CN101355122A - Method for preparing gallium nitride substrate - Google Patents
Method for preparing gallium nitride substrate Download PDFInfo
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- CN101355122A CN101355122A CNA2007101391356A CN200710139135A CN101355122A CN 101355122 A CN101355122 A CN 101355122A CN A2007101391356 A CNA2007101391356 A CN A2007101391356A CN 200710139135 A CN200710139135 A CN 200710139135A CN 101355122 A CN101355122 A CN 101355122A
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- gallium nitride
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- stone
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Abstract
A method for preparing a gallium nitride substrate comprises the following: firstly, a step of preparation, during which an epitaxial substrate made from a gallium nitride material through epitaxy is prepared; a step of bump forming, during which, a plurality of bumps which are distributed at intervals and mainly formed by the gallium nitride material are formed upwards on the epitaxial substrate; a step of horizontal epitaxy, during which, a foundation layer is formed on the end part of each bump through horizontal epitaxy; a step of thickening, during which the foundation layer is thickened to no less than 500 mu m so as to form the gallium nitride substrate; and finally, a step of temperature variation, during which, the temperature is cooled down from the temperature range of the thickening step so as to ensure that the gallium nitride substrate and the epitaxial substrate release thermal stress to destroy the piers of the bumps, and then the epitaxial substrate is directly separated from the gallium nitride substrate so as to obtain the gallium nitride substrate, the thickness of which is more than 50 mu m.
Description
Technical field
The present invention relates to a kind of manufacture method of gallium nitride substrate, the high-quality gallium nitride that particularly relates to the not little 500 μ m of a kind of thickness is the manufacture method of substrate.
Background technology
The used gallium nitride substrate of light-emitting diode that is used for the gallium nitride based material of building crystal to grow (gallium nitride-based) at present generally is after utilizing brilliant substrate building crystal to grow of heap of stone, to cooperate laser lift-off (Laser Lift-Off) technology made again.
Consult Fig. 1, the manufacturing process of gallium nitride substrate 10 is to select for example carborundum (SiC) or sapphire (α-Al earlier for use at present
2O
3) etc. the substrate that material constituted that is complementary of lattice constant and gallium nitride based material as brilliant substrate 11 of heap of stone, for example then utilize Metalorganic chemical vapor deposition method (MOCVD) building crystal to grow thickness at the film 12 of the gallium nitride based material of 2～10 μ m, and then thicken to 100 μ m～300 μ m and become this gallium nitride substrate 10 with hydride gas phase accumulation pattern of growth (HVPE) accumulation, at last, utilize high-octane laser action at the interface (as in figure arrow shown in) of brilliant substrate 11 of heap of stone again with gallium nitride substrate 10 bindings, with gallium nitride substrate 10 brilliant substrate 11 sur-face peelings (Lift-Off) certainly of heap of stone, and make gallium nitride substrate 10.
When the little 300 μ m of the thickness of the gallium nitride substrate 10 of required making, the manufacture method of above-mentioned making gallium nitride substrate 10 not only can make suitable gallium nitride substrate 10, simultaneously can also repeat to reclaim the higher of heap of stone brilliant substrate 11 of use cost, and effectively reduce production costs.
Owing to increase the thickness of gallium nitride substrate 10, can reduce the defect concentration of gallium nitride substrate 10, and thicken to 5mm when above when gallium nitride substrate 10, can make defect concentration less than 10
6Cm
-2Therefore, in order to make the gallium nitride substrate 10 than fabricating low-defect-density, the industry tendency is utilized the thicker gallium nitride substrate 10 of preparation earlier at present, cuts into required thickness again.
Along with the thickness of required gallium nitride substrate 10 increases day by day, accumulation thickens gallium nitride film must be greater than more than the 500 μ m, even thicken into 10mm, though go out enough thick gallium nitride substrate 10 and can directly upwards build crystalline substances at present from brilliant substrate 11 of heap of stone, but but can be in the temperature-fall period after brilliant (temperature is about 950 ℃) of heap of stone, because of the thermal expansion variation difference of the two, and the structural strength of brilliant substrate 11 of heap of stone is bigger, and gallium nitride substrate 10 full wafers that make crystalline substance of heap of stone go out are cracked, and more leisure opinion is follow-up to have obtained thick gallium nitride substrate 10 with laser lift-off technique.
In addition, the method also has the lattice defect of brilliant substrate 11 of heap of stone can directly extend upwardly to the gallium nitride substrate 10 that is become, and then the shortcoming of the quality of the light-emitting diode that forms is made in influence with this gallium nitride substrate 10.
So industry need a kind ofly can be made thick and manufacture method brilliant the second best in quality gallium nitride substrate 10 of heap of stone at present, be applied to produce the gallium nitride substrate 10 of light-emitting diode with making.
Summary of the invention
The objective of the invention is is providing a kind of low cost, high process rate, and can obtain the manufacture method of the gallium nitride substrate of high crystalloid amount of heap of stone.The present invention makes the method for gallium nitride substrate, and comprise a preparation process, projection and form step, brilliant step laterally of heap of stone, one and thicken step, and a temperature change steps.
This preparation process is to prepare an of heap of stone brilliant substrate that is used for the gallium nitride based material of building crystal to grow.
It is upwards to form a plurality of projections that scatter and mainly be made of gallium nitride based material at interval that present from this piece brilliant substrate of heap of stone that this projection forms step, and this each projection has one from the pier portion that should brilliant substrate of heap of stone upwards forms, and an end that upwards forms from this pier portion.
Should brilliant step laterally of heap of stone be that end cross building crystal to grow from this a plurality of projections forms one deck and connects this a plurality of projections end and define the basal layer of the gallium nitride based material in a space jointly with this pier portion that builds brilliant substrate, a plurality of projections.
This thickens step is that accumulation thickens this basal layer and forms this gallium nitride substrate to being not less than 500 μ m.
This temperature change steps is to thicken the temperature range cooling that step is implemented from this, make this gallium nitride substrate and brilliant substrate of heap of stone disengage thermal stress and destroy the pier portion of these a plurality of projections, and then this brilliant substrate of heap of stone is separated with this gallium nitride substrate make this gallium nitride substrate.
Beneficial effect of the present invention is: after forming projection on the brilliant substrate of heap of stone, laterally of heap of stonely more brilliantly form and build that brilliant substrate only is connected with the pier portion of projection and thickness, gallium nitride substrate that structural strength is enough, and then can directly utilize the variations in temperature of temperature-fall period and make described pier portion destroyed, and separate brilliant substrate of heap of stone and gallium nitride silicon substrate, directly making thickness is substrate above the high-quality gallium nitride of 500 μ m.
Description of drawings
Fig. 1 is a flow chart, and the existing method of utilizing laser lift-off technique to make gallium nitride substrate is described;
Fig. 2 is a flow chart, illustrates that the present invention makes one first preferred embodiment of the method for gallium nitride substrate;
Fig. 3 is a cross-sectional schematic, in the method for key diagram 2 explanations, forms one deck resilient coating on a brilliant substrate of heap of stone;
Fig. 4 is a cross-sectional schematic, in the method for key diagram 2 explanations, forms the convex body of a plurality of islands on a resilient coating;
Fig. 5 is a cross-sectional schematic, and in the method for key diagram 2 explanations, the barrier layer that forms one deck silicon nitride on a plurality of convex body pieces forms a plurality of projections;
Fig. 6 is a cross-sectional schematic, in the method for key diagram 2 explanations, carries out horizontal building crystal to grow from the projection end and becomes one deck basal layer;
Fig. 7 is a cross-sectional schematic, and in the method for key diagram 2 explanations, accumulation thickens this basal layer and becomes a gallium nitride substrate;
Fig. 8 is a cross-sectional schematic, and in the method for key diagram 2 explanation, projection pier portion is destroyed because of the thermal stress influence of temperature-fall period, separates brilliant substrate of heap of stone and gallium nitride substrate and makes this gallium nitride substrate.
Embodiment
The present invention is described in detail below in conjunction with drawings and Examples:
Consult Fig. 2, the present invention makes one first preferred embodiment of the method for gallium nitride substrate 40, is suitable for to make the gallium nitride based semi-conducting material (Al of thickness greater than 500 μ m
xIn
yGa
1-x-yN, x 〉=0, y 〉=0,1-x-y＞0) gallium nitride substrate 40, be used for the follow-up brilliant light-emitting diode of making of heap of stone.
At first carry out preparation process 21, prepare a sapphire (α-Al who is used for the gallium nitride based semi-conducting material of building crystal to grow
2O
3) the of heap of stone brilliant substrate 41 that constitutes of material.In fact, the constituent material of brilliant substrate 41 of heap of stone also can be carborundum, zinc oxide, aluminium nitride except sapphire, or silicon.
Consult Fig. 3 simultaneously, then carry out projection and form step 22, brilliant substrate 41 of heap of stone is inserted on the carrier (figure does not show) of a bank of reactor, then heat carrier to 600 ℃, then in reactor, feed silane (SiH4, flow is 40sccm) and ammonia (NH3, flow are 40slm), make silane and ammonia via chemical reaction generate on these brilliant substrate of heap of stone 41 surfaces thickness greater than
The resilient coating 42 (buffer layer) of silicon nitride material; Again as shown in Figure 4, feed hydrogen and elevated temperature to 1100 and ℃ carry out The high temperature anneal (annealing); Be cooled to 800 ℃ growth temperature then, feed the trimethyl gallium (Trimethylgallium of flow 50sccm, TMGa (g), the organic metal gas that promptly contains gallium) with the ammonia of 20slm, and feed the silane of flow 0.5sccm simultaneously, and on this resilient coating 42, become to grow the convex body 43 of gallium nitride based material of the island of the independent branch of a plurality of difference; Please cooperate again and consult Fig. 5, in reactor, feed silane (flow is 40sccm) then, and keep the supply of ammonia, make silane and ammonia form on described convex body 43 surfaces layer thicknesses greater than
The barrier layer 44 of silicon nitride material, a plurality ofly have one respectively and form, and a projection 45 of an end 452 that more upwards forms from this pier portion 451 from the pier portion 451 that this resilient coating 42 upwards forms.
It should be noted that at this this step mainly is to use the Metalorganic chemical vapor deposition method to carry out with organic metal gas and the ammonia that contains gallium; When not feeding silane, still can generate described projection 45, but the depth-width ratio of the projection 45 that generates can reduce; In addition, this step also can adopt hydride vapour deposition pattern of growth to carry out, and owing to the detailed process of these building crystal to grow modes is known by industry, and is not emphasis of the present invention place, so no longer add to describe in detail at this.
Consult Fig. 2, Fig. 6, then carry out brilliant step 23 laterally of heap of stone, under about 1000 ℃ temperature, (get final product) greater than 900 ℃, feed the trimethyl gallium of flow 120sccm and the ammonia of 20slm, and the hydrogen of 20slm, carry out horizontal building crystal to grow from above-mentioned projection 45 ends 452 with the direction of arrow as shown in FIG. and should couple together a plurality of projections 45 ends 452, form a layer thickness and about number mm and with pier portion 451 of this brilliant substrate 41 of heap of stone, a plurality of projection 45, define the basal layer 47 in a space 46 jointly.
Consult Fig. 2, Fig. 7, proceed to thicken step 24, the mode of utilizing the hydride vapour deposition to grow up crystalline substance of heap of stone thickens this basal layer 47 to being not less than 500mm, make it have enough structural strengths and become thick, can be actually used in the brilliant gallium nitride substrate 40 of making light-emitting diode of heap of stone.
Consult Fig. 2, Fig. 8, carry out temperature change steps 25 at last, temperature (about 900 ℃～1100 ℃) when implementing to thicken step, to be cooled to normal temperature naturally, and make the of heap of stone brilliant substrate 41 that links by a plurality of projection 45 pier portions 451 disengage thermal stress with gallium nitride substrate 40, and then make these a plurality of projections 45 pier portion 451 by brilliant substrate 41 of heap of stone and gallium nitride substrate 40 each other deformation pull and destroy, separate brilliant substrate 41 of heap of stone and gallium nitride substrate 40, make the gallium nitride substrate 40 that thickness is not less than 500mm.In fact, the speed of temperature-fall period is not limited to nature cooling, and 3 ℃/minute～100 ℃/minute rate of temperature fall all can destroy honest portion 451 and separate and obtain gallium nitride substrate 40.
What need explanation in addition is, form in the step 22 at the present embodiment projection, on brilliant substrate of heap of stone, form one deck resilient coating 42 earlier, and be omissible in the process that the convex body 43 that forms forms one deck barrier layer 44 again, and can not produce great quality influence to produced gallium nitride substrate 40.
As shown in the above description, when making gallium nitride substrate 40 with method of the present invention, owing to only carry out horizontal building crystal to grow,, only be 10 approximately and obtain defect concentration so can effectively reduce from building the direct upwardly extending problem of lattice defect of brilliant substrate 41 or resilient coating 42 from projection 45 ends 452
6～10
8Cm
-2, even lower gallium nitride substrate 40 (with 500 μ m is the thickness benchmark relatively), and then can significantly promote with this gallium nitride substrate 40 of heap of stone brilliant when making light-emitting diode, the quality of the light-emitting diode that makes.
The more important thing is, the present invention not only can be by carrying out horizontal building crystal to grow from projection 45 ends 452, and then crystalline substance of heap of stone goes out the gallium nitride substrate 40 that thickness is not less than 500 μ m (meaning that also structural strength is enough simultaneously when thickness is enough thick) and high-quality (defect concentration is low), more can be by linking of heap of stone brilliant substrate 41 that crystalline substance of heap of stone finishes projection 45 pier portions 451 with gallium nitride substrate 40, the thermal stress that absorption disengages from brilliant substrate 41 of heap of stone in the temperature-fall period and gallium nitride substrate 40 and destroyed, and keeping under the complete situation of brilliant substrate 41 of heap of stone and gallium nitride substrate 40, directly separate brilliant substrate 41 of heap of stone and gallium nitride substrate 40, make complete gallium nitride substrate 40, solve present industry and can't build the brilliant puzzlement that thickness is not less than the gallium nitride substrate 11 of 500 μ m of making.
The present invention makes one second preferred embodiment of the method for gallium nitride substrate 40, is similar to last example, and it does not exist together and only is that this projection forms the process that applies of step 22, below only does detailed explanation at this process.
It is in reactor under the growth temperature and ammonia flow 20slm with 600 ℃ (500 ℃～700 ℃ all can) that in the present embodiment projection forms step, in brilliant substrate surface cover type ground growth one deck of heap of stone constituted by gallium nitride based semi-conducting material and thickness greater than
Transition layer, then elevated temperature to 950 ℃ (900 ℃～1100 ℃ all can), and control ammonia flow is at 6slm, and makes the transition layer that grows up to because the atmosphere transformation changes kenel with temperature change, is transformed into the island convex body of a plurality of intervals distribution from stratiform; Then in reactor, feed silane (flow is 40sccm), keep the supply of ammonia simultaneously, and on described convex body, form a layer thickness greater than
And coat the barrier layer of the silicon nitride of described convex body, and form a plurality of projections that have pier portion and the end that upwards forms from pier portion respectively.
Similarly, in the projection formation step of present embodiment, also can behind the resilient coating that forms one deck silicon nitride on the brilliant substrate of heap of stone earlier, form one deck island projection again; The step that forms barrier layer also can be omitted, so as to simplifying processing procedure, reducing production costs.
In addition, brilliant step laterally of heap of stone also can adopt the mode of hydride vapor deposition to carry out, and with after the step that thickens form continuous processing procedure, with the complexity of reduction implementation process.
Conclude above-mentioned, the present invention makes the method for gallium nitride substrate 40, it mainly is the projection 45 that on brilliant substrate 41 of heap of stone, forms a plurality of islands, utilize the mode of horizontal building crystal to grow again, the enough thick gallium nitride substrate 40 that formation utilizes projection 45 pier portions 451 and brilliant substrate 41 of heap of stone to link, reduce the direct upwardly extending probability of lattice defect whereby, and can significantly reduce the defect concentration of the gallium nitride substrate 40 that is become, and then can promote the element quality of the light-emitting diode made from this gallium nitride substrate 40.Simultaneously, it is destroyed with a plurality of projections 45 pier portions, 451 the two thermal stress deformation that disengage of absorption of the gallium nitride substrate 40 of moulding to link brilliant substrate 41 of heap of stone by these, and can ensure the complete of gallium nitride substrate 40, and can separate brilliant substrate 41 of heap of stone and gallium nitride substrate 40 naturally because pier portion 451 is destroyed at the temperature-fall period after crystalline substance of heap of stone is finished, obtain complete gallium nitride substrate 40, really improve of heap of stone at present brilliant when making the bigger gallium nitride substrate 10 of thickness, because the ability that 11 pairs of thermal stress of gallium nitride film 12 that crystalline substance of heap of stone forms and brilliant substrate of heap of stone discharge is different, and cause whole layer gallium nitride film 12 cracked, can't make the problem of gallium nitride substrate 10 at all, reach creation purpose of the present invention really.
Claims (11)
1. method of making gallium nitride substrate; It is characterized in that, comprise:
A preparation process is prepared an of heap of stone brilliant substrate that is used for the gallium nitride based material of building crystal to grow,
Projection forms step, and this piece brilliant substrate of heap of stone upwards forms a plurality of projections that scatter and mainly be made of gallium nitride based material at interval that present certainly, and this each projection has one from the pier portion that should brilliant substrate of heap of stone upwards forms, and an end that upwards forms from this pier portion,
A brilliant step laterally of heap of stone, the end cross building crystal to grow of these a plurality of projections formation one deck connects this a plurality of projections end and defines the basal layer of the gallium nitride based material in a space jointly with this pier portion that builds brilliant substrate, a plurality of projections certainly,
One thickens step, and accumulation thickens this basal layer and forms this gallium nitride substrate to being not less than 500 microns, and
A temperature change steps, thicken the temperature range cooling that step is implemented from this, make this gallium nitride substrate and brilliant substrate of heap of stone disengage thermal stress and destroy the pier portion of these a plurality of projections, and then this brilliant substrate of heap of stone is separated with this gallium nitride substrate make this gallium nitride substrate.
2. the method for making gallium nitride substrate as claimed in claim 1 is characterized in that: this temperature change steps is to be cooled to normal temperature with 3 ℃/minute～100 ℃/minute rate of temperature fall.
3. the method for making gallium nitride substrate as claimed in claim 2 is characterized in that: this projection form step be earlier this brilliant substrate surface of heap of stone form a layer thickness greater than
The resilient coating of silicon nitride material, upwards form a plurality of convex bodys that present the gallium nitride based material that scatters at interval in this buffer-layer surface again, and then form in this a plurality of convex bodys surface a layer thickness greater than
The barrier layer of silicon nitride material, and make the barrier layer of this convex body and formation constitute this projection.
4. the method for making gallium nitride substrate as claimed in claim 3, it is characterized in that: these a plurality of convex bodys are to form with ammonia and the organic metal gas that contains gallium with the Metalorganic chemical vapor deposition method, and this resilient coating is with silane and ammonia gas react generation with this barrier layer.
5. the method for making gallium nitride substrate as claimed in claim 4 is characterized in that: the material of this brilliant substrate of heap of stone is to be selected from sapphire, carborundum, zinc oxide, aluminium nitride, or silicon, and the chemical formula of this gallium nitride based material is Al
xIn
yGa
1-x-yN, x 〉=0, y 〉=0,1-x-y＞0.
6. the method for making gallium nitride substrate as claimed in claim 5, it is characterized in that: this brilliant step laterally of heap of stone is under greater than 900 ℃ temperature, with ammonia and the organic metal gas that contains gallium by the end cross of these a plurality of projections brilliant this basal layer that forms of heap of stone, and this to thicken step be to accumulate pattern of growth with the hydride gas phase to carry out.
7. the method for making gallium nitride substrate as claimed in claim 5 is characterized in that: it all is to carry out with hydride gas phase accumulation pattern of growth that this brilliant step laterally of heap of stone and this thicken step.
8. the method for making gallium nitride substrate as claimed in claim 2 is characterized in that: this projection form step be earlier 500 ℃～700 ℃ and predetermined ammonia branch depress generate a layer thickness greater than
The transition layer of gallium nitride based material, then elevated temperature to 900 ℃～1100 ℃, and the dividing potential drop of control ammonia is lower than the ammonia dividing potential drop when generating this transition layer, and make this transition layer change into a plurality of convex bodys that present the gallium nitride based material that scatters at interval, and then in this a plurality of convex bodys surface with silane and ammonia gas react generate a layer thickness greater than
The barrier layer of silicon nitride material, and make the barrier layer of this convex body and formation constitute this projection.
9. the method for making gallium nitride substrate as claimed in claim 8 is characterized in that: the material of this brilliant substrate of heap of stone is to be selected from sapphire, carborundum, zinc oxide, aluminium nitride, or silicon, and the chemical formula of this gallium nitride based material is Al
xIn
yGa
1-x-yN, x 〉=0, y 〉=0,1-x-y＞0.
10. the method for making gallium nitride substrate as claimed in claim 9, it is characterized in that: this brilliant step laterally of heap of stone is under greater than 900 ℃ temperature, with ammonia and the organic metal gas that contains gallium by the end cross of these a plurality of projections brilliant this basal layer that forms of heap of stone, and this to thicken step be to accumulate pattern of growth with the hydride gas phase to carry out.
11. the method for making gallium nitride substrate as claimed in claim 9 is characterized in that: it all is to carry out with hydride gas phase accumulation pattern of growth that this brilliant step laterally of heap of stone and this thicken step.
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|---|---|---|---|
| CNA2007101391356A CN101355122A (en) | 2007-07-26 | 2007-07-26 | Method for preparing gallium nitride substrate |
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|---|---|---|---|
| CNA2007101391356A CN101355122A (en) | 2007-07-26 | 2007-07-26 | Method for preparing gallium nitride substrate |
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ID=40307807
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315347A (en) * | 2010-07-05 | 2012-01-11 | 展晶科技(深圳)有限公司 | Light emitting diode epitaxial structure and manufacture method thereof |
| WO2017113844A1 (en) * | 2015-12-30 | 2017-07-06 | 大族激光科技产业集团股份有限公司 | Laser separation method for wafer |
-
2007
- 2007-07-26 CN CNA2007101391356A patent/CN101355122A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102315347A (en) * | 2010-07-05 | 2012-01-11 | 展晶科技(深圳)有限公司 | Light emitting diode epitaxial structure and manufacture method thereof |
| US8501582B2 (en) | 2010-07-05 | 2013-08-06 | Advanced Optoelectronic Technology, Inc. | Semiconductor structure having low thermal stress and method for manufacturing thereof |
| WO2017113844A1 (en) * | 2015-12-30 | 2017-07-06 | 大族激光科技产业集团股份有限公司 | Laser separation method for wafer |
| TWI646592B (en) * | 2015-12-30 | 2019-01-01 | 大陸商大族激光科技產業集團股份有限公司 | Wafer laser stripping method |
| US10515854B2 (en) | 2015-12-30 | 2019-12-24 | Han's Laser Technology Industry Group Co., Ltd. | Laser lift-off method of wafer |
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Open date: 20090128 |