CN105514224B - A kind of preparation method of the low-stress state compound substrate for GaN growth - Google Patents
A kind of preparation method of the low-stress state compound substrate for GaN growth Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of low-stress state compound substrate for GaN growth.GaN single crystal epitaxial layer is first prepared on a sapphire substrate；And substrate back deposition stress compensation layer is shifted in dystectic thermal conductivity；Then dystectic bonding medium layer is prepared respectively in GaN epitaxy film and transfer substrate surface；Use High temperature diffusion bonding techniques by GaN epitaxy piece together with the thermal conductivity substrate bonding later；Finally Sapphire Substrate is removed with substrate desquamation technology；It then obtains can be used for stablizing at a high temperature of GaN growth and the compound substrate of low-stress state.Compound substrate prepared by the present invention, both the advantages of having taken into account homoepitaxy that the compound substrate that previous transfer is realized has and can directly having prepared vertical structure device, there is low-stress state and high-temperature stability again, the quality of subsequent GaN epitaxy growth and chip preparation can be effectively improved.
Description
Technical field
The present invention relates to semiconductor photoelectronic device technical fields, in particular to use High temperature diffusion bonding technology by GaN
Epitaxial film is transferred on thermal conductivity substrate, and stress compensation layer is combined to realize that the low-stress state for GaN homoepitaxy is led
The preparation method of thermal conducting compound substrate.
Background technique
Broad stopband GaN base semiconductor material have excellent photoelectric characteristic, be widely used in make light emitting diode,
Laser, ultraviolet detector and high temperature, high frequency, high power electronic device, and can apply to high-end micro- needed for preparation aerospace
Electronic device has become international photoelectron neck such as high mobility transistor (HEMT) and heterojunction transistor (HFET)
The research hotspot in domain.
Since preparing for GaN body monocrystalline is extremely difficult, large size single crystal GaN is difficult to directly obtain, and expensive, GaN
The epitaxial growth of material system is mainly based upon the heterogeneous epitaxial technology of big mismatch.Currently, industry the most commonly used is stability compared with
Two-step growth method extension GaN material is used in the Sapphire Substrate of good relative low price, it is this heterogeneous outer based on buffer layer
Prolong technology and achieve huge success, wherein blue and green light LED has been carried out commercialization, but process for sapphire-based GaN compound substrate
Shown biggish limitation, problem is mainly reflected in: (1) sapphire is insulating materials, and related device is caused to cannot achieve
Vertical structure can only use ipsilateral step electrode structure, and electric current is lateral injection, cause the current unevenness for flowing through active layer even,
Cause electric current to cluster round effect, reduce stock utilization, while increasing lithography and etching technique in device preparation, dramatically increases
Cost；(2) sapphire heating conduction is bad, and at 1000 DEG C, thermal conductivity is about 0.25W/cmK, and heat dissipation problem is prominent, influences
The electricity of GaN base device, optical characteristics and long-range functional reliability, and limit its answering on high temperature and high power device
With；(3) sapphire hardness is higher, and there are one 30 ° of angles between sapphire crystal lattice and GaN lattice, so being not easy cleavage, no
The Cavity surface of GaN base device can be obtained by the method for cleavage.
Silicon substrate have thermal conductivity is excellent, cost is relatively low, it is easy to accomplish large scale and it is integrated the advantages that, become close
One of the important subject of several years GaN base LED fields, however the lattice mismatch and thermal mismatching between silicon and GaN are serious, at present silicon
The technology also prematurity of GaN epitaxial layer is grown on substrate, compound substrate Dislocations density is higher, or even occurs being cracked and crackle.
Silicon carbide is the ideal substrate of extension GaN, its lattice mismatch and thermal mismatching between GaN is smaller, and has good thermally conductive lead
Electrical property can greatly simplify manufacture craft, but silicon carbide substrates is expensive, and there are adhesivenesses etc. between epitaxial layer and substrate
Problem should not carry out industrialized production.
With going deep into for research, there is a growing awareness that homoepitaxy is to obtain the optimal selection of high-performance GaN substrate.
In view of the high price of GaN single crystal substrate, some research institution begins to focus on medium bonding and mutually ties with laser lift-off
GaN epitaxy single crystalline layer is transferred on the substrate of the high conductivity of high heat conductance by the technology of conjunction, to eliminate the unfavorable of Sapphire Substrate
It influences.Patent (number of patent application are as follows: 201210068033.0 and number of patent application are as follows: 201210068026.0) to based on low temperature
The compound substrate and preparation method thereof of bonding and laser lift-off technique preparation for GaN growth is described, but uses before this
Medium bonding and laser lift-off prepare thermal conductivity GaN compound substrate, and there are the following problems: (1) previous main using 600
DEG C or less lower temperature bonding, high-temperature stability is poor, has formed when epitaxial growth GaN under subsequent 1000 DEG C or more high temperature
Bonding structure can change again again, seriously affect later period homoepitaxy and chip preparation quality；(2) substrate shifts work
Larger stress is generated in the substrate of the variation of skill and thermal conductivity substrate after the transfer, causes compound substrate that certain warpage occurs,
Wrinkle even are formed on GaN epitaxy film, it is difficult to realize high-performance GaN single crystal extension and chip preparation.Poor high-temperature stable
Property and serious stress remnants be to restrict the main original further applied in high-performance GaN compound substrate of substrate transfer technology
Cause.
Summary of the invention
The object of the present invention is to provide a kind of for the low-stress state compound substrate of GaN growth and its preparation side
GaN epitaxy film is transferred on thermal conductivity substrate by method using High temperature diffusion bonding and substrate desquamation technique from Sapphire Substrate,
And stress compensation layer is prepared in thermal conductivity transfer substrate back, to offset most of stress in transfer process in substrate, institute
Obtained compound substrate is suitable for homoepitaxy and prepares vertical structure LED device, is provided simultaneously with low-stress state and high temperature is steady
It is qualitative, the quality of subsequent GaN epitaxy and chip preparation can be effectively improved, there is biggish development prospect.
A kind of preparation method of the low-stress state compound substrate for GaN growth of the present invention, including thermal conductivity substrate,
High-melting-point thermal conductivity bonding medium layer, GaN single crystal epitaxial layer on the substrate and on thermal conductivity substrate back
The preparation method of stress compensation layer.
As shown in Figure 1, a kind of low-stress state compound substrate for GaN growth proposed by the present invention, including (from it is lower to
On be arranged successively) stress compensation layer, thermal conductivity substrate, thermal conductivity bonding medium layer disposed thereon and GaN single crystal extension
Layer.
Above-mentioned thermal conductivity bonding medium layer with a thickness of 10 nanometers to 100 microns；Thermal conductivity substrate with a thickness of 10
Micron is to 3000 microns；Stress compensation layer with a thickness of 0.1 micron to 300 microns.
Above-mentioned bonding medium layer, thermal conductivity substrate and stress compensation layer are required to have following feature: 1) resistance to height
Temperature, fusing point are more than 1000 DEG C, and without violent diffusion phenomena；(2) there is thermal conductivity.
The GaN epitaxy that above-mentioned stress compensation layer must come in the stress that thermal conductivity substrate back generates with transfer
On the contrary, the stress compensation layer material, fusing point is higher than 1000 DEG C and has good heat conductive electric conductivity stress caused by layer,
It can be GaN, SiNxEqual nitride materials or molybdenum (Mo), titanium (Ti), palladium (Pd), gold (Au), copper (Cu), tungsten (W), nickel
(Ni), one of chromium (Cr) elemental metals or several alloys.
By requirements above, the thermal conductivity bonding medium layer material, fusing point is higher than 1000 DEG C and has good heat conductive conductive
Performance can be one of molybdenum (Mo), titanium (Ti), palladium (Pd), golden (Au), copper (Cu), tungsten (W), nickel (Ni), chromium (Cr) simple substance
Metal or several alloys or resin matrix and conducting particles silver-colored (Ag), golden (Au), copper (Cu), aluminium (Al), zinc (Zn),
The conducting polymer or one of the above or a variety of conductions of one of iron (Fe), nickel (Ni), graphite (C) or a variety of compositions
The particle of particle and electrocondution slurry or silicate-base high-temperature electric conduction glue (HSQ) composed by adhesive, solvent, auxiliary agent,
The either high temperature alloy slurry of the metals such as nickel (Ni), chromium (Cr), silicon (Si), boron (B) formation.
By requirements above, which shifts substrate material, and fusing point is higher than 1000 DEG C and has good heat conductive electric conductivity
Can, it can be one of molybdenum (Mo), titanium (Ti), palladium (Pd), copper (Cu), tungsten (W), nickel (Ni), chromium (Cr) elemental metals or several
The alloy or silicon (Si) crystal, silicon carbide (SiC) crystal or AlSi crystal of kind.
Above-mentioned stress compensation layer and thermal conductivity bonding medium layer, may each be single or multi-layer structure.
GaN epitaxial layer used in above-mentioned substrate transfer process with a thickness of 1 micron to 100 microns, and GaN is with monocrystalline
Form exists.
A kind of preparation method of above-mentioned low-stress state compound substrate for GaN growth, includes the following steps:
A) GaN single crystal epitaxial layer is prepared on a sapphire substrate；
B) in the backside deposition stress compensation layer of thermal conductivity transfer substrate；
C) thermal conductivity bonding medium layer is prepared on the surface of GaN epitaxy film and high heat-conductivity conducting transfer substrate respectively；
D) High temperature diffusion bonding technology is used, the GaN epitaxial layer in Sapphire Substrate is passed through into key with thermal conductivity substrate
Dielectric layer is closed to link together；
E) then Sapphire Substrate is removed using substrate desquamation technology, obtains the low-stress state that can be used for GaN growth
And the compound substrate of high-temperature stable.Preparation flow is as shown in Figure 2.
It is prepared in GaN single crystal epitaxial layer in above-mentioned steps a) Sapphire Substrate, if directly extension is raw on a sapphire substrate
MOCVD method or HVPE method well-known to those skilled in the art or MOCVD can be used in long GaN single crystal layer, the extension of GaN
The technology combined with HVPE method；It, will using epoxies binder if the process for sapphire-based GaN substrate shifted using gluing
GaN epitaxial layer is transferred in Sapphire Substrate from epitaxial substrate, and sapphire is as temporary support at this time；If being served as a contrast in sapphire
The sacrificial release layers such as bottom and GaN epitaxy Intercalation reaction ZnO then first can prepare sacrificial release layers using technologies such as magnetron sputterings, then
The extension of GaN is carried out using the technology that MOCVD method or HVPE method or MOCVD and HVPE method combine.
In above-mentioned steps b), stress compensation layer may be selected to use magnetron sputtering, molecular beam epitaxy, plasma enhancing
Learn vapor deposition, Metallo-Organic Chemical Vapor deposition either vacuum thermal evaporation technology, the single-layer or multi-layer membrane structure of preparation.
In step c), on the surface of both GaN epitaxy film or thermal conductivity substrate, magnetron sputtering or vacuum thermal evaporation are utilized
Or wet processing prepares single-layer or multi-layer membrane structure as bonding medium layer, can also only turn in GaN epitaxy film, thermal conductivity
It moves in substrate and selects one kind and deposit bonding medium layer on its surface, then carry out step d).
In above-mentioned steps d), bonding uses High temperature diffusion bonding method.In temperature >=900 DEG C, 100 Kgfs of pressure/flat
Under conditions of square inch to 4 tons/square inch, by the abundant diffusion of bonding medium layer, GaN epitaxy film and thermal conductivity are served as a contrast
The front at bottom is bonded together.
In above-mentioned steps e), if using the GaN single crystal layer of direct extension on a sapphire substrate in step a), at this time
Sapphire Substrate is removed using laser lift-off technique；If the process for sapphire-based GaN substrate shifted in step a) using gluing,
Epoxy adhesive is carbonized during bonding heating, and Sapphire Substrate can be from GaN epitaxy film surface Automatic-falling；If in step a)
Middle elder generation is prepared for the sacrificial release layers such as ZnO, then extension GaN single crystal layer on a sapphire substrate, then step e) uses chemical stripping
Technology removes Sapphire Substrate.
A kind of preparation method of the low-stress state compound substrate for GaN growth of the present invention, including province's destressing
The preparation method of the smaller stress state compound substrate of compensation layer structure, for example, weighing performance and cost and saving stress compensation
Layer preparation process only uses High temperature diffusion bonding techniques and realizes for stablizing at a high temperature of GaN growth and answering compared with low residual stress
The preparation method of substrate (as shown in Figure 3) is closed, also when the range for belonging to this patent and including.
Compound substrate described in preparation method of the present invention, both having had can be used for GaN homoepitaxy and prepares vertical structure LED
The advantage of chip, and the characteristics of High temperature diffusion is bonded with the high-temperature stable of stress compensation technology, low-stress state is combined, therefore
Have many unique advantages:
(1) compound substrate described in preparation method of the present invention, with one layer of GaN, it can be achieved that the homoepitaxy of GaN, is improved outer
Prolong growth quality, and its thermal conductivity is preferable, can be directly used for preparing vertical structure LED device.To efficiently solve
Process for sapphire-based GaN substrate thermal conductivity is poor, can not prepare vertical structure LED, stock utilization is low, hetero-epitaxy matter
Measure the complex process of epitaxial growth in poor and Si substrate and SiC substrate, it is with high costs the problems such as.
(2) realize that GaN epitaxy film is connect with thermal conductivity substrate using High temperature diffusion bonding techniques, in its heating and cooling process
Middle bonding medium layer and diffusion and the phase transformation of shifting substrate etc. are completed entirely, under the hot conditions of subsequent epitaxial, bonding medium
Layer and transfer substrate will not generate variation (e.g., phase transformation, chemical reaction, physical diffusion, peeling etc.) again, i.e., diffusion interlinked technology obtains
The compound substrate obtained has very excellent high-temperature stability, so as to significantly improve the quality of GaN homoepitaxy.
(3) High temperature diffusion bonding techniques are used, the range of choice of alternative bonding medium layer material is had greatly expanded,
The refractory metal or high-temperature alloy material that some chemical activities are smaller, adhesiveness is poor can be used as dielectric layer, very small
Bonding pressure can obtain high-intensitive stable connection, therefore, be highly suitable for realizing that GaN turns to the brittleness substrate such as Si very much
It moves.
(4) required pressure is very small when High temperature diffusion is bonded, therefore the longitudinal stress applied is substantially reduced, and passes through tune
Temperature-fall period after control key closes can play the role of stress relieving by annealing, so the residual stress in substrate can be effectively reduced.
(5) introducing of stress compensation layer can then offset the major part in the GaN epitaxy film being transferred on thermal conductivity substrate
Stress makes compound substrate be in lower stress state, inhibits the formation of substrate warpage and epitaxial film wrinkle, crackle, obtains high
The GaN compound substrate of performance, it is very useful to the improvement of subsequent epitaxial quality.
(6) High temperature diffusion bonding and stress compensation technology are combined, high-temperature stable is finally obtained and is in low-stress state
GaN compound substrate can be good at the homoepitaxy and chip preparing process that adapt to subsequent GaN at high temperature.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of low-stress state compound substrate for GaN growth.
Fig. 2 is a kind of preparation method schematic diagram of the low-stress state compound substrate for GaN growth of the present invention.
Fig. 3 is a kind of structural representation of smaller stress state compound substrate for GaN growth without stress compensation layer
Figure.
Fig. 4, which is embodiment 1., to be made thermal conductivity substrate using CuMo, is mended using Ni and conduction Ag paste as stress
It repays layer and bonding medium layer obtains the preparation flow figure of the low-stress state compound substrate for GaN growth.Wherein, (a) be
The schematic diagram of deposition stress compensation layer on CuMo thermal conductivity substrate；It (b) is made using spin coating proceeding preparation conduction Ag paste
For the schematic diagram of bonding medium layer；It (c) is to be bonded showing for GaN epitaxial layer and thermal conductivity substrate using High temperature diffusion bonding method
It is intended to；It (d) is the schematic diagram that Sapphire Substrate is removed using laser lift-off technique；It (e) is that being made with CuMo of finally obtaining is thermally conductive
Conductive substrates are illustrated using Ni and conduction Ag paste respectively as the composite substrate structure of stress compensation layer and bonding medium layer
Figure.
Fig. 5, which is embodiment 2., makees thermal conductivity substrate using Si, using Au/Pd and Ti/Pd as stress compensation layer and
Bonding medium layer obtains the preparation flow figure of the low-stress state compound substrate for GaN growth.Wherein, (a) uses UV anaerobism
GaN epitaxial layer is transferred to the schematic diagram of sapphire temporary substrates by glue；It (b) is to make to deposit Au/Pd on thermal conductivity substrate in Si
The schematic diagram of double-layer structure stress compensation layer；It (c) is that magnetron sputtering is used to prepare Ti/Pd as the schematic diagram of bonding medium layer；
It (d) is after being bonded GaN epitaxial layer and thermal conductivity substrate using High temperature diffusion bonding method, to peel sapphire signal off
Figure；(e) be finally obtain thermal conductivity substrate is made using Si substrate, using Au/Pd and Ti/Pd as stress compensation layer and
The composite substrate structure schematic diagram of bonding medium layer.
Fig. 6 is that embodiment 3. with AlSi makees thermal conductivity substrate, using SiNxWith Au respectively as stress compensation layer and key
It closes dielectric layer and obtains the preparation flow figure of the low-stress state compound substrate for GaN growth.
Fig. 7, which is embodiment 4., makees thermal conductivity substrate using CuW, using GaN and Pd as stress compensation layer and bonding
Dielectric layer, the preparation flow figure that low-stress state compound substrate for GaN growth is obtained using ZnO as sacrificial release layers.
Fig. 8 is the preparation section that example 5. saves stress compensation layer, makees thermal conductivity substrate with W, high temperature alloy slurry is made
The preparation flow figure of the smaller compound substrate of high-temperature stable and residual stress for GaN growth is obtained for diffusion interlinked dielectric layer.
Wherein, (a) is that spin coating proceeding is used to prepare high temperature alloy slurry as the schematic diagram of bonding medium layer；It (b) is expanded using high temperature
Dissipate the schematic diagram of bonding method bonding GaN epitaxial layer and thermal conductivity substrate；It (c) is to remove sapphire using laser lift-off technique
The schematic diagram of substrate；(d) be finally obtain without stress compensation layer W substrate high temperature alloy slurry bonding composite lining bear building-up
Structure schematic diagram.
Specific embodiment
Below with reference to attached drawing of the invention, a kind of system of low-stress state compound substrate for GaN growth is described in detail
Preparation Method.First it should be noted that those skilled in the art's basic thought according to the present invention, various modifications may be made or changes
Into as long as they do not deviate from the basic of the present invention, being all within the scope of the present invention.
Embodiment 1: it uses Ni as stress compensation layer, conduction Ag paste bonding CuMo metal substrate and GaN epitaxial layer, obtains
To the preparation method of the low-stress state compound substrate for GaN growth:
(1) epitaxial growth GaN single crystal layer on a sapphire substrate: in 2 inches 430 microns thick of plate Sapphire Substrate
On, GaN single crystal layer first thick using 4 microns of MOCVD technology epitaxial growth, then growth thickeies its thickness of GaN layer extremely in HVPE
15 microns.
(2) in 300 microns of thickness CuMo metal substrates (wherein the mass percent of Mo and Cu is respectively 20% to 80%)
The Ni thin layer that the back side is 500 nanometers using magnetron sputtering deposition thickness, as stress compensation layer, as shown in Fig. 4 (a).
(3) face GaN in above-mentioned process for sapphire-based GaN compound substrate and 300 microns thick of CuMo substrate face, revolve respectively
The conductive Ag paste for turning 10 microns of coating layer, as bonding medium layer, as shown in Fig. 4 (b), then in temperature 1100
DEG C, pressure is the High temperature diffusion bonding carried out under 1.5T 30 minutes, and realization GaN epitaxial layer is bonded with CuMo metal substrate, such as
Shown in Fig. 4 (c).
(4) laser lift-off technique is used, Sapphire Substrate is removed, hydrochloric acid, third are carried out to metal composite substrate obtained
The surface cleans technique such as ketone obtains conductive Ag paste bonding, device architecture as at a high temperature of GaN/Ag Paste/CuMo/Ni
Stablize the low-stress state compound substrate for being suitable for GaN isoepitaxial growth, as shown in Fig. 4 (d) and 4 (e).
Embodiment 2: Au/Pd is used to obtain as the GaN epitaxial layer of stress compensation layer, Ti/Pd bonding Si substrate and gluing transfer
To the preparation method of the outward-facing low-stress state compound substrate for GaN growth of gallium polarity:
(1) the process for sapphire-based GaN compound substrate of preparation gluing transfer: in 2 inches 430 microns thick of plate Sapphire Substrate
On, GaN single crystal layer first thick using 4 microns of MOCVD technology epitaxial growth, then growth thickeies GaN layer thickness extremely in HVPE
15 microns, then the GaN epitaxy film is adhered on 2 inches 430 microns thick sapphire temporary substrates using UV anaerobic adhesive, new
Sapphire Substrate is later removed former extension Sapphire Substrate to get arriving using laser lift-off technique as transfer support substrate
The GaN single crystal layer being bonded in new Sapphire Substrate, as shown in Fig. 5 a).
(2) at the back side of 300 microns of thickness Si substrates, 3 microns of Au layer and 10 microns of Pd layer are prepared using magnetron sputtering,
As stress compensation layer.
(3) face GaN of the GaN single crystal in bonding on a sapphire substrate and Si substrate face use magnetron sputtering respectively
The Ti layer and 500 nanometers of Pd layer of 50 nanometers of preparation, as thermal conductivity bonding medium layer, then at 1000 DEG C of temperature, pressure
For the High temperature diffusion bonding under 2.5T, carrying out 20 minutes, realization GaN epitaxial layer is bonded with Si substrate.
(4) in bonding process, UV anaerobic adhesive is carbonized at high temperature, and Sapphire Substrate takes off automatically from GaN epitaxy film surface
It falls, the surface cleans techniques such as hydrochloric acid, acetone is carried out to compound substrate obtained, due to have passed through gluing before and after GaN epitaxial layer
It is overturn twice with Ti/Pd metal medium, therefore finally obtained is Ti/Pd bonding, device architecture GaN/Ti/Pd/Pd/Ti/
The gallium polarity of Si/Au/Pd faces outwardly, high temperatures are suitable for the low-stress state compound substrate of GaN isoepitaxial growth, tool
Preparation is as shown in Figure 5.
Embodiment 3: SiN is usedxIt is used for as stress compensation layer, AuAu bonding AlSi metal substrate and GaN epitaxial layer
The preparation method of the low-stress state compound substrate of GaN growth, specific process step are following (as shown in Figure 6):
(1) epitaxial growth GaN single crystal layer on a sapphire substrate: in 2 inches 430 microns thick of plate Sapphire Substrate
On, GaN single crystal layer first thick using 4 microns of MOCVD technology epitaxial growth, then growth thickeies GaN layer thickness to 15 in HVPE
Micron.
(2) in 150 microns of thickness AlSi metal substrates, (group that wherein, the group of Al is divided into 30%, Si is divided into the back side 70%)
The SiN with a thickness of 5 microns is prepared using plasma enhanced chemical vapor depositionxThin layer, as stress compensation layer.
(3) in the face GaN of above-mentioned process for sapphire-based GaN compound substrate, the Au for preparing 1 micron thick using magnetron sputtering is conductive
Bonding medium layer, then at 950 DEG C of temperature, pressure is the High temperature diffusion bonding carried out under 2T 20 minutes, realizes GaN epitaxial layer
With being bonded for AlSi metal substrate.
(4) laser lift-off technique is used, Sapphire Substrate is removed, hydrochloric acid, third are carried out to metal composite substrate obtained
The surface cleans technique such as ketone obtains AuAu bonding, device architecture GaN/Au/AlSi/SiNxAt a high temperature of stablize be suitable for GaN
The low-stress state compound substrate of isoepitaxial growth.
Embodiment 4: it uses GaN as stress compensation layer, Pd bonding CuW substrate and GaN epitaxial layer, obtains for GaN growth
Low-stress state compound substrate preparation method (as shown in Figure 7):
(1) process for sapphire-based GaN compound substrate of the ZnO as sacrificial release layers is prepared: in 2 inches of 430 microns of thick plates
In Sapphire Substrate, ZnO sacrificial release layers first are deposited using magnetron sputtering technique, then 4 microns of epitaxial growth thick in MOCVD
GaN single crystal layer, then growth thickeies GaN layer thickness to 15 microns in HVPE.
(2) it is mended using 15 microns of GaN layer of HVPE technology extension as stress at the back side of 200 microns of thickness CuW substrates
Repay layer.
(3) in the front of CuW substrate, 1000 nanometers of Pd layer is prepared using magnetron sputtering, is bonded and is situated between as thermal conductivity
Matter layer, then at 1200 DEG C of temperature, pressure is the High temperature diffusion bonding carried out under 3.5T 20 minutes, realize GaN epitaxial layer with
The bonding of CuW substrate.
(4) chemical stripping technology is used, i.e., corrodes ZnO sacrificial release layers using chemical reagent, to remove sapphire lining
Bottom carries out the surface cleans techniques such as hydrochloric acid, acetone to compound substrate obtained, obtains PdPd bonding, device architecture GaN/
Stablize the low-stress state compound substrate for being suitable for GaN isoepitaxial growth at a high temperature of Pd/CuW/GaN.
Embodiment 5:[tradeoff performance and cost and for it] save stress compensation layer preparation section, only use high temperature alloy slurry
Expect (NiCrSiB) High temperature diffusion bonding W metal substrate and GaN epitaxial layer, obtains unstressed compensation layer and residual stress is lesser
The preparation method of compound substrate:
(1) epitaxial growth GaN single crystal layer in Sapphire Substrate: in 2 inches 430 microns thick of plate Sapphire Substrate,
First using the thick GaN single crystal layer of 4 microns of MOCVD technology epitaxial growth, then growth thickeies GaN layer thickness to 15 micro- in HVPE
Rice.
(2) face GaN in above-mentioned process for sapphire-based GaN compound substrate and 150 microns thick of W substrate surface, rotate respectively
It is coated with the NiCrSiB high temperature alloy slurry that a layer thickness is 5 microns, as conductive bond dielectric layer, as shown in Fig. 8 (a), then
At 1200 DEG C of temperature, pressure is the High temperature diffusion bonding carried out under 2T 20 minutes, realizes the key of GaN epitaxial layer and W metal substrate
It closes, as shown in Fig. 8 (b).
(3) Sapphire Substrate is removed using laser lift-off technique, the tables such as hydrochloric acid, acetone is carried out to compound substrate obtained
Face cleaning process obtains the bonding of NiCrSiB high temperature alloy slurry, device architecture is being applicable in for GaN/NiCrSiB/NiCrSiB/W
The stable and lesser state compound substrate of residual stress at a high temperature of GaN isoepitaxial growth, as shown in Fig. 8 (c) and 8 (d).
Claims (10)
1. a kind of preparation method of the low-stress state compound substrate for GaN growth, includes the following steps:
A) on a sapphire substrate, GaN single crystal epitaxial layer is prepared；
B) in the back side of thermal conductivity transfer substrate, deposition stress compensation layer；
C) bonding medium layer is prepared on the surface of GaN epitaxy film, high heat-conductivity conducting transfer substrate respectively；
D) High temperature diffusion bonding techniques are used, by bonding medium layer, by the GaN epitaxial layer and thermal conductivity in Sapphire Substrate
Substrate bonding is together；
E) substrate desquamation technology is used, Sapphire Substrate is removed；
Then obtain the low-stress state compound substrate that can be used for the high-temperature stable of GaN growth.
2. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
It is, step a) is described on a sapphire substrate, prepares GaN single crystal epitaxial layer, including directly extension is raw on a sapphire substrate
Long GaN single crystal layer, or using epoxy adhesive GaN single crystal epitaxial layer to be transferred to sapphire from its epitaxial substrate interim
In support substrate, or ZnO sacrificial release layers, then extension GaN single crystal layer are first deposited on a sapphire substrate.
3. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
It is, the back side in thermal conductivity transfer substrate step b), deposition stress compensation layer is using magnetron sputtering, molecular beam
The either vacuum thermal evaporation technology preparation of extension, plasma enhanced chemical vapor deposition, Metallo-Organic Chemical Vapor deposition
Single-layer or multi-layer membrane structure.
4. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
Be, step c) it is described respectively GaN epitaxy film, high heat-conductivity conducting transfer substrate surface, prepares bonding medium layer, be using
Magnetron sputtering, vacuum thermal evaporation or wet processing techniques prepare single-layer or multi-layer membrane structure.
5. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
It is, step d) the High temperature diffusion bonding techniques first prepare bonding medium layer by step c) is described, later, in temperature >=900
DEG C, under the conditions of pressure 100 Kgf/square inch to 4 tons/square inch, by Sapphire Substrate GaN epitaxy film with it is thermally conductive
Conductive substrates are bonded together by bonding medium layer.
6. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
It is, if using directly the GaN single crystal layer of extension, step e) use laser lift-off skill on a sapphire substrate in step a)
Art removes Sapphire Substrate；If the process for sapphire-based GaN substrate shifted in step a) using gluing, during bonding heating
Epoxy adhesive carbonization, Sapphire Substrate can be from GaN epitaxy film surface Automatic-falling；If first being served as a contrast in sapphire in step a)
ZnO sacrificial release layers, then extension GaN single crystal layer are prepared on bottom, then step e) is using chemical stripping technology removal sapphire lining
Bottom.
7. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
It is, it is GaN, SiN that step b) the stress compensation layer material, which is that fusing point is higher than 1000 DEG C and has thermal conductivity,xNitrogen
Compound material or one of molybdenum (Mo), titanium (Ti), palladium (Pd), golden (Au), copper (Cu), tungsten (W), nickel (Ni), chromium (Cr)
Elemental metals or several alloys.
8. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
It is, it is molybdenum (Mo), titanium that step c) the bonding medium layer material fusing point, which is higher than 1000 DEG C and has thermal conductivity,
(Ti), one of palladium (Pd), golden (Au), copper (Cu), tungsten (W), nickel (Ni), chromium (Cr) elemental metals or several alloys, or
Person is resin matrix and conducting particles silver (Ag), gold (Au), copper (Cu), aluminium (Al), zinc (Zn), iron (Fe), nickel (Ni), graphite
One of (C) or the particle and adhesive of the conducting polymer or one of the above of a variety of compositions or a variety of conducting particles,
Electrocondution slurry silicate-base high-temperature electric conduction glue (HSQ) or nickel (Ni) composed by solvent, auxiliary agent, chromium (Cr),
The high temperature alloy slurry that silicon (Si), boron (B) metal are formed.
9. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, feature
Be, step c) thermal conductivity transfer substrate material fusing point is higher than 1000 DEG C and has thermal conductivity, be molybdenum (Mo),
One of titanium (Ti), palladium (Pd), copper (Cu), tungsten (W), nickel (Ni), chromium (Cr) elemental metals or several alloy or silicon
(Si) crystal, silicon carbide (SiC) crystal or AlSi crystal.
10. a kind of preparation method of low-stress state compound substrate for GaN growth according to claim 1, special
Sign is, wherein the system including saving the smaller stress state compound substrate for GaN growth of stress compensation layer preparation section
Preparation Method also includes that step c) only selects one kind in GaN epitaxy film, thermal conductivity transfer substrate, deposits bonding on its surface and be situated between
After matter layer, the preparation method that High temperature diffusion bonding prepares low-stress state compound substrate is carried out.
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| CN106449912A (en) * | 2016-11-28 | 2017-02-22 | 东莞市中镓半导体科技有限公司 | GaN-based composite substrate with stress balance structural layer and method for preparing GaN-based composite substrate |
| CN108231695A (en) * | 2016-12-15 | 2018-06-29 | 上海新微技术研发中心有限公司 | Composite substrate and method for manufacturing the same |
| CN106611809B (en) * | 2017-01-11 | 2018-09-25 | 东莞市中镓半导体科技有限公司 | A kind of compound substrate preparation method with isolated protective layer for GaN growth |
| CN106952812A (en) * | 2017-03-31 | 2017-07-14 | 成都海威华芯科技有限公司 | A kind of GaN device bonding method |
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| CN108315823A (en) * | 2018-02-07 | 2018-07-24 | 山东大学 | A method of utilizing laser treatment substrate growth low stress Free-standing GaN monocrystalline |
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| CN113097124B (en) * | 2021-04-02 | 2023-12-05 | 中国科学院上海微系统与信息技术研究所 | Preparation method of heterogeneous integrated GaN film and GaN device |
| CN115295701B (en) * | 2022-09-29 | 2022-12-30 | 江西兆驰半导体有限公司 | Silicon-based gallium nitride aluminum epitaxial wafer and preparation method thereof |
| CN115332408B (en) * | 2022-10-18 | 2023-01-31 | 江西兆驰半导体有限公司 | Deep ultraviolet LED epitaxial wafer, preparation method thereof and LED |
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