CN105390532A - Unintentionally doped high resistance GaN film with InGaN insertion layer and preparation method thereof - Google Patents

Unintentionally doped high resistance GaN film with InGaN insertion layer and preparation method thereof Download PDF

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CN105390532A
CN105390532A CN201510712168.XA CN201510712168A CN105390532A CN 105390532 A CN105390532 A CN 105390532A CN 201510712168 A CN201510712168 A CN 201510712168A CN 105390532 A CN105390532 A CN 105390532A
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layer
insert layer
high resistant
ingan
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梁红伟
刘建勋
柳阳
夏晓川
杜国同
蒋建华
闫晓密
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JIANGSU XINGUANGLIAN TECHNOLOGY Co Ltd
Dalian University of Technology
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JIANGSU XINGUANGLIAN TECHNOLOGY Co Ltd
Dalian University of Technology
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    • H01L29/00Semiconductor devices specially adapted for rectifying, amplifying, oscillating or switching and having potential barriers; Capacitors or resistors having potential barriers, e.g. a PN-junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
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    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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Abstract

The present invention provides an unintentionally doped high resistance GaN film with an InGaN insertion layer and a preparation method thereof. The unintentionally doped high resistance GaN film comprises a substrate, a low-temperature GaN nucleation layer, a GaN buffer layer, an InGaN insertion layer reconstructed by annealing and a high resistance GaN layer which are orderly arranged from bottom to top. Through introducing the InGaN insertion layer and carrying out high-temperature annealing, in the condition of not reducing GaN growth pressure and ensuring high crystal quality of the film, an appropriate amount of edge dislocations is introduced, a small amount of screw dislocations is increased, by using the edge dislocations, the carbon acceptor in a reaction chamber is induced into the GaN film, thus background electrons are compensated, and the high resistance GaN film is realized.

Description

A kind of involuntary doping high resistant GaN film with InGaN insert layer and preparation method thereof
Technical field
The present invention relates to semiconductor material technology, particularly relate to a kind of involuntary doping high resistant GaN film with InGaN insert layer and preparation method thereof.
Background technology
At present, the third generation semiconductor material with wide forbidden band taking GaN as representative, because its energy gap is large, disruptive field intensity is high, electronics saturation drift velocity is high, corrosion-resistant and the outstanding advantages such as Flouride-resistani acid phesphatase, plays very important effect in the electronic devices such as making high frequency, high power, radioresistance.The High Electron Mobility Transistor (HEMT) prepared with AlGaN/GaN heterojunction has the two-dimensional electron gas of high density and high mobility, is the ideal material of development microwave power device.At present, the technology preparing GaN material device the most frequently used is metal-organic chemical vapor deposition equipment (MOCVD) technology, but contain the Shi zhiming such as a large amount of O impurity and N room by the GaN film that MOCVD grows, very high concentration of background carriers can be produced, thus make GaN film present N-shaped conduction type, be difficult to realize high resistance film.There is serious electrical leakage problems in the AlGaN/GaN HEMT that the GaN resilient coating of this non-high resistant grows, the high frequency performance of extreme influence AlGaN/GaN based hemts and pinch-off behavior, add the caloric value of device simultaneously.
In order to overcome the above problems, need the GaN epitaxial layer preparing high resistivity, low carrier concentration.At present, employing MOCVD technology acquisition high resistant GaN film mainly contains the impurity doping introducing deep energy level acceptors such as deliberate C, Fe and is controlled to stratum nucleare growth parameter(s) and introduces dislocation thus induce the methods such as C is incorporated to.But these methods have respective shortcoming, such as cause chamber contamination, reduce film crystal quality and electrical properties, the extremely narrow and device growth of growth parameter(s) window is repeated bad etc.Also have a kind of method to control being incorporated to of involuntary doping carbon atom by low-pressure growth, thus introduce carbon acceptor level, compensate for background charge carrier.Although this method technique is simple, usually can introduce highdensity polytype dislocation, and due to the auto-compensation of carbon impurity, be difficult to ensure again higher crystal mass while acquisition high resistivity.
Summary of the invention
The object of the invention is to, for above-mentioned existing GaN epitaxial layer be difficult to take into account high resistivity and compared with the problem of high-crystal quality, a kind of involuntary doping high resistant GaN film with InGaN insert layer is proposed, this film is not when reducing GaN growth pressure and ensure film compared with introducing appropriate edge dislocation when high-crystal quality, and increase helical dislocation on a small quantity, the carbon acceptor in edge dislocation induced reaction room is utilized to be incorporated to GaN film, and then compensate for background electronics, realize high resistant GaN film.
For achieving the above object, the technical solution used in the present invention is: a kind of involuntary doping high resistant GaN film with InGaN insert layer, comprise set gradually from bottom to top substrate, low temperature GaN nucleating layer, GaN resilient coating, annealing reconstruct InGaN insert layer and high resistant GaN layer.
Further, described substrate is sapphire.
Further, described low temperature GaN nucleating layer thickness is 10 ~ 200nm, is preferably 50-100nm; Described GaN buffer layer thickness is 1 ~ 5 μm, is preferably 2-3 μm; The InGaN insert layer thickness of described annealing reconstruct is 50 ~ 200nm, is preferably 60-120nm; Described high resistant GaN layer thickness is 100nm ~ 20 μm, is preferably 500nm-10 μm.
Another object of the present invention, provides a kind of preparation method of the involuntary doping high resistant GaN film with InGaN insert layer, comprises the following steps:
Step 1: substrate is put heat treatment in the reaction chamber;
Step 2: adopt two-step growth method, at Grown one deck low temperature GaN nucleating layer;
Step 3: grow the involuntary Doped GaN resilient coating of one deck on GaN nucleating layer;
Step 4: grow one deck InGaN insert layer on GaN resilient coating;
Step 5: carry out high annealing to InGaN insert layer and obtain the InGaN insert layer reconstructed of annealing, During Annealing continues to pass into a certain amount of TEG and NH 3;
Step 6: the high resistant GaN layer growing the involuntary doping of one deck in the InGaN insert layer of annealing reconstruct.
Further, described low temperature GaN nucleating layer growth temperature is 450 ~ 600 DEG C, and reative cell pressure is 400 ~ 550Torr.
Further, the growth temperature of described GaN resilient coating is 900 ~ 1100 DEG C, reative cell pressure 150 ~ 300Torr.
Further, the growth temperature of described InGaN insert layer is 600 ~ 800 DEG C, reative cell pressure 150 ~ 300Torr.
Further, the annealing temperature of the InGaN insert layer of described annealing reconstruct is more than 1000 DEG C, and annealing time 1 ~ 1200s, be preferably 200-800s, During Annealing continues TEG and NH passing into certain flow 3, wherein TEG flow is 5 ~ 100sccm, is preferably 20-50sccm, NH 3flow is 2000 ~ 8000sccm, is preferably 3000-5000sccm, and keeps reative cell pressure to stablize.
Further, the growth temperature of described high resistant GaN layer is more than 900 ~ 1100 DEG C, reative cell pressure 150 ~ 300Torr.
Further, adopt MOCVD technology growth with the involuntary doping high resistant GaN film of InGaN insert layer.
Further, with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, comprise the following steps:
Step 1: substrate is put heat treatment in the reaction chamber;
Step 2: adopt two-step growth method, with H 2for carrier gas, with TMG and NH 3for growth source, at Grown one deck low temperature GaN nucleating layer;
Step 3: under high temperature 900 ~ 1100 DEG C, constant-pressure conditions, with H 2for carrier gas, with TMG and NH 3for growth source, GaN nucleating layer grows the involuntary Doped GaN resilient coating that one deck 1 ~ 5 μm is thick;
Step 4: keep pressure constant, reduce temperature to 600 ~ 800 DEG C, carrier gas is N 2, gallium source switches to TEG, NH 3for nitrogenous source, GaN resilient coating grows one deck InGaN insert layer, thickness is 50 ~ 200nm;
Step 5: keep pressure constant, carry out high annealing to InGaN insert layer, During Annealing continues to pass into a certain amount of TEG and NH 3, wherein TEG flow is 5 ~ 100sccm, NH 3flow is 2000 ~ 8000sccm;
Step 6: under keeping temperature 900 ~ 1100 DEG C, pressure 150 ~ 300Torr condition, nitrogenous source is ammonia (NH 3), carrier gas is H 2, gallium source is TMG, and the InGaN insert layer of annealing reconstruct grows the high resistant GaN layer of the involuntary doping of one deck.
A kind of involuntary doping high resistant GaN film scientific structure with InGaN insert layer of the present invention, rationally, its preparation method is simple, easy, compared with prior art, has the following advantages:
1, the present invention passes through with the involuntary doping high resistant GaN film of InGaN insert layer the InGaN insert layer introducing annealing reconstruct, the GaN layer edge dislocation density that this insert layer grows is increased, thus induced carbon impurity is incorporated to GaN film, the carbon acceptor introduced can compensate for background charge carrier, and the resistivity of GaN epitaxial layer is improved greatly.
2, the present invention is simple with preparation method's technique of the involuntary doping high resistant GaN film of InGaN insert layer, reproducible, growth parameter(s) controllability is strong, do not need the dopant material that extra introducing is new, memory-less effect, can meet the demand that industrial production manufactures better, and crystal mass is better than the high resistant GaN film adopting traditional handicraft low-pressure growth.
Accompanying drawing explanation
Fig. 1 is the structural representation of the involuntary doping high resistant GaN film with InGaN insert layer;
Fig. 2 is the secondary ion mass spectroscopy test result of the involuntary doping high resistant GaN film with InGaN insert layer.
Embodiment
Below in conjunction with embodiment, the present invention is further described:
Embodiment 1
As shown in Figure 1, present embodiments provide a kind of involuntary doping high resistant GaN film with InGaN insert layer, comprising:
-substrate, its material is sapphire;
-low temperature GaN nucleating layer, it is produced on substrate, and wherein the thickness of low temperature GaN nucleating layer is 25nm;
-GaN resilient coating, it is produced on low temperature GaN nucleating layer, and growth temperature is at 1045 DEG C, and thickness is 3.2 μm;
The InGaN insert layer of-annealing reconstruct, it is produced on GaN resilient coating, and thickness is about 65nm; The growth temperature of InGaN insert layer is 770 DEG C, is warming up to 1050 DEG C of high annealing 600s after growth terminates.
-high resistant GaN layer, it is produced in the InGaN insert layer of annealing reconstruct, and growth temperature is 1050 DEG C, and thickness is 650nm.
The present embodiment, with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, comprises following processing step:
Step 1: by substrate heat treatment in MOCVD device;
Step 2: adopt two-step growth method, with H 2for carrier gas, with TMG and NH 3for growth source, at Grown one deck low temperature GaN nucleating layer, thickness 25nm;
Step 3: be warming up to 1045 DEG C, Pressure Drop is low to moderate 188Torr, GaN nucleating layer grows the involuntary Doped GaN resilient coating of one deck, and thickness is 3.2 μm;
Step 4: be cooled to 770 DEG C, reative cell pressure maintains 188Torr, and carrier gas switches to N 2, gallium source switches to TEG, and GaN resilient coating grows one deck InGaN insert layer, and thickness is about 65nm;
Step 5: raised temperature to 1050 DEG C, reative cell pressure maintains 188Torr, and to InGaN insert layer high annealing 600s, it is 11sccm, NH that During Annealing continues to pass into TEG flow 3flow is 5000sccm;
Step 6: after annealing terminates, keep temperature 1050 DEG C, pressure 188Torr, carrier gas switches to H 2, gallium source switches to TMG, growing high resistant GaN layer, and thickness is 650nm.
After testing the present embodiment with the involuntary doping high resistant GaN film square resistance of InGaN insert layer up to 2.09 × 10 8Ω/sq.High-resolution X-ray diffraction result shows, sample (002) face and (102) face halfwidth are respectively 318.4 " and 464.4 ".
Fig. 2 gives the secondary ion mass spectroscopy testing result of the involuntary doping high resistant GaN film that the present embodiment proposes.As shown in Figure 2, the concentration of carbon of involuntary doping starts to increase gradually after InGaN insert layer, is reaching maximum 4.84 × 10 17cm -3tend towards stability gradually afterwards.Involuntary doping carbon acceptor is to the compensation of background carriers just, makes sample present high resistant characteristic.
By the existing higher resistivity of involuntary doping high resistant GaN that this kind of method obtains, higher crystal mass can be ensured again.This kind of method avoids the deliberately destruction of doping to crystal mass, and do not limit by growth number of times, growth parameter(s) window is wide simultaneously, and controllability is good and can not cause chamber contamination, and for realizing high-quality, high resistant GaN opens a new way.
Embodiment 2
Present embodiment discloses a kind of involuntary doping high resistant GaN film with InGaN insert layer, by introducing InGaN insert layer and high annealing, when not reducing GaN growth pressure and ensure film compared with introducing appropriate edge dislocation when high-crystal quality, and increase helical dislocation on a small quantity, the carbon acceptor in edge dislocation induced reaction room is utilized to be incorporated to GaN film, and then compensate for background electronics, realize high resistant GaN film.
Particularly, should comprise with the involuntary doping high resistant GaN film of InGaN insert layer: comprise set gradually from bottom to top sapphire layer, low temperature GaN nucleating layer, GaN resilient coating, annealing reconstruct InGaN insert layer, high resistant GaN layer.Described low temperature GaN nucleating layer thickness is 30nm, and described GaN buffer layer thickness is 2 μm; Described annealing reconstruct InGaN insert layer thickness for high resistant GaN layer thickness described in 100nm be 1 μm.
The preparation method of the described involuntary doping high resistant GaN film with InGaN insert layer, comprises the following steps:
Step 1: substrate is placed on heat treatment in MOCVD device;
Step 2: adopt two-step growth method, with H 2for carrier gas, with TMG and NH 3for growth source, at Grown one deck low temperature GaN nucleating layer;
Step 3: be low to moderate 200Torr at high temperature 1060 DEG C, Pressure Drop, GaN nucleating layer grows the involuntary Doped GaN resilient coating of one deck;
Step 4: keep pressure constant, reduce temperature to 790 DEG C, reative cell pressure maintains 200Torr, and carrier gas switches to N 2, gallium source switches to TEG, and GaN resilient coating grows one deck InGaN insert layer;
Step 5: keep pressure constant, carry out high annealing to InGaN insert layer, annealing temperature is 1100 DEG C, annealing time 500s, and During Annealing continues to pass into a certain amount of TEG and NH 3, wherein TEG flow is 40sccm, NH 3flow is 6000sccm;
Step 6: under keeping temperature 1060 DEG C, pressure 200Torr condition, with H 2for carrier gas, with TMG and NH 3for growth source, the InGaN insert layer of annealing reconstruct grows the GaN layer of the involuntary doping of one deck, and namely this GaN layer has high resistant character.
The present embodiment is with the involuntary doping high resistant GaN film of InGaN insert layer after testing, and square resistance is up to 8.45 × 10 7Ω/sq.High-resolution X-ray diffraction result shows, sample (002) face and (102) face halfwidth are respectively 352.3 " and 489.6 ".
Embodiment 3
Present embodiment discloses a kind of involuntary doping high resistant GaN film with InGaN insert layer, comprise: a kind of involuntary doping high resistant GaN film with InGaN insert layer, comprise set gradually from bottom to top substrate, low temperature GaN nucleating layer, GaN resilient coating, annealing reconstruct InGaN insert layer, high resistant GaN layer.Described low temperature GaN nucleating layer thickness is 30nm; Described GaN buffer layer thickness is 4 μm; The InGaN insert layer thickness of described annealing reconstruct is 90nm; Described high resistant GaN layer thickness is 1.5 μm.
The present embodiment, with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, comprises the following steps:
Step 1: substrate is put heat treatment in the reaction chamber;
Step 2: adopt two-step growth method, at Grown one deck low temperature GaN nucleating layer;
Step 3: under high temperature 1050 DEG C, pressure 165Torr constant-pressure conditions, GaN nucleating layer grows the involuntary Doped GaN resilient coating of one deck;
Step 4: keep pressure constant, reduce temperature to 750 DEG C, GaN resilient coating grows one deck InGaN insert layer;
Step 5: keep pressure constant, high annealing is carried out to InGaN insert layer, annealing temperature 1000 DEG C, annealing time 100s.During Annealing continues to pass into a certain amount of TEG and NH 3, wherein TEG flow is 50sccm, NH 3flow is 7000sccm;
Step 6: under keeping temperature 1050 DEG C, pressure 165Torr condition, with H 2for carrier gas, with TMG and NH 3for growth source, the InGaN insert layer of annealing reconstruct grows the GaN layer of the involuntary doping of one deck, and namely this GaN layer has high resistant character.
The present embodiment is with the involuntary doping high resistant GaN film of InGaN insert layer after testing, and square resistance is up to 6.75 × 10 8Ω/sq.High-resolution X-ray diffraction result shows, sample (002) face and (102) face halfwidth are respectively 364.4 " and 547.2 ".
Last it is noted that above each embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to foregoing embodiments to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein some or all of technical characteristic; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.

Claims (10)

1., with an involuntary doping high resistant GaN film for InGaN insert layer, it is characterized in that, comprise set gradually from bottom to top substrate, low temperature GaN nucleating layer, GaN resilient coating, annealing reconstruct InGaN insert layer and high resistant GaN layer.
2., according to claim 1 with the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, described substrate is sapphire.
3. according to claim 1 with the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, described low temperature GaN nucleating layer thickness is 10 ~ 200nm; Described GaN buffer layer thickness is 1 ~ 5 μm; The InGaN insert layer thickness of described annealing reconstruct is 50 ~ 200nm; Described high resistant GaN layer thickness is 100nm ~ 20 μm.
4. described in claim 1-3 any one with a preparation method for the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, comprise the following steps:
Step 1: substrate is put heat treatment in the reaction chamber;
Step 2: adopt two-step growth method, at Grown one deck low temperature GaN nucleating layer;
Step 3: grow the involuntary Doped GaN resilient coating of one deck on GaN nucleating layer;
Step 4: grow one deck InGaN insert layer on GaN resilient coating;
Step 5: carry out high annealing to InGaN insert layer, obtain the InGaN insert layer reconstructed of annealing, During Annealing continues to pass into a certain amount of TEG and NH 3;
Step 6: the high resistant GaN layer growing the involuntary doping of one deck in the InGaN insert layer of annealing reconstruct.
5. according to claim 4 with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, described low temperature GaN nucleating layer growth temperature is 450 ~ 600 DEG C, and reative cell pressure is 400 ~ 550Torr.
6. according to claim 4 with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, the growth temperature of described GaN resilient coating is 900 ~ 1100 DEG C, reative cell pressure 150 ~ 300Torr.
7. according to claim 4 with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, the growth temperature of described InGaN insert layer is 600 ~ 800 DEG C, reative cell pressure 150 ~ 300Torr.
8. according to claim 4 with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, the annealing temperature of the InGaN insert layer of described annealing reconstruct is more than 1000 DEG C, and annealing time 1 ~ 1200s, During Annealing continues TEG and NH passing into certain flow 3, wherein TEG flow is 5 ~ 100sccm, NH 3flow is 2000 ~ 8000sccm, and keeps reative cell pressure to stablize.
9. according to claim 4 with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, the growth temperature of described high resistant GaN layer is more than 900 ~ 1100 DEG C, reative cell pressure 150 ~ 300Torr.
10., according to claim 4 with the preparation method of the involuntary doping high resistant GaN film of InGaN insert layer, it is characterized in that, adopt MOCVD technology growth with the involuntary doping high resistant GaN film of InGaN insert layer.
CN201510712168.XA 2015-10-28 2015-10-28 Unintentionally doped high resistance GaN film with InGaN insertion layer and preparation method thereof Pending CN105390532A (en)

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CN106935691A (en) * 2017-02-13 2017-07-07 中山大学 A kind of epitaxial preparation method of InGaN
CN108767008A (en) * 2018-04-17 2018-11-06 厦门市三安集成电路有限公司 A kind of HEMT and preparation method thereof with high resistant GaN buffer layer
WO2020228164A1 (en) * 2019-05-15 2020-11-19 中国电子科技集团公司第五十五研究所 Epitaxial growth method for reducing interfacial thermal resistance of gallium nitride high electron mobility field-effect transistor

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CN102931229A (en) * 2012-11-06 2013-02-13 中国电子科技集团公司第五十五研究所 AlGaN/GaN/InGaN double hetero-junction material and production method thereof
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CN106935691A (en) * 2017-02-13 2017-07-07 中山大学 A kind of epitaxial preparation method of InGaN
CN106935691B (en) * 2017-02-13 2019-07-16 中山大学 A kind of epitaxial preparation method of InGaN
CN108767008A (en) * 2018-04-17 2018-11-06 厦门市三安集成电路有限公司 A kind of HEMT and preparation method thereof with high resistant GaN buffer layer
CN108767008B (en) * 2018-04-17 2021-04-16 厦门市三安集成电路有限公司 HEMT (high electron mobility transistor) with high-resistance GaN buffer layer and preparation method thereof
WO2020228164A1 (en) * 2019-05-15 2020-11-19 中国电子科技集团公司第五十五研究所 Epitaxial growth method for reducing interfacial thermal resistance of gallium nitride high electron mobility field-effect transistor
KR20220020817A (en) * 2019-05-15 2022-02-21 차이나 일렉트로닉스 테크놀로지 그룹 코포레이션 넘버 55 리서치 인스티튜트 Epitaxial Growth Method for Reduction of Interfacial Thermal Resistance of Gallium Nitride High Electron Mobility Field Effect Transistor
KR102452739B1 (en) 2019-05-15 2022-10-11 차이나 일렉트로닉스 테크놀로지 그룹 코포레이션 넘버 55 리서치 인스티튜트 Epitaxial Growth Method for Reducing Interfacial Thermal Resistance of Gallium Nitride High Electron Mobility Field Effect Transistor

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Application publication date: 20160309