CN103325895B - The method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode - Google Patents
The method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode Download PDFInfo
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Abstract
The invention provides a kind of method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, comprise the following steps, S1, the gallium nitride monocrystal substrate of non-polar plane is warming up to the growth temperature range of N-shaped conductive layer, growing gallium nitride N-shaped conductive layer; S2, grown quantum well layer on N-shaped conductive layer; S3, growing gallium nitride p-type electric-conducting layer on quantum well layer.The present invention is by changing the crystallographic direction of gallium nitride substrate growing surface, reduce the electronics and hole being separated in the direction of growth that cause due to pressure polarization electric field and spontaneous polarization electric field in quantum well layer, thus improve the light radiation combined efficiency of charge carrier at luminescent layer.
Description
Technical field
The present invention relates to field of illuminating lamps, particularly relate to a kind of production method of light-emitting diode.
Background technology
Existing gallium nitride-based epitaxial layer primary growth is on <0001>c surface sapphire or SiC substrate, sapphire and gallium nitride belong to six side system crystal together, as shown in Figure 1a, upper and lower two lattice planes are <0001>c face, and face, six, side is <10-10>m face.The epitaxial layer of gallium nitride that c surface sapphire substrate grows can obtain enough good crystal mass, the LED with good luminous efficiency and reliability can be obtained further, so <0001>c surface sapphire substrate is used in a large number in LED epitaxial growth at present.But the gallium nitride belonging to hexagoinal lattice equally also exists spontaneous polarization electric field on <0001>c face, add the pressure polarization electric field action that the stress of indium gallium nitrogen and gallium nitrogen heterojunction produces, cause electronics and hole to be separated in the space of (being also current delivery direction) in the direction of growth, cause InGaN/GaN quantum well radiation efficiency in epitaxial loayer to reduce further.As shown in Figure 3,1 is p-type electric-conducting layer, and 2 is N-shaped conductive layer, and 3 is quantum well layer.
Applicant finds, as shown in Figure 1a, when changing the growth crystal face of gallium nitride, the polarized electric field size in quantum well layer changes.Such as when adopting the crystal face vertical with <0001>c face as <10-10>m (shown in Fig. 1 a) or <11-20>a face (shown in Fig. 1 b), because polarized electric field direction and base chip are to vertical, electronics and the hole space in the direction of growth is separated minimum, thus polarized electric field can not under LED component is energized condition of work to charge carrier in the flow direction (electronics and hole) apply electric field force, thus charge carrier can not be made to misplace in the transmit direction, as shown in Figure 4, 1 is p-type electric-conducting layer, 2 is N-shaped conductive layer, 3 is quantum well layer.Above-mentioned the charge carrier radiation recombination efficiency that effectively can improve quantum well layer 3 is set, greatly improves luminous efficiency.
<10-10>m face and <11-20>a face, due to vertical with <0001>c face, growth course direction is vertical with polarized electric field direction, therefore is called nonpolarity.Applicant also finds, crystal face between nonpolarity (a face) and polar surface (c face), as <20-21>e2 face and <20-2-1>e2' face, also can obtain qualified aufwuchsplate.This area is that the normal direction in the <0001>c face of end atom is for positive direction with Ga with plane of crystal, the normal in <20-21>e2 face becomes 75 ° of angles with positive direction, <20-2-1>e2' face normal becomes 105 ° of angles with positive direction.
<20-21>e2 face and <20-2-1>e2' surface polarization electric field strength are between polar surface c face and nonpolarity a face or m face, be called semi-polarity face in the application, semi-polarity face and nonpolarity face are referred to as non-polar plane.
Fig. 2 be aufwuchsplate polarity along with normal is relative to the variation tendency table of the angle of positive direction, in table, x represents In
xga
1-xthe value of the x of Indium in N, transverse axis represents the angle of normal relative to positive direction of crystal face, and the longitudinal axis represents the size of pressure polarization electric field, unit be coulomb/square metre.
Further, in actual applications, the crystal mass that a face is nonpolar and the more difficult acquisition of most of semi-polarity face GaN crystal is qualified is to be applicable to GaN epitaxial growth.Simple employing original c face epitaxy technique parameter easily forms the crystal defects such as fault, and the process conditions therefore in semi-polarity or non-polar plane are distinguished to some extent.
Summary of the invention
Object of the present invention provides a kind of method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, improves the light radiation combined efficiency of luminescent layer.
The invention provides a kind of method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, comprise the following steps,
S1, is warming up to the growth temperature range of N-shaped conductive layer by the gallium nitride monocrystal substrate of non-polar plane, and under the atmosphere of ammonia growing gallium nitride N-shaped conductive layer;
S2, grown quantum well layer on N-shaped conductive layer;
S3, growing gallium nitride p-type electric-conducting layer on quantum well layer.
The present invention is by changing the crystallographic direction of gallium nitride substrate growing surface, reduce the electronics and hole being separated in the direction of growth that cause due to pressure polarization electric field and spontaneous polarization electric field in quantum well layer, thus improve the light radiation combined efficiency of charge carrier at luminescent layer.
In some embodiments, in S1, non-polar plane is nonpolarity <11-20>a face or <10-10>m face.Because a face, m face are all vertical with c face, so polarized electric field disappears completely in the direction of growth, the gallium nitride homo-substrate in current m face more easily obtains, and better in the gallium nitride quality of m face Grown.
In some embodiments, in S1, non-polar plane is <20-21>e2 face, semi-polarity face.<20-21>e2 face normal direction becomes 75 ° of angles with positive direction, thus polarized electric field is also less in the direction of growth.On this face, grow wavelength longer (such as green glow) extension can need less indium simultaneously, thus produces less stress, avoids due to the excessive generation misfit dislocation of stress.
In some embodiments, in S1, non-polar plane is <20-2-1>e2' face, semi-polarity face.<20-2-1>e2' face normal direction becomes 105 ° of angles with positive direction, thus polarized electric field is also less in the direction of growth.Under the condition obtaining same wavelength, use this semi-polarity face substrate to grow at a higher temperature, thus or obtain better crystalline quality.
In some embodiments, first grow the bottom of a non-impurity-doped gallium nitride in S1 before growing gallium nitride N-shaped conductive layer, the thickness of bottom is 0.5 ~ 1um.For the preparation layer of N-shaped conductive layer growth.
In some embodiments, in S1, the growth temperature range of N-shaped conductive layer is 900 ~ 1000 DEG C, and the impurity element of N-shaped conductive layer is Si, and dopant concentration is 1 × 10
18~ 2 × 10
19/ cm
3, thickness is that 2 ~ 4um is to obtain the contact of good N-shaped.In the present invention, alleged dopant concentration is in the number of foreign atom in cubic unit centimetre.
In some embodiments, before being also included in grown quantum well layer, first growth is without the separator of the gallium nitride mixed for S2, and the growth temperature of separator is 750 ~ 900 DEG C, and thickness is 10 ~ 40nm.For the preparation layer of quantum trap growth.
In some embodiments, in S2, quantum well layer comprises the well layer of indium gallium nitrogen and the barrier layer of gallium nitride, well layer thickness is 2.0 ~ 3.5nm, barrier layer thickness is 6 ~ 12nm, logarithm is 6 ~ 12 right, the growth temperature of quantum well layer is 740 ~ 860 DEG C, and growth atmosphere is the gaseous mixture of nitrogen or nitrogen and hydrogen.
In some embodiments, first grow electronic barrier layer before also comprising growth p-type electric-conducting layer in S3, electronic blocking layer thickness is 10 ~ 30nm, and mixing element is magnesium, and ginseng magnesium density is 1 × 10
19~ 1 × 10
20/ cm
3.Non-radiative recombination is carried out to p-type layer to reduce electron transition.
In some embodiments, p-type electric-conducting layer in S3, thickness is 100 ~ 200nm, and ginseng magnesium density is 1 × 10
19~ 1 × 10
20/ cm
3, to obtain good p-type current spread.
In some embodiments, the present invention also comprises the S4 after S3, on p-type electric-conducting layer, grow contact layer, and contact layer thickness is 10 ~ 20nm, and ginseng magnesium density is 1 × 10
20~ 1 × 10
21/ cm
3.To obtain good p-type contact.
Accompanying drawing explanation
Fig. 1 a is each structural representation of six side system gallium nitride;
Fig. 1 b is a face position view of six side system gallium nitride;
Fig. 1 c is the e2 face position view of six side system gallium nitride, and wherein A is to being positive direction, and B is to being e2 face normal direction;
Fig. 1 d is the e2' face position view of six side system gallium nitride, and wherein A is to being positive direction, and B' is to being e2' face normal direction;
Fig. 2 is that aufwuchsplate polarity is along with normal is relative to the variation tendency table of the angle of positive direction;
Fig. 3 is that c looks unfamiliar the structural representation of long lower quantum well layer;
Fig. 4 is that m looks unfamiliar the structural representation of long lower quantum well layer;
Fig. 5 is the structural representation of the product that the method for a kind of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode provided by the invention obtains.
Embodiment
Embodiment 1:
The invention provides a kind of method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, comprise the following steps,
S1, is warming up to 950 DEG C by the gallium nitride monocrystal substrate in nonpolarity <11-20>a face, and under ammonia atmosphere, first grows the bottom 4 of the non-impurity-doped gallium nitride of 0.8um thickness, then mix 5 × 10
18/ cm
3si grow the N-shaped conductive layer 2 of 3um thickness.
S2, on N-shaped conductive layer 2, growth is without the separator 5 of gallium nitride mixed, and the growth temperature of separator 5 is 800 DEG C, and thickness is 30nm, then on separator 5 grown quantum well layer 3; Quantum well layer 3 comprises the well layer of indium gallium nitrogen and the barrier layer of gallium nitride, and well layer thickness is 2.5nm, and barrier layer thickness is 8nm, and logarithm is 9 right, and the growth temperature of quantum well layer 3 is 800 DEG C, and carrier gas is nitrogen.
S3, first grows electronic barrier layer 6 on quantum well layer 3, and electronic barrier layer 6 thickness is 20nm, and mixing element is magnesium, and ginseng magnesium density is 5 × 10
19/ cm
3.On electronic barrier layer 6, grow p-type electric-conducting layer 1 again, thickness is 150nm, and ginseng magnesium density is 5 × 10
19/ cm
3gallium nitride p-type electric-conducting layer 1.
S4, grows contact layer 7 on p-type electric-conducting layer 1, and contact layer 7 thickness is 15nm, and ginseng magnesium density is 5 × 10
20/ cm
3.
Embodiment 2:
A kind of method that the invention provides gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode comprises the following steps,
S1, is warming up to 900 DEG C by the gallium nitride monocrystal substrate of semi-polarity face <20-21>e2, and under ammonia atmosphere, first grows the bottom 4 of the non-impurity-doped gallium nitride of 0.5um thickness, then mix 1 × 10
18/ cm
3si grow the N-shaped conductive layer 2 of 2um thickness.
S2, on N-shaped conductive layer 2, growth is without the separator 5 of gallium nitride mixed, and the growth temperature of separator 5 is 750 DEG C, and thickness is 10nm, then on separator 5 grown quantum well layer 3; Quantum well layer 3 comprises the well layer of indium gallium nitrogen and the barrier layer of gallium nitride, and well layer thickness is 2.0nm, and barrier layer thickness is 6nm, and logarithm is 6 right, and the growth temperature of quantum well layer 3 is 740 DEG C, and carrier gas is the gaseous mixture of nitrogen or nitrogen and a small amount of hydrogen.
S3, first grows electronic barrier layer 6 on quantum well layer 3, and electronic barrier layer 6 thickness is 10nm, and mixing element is magnesium, and ginseng magnesium density is 1 × 10
19/ cm
3.On electronic barrier layer 6, grow p-type electric-conducting layer 1 again, thickness is 100nm, and ginseng magnesium density is 1 × 10
19/ cm
3gallium nitride p-type electric-conducting layer 1.
S4, grows contact layer 7 on p-type electric-conducting layer 1, and contact layer 7 thickness is 10nm, and ginseng magnesium density is 1 × 10
20/ cm
3.
Embodiment 3:
The invention provides a kind of method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, comprise the following steps,
S1, is warming up to 1000 DEG C by the gallium nitride monocrystal substrate in <20-2-1>e2' face, semi-polarity face, and under ammonia atmosphere, first grows the bottom 4 of the non-impurity-doped gallium nitride of 1um thickness, then mix 2 × 10
19/ cm
3si grow the N-shaped conductive layer 2 of 4um thickness.
S2, on N-shaped conductive layer 2, growth is without the separator 5 of gallium nitride mixed, and the growth temperature of separator 5 is 900 DEG C, and thickness is 40nm, then on separator 5 grown quantum well layer 3; Quantum well layer 3 comprises the well layer of indium gallium nitrogen and the barrier layer of gallium nitride, and well layer thickness is 3.5nm, and barrier layer thickness is 12nm, and logarithm is 12 right, and the growth temperature of quantum well layer 3 is 860 DEG C, and carrier gas is the gaseous mixture of nitrogen or nitrogen and a small amount of hydrogen.
S3, first grows electronic barrier layer 6 on quantum well layer 3, and electronic barrier layer 6 thickness is 30nm, and mixing element is magnesium, and ginseng magnesium density is 1 × 10
20/ cm
3.On electronic barrier layer 6, grow p-type electric-conducting layer 1 again, thickness is 200nm, and ginseng magnesium density is 1 × 10
20/ cm
3gallium nitride p-type electric-conducting layer 1.
S4, grows contact layer 7 on p-type electric-conducting layer 1, and contact layer 7 thickness is 10 ~ 20nm, and ginseng magnesium density is 1 × 10
21/ cm
3.
Embodiment 4:
The invention provides a kind of method of gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, comprise the following steps,
S1, is warming up to 960 DEG C by the gallium nitride monocrystal substrate in nonpolarity <10-10>m face, and under ammonia atmosphere, first grows the bottom 4 of the non-impurity-doped gallium nitride of 0.9um thickness, then mix 8 × 10
18/ cm
3si grow the N-shaped conductive layer 2 of 3um thickness.
S2, on N-shaped conductive layer 2, growth is without the separator 5 of gallium nitride mixed, and the growth temperature of separator 5 is 850 DEG C, and thickness is 30nm, then on separator 5 grown quantum well layer 3; Quantum well layer 3 comprises the well layer of indium gallium nitrogen and the barrier layer of gallium nitride, and well layer thickness is 2.5nm, and barrier layer thickness is 8nm, and logarithm is 9 right, and the growth temperature of quantum well layer 3 is 800 DEG C, and carrier gas is nitrogen.
S3, first grows electronic barrier layer 6 on quantum well layer 3, and electronic barrier layer 6 thickness is 20nm, and mixing element is magnesium, and ginseng magnesium density is 5 × 10
19/ cm
3.On electronic barrier layer 6, grow p-type electric-conducting layer 1 again, thickness is 150nm, and ginseng magnesium density is 5 × 10
19/ cm
3gallium nitride p-type electric-conducting layer 1.
S4, grows contact layer 7 on p-type electric-conducting layer 1, and contact layer 7 thickness is 15nm, and ginseng magnesium density is 5 × 10
20/ cm
3.
The above is only optimal way of the present invention; it should be pointed out that to those skilled in the art, without departing from the concept of the premise of the invention; can also make some similar distortion and improvement, these also should be considered as within protection scope of the present invention.
Claims (4)
1. the method for gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode, is characterized in that, comprise the following steps,
S1, is warming up to the growth temperature range of N-shaped conductive layer by the gallium nitride monocrystal substrate of non-polar plane, growing gallium nitride N-shaped conductive layer (2);
S2, in the upper grown quantum well layer (3) of described N-shaped conductive layer (2);
S3, in the upper growing gallium nitride p-type electric-conducting layer (1) of described quantum well layer (3);
First grow the bottom (4) of a undoped gallium nitride before the N-shaped of growing gallium nitride described in S1 conductive layer (2), the thickness of described bottom (4) is 0.5 ~ 1um;
The growth temperature range of the conductive layer of N-shaped described in S1 (2) is 900 ~ 1000 DEG C, and the impurity element of described N-shaped conductive layer (2) is Si, and doping content is 1 × 10
18~ 2 × 10
19/ cm
3, thickness is 2 ~ 4um;
S2 first grows the separator (5) of undoped gallium nitride before being also included in grown quantum well layer (3), the growth temperature of described separator (5) is 750 ~ 900 DEG C, and thickness is 10 ~ 40nm;
Quantum well layer described in S2 (3) comprises the well layer of indium gallium nitrogen and the barrier layer of gallium nitride, described well layer thickness is 2.0 ~ 3.5nm, described barrier layer thickness is 6 ~ 12nm, logarithm is 6 ~ 12 right, the growth temperature of described quantum well layer (3) is 740 ~ 860 DEG C, and carrier gas is the gaseous mixture of nitrogen or nitrogen and hydrogen;
First grow electronic barrier layer (6) before also comprising growth p-type electric-conducting layer (1) in S3, described electronic barrier layer (6) thickness is 10 ~ 30nm, and doped chemical is magnesium, and mixing magnesium density is 1 × 10
19~ 1 × 10
20/ cm
3;
The layer of p-type electric-conducting described in S3 (2), thickness is 100 ~ 200nm, and mixing magnesium density is 1 × 10
19~ 1 × 10
20/ cm
3.
2. the method for gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode according to claim 1, it is characterized in that, non-polar plane described in S1 is nonpolarity <11-20>a face or <10-10>m face.
3. the method for gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode according to claim 1, it is characterized in that, non-polar plane described in S1 is <20-21>e2 face, semi-polarity face.
4. the method for gallium nitride single crystal non-polar plane substrate growth gallium nitride light-emitting diode according to claim 1, it is characterized in that, non-polar plane described in S1 is <20-2-1>e2' face, semi-polarity face.
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| TWI583831B (en) * | 2016-05-31 | 2017-05-21 | 國立中山大學 | Fabrication of m-plane gallium nitride |
| CN108389942A (en) * | 2018-02-07 | 2018-08-10 | 赛富乐斯股份有限公司 | Light-emitting device and its manufacturing method |
| CN110289343B (en) * | 2018-12-03 | 2020-05-29 | 东莞理工学院 | Nonpolar plane gallium nitride substrate epitaxial structure and preparation method and application thereof |
| CN111434809B (en) * | 2019-01-14 | 2022-04-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Non-polar/semi-polar gallium nitride single crystal and growth method thereof by flux method |
| CN110071197A (en) * | 2019-03-27 | 2019-07-30 | 北京大学 | A kind of high polarization degree spin LED and preparation method thereof based on non-polar plane gallium nitride |
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