CN108439993A - It is a kind of with AlN/C be bury burn powder high heat conductance AlN ceramic and preparation method thereof - Google Patents
It is a kind of with AlN/C be bury burn powder high heat conductance AlN ceramic and preparation method thereof Download PDFInfo
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Abstract
It is to bury the high heat conductance AlN ceramic and preparation method thereof for burning powder that the invention discloses a kind of with AlN/C, and this method is mainly to bury burning powder raw material with aluminium nitride, and the carbon dust that mass fraction is 0.1% ~ 0.6% is added.Simultaneously, using aluminium nitride as AlN ceramic base stock, use rare earth metal fluoride, rare-earth oxide, alkali earth metal fluoride, rare-earth oxide or their compound to be sintered sintering aid, through wet-milling mixing, it is dry, be granulated, molding, burnt powder and buried burning with burying.Gained aluminium nitride ceramics thermal conductivity is in 150 ~ 230W/ (m.), K fine and close Du≤99.0%.Advantage is, it is simple for process, aluminium nitride ceramics the second phase content and its existence form can be carried out to regulate and control and not introduce new impurity by burying burning powder, promote densification sintering, ensure that the aluminium nitride ceramics prepared above has clean crystal boundary microcosmic, and then realizes the preparation of high-heat conductivity aluminium nitride ceramics pressureless sintering.
Description
Technical field
The present invention relates to AlN ceramic purify sintering technology, and in particular to it is a kind of with AlN/C be bury burn powder high heat conductance
AlN ceramic and preparation method thereof.
Background technology
AlN is covalent key compound, and without free electron, heat transfer mechanism is phonon thermal conduction, and crystal structure meets it
Have the characteristics that high heat conductance, pure aluminium nitride theory thermal conductivity reach 320W/ (m.k).Its excellent heat conductivility obtains
It is extensive to pay attention to.However, be easily introduced impurity in aluminium nitride, in all impurity, oxygen be influence AlN thermal conductivities it is main because
Element is easy to form oxygen defect because the oxygen in lattice has high displacement soluble.For this purpose, in addition to improving aln raw material purity
And its while preservation condition, people are by adding some sintering aids, such as rare earth element, alkali earth metal, alkali metal member
Oxide, the fluoride of element（Y2O3、CaO、Li2O、YF3、CaF2, LiF etc.）, miscellaneous to reduce and remove AlON in aluminium nitride ceramics
Phase can effectively avoid solid solution of the oxygen atom in aluminium nitride.But in sintering process, the reactant of formation is not easy to be discharged, and shape
At new impurity, it is easy to accumulate in aluminium nitride grain boundaries, produces the second phase, influence the transmission of heat.It prepares highly thermally conductive
Rate AlN ceramic becomes a kind of problem, and therefore, the impurity removed in aluminium nitride is most important.
Invention content
The purpose of this method be to provide it is a kind of with AlN/C be bury burn powder high heat conductance AlN ceramic and preparation method thereof, should
Method can remove oxygen impurities, reduce the content of the second phase, and crystal boundary is purified while purifying lattice.
The object of the invention is achieved by the following technical programs.
It is a kind of with AlN/C be bury burn powder high heat conductance AlN ceramic preparation method, include the following steps：
（1）AlN, sintering aid are mixed, ball milling obtains mixture；
（2）By step（1）Gained mixture is dried, and is then granulated；
（3）By step（2）Isostatic cool pressing processing is carried out after gained particle is dry-pressing formed, obtains aluminium nitride sample；
（4）Powder is burnt to step with burying（3）Gained aluminium nitride sample carries out burying burning, obtains AlN ceramic；
The burning powder that buries includes AlN and C.
Preferably, step（1）The sintering aid is rare earth metal fluoride, rare-earth oxide, alkaline-earth metal fluorine
It is one or more in compound and rare-earth oxide.
Preferably, step（1）The addition of the sintering aid is the 1% ~ 7% of AlN and sintering aid gross mass, further
Preferably 4%.
Preferably, step（1）Solvent isopropanol is added when the ball milling；The time of the ball milling is 24 ~ 48 hours, into one
Step preferably 36 hours.
Preferably, step（2）The temperature of the drying is 100 DEG C, and the time is 10 hours.
Preferably, step（3）The dry-pressing formed pressure is 20 ~ 30MPa, and the dwell time is 0.5 ~ 1min；Further
Preferably 25MPa, pressurize 0.75min.
Preferably, step（3）The pressure of the isostatic cool pressing is 150 ~ 200MPa, and the dwell time is 1 ~ 2min；Further
Preferably 175MPa, pressurize 1.5min.
Preferably, step（4）The mass ratio for burying AlN and C in burning powder is 100:0.1~100:0.6.
Preferably, the mass ratio for burying AlN and C in burning powder is 100:0.35.
Preferably, step（4）The firing degree that buries is：Atmosphere furnace, nitrogen keep the temperature 4 at 1650 ~ 1700 DEG C as protection gas
Then ~ 6h is cooled to 1500 ~ 1550 DEG C of 30 ~ 60min of heat preservation.
Made from above-described preparation method it is a kind of with AlN/C be bury burn powder high heat conductance AlN ceramic.
The novel manufacturing process flow for burying burning method that the present invention prepares high-thermal conductivity A 1 N is as follows：
Raw material test → dispensing → ball milling → drying → granulation → dry-pressing formed → isostatic cool pressing → firing → finished product.
The thermal conductivity of gained AlN ceramic of the invention is in 150 ~ 230W/ (m.), K fine and close Du≤99.0%.The advantage is that technique
Simply, aluminium nitride ceramics the second phase content and its existence form can be carried out to regulate and control and not introduce new impurity by burying burning powder,
Promote densification sintering, it is ensured that the aluminium nitride ceramics of preparation above has clean crystal boundary microcosmic, and then realizes high heat conductance nitrogen
Change the preparation of aluminium ceramics pressureless sintering.
Compared with prior art, the invention has the advantages that：
The firing method that buries of the present invention effectively removes the oxygen impurities in AlN and the content of the second phase is made to reduce, and purifies crystal boundary, has
The thermal conductivity for improving AlN of effect.
Description of the drawings
Fig. 1 is to bury burning schematic diagram.
Specific implementation mode
The specific implementation of the present invention is further described with reference to specific embodiment, but embodiments of the present invention
It is without being limited thereto.
Embodiment 1
The AlN ceramic raw material of the present embodiment is grouped as by the group of following mass fraction：YF3:4%; AlN：96%；Bury burn powder by with
The group of lower mass fraction is grouped as：AlN：C=100:0.35.
Raw materials used formula is calculated according to formula rate as above, selects YF in the present embodiment3 0.4g, AlN 9.6g conducts
Raw material.Add isopropanol ball milling 24 hours.It is dry after ball milling.Then it is granulated.First dry-pressing formed and then isostatic cool pressing, it is dry-pressing formed
Pressure is 20MPa, dwell time 1min；The pressure of isostatic cool pressing is 200MPa, dwell time 2min.Burning is buried with 10g
Powder buries burning, under atmospheric pressure kiln, nitrogen atmosphere, at 1650 DEG C, keeps the temperature 4 hours.Then 1500 DEG C of heat preservation 30min are cooled to burn
At obtaining AlN ceramic.It is as shown in Figure 1 to bury burning schematic diagram.
AlN ceramic thermal conductivity obtained by the present embodiment is 165W/ (m.K), consistency reaches 99.2%.
Embodiment 2
The AlN ceramic raw material of the present embodiment is grouped as by the group of following mass fraction：Y2O3:7%；AlN：93%；Bury burn powder by with
The group of lower mass fraction is grouped as：AlN：C=100:0.1.
Raw materials used formula is calculated according to formula rate as above, selects Y in the present embodiment2O3 0.7g, AlN 9.3g make
For raw material.Add isopropanol ball milling 48 hours.It is dry after ball milling.Then it is granulated.First dry-pressing formed and then isostatic cool pressing, it is dry-pressing formed
Pressure be 25MPa, dwell time 0.5min；The pressure of isostatic cool pressing is 150MPa, dwell time 1.5min.Use 10g
Bury burn powder bury burnings, under atmospheric pressure kiln, nitrogen atmosphere, at 1675 DEG C, heat preservation 6 hours.Then 1550 DEG C of heat preservations are cooled to
45min is burnt into, and obtains AlN ceramic.
AlN ceramic thermal conductivity obtained by the present embodiment is 175W/ (m.K), consistency reaches 99.4%.
Embodiment 3
The AlN ceramic raw material of the present embodiment is grouped as by the group of following mass fraction：CaO:1%；AlN：99%；It buries and burns powder by following
The group of mass fraction is grouped as：AlN：C=100:0.6.
Raw materials used formula is calculated according to formula rate as above, selects CaO 0.1g, AlN 9.9g to make in the present embodiment
For raw material.Add isopropanol ball milling 36 hours.It is dry after ball milling.Then it is granulated.First dry-pressing formed and then isostatic cool pressing, it is dry-pressing formed
Pressure be 25MPa, dwell time 0.75min；The pressure of isostatic cool pressing is 175MPa, dwell time 1min.With 10g's
It buries burning powder and buries burning, in a nitrogen atmosphere, at 1700 DEG C, keep the temperature 5 hours.Then 1525 DEG C of heat preservation 60min firings are cooled to, are obtained
AlN ceramic.
AlN ceramic thermal conductivity obtained by the present embodiment is 160W/ (m.K), consistency reaches 99.1%.
Embodiment 4
The AlN ceramic raw material of the present embodiment is grouped as by the group of following mass fraction：CaF2:2%；AlN：98%；Bury burn powder by with
The group of lower mass fraction is grouped as：AlN：C=100:0.5.
Raw materials used formula is calculated according to formula rate as above, selects CaF in the present embodiment2 0.2g, AlN 9.8g make
For raw material.Add isopropanol ball milling 24 hours.It is dry after ball milling.Then it is granulated.First dry-pressing formed and then isostatic cool pressing, it is dry-pressing formed
Pressure be 25MPa, dwell time 0.5min；The pressure of isostatic cool pressing is 300MPa, dwell time 1.5min.Use 10g
Bury burn powder bury burnings, in a nitrogen atmosphere, at 1650 DEG C, heat preservation 4 hours.Then 1525 DEG C of heat preservation 60min firings are cooled to,
Obtain AlN ceramic.
AlN ceramic thermal conductivity obtained by the present embodiment is 150W/ (m.K), consistency reaches 99.0%.
Embodiment 5
The AlN ceramic raw material of the present embodiment is grouped as by the group of following mass fraction：YF3:5%；CaF2:2%；AlN：93%；Bury burning
Powder is grouped as by the group of following mass fraction：AlN：C=100:0.35.
Raw materials used formula is calculated according to formula rate as above, selects YF in the present embodiment3 0.5g、CaF2 0.2g、
AlN 9.3g are as raw material.Add isopropanol ball milling 24 hours.It is dry after ball milling.Then it is granulated.It is first dry-pressing formed and then cold etc. quiet
Pressure, dry-pressing formed pressure are 25MPa, dwell time 1min；The pressure of isostatic cool pressing is 200MPa, and the dwell time is
2min.Burning is buried with the burning powder that buries of 10g, in a nitrogen atmosphere, at 1700 DEG C, keeps the temperature 4 hours.Then 1500 DEG C of heat preservations are cooled to
60min is burnt into, and obtains AlN ceramic.
AlN ceramic thermal conductivity obtained by the present embodiment is 190W/ (m.K), consistency reaches 99.5%.
Embodiment 6
The AlN ceramic raw material of the present embodiment is grouped as by the group of following mass fraction：Y2O3:5%；CaF2:1%；CeO2:1%；AlN：
93%；Burning powder is buried to be grouped as by the group of following mass fraction：AlN：C=100:0.6.
Raw materials used formula is calculated according to formula rate as above, selects Y in the present embodiment2O3 0.5g、CaF2 0.1g、
CeO2 0.1g, AlN 9.3g are as raw material.Add isopropanol ball milling 36 hours.It is dry after ball milling.Then it is granulated.It is first dry-pressing formed right
Isostatic cool pressing afterwards, dry-pressing formed pressure are 20MPa, dwell time 1min；The pressure of isostatic cool pressing is 200MPa, when pressurize
Between be 2min.Burning is buried with the burning powder that buries of 10g, in a nitrogen atmosphere, at 1700 DEG C, keeps the temperature 5 hours.Then 1525 DEG C are cooled to
60min firings are kept the temperature, AlN ceramic is obtained.
AlN ceramic thermal conductivity obtained by the present embodiment is 230W/ (m.K), and consistency reaches 99.8%.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
All any modification, equivalent and improvement etc., should be included in the claims in the present invention made by within the spirit and principle of invention
Protection domain within.
Claims (10)
1. it is a kind of with AlN/C be bury burn powder high heat conductance AlN ceramic preparation method, which is characterized in that include the following steps：
（1）AlN, sintering aid are mixed, ball milling obtains mixture；
（2）By step（1）Gained mixture is dried, and is then granulated；
（3）By step（2）Isostatic cool pressing processing is carried out after gained particle is dry-pressing formed, obtains aluminium nitride sample；
（4）Powder is burnt to step with burying（3）Gained aluminium nitride sample carries out burying burning, obtains AlN ceramic；
The burning powder that buries includes AlN and C.
2. preparation method as described in claim 1, which is characterized in that step（1）The sintering aid is fluorinated for rare earth metal
It is one or more in object, rare-earth oxide, alkali earth metal fluoride and rare-earth oxide.
3. preparation method as described in claim 1, which is characterized in that step（1）The addition of the sintering aid be AlN and
The 1% ~ 7% of sintering aid gross mass.
4. preparation method as described in claim 1, which is characterized in that step（1）Solvent isopropanol is added when the ball milling；Institute
The time for stating ball milling is 24 ~ 48 hours.
5. preparation method as described in claim 1, which is characterized in that step（3）The dry-pressing formed pressure be 20 ~
30MPa, dwell time are 0.5 ~ 1min.
6. preparation method as described in claim 1, which is characterized in that step（3）The pressure of the isostatic cool pressing be 150 ~
200MPa, dwell time are 1 ~ 2min.
7. preparation method as described in claim 1, which is characterized in that step（4）It is described to bury the mass ratio for burning AlN and C in powder
It is 100:0.1~100:0.6.
8. preparation method as claimed in claim 7, which is characterized in that the mass ratio for burying AlN and C in burning powder is 100:
0.35。
9. preparation method as described in claim 1, which is characterized in that step（4）The firing degree that buries is：Atmosphere furnace, nitrogen
As protection gas, 4 ~ 6h is kept the temperature at 1650 ~ 1700 DEG C, is then cooled to 1500 ~ 1550 DEG C of 30 ~ 60min of heat preservation.
10. made from claim 1-9 any one of them preparation methods it is a kind of with AlN/C be bury burn powder high heat conductance
AlN ceramic.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115124355A (en) * | 2022-07-21 | 2022-09-30 | 新乡市固元陶瓷科技有限公司 | Method for burning large-size ceramic spheres in buried mode |
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|---|---|---|---|---|
| JPS60255677A (en) * | 1984-05-29 | 1985-12-17 | 日本電気株式会社 | Manufacture of aluminum nitride sintered body |
| CN101333114A (en) * | 2008-07-31 | 2008-12-31 | 潮州三环（集团）股份有限公司 | Method for making high-thermal-conductivity aluminium nitride ceramics substrate |
| CN101570437A (en) * | 2009-04-30 | 2009-11-04 | 潮州三环（集团）股份有限公司 | Method for continuous low temperature sintering of high thermal coefficient AIN ceramics and product thereof |
| CN106542828A (en) * | 2016-10-18 | 2017-03-29 | 华中科技大学 | A kind of aluminium nitride ceramics of low-temperature sintering high heat conductance and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN115124355B (en) * | 2022-07-21 | 2023-09-01 | 新乡市固元陶瓷科技有限公司 | Method for burying and burning large-size ceramic spheres |
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