li2CO3Substitute Li2O etc..These sintering aid systems generally require the guarantor grown very much
The warm time, and liquid phase can be generated with aluminum oxide after Ca introducings, there is good wetability to AlN particles, often lead to heat
Conductance declines seriously, more can not effectively reduce cost.
The content of the invention
In view of the above-mentioned problems, the present invention proposes a kind of low-temperature sintering adjuvant system for aluminium nitride ceramics, it is described low
Warm sintering aid system includes component A and component B；
The component A is TiO2、ZrO2、HfO2At least one of, preferably TiO2、ZrO2、HfO2In one kind；
The component B is V2O5、Nb2O5、Ta2O5At least one of, preferably V2O5、Nb2O5、Ta2O5In one kind.
A kind of sintering research of the present invention based on long-term aluminium nitride ceramics, it is proposed that new sintering aid system.Using two
First component, component A include TiO2, ZrO2, HfO2At least one of；B component includes V2O5, Nb2O5, Ta2O5In at least one
Kind.Liquid phase can be formed in lower temperature as sintering aid, wherein the sintering aid system using combinations thereof, utilize liquid
Phase acceleration of sintering, meanwhile, sintering aid system and oxa- qualitative response form aluminate, separate out the second phase during cooling, utilize second
Mutually oxygen is consolidated on crystal boundary, reduces the oxygen content of sintered body, is advantageous to improve the thermal conductivity of aluminium nitride ceramics.
It is preferred that the component A and component B mass ratio is 1：(1~5).During the span, crystal boundary is advantageously reduced
The viscosity of phase, promote low-temperature sintering, and ensure the thermal conductivity of aluminium nitride ceramics.
It is preferred that the particle diameter distribution of the low-temperature sintering adjuvant system is 50nm~50 micron.
On the other hand, present invention also offers a kind of preparation method of aluminium nitride ceramics, including：
Aluminium nitride powder and above-mentioned temperature sintering aid system are dissolved in organic solvent, add dispersant, binding agent, plasticity
Uniformly mixed after agent, be made base substrate, the mass ratio of the aluminium nitride powder and low-temperature sintering adjuvant system is (90~95)：(5~
10)；
Gained base substrate is calcined into 1-12 hours at 1600~1700 DEG C, obtains aluminium nitride ceramics.
Specifically, low-temperature sintering auxiliary agent proposed by the present invention has the characteristics that.First, the sintering aid will not be dissolved
Into aluminium nitride lattice, the degradation of the aluminium nitride thermal conductivity caused by solid solution is avoided；Secondly, the sintering aid system can be with
Low temperature liquid phase is generated in sintering process, effective wetting aluminium nitride ceramics particle surface, promotes particle re-arrangement and sintering process, drop
Sintering temperature and low (1600~1700 DEG C)；Densification process can also be realized within the shorter time (1-2 hours).In addition,
After sintering, the wetability of the sintering aid and aluminum nitride particle is poor, easily moves back to three trouble grain boundary sites, it is ensured that nitridation
Aluminium grain can be contacted with each other, and condition is created for the thermal conductivity control of aluminium nitride ceramics.Therefore, using burning proposed by the present invention
Adjuvant system is tied, the densification process of aluminium nitride ceramics can be realized in the short period of time, be high heat conduction aluminium nitride ceramics body
The preparation of system is laid a good foundation.
It is preferred that the organic solvent is ethanol, butanone, toluene, n-hexane, methanol, dimethylbenzene, normal propyl alcohol and n-butanol
At least one of, preferably ethanol/butanone, ethanol/toluene, ethanol/n-hexane, butanone/methanol, dimethylbenzene/normal propyl alcohol or
Dimethylbenzene/n-butanol, addition are 15~30wt% of the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system.
It is preferred that the dispersant is olein, phosphate ester, castor oil herring oil, ascorbic acid and terpinol
At least one of, addition is 0.5~4wt% of the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system.
It is preferred that the binding agent is polyvinyl butyral resin or/and polymethyl methacrylate, addition is aluminium nitride
6~9wt% of the gross mass of powder and low-temperature sintering adjuvant system.
It is preferred that the plastic agent is the dibutyl phthalate DBP or/and fourth Bian ester BBP of phthalic acid two, add
Measure 7~12wt% of the gross mass for aluminium nitride powder and low-temperature sintering adjuvant system.
It is preferred that the heating rate of the calcining is 1~15 DEG C/min.It is preferred that the particle diameter of the aluminium nitride powder is
100nm~10 μm.
Another further aspect, present invention also offers a kind of aluminium nitride ceramics prepared according to above-mentioned method.
Sintering aid scheme proposed by the present invention, compared with the scheme of current document report, can be in the short period of time
The densification process of material, simple and reliable process are realized, and higher thermal conductivity can be obtained.Burnt so as to substantially reduce
Form this.The present invention is applied to the low-temperature sintering of aluminium nitride ceramics, disclosure satisfy that each side such as industry, Aeronautics and Astronautics and national defence
Demand.Heretofore described system in relatively low temperature, can realize the sintering of aluminium nitride ceramics within a short period of time,
Consistency reaches more than 99%.
Embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
The present invention sinters the problem of cost is high for aluminium nitride ceramic substrate, in order to further shorten sintering time, reduces
Sinter cost, there is provided a kind of new low-temperature sintering adjuvant system for aluminium nitride ceramics.The sintering aid includes two kinds of groups
Point：Component A and component B.Described sintering aid component A is transition elements oxide of mutually, including TiO2、ZrO2、HfO2Deng.It is described
Sintering aid component B be high-valence state transition elements oxide of mutually, including V2O5、Nb2O5、Ta2O5Deng.Wherein, component A and component B
Weight ratio can be 1:1 to 1:5.The grain diameter of two kinds of sintering aids (component A and component B) is from 50nm to 50 micron.Total
For, the bi-component transition metal of the present invention for the low sintering sintering aid system of aluminium nitride ceramics using low cost
Oxide generates liquid phase by low temperature, promotes mass transport process, reach densification as complex sintering aids system.And liquid phase exists
Crystalline phase can be generated after sintering, the thermal conductivity of ceramics is influenceed smaller.Low-temperature sintering adjuvant system proposed by the present invention, not only into
This is relatively low, and can effectively realize the low-temperature sintering of aluminium nitride ceramics, smaller to the Effect of Thermal Performance of final aluminium nitride ceramics.
Preparation and LED field application suitable for inexpensive aluminium nitride ceramic substrate.
Low-temperature sintering scheme proposed by the present invention, simple and reliable process, cost is low, easy operation.It is suitable for aluminium nitride pottery
The low-temperature sintering of porcelain.Illustrate to following exemplary the preparation method of aluminium nitride ceramics provided by the invention.
Ceramic powder and sintering aid are mixed, disperseed in organic solvent.Specifically, by aluminium nitride powder and above-mentioned
Low-temperature sintering adjuvant system is dissolved in organic solvent, is uniformly mixed after adding dispersant, binding agent, plastic agent, base is made
The mass ratio of body, the aluminium nitride powder and low-temperature sintering adjuvant system can be (5~10)：(90~95).It is proposed by the present invention
Low-temperature sintering adjuvant system includes component A (TiO2、ZrO2、HfO2Deng) and component B (V2O5、Nb2O5、Ta2O5Deng).Component A and group
The weight ratio for dividing B can be 1:1 to 1:5.The particle diameter of the aluminium nitride powder can be 100nm~10 μm.In addition, the side of base substrate is made
Method, the methods of including but are not limited to flow casting molding, dry-pressing formed, cold isostatic compaction, gel casting forming.
In the present invention, the organic solvent can be ethanol, butanone, toluene, n-hexane, methanol, dimethylbenzene, normal propyl alcohol and just
At least one of butanol, preferably ethanol/butanone, ethanol/toluene, ethanol/n-hexane, butanone/methanol, dimethylbenzene/positive third
Alcohol or dimethylbenzene/n-butanol.Its addition can be the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system 15~
30wt%.
In the present invention, conventional dispersant is olein, phosphate ester, castor oil herring oil, ascorbic acid, pine tar
Alcohol etc., addition can be 0.5~4wt% of the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system.
In the present invention, conventional binding agent has polyvinyl butyral resin, polymethyl methacrylate etc., and its addition can be
6~9wt% of the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system.
In the present invention, conventional plastic agent has dibutyl phthalate (DBP), the fourth Bian ester (BBP) of phthalic acid two,
Its addition can be 7~12wt% of the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system.
Gained base substrate is calcined 1~12 hour at 1600~1700 DEG C, obtains aluminium nitride ceramics.The heating of the calcining
Speed is 1~15 DEG C/min.
The present invention uses Archimedes's drainage-measure the consistency of aluminium nitride ceramics as 99~99.5%.The present invention adopts
The thermal conductivity that aluminium oxide ceramics is measured with laser conductometer is 130~160Wm-1·K-1。
The present invention proposes using the method for low-temperature sintering auxiliary agent to reduce sintering cost, can be in 1600-1700 DEG C of temperature
In the range of sintering obtain fine and close aluminium nitride ceramics.The conventional low-temperature sintering auxiliary agent reported both at home and abroad is compared, and this sintering aid can
To use the method for Fast Sintering, the densification of material is realized within the relatively short time, so as to substantially reduce sintering cost,
Application for AlN ceramic substrate creates conditions.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.If without specified otherwise, aluminium nitride in following embodiments
The particle diameter of powder is generally 100nm~10 μm.The particle diameter distribution of the low-temperature sintering adjuvant system is 50nm~50 micron.
Embodiment 1
By 95g aluminium nitride powders and 5g sintering aids titanium oxide, vanadium oxide addition 21g ethanol/butanone solvent system (ethanol and
Acetone quality ratio is 40：60) in, the ratio of titanium oxide and vanadium oxide is 1:1.Using 2g oleins as dispersant,
It is binding agent that 8g PVB are added after ball milling, and 8g DBP are plastic agent, deaeration, curtain coating after ball milling, and prepare thickness 0.15- again
0.2mm casting films.Sintered after casting films unsticking in carbon shirt-circuiting furnace, reach 1650 DEG C with 5 DEG C/min heating rate, be incubated 2h
Realize sintering.Fine and close, complete aluminium nitride chip can be obtained.
Embodiment 2
By 94g aluminium nitride powders and 6g sintering aids titanium oxide, niobium oxide addition 21g ethanol/toluenes dicyandiamide solution (ethanol and
Toluene mass ratio is 40：60) in, the ratio of titanium oxide and niobium oxide is 1:2.Using 2.5g phosphate esters as dispersant, ball milling
It is binding agent to add 8.5g PVB afterwards, and 9g DBP are plastic agent, deaeration, curtain coating after ball milling, and prepare thickness 0.15- again
0.2mm casting films.Sintered after casting films unsticking in carbon shirt-circuiting furnace, reach 1650 DEG C with 5 DEG C/min heating rate, be incubated 2h
Realize sintering.Fine and close, complete aluminium nitride chip can be obtained.
Embodiment 3
By 93g aluminium nitride powders and 7g sintering aids titanium oxide, tantalum oxide addition in 21g ethanol/n-hexane dicyandiamide solution (ethanol
It is 50 with n-hexane mass ratio：50) in, the ratio of titanium oxide and tantalum oxide is 1:3.Using 2.0g castor oil as dispersant,
It is binding agent that 9g PVB are added after ball milling, and 10g DBP are plastic agent, deaeration, curtain coating after ball milling, and prepare thickness again
0.15-0.2mm casting films.Sintered after casting films unsticking in carbon shirt-circuiting furnace, reach 1650 DEG C with 5 DEG C/min heating rate
Degree, insulation 2h realize sintering.Fine and close, complete aluminium nitride chip can be obtained.
Embodiment 4
By 92g aluminium nitride powders and 8g sintering aids zirconium oxide, niobium oxide addition 21g butanone/methanol solvent system (butanone and
Methanol quality ratio is 50：50) in, the ratio of zirconium oxide and niobium oxide is 1:4.Using 2g ascorbic acid as dispersant, ball milling
It is binding agent to add 7.5g PVB afterwards, and 8.5g BBP are plastic agent, deaeration, curtain coating after ball milling, and prepare thickness 0.15- again
0.2mm casting films.Sintered after casting films unsticking in carbon shirt-circuiting furnace, 1650 DEG C of insulation 2h are reached with 5 DEG C/min heating rate
Realize sintering.Fine and close, complete aluminium nitride chip can be obtained.
Embodiment 5
By 90g aluminium nitride powders and 10g sintering aids hafnium oxide, niobium oxide addition in 21g dimethylbenzene/normal propyl alcohol dicyandiamide solution
(dimethylbenzene and normal propyl alcohol mass ratio are 50：50) in, the ratio of hafnium oxide and niobium oxide is 1:5.Using the oleics of 1.8g tri-
It is binding agent that ester adds 8.5g PVB as dispersant, after ball milling, and 10g BBP are plastic agent, again deaeration after ball milling, be cast,
And prepare thickness 0.15-0.2mm casting films.Sintered after casting films unsticking in carbon shirt-circuiting furnace, with 5 DEG C/min heating rate
Reach 1650 DEG C, insulation 2h realizes sintering.Fine and close, complete aluminium nitride chip can be obtained.
Table 1 is the preparation method and performance parameter of gained aluminium nitride chip in 1-5 of the embodiment of the present invention：
。
Claims (10)
- A kind of 1. low-temperature sintering adjuvant system for aluminium nitride ceramics, it is characterised in that the low-temperature sintering adjuvant system bag Include component A and component B；The component A is TiO2、ZrO2、HfO2At least one of；The component B is V2O5、Nb2O5、Ta2O5At least one of.
- 2. low-temperature sintering adjuvant system according to claim 1, it is characterised in that the mass ratio of the component A and component B For 1：（1~5）.
- 3. low-temperature sintering adjuvant system according to claim 1 or 2, it is characterised in that the low-temperature sintering adjuvant system Particle diameter distribution be 50nm~50 micron.
- A kind of 4. preparation method of aluminium nitride ceramics, it is characterised in that including：Low-temperature sintering adjuvant system any one of aluminium nitride powder and claim 1-3 is dissolved in organic solvent, then Uniformly mixed after adding dispersant, binding agent, plastic agent, base substrate, the aluminium nitride powder and low-temperature sintering adjuvant system is made Mass ratio be（5~10）：（90~95）；Gained base substrate is calcined 1~12 hour at 1600~1700 DEG C, obtains aluminium nitride ceramics.
- 5. according to the preparation method described in claim 4, it is characterised in that the particle diameter of the aluminium nitride powder can be 100nm ~10 μm；The organic solvent is at least one in ethanol, butanone, toluene, n-hexane, methanol, dimethylbenzene, normal propyl alcohol and n-butanol Kind, preferably ethanol/butanone, ethanol/toluene, ethanol/n-hexane, butanone/methanol, dimethylbenzene/normal propyl alcohol or dimethylbenzene/just Butanol, addition are 15~30wt% of the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system.
- 6. according to the preparation method described in claim 4 or 5, it is characterised in that the dispersant is olein, phosphorus At least one of sour fat, castor oil herring oil, ascorbic acid and terpinol, addition are that aluminium nitride powder and low-temperature sintering help 0.5~4wt% of the gross mass of agent system.
- 7. according to the preparation method described in any one of claim 4-6, it is characterised in that the binding agent is polyvinyl alcohol Butyral or/and polymethyl methacrylate, addition be the gross mass of aluminium nitride powder and low-temperature sintering adjuvant system 6~ 9wt%。
- 8. according to the preparation method described in any one of claim 4-7, it is characterised in that the plastic agent is O-phthalic The dibutyl phthalate DBP or/and fourth Bian ester BBP of phthalic acid two, addition are aluminium nitride powder and low-temperature sintering adjuvant system 7~12wt% of gross mass.
- 9. according to the preparation method described in any one of claim 4-8, it is characterised in that the heating rate of the calcining is 1~15 DEG C/min.
- A kind of 10. aluminium nitride ceramics prepared by method according to described in any one of claim 4-9.
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