CN102875156A - Preparation method of aluminum nitride ceramic LED lamp thermal-conducting material - Google Patents
Preparation method of aluminum nitride ceramic LED lamp thermal-conducting material Download PDFInfo
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- CN102875156A CN102875156A CN2012103767887A CN201210376788A CN102875156A CN 102875156 A CN102875156 A CN 102875156A CN 2012103767887 A CN2012103767887 A CN 2012103767887A CN 201210376788 A CN201210376788 A CN 201210376788A CN 102875156 A CN102875156 A CN 102875156A
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- led lamp
- preparation
- heat sink
- aluminium nitride
- sink material
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- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 14
- 239000004020 conductor Substances 0.000 title abstract 2
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000009768 microwave sintering Methods 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 6
- 238000004381 surface treatment Methods 0.000 claims abstract description 6
- 229910017083 AlN Inorganic materials 0.000 claims description 23
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 22
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 229910052810 boron oxide Inorganic materials 0.000 claims description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 11
- 239000000292 calcium oxide Substances 0.000 claims description 11
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 7
- 238000007731 hot pressing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000004018 waxing Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000000280 densification Methods 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000008646 thermal stress Effects 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of aluminum nitride ceramic LED lamp thermal-conducting material. The preparation method includes the steps of ball-milling, blanking, evacuating and sintering, surface treatment and the like. By microwave sintering, compacting speed of compacted body is increased, and thermal efficiency of products is improved. The preparation process is simple, production cost is low, and production efficiency is improved greatly.
Description
Technical field
The present invention relates to a kind of preparation method of aluminium nitride ceramics LED lamp heat sink material.
Background technology
Adopt metal substrate and the outer scatterer of metal on the tradition LED structure, because characteristics such as the high thermal stress of metal, high conductivity, there is following some technical bottleneck in therefore traditional LED:
The first, there is the thermal stresses that is difficult to overcome in the traditional metal material, and the metal sheet that is used for the LED heat transmission mainly is aluminium and copper, its thermal expansivity is much larger than the substrate of crystal grain, be operated in the process of cold cycling, crystal grain will bear very large thermal stresses and stress impact, have very big chance to snap, simultaneously, the thermoemitting rate of metal product is lower, as aluminium only be 0.05, copper be 0.1, heat can't diffuse in the air, causes heat can't derive and in the Local enrichment carbonization.
The second, there is potential safety hazard in the metal material poor insulativity.Because the electroconductibility of metal, the Secure Application of LED product is caused certain influence, there are the potential safety hazards such as electric leakage.
In the prior art, the method of processing LED radiating equipment, traditional technology adopts the methods such as die casting aluminium, casting molding machine moulding, the moulding of Extrusion Process of Aluminum Alloy Profile machined into mostly, the shortcoming such as the metal material LED radiating equipment of making exists that production cost is high, complex process, efficient are low, and on-insulated, potential safety hazard is arranged.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of aluminium nitride ceramics LED lamp heat sink material is provided, adopt microwave sintering, improve the densification rate of sintered compact, improve product thermo-efficiency, simultaneously, manufacture craft is simple, and production cost is low, can significantly enhance productivity.
Above-mentioned purpose of the present invention is achieved by following technical solution:
A kind of preparation method of aluminium nitride ceramics LED lamp heat sink material comprises the steps:
(1) aluminum nitride powder is carried out ball milling pretreatment, and add sintering aid, make its even mixing;
(2) above-mentioned batching and wax become just base at the forming under the pressure of 85-90MPa;
(3) with moulding just base place and carry out de-waxing in the retort furnace, form blank;
(4) base substrate is placed in the nitrogen atmosphere stove, vacuumize processing after the sealing;
(5) under the flowing nitrogen atmosphere base substrate is being carried out microwave presintering 1.8-4.5 hours under 300-400 ℃;
(6) base substrate after the pre-burning is placed hot pressing furnace, carry out microwave sintering in the nitrogen atmosphere under 1200-1300 ℃, and be incubated 0.5 hour;
(7) according to the warm change curve that moves back of setting, make it be cooled to room temperature, moved back warm process approximately 5-6 hours;
(8) carry out surface treatment to burning till blank, grind off burr, become aluminium nitride ceramics LED lamp heat sink material.
The weight ratio of described aluminum nitride powder and sintering aid is 1:0.008-0.01; Sintering aid is the mixture of calcium oxide and boron oxide; The weight ratio of calcium oxide and boron oxide is 2:1.
Described step (1) utilizes high energy ball mill that aluminum nitride powder is carried out pre-treatment, it is evenly mixed with sintering aid, improve the grain composition of material, guarantee that the material particles size is little, particle distribution range is narrow, improve its sintering character, improve the density of aluminium nitride ceramics material.
Add wax in the described step (2) and prepare burden at the thermal high compacted under, reach the effect that helps forming ingredient, prevent that just base produces bubble and slight crack in moulding process, affect molding effect.
It is in order to build pure nitrogen atmosphere, for sintering step is made sufficient preparation that described step (3) vacuumizes.
Microwave sintering is adopted in described step (5) and (6), and the heat-processed that makes blank is to carry out simultaneously in the whole volume, heats up rapidly, and temperature is even.But be conducive to improve densification rate and the establishment grain growing of sintered compact, make into the performance of blank and the blank that structure all is better than the normal sintering gained; Simultaneously, the thermo-efficiency of microwave sintering is high, saves energy consumption, shortens the production cycle, thereby enhance productivity.Wherein step (5) is carried out presintering under flowing nitrogen atmosphere, the moisture that absorbs in depositing process to get rid of molding blank.
Because the aluminium nitride self-diffusion coefficient is very little, sintering is very difficult, adds the sintering that sintering aid promotes aluminium nitride.By adding the mixture of calcium oxide and boron oxide, can generate various metallic aluminium salt liquid phases (Grain-Boundary Phase) with residual aluminum oxide reaction in the aluminum nitride powder on the one hand, reduce sintering temperature, acceleration of sintering makes blank Densification; On the other hand, the content of impurity oxygen can reduce with the discharge of Grain-Boundary Phase, thereby improves the thermal conductivity of aluminium nitride.In addition, ratio is suitable, can not increase foreign matter content, thereby affect thermal conductivity because of too much hindering particle diameter to grow up, or because measuring the very few effect that loses sintering aid.
Compared with prior art, the present invention has following beneficial effect:
1. employing microwave sintering improves the densification rate of sintered compact, and thermo-efficiency is high, thereby enhances productivity;
2. manufacture craft is simple, and production cost is low;
3. product has higher thermoemitting performance, and the thermoemitting rate reaches 0.97, so that heat diffuses in the air better, thereby effectively helps the LED lamp pearl heat that sheds;
4. the product insulativity is high, and is high pressure resistant, do not have the danger of traditional metal electric leakage, high safety;
5. can in time LED lamp pearl heat in time be shed, thereby effectively prolong power source life, improve the whole lamp life-span.
Embodiment
Below in conjunction with specific embodiment the present invention is further explained, but embodiment does not do any restriction to the present invention.
Embodiment 1
A kind of preparation method of aluminium nitride ceramics LED lamp heat sink material comprises the steps:
(1) aluminum nitride powder is carried out ball milling pretreatment, and add sintering aid, make its even mixing;
(2) above-mentioned batching and wax become just base at the forming under the pressure of 85-90MPa;
(3) with moulding just base be positioned over and carry out de-waxing in the retort furnace, form blank;
(4) base substrate is positioned in the nitrogen atmosphere stove, vacuumizes processing after the sealing;
(5) under 400 ℃, carry out microwave presintering 1.8 hours at the base substrate to compression moulding under the flowing nitrogen atmosphere;
(6) base substrate after the pre-burning is placed hot pressing furnace, carry out microwave sintering in the nitrogen atmosphere under 1200 ℃, and be incubated 0.5 hour;
(7) according to the warm change curve that moves back of setting, make it be cooled to room temperature, moved back warm process approximately 5 hours;
(8) carry out surface treatment to burning till blank, grind off burr, become aluminium nitride ceramics LED lamp heat sink material.
The weight ratio of described aluminum nitride powder and sintering aid is 1:0.008; Sintering aid is the mixture of calcium oxide and boron oxide; The weight ratio of calcium oxide and boron oxide is 2:1.
The aluminium nitride ceramics LED lamp heat sink material thermoemitting rate that obtains by above step can reach 0.92, thermal conductivity 〉=39 W/mk.
Embodiment 2
A kind of preparation method of aluminium nitride ceramics LED lamp heat sink material comprises the steps:
(1) aluminum nitride powder is carried out ball milling pretreatment, and add sintering aid, make its even mixing;
(2) above-mentioned batching and wax become just base at the forming under the pressure of 85-90MPa;
(3) with moulding just base place and carry out de-waxing in the retort furnace, form blank;
(4) base substrate is placed in the nitrogen atmosphere stove, vacuumize processing after the sealing;
(5) under 350 ℃, carry out microwave presintering 4 hours at the base substrate to compression moulding under the flowing nitrogen atmosphere;
(6) base substrate after the pre-burning is placed hot pressing furnace, carry out microwave sintering in the nitrogen atmosphere under 1250 ℃, and be incubated 0.5 hour;
(7) according to the warm change curve that moves back of setting, make it be cooled to room temperature, moved back warm process approximately 5.5 hours;
(8) carry out surface treatment to burning till blank, grind off burr, become aluminium nitride ceramics LED lamp heat sink material.
The weight ratio of described aluminum nitride powder and sintering aid is 1:0.009; Sintering aid is the mixture of calcium oxide and boron oxide; The weight ratio of calcium oxide and boron oxide is 2:1.
The aluminium nitride ceramics LED lamp heat sink material thermoemitting rate that obtains by above step can reach 0.97, thermal conductivity 〉=39 W/mk.
Embodiment 3
A kind of preparation method of aluminium nitride ceramics LED lamp heat sink material comprises the steps:
(1) aluminum nitride powder is carried out ball milling pretreatment, and add sintering aid, make its even mixing;
(2) above-mentioned batching and wax become just base at the forming under the pressure of 85-90MPa;
(3) with moulding just base place and carry out de-waxing in the retort furnace, form blank;
(4) base substrate is placed in the nitrogen atmosphere stove, vacuumize processing after the sealing;
(5) under 300 ℃, carry out microwave presintering 3 hours at the base substrate to compression moulding under the flowing nitrogen atmosphere;
(6) base substrate after the pre-burning is placed hot pressing furnace, carry out microwave sintering in the nitrogen atmosphere under 1300 ℃, and be incubated 0.5 hour;
(7) according to the warm change curve that moves back of setting, make it be cooled to room temperature, moved back warm process approximately 6 hours;
(8) carry out surface treatment to burning till blank, become aluminium nitride ceramics LED lamp heat sink material.
The weight ratio of described aluminum nitride powder and sintering aid is 1:0.01; Sintering aid is the mixture of calcium oxide and boron oxide; The weight ratio of calcium oxide and boron oxide is 2:1.
The aluminium nitride ceramics LED lamp heat sink material thermoemitting rate that obtains by above step can reach 0.96, thermal conductivity 〉=39 W/mk.
Claims (4)
1. the preparation method of an aluminium nitride ceramics LED lamp heat sink material is characterized in that, comprises the steps:
(1) aluminum nitride powder is carried out ball milling pretreatment, and add sintering aid, make its even mixing;
(2) above-mentioned batching and wax become just base at the forming under the pressure of 85-90MPa;
(3) with moulding just base place and carry out de-waxing in the retort furnace, form blank;
(4) base substrate is placed in the nitrogen atmosphere stove, vacuumize processing after the sealing;
(5) under the flowing nitrogen atmosphere base substrate is being carried out microwave presintering 1.8-4.5 hours under 300-400 ℃;
(6) base substrate after the pre-burning is placed hot pressing furnace, carry out microwave sintering in the nitrogen atmosphere under 1200-1300 ℃, and be incubated 0.5 hour;
(7) according to the warm change curve that moves back of setting, make it be cooled to room temperature, moved back warm process approximately 5-6 hours;
(8) carry out surface treatment to burning till blank, grind off burr, become aluminium nitride ceramics LED lamp heat sink material.
2. the preparation method of aluminium nitride ceramics LED lamp heat sink material according to claim 1 is characterized in that, the weight ratio of described aluminum nitride powder and sintering aid is 1:0.008-0.01.
3. the preparation method of aluminium nitride ceramics LED lamp heat sink material according to claim 1 is characterized in that, sintering aid is the mixture of calcium oxide and boron oxide.
4. the preparation method of aluminium nitride ceramics LED lamp heat sink material according to claim 3 is characterized in that, the weight ratio of calcium oxide and boron oxide is 2:1.
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| CN2012103767887A CN102875156A (en) | 2012-10-08 | 2012-10-08 | Preparation method of aluminum nitride ceramic LED lamp thermal-conducting material |
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| CN2012103767887A CN102875156A (en) | 2012-10-08 | 2012-10-08 | Preparation method of aluminum nitride ceramic LED lamp thermal-conducting material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224398A (en) * | 2013-04-26 | 2013-07-31 | 湖南凯新陶瓷科技有限公司 | Nitride ceramic material microwave sintering method |
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| CN1749213A (en) * | 2005-07-29 | 2006-03-22 | 四川艺精长运超硬材料有限公司 | Process for preparing AIN ceramic material |
| CN101985396A (en) * | 2010-11-03 | 2011-03-16 | 刘述江 | Method for preparing aluminum nitride ceramic substrate by clinker slicing |
| CN102344286A (en) * | 2010-07-27 | 2012-02-08 | 台盐实业股份有限公司 | Aluminum nitride ceramic radiating fin and manufacturing method thereof |
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2012
- 2012-10-08 CN CN2012103767887A patent/CN102875156A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1749213A (en) * | 2005-07-29 | 2006-03-22 | 四川艺精长运超硬材料有限公司 | Process for preparing AIN ceramic material |
| CN102344286A (en) * | 2010-07-27 | 2012-02-08 | 台盐实业股份有限公司 | Aluminum nitride ceramic radiating fin and manufacturing method thereof |
| CN101985396A (en) * | 2010-11-03 | 2011-03-16 | 刘述江 | Method for preparing aluminum nitride ceramic substrate by clinker slicing |
Non-Patent Citations (2)
| Title |
|---|
| 徐耕夫等: "氮化铝陶瓷的微波烧结研究", 《硅酸盐学报》, vol. 25, no. 1, 28 February 1997 (1997-02-28), pages 89 - 95 * |
| 李友芬等: "ALN陶瓷烧结技术研究进展", 《现代技术陶瓷》, no. 1, 31 December 2006 (2006-12-31), pages 28 - 31 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224398A (en) * | 2013-04-26 | 2013-07-31 | 湖南凯新陶瓷科技有限公司 | Nitride ceramic material microwave sintering method |
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Application publication date: 20130116 |