CN106783551A - A kind of method of the alternate GaN structures of growth polarity in N polar GaN templates - Google Patents
A kind of method of the alternate GaN structures of growth polarity in N polar GaN templates Download PDFInfo
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
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- H01L21/02538—Group 13/15 materials
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Abstract
A kind of method of the alternate GaN structures of growth polarity in N polar GaN templates, belongs to semiconductor technology and devices field.N polar GaNs using the growths of MOCVD on a sapphire substrate are used as template,Mask layer is used as by the photoresist of photoetching process fabricating patterned in the template,The AlN for reversal is grown with T ALD method choices on the mask layer,T ALD methods can make technological temperature less than the fusing point of mask layer,Ensure that mask layer is indeformable,Uniformity can be prepared good,Thickness can be with the AlN films of precise control,Lift-off mask pattern layers AlN,Eliminate the etch step of conventional patterning process,Avoid infringement of the etching to device architecture,It is last to carry out thick film GaN growth using HVPE methods on the AlN of exposed N polar GaNs template and patterning,It is expected to obtain thickness up to the GaN structures of the alternating polarity of 1mm,To meet requirement of the high-power component to thick film alternately polarity GaN.
Description
Technical field
The present invention relates to semiconductor technology and devices field, referring specifically to a kind of growth on a sapphire substrate has difference
The method of polar GaN structure.
Background technology
The GaN of wurtzite structure has hexagonal crystallographic texture, is not centrosymmetric, tool in the positive and negative charge of C- direction of principal axis
There is intrinsic polarity effect, in N is bonded with Ga, covalent bonding electron is partial to N, so the direction of spontaneous polarization is N to Ga, in+C
(0001) direction is Ga to N, shows as Ga- polarity, so showing N- polarity in-C (000-1) direction, they have obvious
Different characteristics, such as chemism, doping efficiency, polarised direction, work function, configuration of surface and internal electric field.Although six sides'
GaN semiconductors have this different polarity, but current GaN base device is still substantially taken using single polarity or single crystal
To.For example, in electronic device such as light emitting diode, semiconductor laser and microwave high-power transistor frequently be
Ga- polar GaNs.In recent years, in order to the different characteristic of opposed polarity GaN is combined, researcher is devoted in same template
Upper growth has the research of alternately Ga- polarity and N- polar GaN structures.
There is important application field in optically and electrically device with alternately polarity GaN structures.GaN has big secondary
Nonlinear factor, such as combines its high heat conductance, broad-band gap and transparent window wide, is quasi-phase matched (quasi-phase
Matching) the ideal material of type frequency conversion.In quasi-phase matching, the periodic arrangement of crystal orientation conversion can be used
Relative phase during correcting light by crystal, this is that current nonlinear optical material to be met.
At present, the implementation method of this alternately polarity GaN structures is still evolving, mainly using foreign substrate (such as indigo plant
Jewel substrate, SiC substrate), by using different substrate orientation and growth conditions, doped level and cushion and nucleating layer
To control the polarity of epitaxial layer GaN.For example, growing GaN using MOCVD on SiC (0001) substrate that lattice mismatch is 3.4%
When, can in the SiC substrate of Si polar surfaces extension Ga- polar GaNs, on C faces obtain N- polar GaNs.It is previously used for GaN- poles
The technology of sex reversal is mainly the reversion of induction of being adulterated by Mg, and Ga- polar GaNs can be become N- poles by the P-type layer of Mg heavy doping
Property GaN, but this method can cause doping aggregation in film, influence the quality of film and the performance of composite structure.In addition, individual layer
Mg and MgxNyThe Ga- poles of GaN can be also converted to N- polarity by thin layer, although the problem that they do not have doping aggregation occurs, but
It is inverting domain boundary occur in the interface of N- polarity and Ga- polar materials.Later in the case where not using Mg to induce reversion, adopt
The growth of Ga- the polar GaNs, (S.Mita.J.Cryst.Growth.311 of document 1 are controlled with one layer thin of polarity inversion layer AlN
(2009) 3044-3048) report, growth polarity inversion layer AlN on a sapphire substrate, then obtained by photoetching and etching technics
Patterning AlN, then grows the GaN structures converted with alternately polarity using MOCVD methods.The method is due to using life
The slower epitaxy technology of speed long, it is unfavorable to realizing thick film growth, and etch step can cause partial destruction to the structure of device.
There is thermal conductivity and relatively low laser threshold high in view of GaN, this characteristic can be used for the frequency of power-type
Rate converter part, current nonlinear optical material can not meet requirement.To this high power applications, it is necessary to thickness is up to 1 millimeter
The alternating polarity GaN structures of left and right.Currently, although prepare GaN body materials using HVPE and the hot method of ammonia and reach its maturity, but GaN is served as a contrast
Bottom cost still remains high, and is orientated using GaN substrate growth cycle and the still more difficult popularization of thicker GaN structures.
The content of the invention
In order to solve the above problems, the present invention proposes on a sapphire substrate the GaN template of growth N- polarity in advance, in mould
Mask layer selective growth on plate by patterning is used for AlN, the lift-off mask pattern layers AlN of reversal, finally exists
Thick film GaN is grown using HVPE in the GaN template and patterning AlN of exposed N- polarity, high-power component needs thickness is met
Up to the GaN requirements of the alternating polarity of 1mm.
The present invention is achieved by the following technical solutions：
A kind of method of the growth with opposed polarity GaN structures on a sapphire substrate, the described method comprises the following steps：
(1) N- polar GaNs are grown on a sapphire substrate, obtain Sapphire Substrate/N- polar GaN structures as template；Generation
Replaced relatively costly GaN substrate, and avoid directly with Sapphire Substrate when in foreign substrate because of lattice mismatch and heat
The defect that mismatch is produced；
(2) by photoetching process, the photoresist of fabricating patterned is used as mask layer in the template, obtain Sapphire Substrate/
N- polar GaNs/patterning photoresist structure；
The patterning photoresist refers to same according to certain pattern removal part photoresist reservation remainder photoresist
When make accordingly positioned at removal part photoresist lower floor N- polar GaNs it is exposed.
(3) the selective growth polarity inversion layer AlN on the mask layer and exposed N- polar GaNs, obtains sapphire lining
Bottom/N- polar GaNs/patterning photoresist/AlN structures.
(4) lift-off mask layer, obtains Sapphire Substrate/N- polar GaNs/patterning AlN structures；Eliminate tradition design chemical industry
Etch step in skill；
Patterning AlN refers to removal patterning photoresist while making lower floor accordingly positioned at removal part photoresist
N- polar GaNs it is exposed.
(5) GaN is grown in the Sapphire Substrate/N- polar GaNs/patterning AlN structures, in the remainder
The GaN grown on AlN is Ga- polarity, and the GaN grown on the exposed N- polar GaNs is N- polarity, is obtained in sapphire
Grown has opposed polarity GaN structures.
Further, the step (1) using c-plane sapphire as before substrate, including growth N- polar GaNs to the indigo plant
Jewel substrate carries out nitrogen treatment.
Further, photoresist used in the step (2) is resistant to elevated temperatures positive glue AZ6130.
Further, the photoetching process described in the step (2) includes spin coating, exposure, development.
Further, the step (3) is using low temperature plasma enhancing ald (PEALD) choice of technology life
AlN long, compared to traditional CVD technology, it can directly by the way that selective growth uniformity on the photoresist that patterns is good, thickness
Can be with the AlN films of precise control；
Described low temperature is 150 DEG C；
Al sources are TMA (trimethyl aluminium) during described PEALD prepares AlN
；N sources are Ar, N2And H2Mixed gas；
Each gas volume fractions are Ar in the mixed gas：N2：H2=1:3:6；
Described selective growth refer to only in exposed N- polar GaN region growing AlN, and on mask layer be difficult growth
AlN。
Further, the step (4) is using acetone lift-off mask layer.
Further, the step (5) uses hydride gas-phase epitaxy (HVPE) method growing pullets of very fast growth rate
The alternate GaN structures of property, compared with the slower MOCVD epitaxy method of growth rate, are more expected to meet power-type frequency converter
GaN requirement of the thickness needed for part up to the alternating polarity of 1mm.
Further, the step (5) is specially that hydrogen chloride is carried at gallium boat using nitrogen and is reacted with gallium, raw
Into gallium chloride, ammonia and the gallium chloride are introduced into vitellarium in the Sapphire Substrate/N- polar GaNs/patterning AlN respectively
Body structure surface generates GaN, and GaN thickness can be controlled by controlling growth time；
Temperature at the gallium boat is 800-850 DEG C；
The vitellarium temperature is 1050-1070 DEG C；
The flow velocity of the hydrogen chloride is 0.01slm；
The flow velocity of the ammonia is 0.6-1slm.
Further, the thickness of N- polar GaNs is 1.5-2um in the step (1).
Further, the thickness of mask layer is 0.1-1um in the step (2).
Further, the thickness of polarity inversion layer AlN is 20-45nm in the step (3).
Further, the pattern in the step (2) is wide, equidistant strip structure.
Advantageous Effects of the invention：
(1) present invention is, using epitaxial growth GaN layer on a sapphire substrate as template, to instead of relatively costly GaN
Substrate, and avoid directly with Sapphire Substrate when in foreign substrate because of defect that lattice mismatch and thermal mismatching are produced.
(2) present invention uses the direct selective growth polarity on patterned mask layer and exposed template of PEALD technologies
Inversion layer AlN, compared with (about 700 DEG C) AlN of growth of MOCVD, the method can be equal to preparation under the conditions of 150 DEG C in low temperature
Even, thickness with the AlN films of precise control, and can ensure that mask layer stands intact；Selective growth is caused will not on mask layer
There is AlN to generate, obtain patterning AlN after stripping, eliminate the etch step in conventional patterning process, it is to avoid etching is right
The damage of device architecture.
(3) present invention using very fast growth rate the alternate GaN structures of HVPE method growth polarities, with growth rate compared with
Slow MOCVD epitaxy method is compared, and is more expected to meet thickness needed for power-type frequency conversion device up to the alternating polarity of 1mm
GaN requirements.
Brief description of the drawings
Fig. 1, present invention method flow chart.
Fig. 2, be the present invention provide on a sapphire substrate grow N- polar GaN templates structure chart.
Fig. 3, be the present invention provide the structure chart of the mask layer photoresist of fabricating patterned in template.
Fig. 4, be the present invention provide selective growth polarity inversion layer AlN structure chart.
Fig. 5, be the present invention provide patterning AlN structure chart.
Fig. 6, be the present invention provide the alternate GaN structure charts of growth polarity in N- polar GaN templates.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
Conversely, the present invention covers any replacement done in spirit and scope of the invention being defined by the claims, repaiies
Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to of the invention thin
It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art
Description can also completely understand the present invention.
Embodiment 1
The method that Grown on Sapphire Substrates replaces Ga- and N- polar GaN structures：
Step 1：By Sapphire Substrate isopropanol, acetone, methyl alcohol, alcohol, deionized water, ultrasound is clear successively at room temperature
Wash 5 minutes, finally use N2Drying.
Step 2：Sapphire Substrate after cleaning is put in the MOCVD reative cells rich in N, is carried out at nitridation at high temperature
After reason, with triethyl-gallium TEG and NH3It it is 1100 DEG C in temperature respectively as Ga and N sources, chamber pressure is 150Torr, V/III ratios
It is the N- polar GaNs of 1.5-2um to grow thickness under conditions of 600-3000.
Step 3：With N- polar GaNs as template, the photoresist of patterning is prepared with photoetching process：Above-mentioned sample is placed on
Soaked 2 minutes in ionized water, then with 80 DEG C of standard cleaning liquid SC1 (NH40H:H2O2：H2O=1：1：5) clean 10 minutes,
Cleaned with deionized water again and nitrogen drying, a layer thickness is prepared between 0.1-1um in template surface using whirl coating
Positive glue (AZ6130), be placed on 95 DEG C of baking boxs toast 2.5 minutes, the sample after drying is put into litho machine, by covering
Film version carries out selective uv-exposure to it, finally photoresist is placed in acetone and developed, and the pattern transfer on mask plate is arrived
In N- polar GaN templates, the photoresist (AZ6130) for being patterned.
Step 4：PEALD deposits AlN layers for reversed polarity：Above-mentioned sample deionized water rinsing and nitrogen are dried up
Afterwards in feeding PEALD reative cells, the temperature of sample stage is increased to 150 DEG C, is made respectively using trimethyl aluminium TMA and Ar/N2/H2
It is Al and N sources, is in growth parameter(s)：Sunk under conditions of 0.1s TMA dose/15s purge/30s plasma/15s purge
The AlN of 20~45nm of product.
Step 5：Above-mentioned sample is put into acetone, photoresist is removed, the N- polar GaN templates under photoresist are exposed
Come, obtain patterning AlN, and clearly dried up with nitrogen with deionized water.
Step 6：Above-mentioned sample is put into hvpe reactor chamber, warm area residing for gallium boat is 800-850 DEG C, chlorine in HVPE systems
Change hydrogen under the carrying of nitrogen by gallium boat, with gallium reaction, generate gallium chloride, gallium chloride introduces growth respectively with ammonia
Area, temperature can be controlled between 1050-1070 DEG C, in N- polar GaNs substrate and AlN Surface Creation GaN, hydrogen chloride during growth
Flow velocity be 0.01slm, ammonia flow can be located between 0.6-1slm, control growth time to grow thicker GaN, in AlN
What is grown on region is Ga- polar GaNs, and N- polar GaNs are obtained on N- polar GaNs, thus obtains alternately polarity GaN structures.
Embodiment 2
1) reference picture 2, by the isopropanol of Sapphire Substrate 101, acetone, methyl alcohol, alcohol, are cleaned by ultrasonic successively at room temperature
5 minutes, then rinsed repeatedly with deionized water, and use N2Drying.Sapphire Substrate 101 after cleaning is put in the MOCVD rich in N
In reative cell, after carrying out nitrogen treatment at high temperature, with triethyl-gallium TEG and NH3Respectively as Ga and N sources, it is in temperature
1100 DEG C, chamber pressure is 150Torr, and V/III ratios are growth 2um N- polar GaNs layer 102 under conditions of 3000.
2) reference picture 3, with N- polar GaNs as template, with the photoresist 103 of photoetching process fabricating patterned：By in upper step
Sample put in deionized water soak 2 minutes, then with 80 DEG C of standard cleaning liquid SC1 (NH40H:H2O2：H2O=1：1：
5) clean 10 minutes, then cleaned with deionized water and nitrogen drying, a layer thickness is prepared in template surface using whirl coating
It is the positive glue (AZ6130) of 100nm, is placed in being toasted 2.5 minutes on 95 DEG C of baking boxs, the sample after drying is put into litho machine,
Selective uv-exposure is carried out to it by mask plate, the 40s that develops is finally putting into acetone, the part that removal is exposed will be covered
Pattern transfer in film version in N- polar GaNs template 102, the photoresist (AZ6130) 103 for being patterned.
3) reference picture 4, the sample obtained in upper step are cleaned with deionized water after being dried up with nitrogen, feeding PEALD reactions
In room, the temperature of sample stage is raised to 150 DEG C, use trimethyl aluminium TMA and Ar/N2/H2Respectively as Al and N sources, join in growth
Number is：200 cycles are deposited under conditions of 0.1s TMA dose/15s purge/30s plasma/15s purge, film is obtained
Thickness is about AlN layers 104 of 30nm.
4) reference picture 5, the sample that will be obtained is put into acetone, lift-off mask layer photoresist, exposes N- polar GaNs, directly
The AlN being grown in N- polar GaN templates retains, AlN layers 104 for being patterned.
5) reference picture 6, above-mentioned sample is put into hvpe reactor chamber, and warm area residing for gallium boat is 850 DEG C, chlorine in HVPE systems
Change hydrogen under the carrying of nitrogen by gallium boat, with gallium reaction, generate gallium chloride, gallium chloride introduces growth respectively with ammonia
Area, is 1070 DEG C, hydrogen chloride, ammonia, N in temperature2The flow of carrier gas is respectively growth under conditions of 0.01slm, 1slm, 3slm
GaN film layer, obtains N- polar GaNs film layer 106 on N- polar GaNs, and what is grown on AlN regions is Ga- polar GaN film layers
105, thus obtain the GaN structures of thicker alternating polarity.
Claims (10)
1. a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, it is characterised in that methods described bag
Include following steps：
(1) N- polar GaNs are grown on a sapphire substrate, obtain Sapphire Substrate/N- polar GaN structures as template；
(2) by photoetching process, the photoresist of fabricating patterned is used as mask layer in the template, obtains Sapphire Substrate/N- poles
Property GaN/ patterning photoresist structure；
The patterning photoresist refers to retain remainder photoresist while making according to certain pattern removal part photoresist
N- polar GaNs accordingly positioned at the lower floor of removal part photoresist are exposed；
(3) the selective growth polarity inversion layer AlN on the mask layer and exposed N- polar GaNs, obtains Sapphire Substrate/N-
Polar GaN/patterning photoresist/AlN structures；
(4) lift-off mask layer, obtains Sapphire Substrate/N- polar GaNs/patterning AlN structures；Patterning AlN refers to removal pattern
Change photoresist makes the N- polar GaNs accordingly positioned at the lower floor of removal part photoresist exposed simultaneously；
(5) GaN is grown in the Sapphire Substrate/N- polar GaNs/patterning AlN structures, on the remainder AlN
The GaN of growth is Ga- polarity, and the GaN grown on the exposed N- polar GaNs is N- polarity, is obtained in Sapphire Substrate
Upper growth has N- polar GaN structures.
2. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
It is that the step (1) is using c surface sapphires as substrate；Including being carried out to the Sapphire Substrate before growth N- polar GaNs
Nitrogen treatment.
3. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
It is that glue used is resistant to elevated temperatures positive glue AZ6130 in the step (2)；Described photoetching process includes spin coating, exposure, shows
Shadow.
4. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
It is that the step (3) uses PEALD choice of technology growing AINs；Described low temperature is 150 DEG C；
The Al sources that described PEALD prepares in AlN are TMA；N sources are Ar, N2And H2Mixed gas；
Each gas volume fractions are Ar in the mixed gas：N2：H2=1:3:6；
Described selective growth refer to only in exposed N- polar GaN region growing AlN, and on mask layer be difficult growing AIN.
5. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
It is that the step (4) is using acetone lift-off mask layer.
6. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
Be that the method for growth GaN is HVPE methods in the step (5), specially using nitrogen by hydrogen chloride be carried at gallium boat with
Gallium reacts, and generates gallium chloride, ammonia and the gallium chloride is introduced into vitellarium respectively, in the Sapphire Substrate/N- poles
Property GaN/ patterning AlN body structure surfaces generation GaN, GaN thickness is controlled by controlling growth time；
Temperature at the gallium boat is 800-850 DEG C；
The vitellarium temperature is 1050-1070 DEG C；
The flow velocity of the hydrogen chloride is 0.01slm；
The flow velocity of the ammonia is 0.6-1slm.
7. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
It is that the thickness of N- polar GaNs is 1.5-2um in the step (1).
8. a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates as described in claim 1 or 3, it is special
Levy and be, the thickness of mask layer is 0.1-1um in the step (2).
9. as claimed in claim 1 a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates, its feature
It is that the thickness of polarity inversion layer AlN is 20-45nm in the step (3).
10. a kind of method of the alternate GaN structures of growth polarity in N- polar GaN templates as described in claim 1 or 3, its
It is characterised by, the figure in the step (2) is wide, equidistant strip structure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108023001A (en) * | 2017-11-30 | 2018-05-11 | 武汉大学 | Etch stop layer structure, the production method containing its epitaxial wafer and the epitaxial wafer |
| CN113539791A (en) * | 2021-06-25 | 2021-10-22 | 中国科学院半导体研究所 | Preparation method of polarity-alternating AlN template |
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| US20120068189A1 (en) * | 2010-09-17 | 2012-03-22 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Method for Vertical and Lateral Control of III-N Polarity |
| CN103579421A (en) * | 2013-11-07 | 2014-02-12 | 无锡英普林纳米科技有限公司 | Preparation method for large-area patterning sapphire substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101135854A (en) * | 2003-11-27 | 2008-03-05 | 株式会社新克 | Positive light sensitivity composition |
| US20120068189A1 (en) * | 2010-09-17 | 2012-03-22 | The Government Of The United States Of America, As Represented By The Secretary Of The Navy | Method for Vertical and Lateral Control of III-N Polarity |
| CN103579421A (en) * | 2013-11-07 | 2014-02-12 | 无锡英普林纳米科技有限公司 | Preparation method for large-area patterning sapphire substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108023001A (en) * | 2017-11-30 | 2018-05-11 | 武汉大学 | Etch stop layer structure, the production method containing its epitaxial wafer and the epitaxial wafer |
| CN113539791A (en) * | 2021-06-25 | 2021-10-22 | 中国科学院半导体研究所 | Preparation method of polarity-alternating AlN template |
| CN113539791B (en) * | 2021-06-25 | 2024-02-27 | 中国科学院半导体研究所 | Preparation method of polarity-alternating AlN template |
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Application publication date: 20170531 |
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