CN1398790A - Rod-like polycrystal GaN and its two-step prepn process - Google Patents
Rod-like polycrystal GaN and its two-step prepn process Download PDFInfo
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- CN1398790A CN1398790A CN 02136638 CN02136638A CN1398790A CN 1398790 A CN1398790 A CN 1398790A CN 02136638 CN02136638 CN 02136638 CN 02136638 A CN02136638 A CN 02136638A CN 1398790 A CN1398790 A CN 1398790A
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Abstract
Rod-like polycrystal GaN is prepared through two-step process including the steps of: firstly, washing substrate with cleaning liquid by use of the hot bath method; secondly hot evaporating metal Ga so as to make Ga atoms uniformly distributed on the surface of the substrate through the steps of setting the cleaned substrate in some tray of an evaporator, setting Ga source inside a quartz crucible of the evaporator, vacuum pumping the evaporator to 1E(-3)-1, Pa heating the substrate to 600-800 deg.c and heating Ga source to 600-900 deg.c; and thirdly nitriding the metal Ga layer in a heating furnace of nitriding equipment at normal pressure or vacuum through heating to 800-1000 deg.C and introducing pure nitrogen before cooling. The product of the present invention is rod-like polycrystal of 0.2-2 micron diameter and 10-20 micron length.
Description
Technical field
The present invention relates to polycrystalline material and preparation method thereof, relate to polycrystal GaN of photoelectric device use and preparation method thereof specifically.
Background technology
For a long time, most photoelectric devices all are to use monocrystal material to be prepared from, yet the growth technique complexity of monocrystal material, conditional request harshness, and size is less, cost an arm and a leg, so the development of polycrystalline photoelectric device becomes important research direction in the semi-conductor industry field naturally.
Summary of the invention
The purpose of this invention is to provide that a kind of cost is low, the simple rod-like polycrystal GaN of growth technique and preparation method thereof.
Rod-like polycrystal GaN of the present invention is that diameter is 200nm～2 μ m, and length is the bar-like polycrystal of 10～20 μ m.
The two-step preparation process of rod-like polycrystal GaN of the present invention may further comprise the steps:
1) adopt hot bath method to clean substrate with scavenging solution;
2) substrate after will cleaning is put on the substrate bracket of heat evaporating device, and gallium (Ga) source is placed in the quartz crucible of heat evaporating device, and heat evaporating device is evacuated down to 1Pa～10
-3Pa, heating makes underlayer temperature be raised to 600～800 ℃, and the gallium source temperature is raised to 600～900 ℃, and the thermal evaporation gallium makes the gallium atom be evenly distributed on substrate surface;
3) with step 2) the gained substrate that deposited the gallium layer puts into the process furnace of ammonia nitrogenize device, under normal pressure or vacuum, is warming up to 800～1000 ℃, feed high-purity ammonia (99.999%), carry out nitrogenize, under the logical ammonia situation of maintenance, cool off then, get product of the present invention with furnace temperature.
Used scavenging solution can be the mixing solutions of acetone or vinylchlorid, acetone and Virahol in the aforesaid method.Substrate adopts quartz usually.The flow of logical ammonia generally be controlled at 40～80ml/min, change ammonia flow, can prepare the rod-like polycrystal GaN of different size.
The invention has the advantages that: growth apparatus is simple, prepared rod-like polycrystal GaN controllable size that goes out and size evenly, low price, purity height.
Description of drawings
Fig. 1 is the heat evaporating device synoptic diagram;
Among the figure, 1 water-cooled tube, 2 bell jars, 3 heater support, 4 graphite heaters, 5 gallium sources, 6 crucible trays, 7 quartz crucibles, 8 substrate brackets, 9 substrates, 10 tungsten heaters
Fig. 2 is an ammonia nitrogenize device synoptic diagram;
Among the figure, 11 injection ports, 12 movable sample holders, 13 silica tubes, 14 inlet mouths, 15 air valves, 16 thermopairs, 17 process furnace
Fig. 3 is the X-ray diffractogram that is grown in rod-like polycrystal GaN on the quartz substrate;
Fig. 4 is the surperficial complexion figure of the captured rod-like polycrystal GaN of AMRAY1840 scanning electron microscope.
Embodiment
Further specify the present invention below in conjunction with accompanying drawing by embodiment.
Present embodiment prepares rod-like polycrystal GaN and specifically may further comprise the steps:
1) adopt hot bath method to clean quartz substrate with the mixing solutions of vinylchlorid, acetone and Virahol;
2) quartz substrate 9 after will cleaning is put on the substrate bracket 8 of heat evaporating device shown in Figure 1, gallium source 5 is placed in the quartz crucible 7 of heat evaporating device, and heat evaporating device is evacuated down to 3 * 10
-3Pa by tungsten heater 10 heated substrate, makes underlayer temperature be raised to 600～650 ℃, by graphite heater 5 heating gallium sources, makes the gallium source temperature be raised to 850 ℃, and the thermal evaporation gallium makes the gallium atom be evenly distributed on quartz substrate surface;
3) with step 2) the gained substrate that deposited the gallium layer puts in the movable sample holder 2 of silica tube 3 of ammonia nitrogenize device shown in Figure 2, under normal pressure, be warming up to 950～1000 ℃, feed high-purity ammonia from inlet mouth 4, carried out nitrogenize about one hour, under the logical ammonia situation of maintenance, cool off then, get product of the present invention with furnace temperature.
Products obtained therefrom is seen Fig. 3, it is polycrystalline six side GaN, the main peak in its three crystal orientation (1010) (0002) (1011) appears at 2 θ respectively and is 32.381 °, 34.543 ° and 36.828 ° and locates, in addition among this figure other small peaks also all corresponding to other crystal orientation of polycrystalline six side GaN.The inclusion-free peak is (as Ga
2O
3The peak) occurs, prove to have obtained purer polycrystal GaN.
The surperficial complexion of products obtained therefrom is seen Fig. 4, can be clear that from figure, and there is the rhabdolith structure that orientation is different, be evenly distributed in sample surfaces, and its diameter is about 1 μ m, and length is 10-20 μ m.
Claims (5)
1. rod-like polycrystal GaN is characterized in that it is that diameter is 200nm～2 μ m, and length is the bar-like polycrystal of 10～20 μ m.
2. by the two-step preparation process of the described rod-like polycrystal GaN of claim 1, it is characterized in that may further comprise the steps:
1) adopt hot bath method to clean substrate with scavenging solution;
2) substrate after will cleaning is put on the substrate bracket of heat evaporating device, the gallium source is placed in the quartz crucible of heat evaporating device, and heat evaporating device is evacuated down to 1Pa～10
-3Pa, heating makes underlayer temperature be raised to 600～800 ℃, and the gallium source temperature is raised to 600～900 ℃, and the thermal evaporation gallium makes the gallium atom be evenly distributed on substrate surface;
3) with step 2) the gained substrate that deposited the gallium layer puts into the process furnace of ammonia nitrogenize device, under normal pressure or vacuum, is warming up to 800～1000 ℃, feed high-purity ammonia, carry out nitrogenize, under the logical ammonia situation of maintenance, cool off then, get product of the present invention with furnace temperature.
3. by the two-step preparation process of the described rod-like polycrystal GaN of claim 2, it is characterized in that scavenging solution is the mixing solutions of acetone or vinylchlorid, acetone and Virahol.
4. by the two-step preparation process of the described rod-like polycrystal GaN of claim 2, it is characterized in that the flow of logical ammonia at 40～80ml/min.
5. by the two-step preparation process of the described rod-like polycrystal GaN of claim 2, it is characterized in that said substrate is quartzy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021366381A CN1182039C (en) | 2002-08-20 | 2002-08-20 | Rod-like polycrystal GaN and its two-step prepn process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021366381A CN1182039C (en) | 2002-08-20 | 2002-08-20 | Rod-like polycrystal GaN and its two-step prepn process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1398790A true CN1398790A (en) | 2003-02-26 |
| CN1182039C CN1182039C (en) | 2004-12-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB021366381A Expired - Fee Related CN1182039C (en) | 2002-08-20 | 2002-08-20 | Rod-like polycrystal GaN and its two-step prepn process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410178C (en) * | 2006-10-25 | 2008-08-13 | 国家纳米技术与工程研究院 | Process for preparing tipped gallium nitride conical stick using self catalytic mode |
| CN100410179C (en) * | 2006-10-25 | 2008-08-13 | 国家纳米技术与工程研究院 | Method for preparing gallium nitride nano crystal using sol-gel method |
| CN101863458A (en) * | 2010-06-23 | 2010-10-20 | 西安理工大学 | Method for preparing GaN nanowires |
-
2002
- 2002-08-20 CN CNB021366381A patent/CN1182039C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410178C (en) * | 2006-10-25 | 2008-08-13 | 国家纳米技术与工程研究院 | Process for preparing tipped gallium nitride conical stick using self catalytic mode |
| CN100410179C (en) * | 2006-10-25 | 2008-08-13 | 国家纳米技术与工程研究院 | Method for preparing gallium nitride nano crystal using sol-gel method |
| CN101863458A (en) * | 2010-06-23 | 2010-10-20 | 西安理工大学 | Method for preparing GaN nanowires |
| CN101863458B (en) * | 2010-06-23 | 2011-12-14 | 西安理工大学 | Method for preparing GaN nanowires |
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| Publication number | Publication date |
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| CN1182039C (en) | 2004-12-29 |
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