CN105254306A - Method for preparing high-thermal-conductivity silicon nitride ceramics - Google Patents
Method for preparing high-thermal-conductivity silicon nitride ceramics Download PDFInfo
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- CN105254306A CN105254306A CN201510640611.7A CN201510640611A CN105254306A CN 105254306 A CN105254306 A CN 105254306A CN 201510640611 A CN201510640611 A CN 201510640611A CN 105254306 A CN105254306 A CN 105254306A
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- silicon nitride
- powder
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- thermal conductive
- high thermal
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Abstract
The invention relates to a method for preparing high-thermal-conductivity silicon nitride ceramics. The method comprises the steps that firstly, thermal treatment and acid pickling treatment are carried out on Si3N4 powder, and then Si3N4 slurry is prepared; an Si3N4 thin layer is prepared through a casting process technology, and porous silicon nitride powder prefabricated bodies are obtained after the thin layer is cut and overlapped; the prefabricated bodies are subjected to liquid silicon penetration through high-purity silicon powder, and compact Si3N4/Si is obtained; nitrogen treatment is carried out on Si3N4/Si in a nitrogenation oven, so that Si in the material is subjected to a nitriding reaction to generate Si3N4. Compared with frequently-used processes for preparing the high-thermal-conductivity silicon nitride ceramics, such as isostatic pressing sintering and hot pressed sintering, a tape casting method is combined with liquid silicon penetration forming and nitriding sintering processes, no or little machining is needed, preparation temperature is low, no sintering additive needs to be added, and the influence of a grain boundary on the thermal conductivity of the material is avoided. The thermal conductivity of the prepared silicon nitride ceramics can reach 80-120 Wm<-1>K<-1>.
Description
Technical field
The invention belongs to function ceramics field, be specifically related to a kind of preparation method of high thermal conductive silicon nitride pottery.
Background technology
Along with the development of unicircuit and power device, the restriction that heat dissipation problem promotes for product performance is more and more serious, and people have higher requirement for the over-all properties of Electronic Packaging substrate and heat sink material.Silicon nitride ceramics has potential high heat conductance, and (its theoretical thermal conductivity can reach 200 ~ 320Wm
-1k
-1), good insulativity, erosion resistance, resistance to sudden heating and outstanding mechanical property, have a good application prospect at electronic package material and heat sink material field.
Because silicon nitride belongs to strong covalent bond compound, being difficult to densified sintering product, therefore, in order to improve the density of silicon nitride ceramics to realize high thermal conductivity, usually needing when sintered silicon nitride ceramic to add Y
2o
3, MgO, Al
2o
3deng oxide sintering aid, more than 1800 DEG C, carry out gas pressure sintering or hot pressed sintering.The introducing of these sintering aids has adverse influence for the thermal conductivity of silicon nitride ceramics: Sauerstoffatom can dissolve in silicon nitride lattice, causes lattice defect, and the phonon for heat conduction plays scattering process; Meanwhile, the oxide compound remained between silicon nitride crystal boundary has lower thermal conductivity, causes obstruct for the propagation of heat between silicon nitride grain.
Document " G.J.Jiang; J.Y.Xu; G.H.Peng; H.R.Zhuang; W.L.Li; S.Y.Xu, etal.Sinteringofsiliconnitrideceramicswithmagnesiumsilic onnitrideandyttriumoxideassinteringaids.3rdInternational CongressonCeramics (Icc3): AdvancedEngineeringCeramicsandComposites, 2011,18 " a kind of preparation method of high thermal conductive silicon nitride is disclosed; the method, using high-purity silicon powder as raw material, adopts Y
2o
3-MgO, as sintering aid, has prepared high thermal conductive silicon nitride pottery to react reheating connection.The method needs to sinter for a long time under the high temperature of 1900 DEG C, and the interpolation of sintering aid has disadvantageous effect for the thermal conductivity improving silicon nitride ceramics.
Summary of the invention
The technical problem solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of preparation method of high thermal conductive silicon nitride pottery, overcomes the problem that existing preparation method's sintering temperature is high, introduce lattice oxygen atom and Grain-Boundary Phase.
Technical scheme
A preparation method for high thermal conductive silicon nitride pottery, is characterized in that step is as follows:
Step 1, Si
3n
4the pre-treatment of powder: by Si
3n
4powder is in 1700 ~ 1900 DEG C, and thermal treatment in nitrogen atmosphere, then carries out pickling with HF acid;
Step 2, preparation Si
3n
4powder precast body: by the Si after process
3n
4powder and solvent, dispersion agent, binding agent, softening agent and defoamer mixing and ball milling, obtain Si
3n
4slurry; The Si that flow casting molding thickness is 0.1 ~ 0.5mm is carried out to slurry
3n
4curtain coating thin layer; Thin layer is cut out and lamination, obtains the Si that base substrate relative density is 30 ~ 60%
3n
4powder precast body; Si in described slurry
3n
4the massfraction of powder is 30 ~ 60%; Described solvent is dehydrated alcohol and butanone 1:1 mixing by volume; The massfraction of described solvent is 30 ~ 50%; The massfraction of described dispersion agent is 2 ~ 4%; The massfraction of described binding agent is 2 ~ 4%; The massfraction of described defoamer is 2 ~ 4%;
Step 3, liquid silicon infiltration: by Si
3n
4powder precast body is embedded in high-purity silicon powder, is placed in vacuum oven, at the temperature of 1450 ~ 1650 DEG C, carry out liquid silicon infiltration, obtains fine and close Si
3n
4/ Si;
Step 4, nitridation sintered: by Si
3n
4/ Si is placed in nitriding furnace, at the temperature of 1200 ~ 1600 DEG C, carries out nitridation sintered in nitrogen atmosphere, obtains fine and close silicon nitride ceramics.
Described ball milling is placed in tumbling ball mill ball milling 12 ~ 24h.
Described dispersion agent is triethyl phosphate.
Described binding agent is polyvinyl butyral acetal.
Described softening agent is glycerol and dioctyl phthalate (DOP) 1:1 mixing by volume.
Described defoamer is propyl carbinol and ethylene glycol 1:1 mixing by volume.
Described Si
3n
4powder footpath is 0.3 ~ 10 μm.
Described high-purity Si powder purity is not less than 99.9%.
Described Si
3n
4powder precast body thickness is 0.5 ~ 5mm.
Beneficial effect
The preparation method of a kind of high thermal conductive silicon nitride pottery that the present invention proposes, first to Si
3n
4powder is heat-treated and cleanup acid treatment, then prepares Si
3n
4slurry, prepares Si with casting technique
3n
4thin layer, to the silicon nitride powder precast body obtaining the more hole after thin layer cutting lamination.Then adopt high-purity silicon powder to carry out liquid silicon infiltration to precast body, obtain fine and close Si
3n
4/ Si.To Si in nitriding furnace
3n
4/ Si carries out nitriding treatment, makes the Si in material that nitrogenizing reaction occur and generates Si
3n
4.With the conventional technique of preparation high thermal conductive silicon nitride pottery as compared with isostatic sintering, hot pressed sintering etc., the present invention adopts casting method shaping in conjunction with liquid silicon infiltration, nitridation sintered technique, do not need or only need a small amount of mechanical workout, preparation temperature is low, and do not need to add sintering aid, avoid the impact of Grain-Boundary Phase for material thermal conductivity.Prepared silicon nitride ceramics thermal conductivity can reach 80 ~ 120Wm
-1k
-1.
The invention has the beneficial effects as follows: adopt casting method shaping in conjunction with liquid silicon infiltration method, be suitable for the production of electronic substrates and radiator element, be conducive to realizing near-net-shape, reduce following process.Compared with conventional sintering technique, the present invention can not add sintering aid and realize the densification of silicon nitride ceramics, eliminates the impact of impurity oxygen atom and Grain-Boundary Phase; Nitridation sintered mold temperature is low, and equipment is relatively simple.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of height thermal conductive silicon nitride pottery of the present invention.
Fig. 2 is the Fracture scan electron microscope shape appearance figure of height thermal conductive silicon nitride pottery of the present invention.
Fig. 3 is the XRD material phase analysis figure of height thermal conductive silicon nitride pottery of the present invention.
Embodiment
Now in conjunction with the embodiments, the invention will be further described for accompanying drawing:
Example 1: selection particle diameter is the β-Si of 1.2 μm
3n
4powder, at 1800 DEG C, 0.3MPaN
2thermal treatment 2 hours under atmosphere, then with massfraction be 5% HF acid to the Si after thermal treatment
3n
4powder carries out pickling 6 hours, dry for standby.Take the Si after 50g process
3n
4powder, adds 50g solvent, and solvent is dehydrated alcohol and butanone 1:1 mixing by volume, and 4g dispersion agent triethyl phosphate, puts into nylon ball grinder, then adds silicon nitride abrading-ball, ball milling 12 hours on tumbling ball mill; Then in ball grinder, add 5g binding agent polyvinyl butyral acetal, 5g softening agent, softening agent is the 1:1 mixing by volume of glycerol and dioctyl phthalate (DOP) and 4g defoamer, defoamer be propyl carbinol and ethylene glycol by volume 1:1 mix; Continue ball milling 12 hours, the Si of the curtain coating that is uniformly dispersed, is suitable for
3n
4slurry.Carry out curtain coating to slurry, obtaining thickness is 0.4mm, Si
3n
4volume fraction is the thin layer of 40%.Thin layer is cut into the size of 40mm × 40mm, every 4 layer laminate hot pressing are 1mm to thickness, obtain Si
3n
4volume fraction is the porous preform of 60%.Precast body is placed in plumbago crucible, spreads high-purity silicon powder in precast body upper and lower surface, in the vacuum high temperature furnace of absolute pressure position 1000Pa, carry out liquid silicon infiltration, siliconising temperature is 1500 DEG C, insulation 2h.By the Si obtained after liquid silicon infiltration
3n
4/ Si carries out the remaining silicon that simple polishing can remove surface, and nitridation sintered in nitriding furnace subsequently, nitriding temperature is 1200 DEG C ~ 1500 DEG C, obtains fine and close high thermal conductive silicon nitride pottery.The flexural strength of material is 300MPa, and thermal conductivity is 80Wm
-1k
-1.
Example 2: select diameter be about 1 μm, length-to-diameter ratio be about 5 β-Si
3n
4column crystal, at 1800 DEG C, 0.3MPaN
2thermal treatment 2 hours under atmosphere, then with massfraction be 5% HF acid to the Si after thermal treatment
3n
4powder carries out pickling 6 hours, dry for standby.Take the Si after 50g process
3n
4powder, adds 50g solvent, and solvent is dehydrated alcohol and butanone 1:1 mixing by volume, and 4g dispersion agent triethyl phosphate, puts into nylon ball grinder, adds silicon nitride abrading-ball, ball milling 12 hours on tumbling ball mill.Then in ball grinder, 5g binding agent polyvinyl butyral acetal is added, 5g softening agent, softening agent is the 1:1 mixing by volume of glycerol and dioctyl phthalate (DOP) and 4g defoamer, defoamer is propyl carbinol and ethylene glycol 1:1 mixing by volume, continue ball milling 12 hours, the Si of the curtain coating that is uniformly dispersed, is suitable for
3n
4slurry.Carry out curtain coating to slurry, obtaining thickness is 0.3mm, Si
3n
4volume fraction is the thin layer of 45%.Thin layer is cut into the size of 40mm × 40mm, every 5 layer laminate hot pressing are 1mm to thickness, obtain Si
3n
4volume fraction is the porous preform of 65%.Precast body is placed in plumbago crucible, spreads high-purity silicon powder in precast body upper and lower surface, in the vacuum high temperature furnace of absolute pressure position 1000Pa, carry out liquid silicon infiltration, siliconising temperature is 1500 DEG C, insulation 2h.By the Si obtained after liquid silicon infiltration
3n
4/ Si carries out the remaining silicon that simple polishing can remove surface, and nitridation sintered in nitriding furnace subsequently, nitriding temperature is 1200 DEG C ~ 1500 DEG C, obtains fine and close high thermal conductive silicon nitride pottery.The flexural strength of material is 400MPa, and thermal conductivity is 90Wm
-1k
-1.Further annealing process is carried out to silicon nitride ceramics: silicon nitride ceramics is placed in 1800 DEG C, 0.5MPaN
2being incubated 4h in atmosphere, can be that the thermal conductivity of silicon nitride ceramics rises to 105Wm
-1k
-1.
Claims (9)
1. a preparation method for high thermal conductive silicon nitride pottery, is characterized in that step is as follows:
Step 1, Si
3n
4the pre-treatment of powder: by Si
3n
4powder is in 1700 ~ 1900 DEG C, and thermal treatment in nitrogen atmosphere, then carries out pickling with HF acid;
Step 2, preparation Si
3n
4powder precast body: by the Si after process
3n
4powder and solvent, dispersion agent, binding agent, softening agent and defoamer mixing and ball milling, obtain Si
3n
4slurry; The Si that flow casting molding thickness is 0.1 ~ 0.5mm is carried out to slurry
3n
4curtain coating thin layer; Thin layer is cut out and lamination, obtains the Si that base substrate relative density is 30 ~ 60%
3n
4powder precast body; Si in described slurry
3n
4the massfraction of powder is 30 ~ 60%; Described solvent is dehydrated alcohol and butanone 1:1 mixing by volume; The massfraction of described solvent is 30 ~ 50%; The massfraction of described dispersion agent is 2 ~ 4%; The massfraction of described binding agent is 2 ~ 4%; The massfraction of described defoamer is 2 ~ 4%;
Step 3, liquid silicon infiltration: by Si
3n
4powder precast body is embedded in high-purity silicon powder, is placed in vacuum oven, at the temperature of 1450 ~ 1650 DEG C, carry out liquid silicon infiltration, obtains fine and close Si
3n
4/ Si;
Step 4, nitridation sintered: by Si
3n
4/ Si is placed in nitriding furnace, at the temperature of 1200 ~ 1600 DEG C, carries out nitridation sintered in nitrogen atmosphere, obtains fine and close silicon nitride ceramics.
2. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described ball milling is placed in tumbling ball mill ball milling 12 ~ 24h.
3. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described dispersion agent is triethyl phosphate.
4. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described binding agent is polyvinyl butyral acetal.
5. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described softening agent is glycerol and dioctyl phthalate (DOP) 1:1 mixing by volume.
6. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described defoamer is propyl carbinol and ethylene glycol 1:1 mixing by volume.
7. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described Si
3n
4powder footpath is 0.3 ~ 10 μm.
8. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described high-purity Si powder purity is not less than 99.9%.
9. the preparation method of high thermal conductive silicon nitride pottery according to claim 1, is characterized in that: described Si
3n
4powder precast body thickness is 0.5 ~ 5mm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105884376A (en) * | 2016-04-01 | 2016-08-24 | 广东工业大学 | Method for preparing silicon-nitride ceramic substrate through silicon-powder tape casting |
| CN107573074A (en) * | 2017-08-30 | 2018-01-12 | 西北工业大学 | A kind of method of RMI methods low temperature preparation stratiform SiC base shock resistance composite ceramic materials |
| CN107604192A (en) * | 2017-08-25 | 2018-01-19 | 巩义市泛锐熠辉复合材料有限公司 | A kind of preparation method of aluminium nitride/aluminium composite material |
| CN109851370A (en) * | 2019-03-22 | 2019-06-07 | 常德科锐新材料科技有限公司 | The production method of high-intensitive high thermal conductivity silicon nitride board |
| CN109987944A (en) * | 2019-03-06 | 2019-07-09 | 清华大学 | A kind of high thermal conductivity silicon nitride ceramic substrate and preparation method thereof |
| CN110078521A (en) * | 2019-05-13 | 2019-08-02 | 西北工业大学 | A kind of submicron order silicon nitride hollow microsphere and preparation method |
| CN110330321A (en) * | 2019-07-01 | 2019-10-15 | 佛山市百瑞新材料技术有限公司 | A kind of curtain coating-temperature and pressure composite molding technique of across the scale hybrid ceramic substrate of micro-nano |
| WO2020177465A1 (en) * | 2019-03-05 | 2020-09-10 | 青岛瓷兴新材料有限公司 | Silicon nitride, ceramic slurry and preparation method |
| CN113149662A (en) * | 2021-04-20 | 2021-07-23 | 中材高新氮化物陶瓷有限公司 | Preparation method and application of high-thermal-conductivity silicon nitride ceramic casting film |
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Cited By (14)
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|---|---|---|---|---|
| CN105884376A (en) * | 2016-04-01 | 2016-08-24 | 广东工业大学 | Method for preparing silicon-nitride ceramic substrate through silicon-powder tape casting |
| CN105884376B (en) * | 2016-04-01 | 2018-09-07 | 广东工业大学 | A kind of method that silica flour curtain coating prepares silicon nitride ceramic substrate |
| CN107604192A (en) * | 2017-08-25 | 2018-01-19 | 巩义市泛锐熠辉复合材料有限公司 | A kind of preparation method of aluminium nitride/aluminium composite material |
| CN107573074A (en) * | 2017-08-30 | 2018-01-12 | 西北工业大学 | A kind of method of RMI methods low temperature preparation stratiform SiC base shock resistance composite ceramic materials |
| CN107573074B (en) * | 2017-08-30 | 2020-12-08 | 西北工业大学 | Method for preparing laminated SiC-based impact-resistant composite ceramic material at low temperature by RMI method |
| WO2020177465A1 (en) * | 2019-03-05 | 2020-09-10 | 青岛瓷兴新材料有限公司 | Silicon nitride, ceramic slurry and preparation method |
| CN109987944B (en) * | 2019-03-06 | 2020-09-01 | 清华大学 | High-thermal-conductivity silicon nitride ceramic substrate and preparation method thereof |
| CN109987944A (en) * | 2019-03-06 | 2019-07-09 | 清华大学 | A kind of high thermal conductivity silicon nitride ceramic substrate and preparation method thereof |
| CN109851370A (en) * | 2019-03-22 | 2019-06-07 | 常德科锐新材料科技有限公司 | The production method of high-intensitive high thermal conductivity silicon nitride board |
| CN110078521A (en) * | 2019-05-13 | 2019-08-02 | 西北工业大学 | A kind of submicron order silicon nitride hollow microsphere and preparation method |
| CN110078521B (en) * | 2019-05-13 | 2021-06-11 | 西北工业大学 | Submicron silicon nitride hollow microsphere and preparation method thereof |
| CN110330321A (en) * | 2019-07-01 | 2019-10-15 | 佛山市百瑞新材料技术有限公司 | A kind of curtain coating-temperature and pressure composite molding technique of across the scale hybrid ceramic substrate of micro-nano |
| CN110330321B (en) * | 2019-07-01 | 2021-09-24 | 佛山市百瑞新材料技术有限公司 | Tape casting-warm pressing composite forming process for micro-nano cross-scale mixed ceramic substrate |
| CN113149662A (en) * | 2021-04-20 | 2021-07-23 | 中材高新氮化物陶瓷有限公司 | Preparation method and application of high-thermal-conductivity silicon nitride ceramic casting film |
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Application publication date: 20160120 |