CN103305917A - Method for manufacturing GaN template substrate and GaN template substrate - Google Patents
Method for manufacturing GaN template substrate and GaN template substrate Download PDFInfo
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- CN103305917A CN103305917A CN2013100549974A CN201310054997A CN103305917A CN 103305917 A CN103305917 A CN 103305917A CN 2013100549974 A CN2013100549974 A CN 2013100549974A CN 201310054997 A CN201310054997 A CN 201310054997A CN 103305917 A CN103305917 A CN 103305917A
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- template substrate
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Abstract
The invention provides a cheap and highly effective method for manufacturing gallium nitride (GaN) template substrates of which the quality is the same as or higher than the GaN template substrates made by metal-organic vapor growth, and the GaN template substrate. The method for manufacturing GaN template substrates includes sequentially growing a nucleating layer (12) containing aluminum nitride (AIN) and a buffer layer (13) containing GaN through hydride vapor growth. During growing the nucleating layer (12), the mole ratio( V/III ratio) of the V-group materials to the III-group materials greater than 0.5 and smaller than 3.
Description
Technical field
The present invention relates to manufacture method and the gallium nitride template substrate of gallium nitride template substrate.
Background technology
Shown in Fig. 1 (a) ~ (d), the gallium nitride template substrate 10 that in white light-emitting diode etc., uses by stack gradually nucleating layer 12, the buffer layer 13 that comprises gan (GaN) that comprises aluminium nitride (AlN) at underlay substrate 11, each epitaxial film such as active coating 14 that comprises GaN is made, but require more cheap and make expeditiously.
Template growth technology as these epitaxial films of growth, the most universal method is to use organo-metallic vapor growth method (MOVPE method), but the method is because except the raw materials cost height, the speed of growth is for per hour counting μ m, therefore exist when the buffer layer 13 of wanting to grow about 10 μ m, need long-time such problem.
Therefore, can consider following method: by comparing the hydride vapor growth method (HVPE method) that raw materials cost cheapness and the speed of growth per hour are the above high speed of 10 μ m ~ 100 μ m with the organo-metallic vapor growth method, the nucleating layer 12 on the underlay substrate 11 of growing and the buffer layer 13 on it.
According to the method, compare with the situation of whole epitaxial film of growing by the organo-metallic vapor growth method, can shorten by leaps and bounds growth time, when batch production gallium nitride template substrate 10, can enhance productivity by leaps and bounds.
In addition, by using sapphire substrate cheap and that easily obtain as underlay substrate 11, can further reduce cost.
The prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2012-012292 communique
Summary of the invention
Yet, use the template growth technology on the sapphire substrate of hydride vapor growth method, compare with the situation of using the organo-metallic vapor growth method, growth controlled poor, thereby the gallium nitride template substrate of high-quality can not stably be provided, expect early stage technology establishment.
Therefore, the object of the invention is to, a kind of manufacture method and the gallium nitride template substrate that can make cheap and expeditiously with the gallium nitride template substrate of the equal above high-quality gallium nitride template substrate of the situation of using the organo-metallic vapor growth method is provided.
Solve the method for problem
The present invention who finishes in order to realize this purpose, it is a kind of manufacture method of gallium nitride template substrate, it is on sapphire substrate, by grow at least successively nucleating layer that comprises aluminium nitride and comprise the manufacture method of gallium nitride template substrate of the buffer layer of gan of hydride vapor growth method, and to make the mol ratio (V/III ratio) of V family raw material and III family raw material when the above-mentioned nucleating layer of growth be more than 0.5 below 3.
Preferably when the above-mentioned nucleating layer of growth, add hydrogen chloride gas.
Preferably in growth during above-mentioned nucleating layer, flow into hydrogen chloride gas when flowing into ammonia as above-mentioned V family raw material, and make the above-mentioned ammonia of its throughput ratio many.
Preferably making growth pressure is below the above 106kPa of 90kPa.
Preferably use during above-mentioned nucleating layer aluminum chloride as above-mentioned III family raw material in growth.
In addition, the present invention is a kind of gallium nitride template substrate, and it is the gallium nitride template substrate of making by aforesaid method, and the thickness of above-mentioned buffer layer is below the 5 μ m, and the halfwidth of the X ray rocking curve of its (0002) face or (0004) face is below 250 seconds.
The invention effect
According to the present invention, can provide a kind of manufacture method and the gallium nitride template substrate that can make cheap and expeditiously with the gallium nitride template substrate of the equal above high-quality gallium nitride template substrate of the situation of using the organo-metallic vapor growth method.
Description of drawings
Fig. 1 is the figure of the manufacture method of explanation gallium nitride template substrate.
Fig. 2 is the sketch chart of expression hydride vapor phase growth subtraction unit.
Fig. 3 represents when changing the throughput ratio of hydrogen chloride gas and ammonia the figure of the relation of the halfwidth of the mol ratio of V family raw material and III family raw material and the X ray rocking curve of (0004) face.
Nomenclature
10: the gallium nitride template substrate; 11: underlay substrate (sapphire substrate); 12: nucleating layer (aluminium nitride); 13: buffer layer (gan); 14: active coating (gan).
Embodiment
Below based on the description of drawings preferred embodiment of the present invention.
Shown in Fig. 1 (a) ~ (d), the manufacture method of the gallium nitride template substrate 10 of present embodiment is characterised in that, on the sapphire substrate as underlay substrate 11, by grow at least successively nucleating layer 12 that comprises aluminium nitride and comprise the buffer layer 13 of gan of hydride vapor growth method, and to make the mol ratio (V/III ratio) of V family raw material and III family raw material when growing into stratum nucleare 12 be more than 0.5 below 3.In addition, Fig. 1 example of the active coating 14 that forms of lamination GaN based material that has been illustrated in further growth on the buffer layer 13.Active coating 14 also can be luminous element or electronic device structure.
Realize that to being used for the hydride epitaxially growing equipment of this manufacture method describes.
As shown in Figure 2, the hydride epitaxially growing equipment 20 of gallium nitride template substrate 10 has been divided into the raw material section 21 of upstream side and the growing part 22 in downstream side, each utilize raw material section well heater 23, growing part well heater 24 separately be heated to respectively about 600 ~ 850 ℃, about 900 ~ 1200 ℃.
Inboard at raw material section well heater 23 and growing part well heater 24 arranges Reaktionsofen 25.In this Reaktionsofen 25, from raw material section 21 towards growing part 22, the supply line of 4 systems is set, that is: be used for supplying with doping agent doping agent supply line 26, be used for supplying with ammonia (NH
3) ammonia supply line 27, be used for to supply with gallium chloride (GaCl) gallium chloride supply line 28, be used for supplying with and contain aluminum chloride (AlCl
3) and the mixed gas supply line 29 of hydrogenchloride (HCl) mixed gas.
When the growth of not mixing, supply with hydrogen (H from doping agent supply line 26
2), nitrogen (N
2) or the mixed gas of hydrogen and nitrogen, in the situation of toasting for the gallium nitride based dirt settling that will adhere in Reaktionsofen 25 removes, with the mixed gas of hydrogen, nitrogen or hydrogen and nitrogen as carrier gas and supply with hydrogen chloride gas, in the situation that mix, hydrogen, nitrogen or hydrogen are supplied with dopant gas with the mixed gas of nitrogen as carrier gas and with hydrogen chloride gas etc.
From ammonia supply line 27, with supply with hydrogen, nitrogen or hydrogen as carrier gas and the mixed gas of nitrogen as the ammonia of V family raw material.
(be positioned at the part of raw material section 21) in the way of gallium chloride supply line 28 the gallium tank 31 that contains gallium (Ga) is set, the melting by raw material section well heater 23 of this gallium forms Gallium solution 32.
In gallium chloride supply line 28, from upstream side, supply with hydrogen chloride gas with hydrogen, nitrogen or hydrogen as carrier gas with the mixed gas of nitrogen, Gallium solution 32 in this hydrogen chloride gas and the gallium tank 31 reacts, generation is as the gallium chloride gas of III raw material, and is supplied to growing part 22.
Mixed gas supply line 29 is merged by aluminum chloride supply line 33 and hydrogenchloride supply line 34.
In the way of aluminum chloride supply line 33, (be positioned at the part of the upstream side of raw material section 21) aluminium pot 36 that contains aluminium (Al) particle 35 is set.
This be because: if the excess Temperature of aluminum particulate 35 can form monochlor(in)ate aluminium (AlCl) during then with the hydrogen chloride gas precursor reactant, thereby make the quartz corrosion that consists of Reaktionsofen 25, supply line etc.This danger can be avoided by the aluminium pot 36 that contains aluminum particulate 35 is set in than 660 ℃ of lower temperature ranges of fusing point of aluminium.
In aluminum chloride supply line 33, from upstream side, supply with hydrogen chloride gas with hydrogen, nitrogen or hydrogen as carrier gas with the mixed gas of nitrogen, aluminum particulate 35 in this hydrogen chloride gas and the aluminium pot 36 reacts, generation is as the aluminum chloride gas of III family raw material, and is supplied to growing part 22.
In addition, in the downstream side of aluminium pot 36, connect the hydrogenchloride supply line 34 that is used for supplying with hydrogen chloride gas.In hydrogenchloride supply line 34, from upstream side, supply with hydrogen chloride gas with hydrogen, nitrogen or hydrogen as carrier gas with the mixed gas of nitrogen, these gases with converge from the aluminum chloride gas of aluminum chloride supply line 33, and be supplied to growing part 22.
In growing part 22, the pallet (tray) 37 with the rotation of the revolution about 3 ~ 100rpm is set, at the face (face be set) 38 relative with the outlet of this supply line underlay substrate 11 is set.The gas that flows through after underlay substrate 11 is discharged from by vapor pipe 39 from downstream portion.
When making gallium nitride template substrate 10 with this hydride epitaxially growing equipment 20, at first the face 38 at pallet 37 arranges underlay substrate 11.Underlay substrate 11 becomes be used to the pedestal that grows into each epitaxial film such as stratum nucleare 12, buffer layer 13 and active coating 14.The below growth of each epitaxial film of explanation, can make growth pressure is to carry out near the above 106kPa of 90kPa of normal pressure following (the above 800Torr of 680Torr is following).
After underlay substrate 11 is set, 22 supply with ammonia from ammonia supply line 27 to growing part, 22 supply with the aluminum chloride gases from aluminum chloride supply line 33 to growing part simultaneously, making as the ammonia of V family material and mol ratio as the aluminum chloride of III family raw material is more than 0.5 below 3, thereby grows into stratum nucleare 12 at underlay substrate 11.
Preferably when this nucleating layer 12 of growth, add hydrogen chloride gas, particularly preferably, flow into hydrogen chloride gas from hydrogenchloride supply line 34 when flowing into ammonia as V family raw material from ammonia supply line 27, and make its throughput ratio ammonia many.At this moment, by supplying with hydrogen chloride gas, capable of regulating its flow via mixed gas supply line 29 to growing part 22 from hydrogenchloride supply line 34.
By growing into stratum nucleare 12 with non-polar underlay substrate 11(sapphire) surface transformation is the aluminium nitride with polarity, thus the thereon buffer layer 13 of growing high quality and the active coating on it 14.
Here, the mol ratio that makes V family raw material and III family raw material when growing into stratum nucleare 12 is the basis below 3 and flow into hydrogen chloride gas and preferably make the many reasons of its throughput ratio ammonia when growing into stratum nucleare 12 more than 0.5, uses Fig. 3 to describe.
Finish when of the present invention, take the thickness of nucleating layer 12 as 20nm, the buffer layer 13 that comprises gan as 4.5 μ m as rigid condition, V family raw material when growing into stratum nucleare 12 and the mol ratio of III family raw material are changed in 0.5 to 1000 scope, by the hydride vapor growth method, made gallium nitride template substrate 10.What use in common organo-metallic vapor growth method, hydride vapor phase growth is the mol ratio (for example value below 1000 or more than it more than 10) of higher V family raw material and III family raw material.In this experiment, as can be known: though the mol ratio (V/III ratio) of the V family raw material that makes aluminium nitride when growth and III family raw material than 3 height, the halfwidth of the X ray rocking curve (locking curve) of (0004) face of the gan of growing thereon still is about 250 seconds.Yet, the mol ratio of the V family raw material that makes aluminium nitride when growth and III family raw material than in the past low, be in the situation below 3, even the thickness of buffer layer 13 is below the 5 μ m, also can to make the halfwidth of X ray rocking curve of (0004) face of gan be below 250 seconds, can improve to some extent with former the comparing of III family material molar ratio than having improved V family raw material.
Since by former use the method for organo-metallic vapor growth method, also can make the gallium nitride template substrate 10 of halfwidth in 300 seconds following scopes more than 200 seconds of X ray rocking curve of (0004) face of gan, so its mean value became the target of the characteristic quality of template substrate in 250 seconds.
That is to say, its meaning is: if the halfwidth of the X ray rocking curve of gan (0004) face is below 250 seconds, then be and the equal above high-quality gallium nitride template substrate 10 of the method for using the organo-metallic vapor growth method.
On the other hand, if in fact the mol ratio less than 0.5 of V family raw material and III family raw material then can't carry out the growth of nucleating layer 12, therefore it is defined as lower value.
Based on above basis, the mol ratio that makes V family raw material and III family raw material when growing into stratum nucleare 12 is more than 0.5 below 3.
And as can be known, make hydrogen chloride gas when growing into stratum nucleare 12 with respect to the throughput ratio (HCl/NH of ammonia
3) in 0 to 2 scope, change, and when having made gallium nitride template substrate 10 by the hydride vapor growth method, along with increasing the flow of hydrogen chloride gas with respect to ammonia, the halfwidth of the X ray rocking curve of (0004) face of gan reduces.In order to confirm hydrogen chloride gas with respect to the upper limit of the flow of ammonia, attempted making this fluctuations in discharge to HCl/NH
3Be 10, the result can grow as can be known without problems.
As mentioned above, when increasing hydrogen chloride gas with respect to the flow of ammonia, the reason that the halfwidth of the X ray rocking curve of (0004) face of gan reduces, think because: because hydrogen chloride gas is in the mixed gas of V family raw material and III family raw material, the gas-phase reaction that therefore can suppress V family raw material and III family raw material, the nucleating layer 12 of growing high quality on underlay substrate 11.Can think: when having gas-phase reaction, the resultant in the gas phase can be attached in the growth of aluminium nitride on underlay substrate 11 surfaces, so the crystal orientation of aluminium nitride is disorderly, and the crystallinity of the gan of growth is deteriorated thereon.
In addition, not only (0004) face uses the halfwidth of the X ray rocking curve of (0002) face also can obtain roughly the same result.This is because only only be the difference of order of reflection.
Based on above reason, obtain such conclusion: preferably when growing into stratum nucleare 12, flow into hydrogen chloride gas, and make its throughput ratio ammonia many.
Grown behind the nucleating layer 12 of before this explanation, 22 supply with ammonia from ammonia supply line 27 to growing part, 22 supply with the gallium chloride gases from gallium chloride supply line 28 to growing part simultaneously, grown buffer layer 13 on nucleating layer 12, further 22 supply with doping agents, growth activity layer 14 on buffer layer 13 from doping agent supply line 26 to growing part if required.
Thus, even in the situation that use the hydride vapor growth method, the thickness of buffer layer 13 also is below the 5 μ m, and in this case, the halfwidth that also can obtain the X ray rocking curve of its (0002) face or (0004) face is the gallium nitride template substrate 10 of the high-quality below 250 seconds.
Below generally speaking, manufacture method according to the gallium nitride template substrate 10 of present embodiment, owing to using the hydride vapor growth method, and the mol ratio that makes V family raw material and III family raw material when growing into stratum nucleare 12 is more than 0.5 below 3, therefore can make inexpensive and expeditiously and the equal above high-quality gallium nitride template substrate 10 of the situation of using the organo-metallic vapor growth method.
In addition, by inflow hydrogen chloride gas when growing into stratum nucleare 12, and make its throughput ratio ammonia many, can make cheap and expeditiously and realize the further gallium nitride template substrate 10 of high-qualityization.
In addition, in embodiment, used aluminum chloride as III family raw material, but the organo-metallic such as use trimethyl aluminium (TMA) also are fine.
In addition, in the present embodiment, make growth pressure for carrying out the growth of each epitaxial film below the close above 106kPa of 90kPa of normal pressure, its reason is: in the situation of the growth of carrying out each epitaxial film under the not enough 90kPa, although also can obtain the measurement result same with present embodiment, but the mol ratio of V family raw material and III family raw material is that the halfwidth of the X ray rocking curve of (0004) face more than 3 is about 400 seconds, the mol ratio of V family raw material and III family raw material be 0.5 and the mol ratio of hydrogenchloride and ammonia be that the best halfwidth that obtains in 2 the situation also is about 300 seconds, do not reach the obtainable effect of present embodiment.
Claims (6)
1. the manufacture method of a gallium nitride template substrate, it is characterized in that, it is on sapphire substrate, by grow at least successively nucleating layer that comprises aluminium nitride and comprise the manufacture method of gallium nitride template substrate of the buffer layer of gan of hydride vapor growth method, and to make mol ratio, the V/III ratio of V family raw material and III family raw material when the described nucleating layer of growth be more than 0.5 below 3.
2. the manufacture method of gallium nitride template substrate according to claim 1 is added hydrogen chloride gas when the described nucleating layer of growth.
3. the manufacture method of gallium nitride template substrate according to claim 2 when the described nucleating layer of growth, flows into hydrogen chloride gas when flowing into ammonia as described V family raw material, and makes the described ammonia of its throughput ratio many.
4. the manufacture method of each described gallium nitride template substrate according to claim 1 ~ 3, making growth pressure is below the above 106kPa of 90kPa.
5. the manufacture method of each described gallium nitride template substrate according to claim 1 ~ 4 uses during described nucleating layer aluminum chloride as described III family raw material in growth.
6. gallium nitride template substrate, it is characterized in that, it is the gallium nitride template substrate of making by each described method in the claim 1 ~ 5, and the thickness of described buffer layer is below the 5 μ m, and the halfwidth of the X ray rocking curve of its (0002) face or (0004) face is below 250 seconds.
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| JP2012051531A JP5829152B2 (en) | 2012-03-08 | 2012-03-08 | Method for manufacturing gallium nitride template substrate and gallium nitride template substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110544619A (en) * | 2018-05-29 | 2019-12-06 | 汉阳大学校产学协力团 | Method for manufacturing gallium nitride substrate by hydride vapor deposition |
| CN113840949A (en) * | 2019-05-27 | 2021-12-24 | 信越化学工业株式会社 | Method for producing group III compound substrate, and group III compound substrate |
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| JP6004849B2 (en) * | 2012-09-07 | 2016-10-12 | 株式会社トクヤマ | Method for producing aluminum halide gas |
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| JP4992616B2 (en) * | 2007-09-03 | 2012-08-08 | 日立電線株式会社 | Method for producing group III nitride single crystal and method for producing group III nitride single crystal substrate |
| JP5668339B2 (en) * | 2010-06-30 | 2015-02-12 | 住友電気工業株式会社 | Manufacturing method of semiconductor device |
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| CN1943051A (en) * | 2005-03-14 | 2007-04-04 | 株式会社东芝 | Light emitting device with fluorescent material |
| US20060281205A1 (en) * | 2005-06-10 | 2006-12-14 | Samsung Electro-Mechanics Co., Ltd. | Method for manufacturing nitride-based semiconductor device |
| US20080197359A1 (en) * | 2007-02-20 | 2008-08-21 | Fujitsu Limited | Compound semiconductor device and method of manufacturing the same |
| CN101816061A (en) * | 2007-10-04 | 2010-08-25 | 应用材料股份有限公司 | Parasitic particle suppression in the growth of III-V nitride films using MOCVD and HVPE |
| JP2012031027A (en) * | 2010-08-02 | 2012-02-16 | Tokyo Univ Of Agriculture & Technology | Method for producing single crystal aluminum nitride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110544619A (en) * | 2018-05-29 | 2019-12-06 | 汉阳大学校产学协力团 | Method for manufacturing gallium nitride substrate by hydride vapor deposition |
| CN110544619B (en) * | 2018-05-29 | 2023-08-29 | 汉阳大学校产学协力团 | Method for manufacturing gallium nitride substrate by hydride vapor deposition method |
| CN113840949A (en) * | 2019-05-27 | 2021-12-24 | 信越化学工业株式会社 | Method for producing group III compound substrate, and group III compound substrate |
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| TW201338205A (en) | 2013-09-16 |
| JP2013187367A (en) | 2013-09-19 |
| TWI546981B (en) | 2016-08-21 |
| JP5829152B2 (en) | 2015-12-09 |
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