CN1333438C - Coaxial air intake for acquiring uniform wide-band gap semiconductor thin film - Google Patents
Coaxial air intake for acquiring uniform wide-band gap semiconductor thin film Download PDFInfo
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- CN1333438C CN1333438C CNB2005100377333A CN200510037733A CN1333438C CN 1333438 C CN1333438 C CN 1333438C CN B2005100377333 A CNB2005100377333 A CN B2005100377333A CN 200510037733 A CN200510037733 A CN 200510037733A CN 1333438 C CN1333438 C CN 1333438C
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 21
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- 239000000376 reactant Substances 0.000 claims abstract description 75
- 239000000463 material Substances 0.000 claims abstract description 28
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- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
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- 238000011160 research Methods 0.000 abstract description 5
- 206010040007 Sense of oppression Diseases 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 48
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
- 230000006698 induction Effects 0.000 description 8
- 239000010408 film Substances 0.000 description 7
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 7
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 7
- 239000011787 zinc oxide Substances 0.000 description 7
- 229910002601 GaN Inorganic materials 0.000 description 5
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- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 2
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Abstract
The present invention discloses a coaxial air inlet method for acquiring a semiconductor thin film with a uniform wide-band gap. The method is carried out in a reactor of a series of coaxial quartz tubes and quartz rings. The method has the following steps: (1), a substrate 6 is arranged on a substrate supporter 7, and is arranged in a reaction chamber with the substrate supporter 7, and the reaction chamber is vacuumized; (2), reactant I enters the reaction chamber from an air inlet pipe 1, reactant II enters the reaction chamber from an air inlet ring 3, isolation air is input from an air inlet ring 2, and oppression air is input from an air inlet ring 4; (3), the substrate is heated to preset temperature, the reactant I and the reactant II are uniformly mixed when approaching to the surface of the substrate 6, and are absorbed on the surface of the substrate 6 at high temperature to carry out decomposition reaction, and thus, a semiconductor thin film with a uniform wide-band gap is generated on the substrate 6. The present invention has the advantages of low cost, low technology difficulty and strong practicability, and is especially suitable for the growth of various wide-band gap structural materials such as GaN groups, ZnO groups, etc., and the research of device structural materials.
Description
One, technical field
The present invention relates to the preparation method of semi-conducting material, relate to a kind of coaxial air intake method of Semiconductor Film Growth specifically.
Two, background technology
Wide bandgap semiconductor materials has become one of center of semiconductor and photoelectron research.This based semiconductor material mainly comprises two classes: a class is to be the III group nitride material of representative with the gallium nitride, and another kind of is to be the II-VI group iii v compound semiconductor material of representative with zinc oxide.This two classes semiconductor material with wide forbidden band has some common advantages,, electron drift saturated velocity height big as energy gap, dielectric constant are little, characteristics such as good heat conductivity, be very suitable for making radioresistance, high frequency, high-power and superintegrated electronic device, and the more important thing is that they all have excellent photoelectric characteristic, be to make indigo plant, green glow and the Laser Devices of ultraviolet light and the preferred material of light-detecting device.
At present, gas phase epitaxy of metal organic compound (MOCVD), molecular beam epitaxy (MBE), hydride gas-phase epitaxy (HVPE) is the main method of preparation wide bandgap semiconductor materials, and the MOCVD technology is owing to can realize the growth of the single crystal epitaxial material of large tracts of land, good uniformity and two-forty, helping the development of high-quality light electric device, is that growth is used for one of most important technology of photoelectric material high-purity epitaxial film at present.Simultaneously, the HVPE technology also is one of major technique that obtains large tracts of land self-supporting GaN substrate at present.
With respect to molecular beam epitaxy technique, MOCVD and HVPE technology all be by with source metal (compound that contains Zn or Ga, the back claims reactant I) gas and V family or VI family gas (back title reactant II) as O
2, NH
3Deng, feed reative cell by different pipelines.Owing to these two kinds of gas molecules need be mixed before arriving at the substrate of film growth fully, obtaining uniform thin-film material, so people usually are pre-mixed these two kinds of reactants.Have extremely strong pre-reaction behavior but be used to develop between the reactant of this class wide bandgap semiconductor materials, this just makes the design of reative cell and obtain to obtain balance and optimization between the material growth uniformity in the pre-reaction of inhibitory reaction thing.
Commercial at present MOCVD equipment has taked various technology to solve this problem, as the Shower technology of Thomas Swan company and planet technology etc., the double-layer air-flow technology of Nichia company etc., but the difficulty of processing of these technology is bigger, simultaneously must be equipped with the substrate rotation technique, to reach high quality devices material and good material homogeneity.These numerous technology integrated makes the development cost of equipment and processing cost very high, relatively is suitable for the large-scale production of various devices.And for many pilot studys, can adopt a kind of cost lower, the structure of reactor that technical difficulty is less is realized than the homogeneous semiconductor growth for Thin Film, just can satisfy the requirement of research fully.
Three, summary of the invention
1. goal of the invention
The objective of the invention is to realize obtaining the coaxial air intake method of uniform wide-band gap semiconductor thin film by adopting the structure of reactor that a kind of cost is lower, technical difficulty is less.
2. technical scheme
This invention proposes to adopt coaxial air-flow air inlet technology, has solved the pre-reaction of existence during wide bandgap semiconductor materials is grown in MOCVD or the HVPE system and the contradiction between the material homogeneity, grows than the material between homogeneity range with realization.This core technology is a series of coaxial quartz ampoules or quartz ring, can be evenly distributed on substrate surface to guarantee above-mentioned reactant I that is carried and II.Adopt a kind of cost lower, the structure of reactor that technical difficulty is less, shown in figure (1), it is made up of air inlet pipe 1, air inlet ring 2, air inlet ring 3, air inlet ring 4, interior pipe 5, outer tube 8, substrate 6, substrate bracket 7 and institutes such as exhaust outlet or vacuum orifice 9.
A kind of coaxial air intake method of obtaining uniform wide-band gap semiconductor thin film, its method step is as follows:
A. at first be placed on the substrate bracket 7 after the material cleaning with substrate 6, put into reative cell in the lump, anti-
Answer the chamber to vacuumize from vacuum pumping opening 9 with mechanical pump and molecular pump; The base vacuum degree is evacuated to 10
-3Pa;
B. reactant I is carried by air inlet pipe 1 input by high-purity gas, reactant II is by 3 inputs of the second air inlet ring, isolate gas by 2 inputs of the first air inlet ring, isolating gas isolates reactant I and reactant II, compressing gas is by 4 inputs of the 3rd air inlet ring, the compressing shortness of breath makes the air-flow of reactant I and the air-flow of reactant II and the air-flow of isolation gas arrive at substrate surface as far as possible, the pressure of control reative cell and the distance D between substrate 6 and the air inlet;
C. substrate 6 is by the electric furnace heating that places under the substrate bracket 7, after being heated to design temperature, reactant I is carried from air inlet pipe 1 by high-purity gas and enters reaction zone, reactant II feeds reaction zone by air inlet ring 3, two kinds of reactants evenly mix during near substrate 6 surfaces, and be adsorbed on the substrate 6 surface generation decomposition reactions that are in high temperature, thereby on substrate 6, grow into uniform wide-band gap semiconductor thin film.
The material of the substrate 6 described in the above-mentioned steps a comprises sapphire or Si, GaAs, ZnO; Substrate bracket 7 is graphite or easy thermal conductive metallic material.
Reactant I described in the above-mentioned steps b comprises the compound of Zn or Ga, and reactant II comprises O
2Or NH
3, high-purity gas bag is drawn together high-purity Ar or N
2
Reactant I is 0.1-50m/s by the air velocity of air inlet pipe 1 input among the above-mentioned steps b, reactant II is 0.1-50m/s by the air velocity of the second air inlet ring (3) input, isolation gas is 0.1-40m/s by the air velocity of the first air inlet ring (2) input, compressing gas is imported by the 3rd air inlet ring (4), and its air velocity is at 0.1-60m/s.
The pressure of the control reative cell described in the above-mentioned steps b can be from low pressure 1Torr district to normal pressure 760Torr district, and distance D is 2-6cm.
The design temperature of substrate 6 heating described in the above-mentioned steps c is 400-700 ℃.
In this invention, the speed of all gases is determined that by separately the gas flow and the sectional area of quartz ampoule or quartz ring the while depends on the operating pressure of reative cell strongly.Exemplary value related in the following description of this invention technical scheme is an example to work in an atmospheric situation all, and other operating pressures all should be optimized and calculate on this basis.The gas velocity of air inlet pipe 1 must satisfy makes gas reactant I can be evenly distributed on substrate surface, this requires the gas velocity must be in certain limit 0.1-2m/s, and concrete numerical value must be optimized design between the internal diameter of air inlet and substrate distance D and air inlet pipe.Isolation gas by 2 inputs of air inlet ring plays a part reactant I and II are spatially isolated, it also is the compressing gas of reactant I air-flow simultaneously, its speed numerical value excursion is in the scope of 0.1-1m/s, its velocity magnitude must guarantee that (1) fully isolates reactant I and II before arriving substrate, reduce arriving the preceding mixability of substrate.(2) force reactant I to be distributed in substrate surface simultaneously as far as possible,, improve growth rate to improve the utilance of reactant I.Gas reactant II is by 3 inputs of air inlet ring, because its air inlet is distributed as ring-type, for guaranteeing the uniformity of reactant II at substrate surface, its air velocity must be slightly less than the speed of reactant I, and this speed will guarantee that this reactant can more arrive at substrate.The exemplary value of this air-flow is generally in the 0.1-0.5m/s scope.Compressing gas is by 4 inputs of air inlet ring, and the speed of this air-flow should be big as much as possible, and its exemplary value is in the 0.1-2m/s scope.Compressing gas just can play the substrate surface that reactant II is urged to as far as possible growth like this, to improve the utilance of reactant.Isolate gas simultaneously and oppress gas and also have an important effect, promptly stop contacting of reactant I or II and quartzy tube wall as far as possible, to reduce the growth of reactant, prevent from the contamination of system and the repeatability that growth moves to system material are produced destruction at reaction chamber wall.
Under the typical airflow condition, we adopt computer modeling technique that the substrate reactant concentration distribution of different distance D is calculated, and the result is shown in Fig. 2-3.Fig. 2 shows that gas reactant II is higher during in the D2 left and right sides at the distributed density of substrate surface, illustrates that on this position, the utilization ratio of reactant II is higher.On the other hand, Fig. 3 shows that the utilization ratio of reactant I descends significantly with the increase of distance D, and less distance D can make film growth rate be controlled on the higher level.Like this, under the standard air-flow, adopting distance is the substrate location of D2, can obtain more equally distributed high-quality thin film material at 2 inches substrate surfaces.Theoretical modeling shows that under typical sizes the surface heterogeneity of semiconductive thin film is ± 10%, can satisfy the growth and the research of semi-conducting material and simple Devices structure fully.
As mentioned above, the same with each pipeline intake velocity, the distance between air inlet and the substrate (Fig. 1 middle distance D) also is main key factor.Generally speaking, the typical sizes of the distance between air inlet and the substrate is 3 to 5cm, and in this size range, reactant can obtain to distribute more uniformly at substrate surface, can guarantee that again the mixability of these two kinds of reactants before arriving at substrate is controlled.
In this invention, higher air velocity is the key point of this invention, because higher air velocity can reduce the transport time of reactant before arriving at substrate greatly, thereby reduces the degree of pre-reaction.Simultaneously, the shortening that transports the time also goes far towards to reduce reactant and arrives at temperature before the substrate, thereby also can suppress the intensity of pre-reaction greatly.In this invention, reactant arrives at the typical time of substrate for below the millisecond magnitude.
Meanwhile, among Fig. 1 the speed of gas outlet (ring) and size also be the realization response thing substrate surface evenly distribute and provide the reactant utilance than key factor.If this gas outlet speed is bigger, will make reactant difficulty arrive at substrate surface and, directly flow away from the gas outlet in the space short circuit, thereby the utilance of reactant is descended greatly, the uniformity of film is relatively poor.And if gas outlet speed is too small, will make reaction gas flow easily form eddy current, thereby reactant is mixed too early, aggravated pre-reaction, the quality of materials of film is descended greatly.In the representative value 0.02-0.1m/s scope of this numerical value.
3. beneficial effect
This invention compared with prior art, the process technology that relates to is not difficult, cost is lower, practical, compatible good, be applicable to various MOCVD, in the design of the reative cell of HVPE and the pre-reaction of various necessary consideration reactant, and chamber pressure can be distinguished from low pressure (1 Torr) district's work to normal pressure (760 Torr).Be particularly suitable for various GaN bases and the growth of the wide bandgap structure material of zno-based and the research of device architecture material.
Four, description of drawings
Fig. 1. the reaction chamber structure schematic diagram
Fig. 2. under the fixed gas flow, different distance D adopts the distribution map of the substrate surface gas reactant II of computer simulation
Fig. 3. under the fixed gas flow, different distance D adopts the distribution map of the substrate surface gas reactant I of computer simulation
The description of symbols of accompanying drawing: 1-advances organ 2-and isolates pipe 6-substrate 7-substrate bracket 8-reative cell outer tube 9-reative cell exhaust outlet or vacuum pumping opening in the gas air inlet ring 3-reactant I air inlet ring 4-compressing gas air inlet ring 5-
Five, embodiment
Embodiment 1:
On Sapphire Substrate, adopt the typical growth step and the condition of MOCVD growing ZnO thin-film as follows:
Be placed on the substrate bracket 7 after at first Sapphire Substrate 6 being cleaned, and in the dress people reative cell, reative cell vacuumizes from vacuum pumping opening 9 with mechanical pump and molecular pump, the base vacuum degree is evacuated to higher vacuum (10
-3Pa).(flow is 50sccm as isolating gas feeding isolation gas air inlet ring 2 with high-purity gas (Ar) then, induction air flow ratio is 8m/s) and compressing gas feeds compressing gas air inlet ring 4, and (flow is 100sccm, induction air flow ratio is 10m/s) import the vitellarium by isolating gas air inlet ring 2 among Fig. 1 with compressing gas air inlet ring 4, the control chamber pressure is 200Pa, and substrate 6 is 3cm with the air inlet distance D.Substrate 6 after being heated to design temperature (550 ℃), is placed on the liquid MO source diethyl zinc (Zn (C in the steel cylinder by the electric furnace heating that places under the substrate bracket 7
2H
5)
2) carry (carrier gas flux 10sccm, causing 1 induction air flow ratio is 16m/s) 1 feeding reaction zone from Fig. 1, reactant IIO by high-purity Ar gas
2(flow 50sccm, causing 3 induction air flow ratios is 20m/s) feed reaction zone by air inlet ring 3, two kinds of reactants evenly mix near substrate 6 surfaces the time, and are adsorbed on the surface generation decomposition reaction of the Sapphire Substrate 6 that is in high temperature, thereby grow into ZnO on substrate 6.The growth rate of the feeding amount decision ZnO of reactant I, it also can be by Zn (C except that being determined by carrier gas flux
2H
5)
2Source bottle temperature is controlled.In this embodiment, source bottle temperature is controlled at 0 ℃, and the speed of growth that causes ZnO is 0.2nm/s.
Embodiment 2:
On Sapphire Substrate, adopt the typical growth step and the condition of HVPE growing GaN film as follows:
This HVPE device prevents placing the electric tube furnace of a pair of warm area, is divided into two zones: first zone is the synthetic district of reactant I, and this zone is in 900 ℃ of high temperature, and gallium source and feeding are by high-purity N
2The HCl gas that carries (flow is respectively 140sccm and 6sccm) reacts reaction of formation thing I GaCl here; Second zone is reaction zone, and the structure among Fig. 1 is located in this zone, and this reaction zone is the flat-temperature zone, and temperature is 1100 ℃, and substrate and air inlet distance D are 4cm.At first the Sapphire Substrate sheet is cleaned back dress people reative cell, the reative cell high-purity N
2Protection: high-purity gas (N
2) (flow is 500sccm as isolating gas, causing 2 induction air flow ratios is 0.1m/s) and oppress gas (flow is 1500sccm, and causing 4 induction air flow ratios is 0.1m/s) by 2 and 4 importing vitellariums among Fig. 1, and discharge from 9,9 exhaust flow velocitys are 0.05m/s, and chamber pressure is an atmospheric pressure.Reactant I is by high-purity N
2Gas carries (carrier gas flux 140sccm, causing air inlet ring 1 induction air flow ratio is 0.2m/s) reactant I air inlet ring 1 from Fig. 1 and feeds reaction zone, reactant II NH
3(flow 350sccm, causing air inlet ring 3 induction air flow ratios is 0.4m/s) feed reaction zone by air inlet ring 3, two kinds of reactants evenly mix near substrate 6 surperficial the time, and decomposition reaction takes place on the surface that is adsorbed on the Sapphire Substrate 6 that is in high temperature, thus on substrate 6 growing GaN.In this embodiment, the growth rate of the feeding amount of reactant I decision ZnO, it is by the decision of GaCl flow, and the growth rate that causes GaN is 15nm/s.
Claims (6)
1. coaxial air intake method of obtaining uniform wide-band gap semiconductor thin film, its method step is as follows:
A. at first be placed on the substrate bracket (7) after the material cleaning with substrate (6), put into reative cell in the lump, reative cell vacuumizes from vacuum pumping opening (9) with mechanical pump and molecular pump, and the base vacuum degree is evacuated to 10
-3Pa;
B. reactant I is carried from air inlet pipe (1) by high-purity gas and imports, reactant II is imported by the second air inlet ring (3), isolating gas is imported by the first air inlet ring (2), isolating gas isolates reactant I and reactant II, compressing gas is imported by the 3rd air inlet ring (4), the compressing shortness of breath makes the air-flow of reactant I and the air-flow of reactant II and the air-flow of isolation gas arrive at substrate surface as far as possible, and the distance D of the pressure of control reative cell and substrate (6) and air inlet;
C. substrate (6) is by the electric furnace heating that places under the substrate bracket (7), after being heated to design temperature, reactant I is carried from air inlet pipe (1) by high-purity gas and enters reaction zone, reactant II feeds reaction zone by the second air inlet ring (3), two kinds of reactants evenly mix during near substrate (6) surface, and be adsorbed on substrate (6) the surface generation decomposition reaction that is in high temperature, thereby on substrate (6), grow into uniform wide-band gap semiconductor thin film.
2. the coaxial air intake method of semiconductive thin film according to claim 1, the material that it is characterized in that the substrate described in the step a (6) comprise sapphire or Si, GaAs, ZnO; Substrate bracket (7) is graphite or easy thermal conductive metallic material.
3. the coaxial air intake method of semiconductive thin film according to claim 1 is characterized in that the reactant I described in the step b comprises the compound of Zn or Ga, and reactant II comprises O
2Or NH
3, high-purity gas bag is drawn together high-purity Ar or N
2
4. the coaxial air intake method of semiconductive thin film according to claim 1, it is characterized in that the air velocity that reactant I is imported by air inlet pipe (1) among the step b is 0.1-50m/s, reactant II by the air velocity of the second air inlet ring (3) input for O.1-50m/s, isolation gas is 0.1-40m/s by the air velocity of the first air inlet ring (2) input, compressing gas is imported by the 3rd air inlet ring (4), and its air velocity is at 0.1-60m/s.
5. the coaxial air intake method of semiconductive thin film according to claim 1 is characterized in that the pressure of the control reative cell described in the step b can be from low pressure 1Torr district to normal pressure 760Torr district, and distance D is 2-6cm.
6. the coaxial air intake method of semiconductive thin film according to claim 1 is characterized in that the design temperature of the substrate described in the step c (6) heating is 400-700 ℃.
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| CN102465277B (en) * | 2010-11-04 | 2013-11-27 | 上海蓝光科技有限公司 | Reverse radial MOCVD reactor |
| CN102465333B (en) * | 2010-11-18 | 2015-04-15 | 南京大学 | Vertical hydride vapor phase epitaxy growth system |
| CN102108547B (en) * | 2010-12-31 | 2012-06-13 | 东莞市中镓半导体科技有限公司 | Multi-substrate large-size hydride vapor phase epitaxy method and device |
| CN103456593B (en) * | 2013-09-02 | 2016-02-10 | 东莞市中镓半导体科技有限公司 | A kind of hydride vapor phase epitaxy apparatus and method improving multiple-piece epitaxial material thickness distributing homogeneity |
| CN103668446B (en) * | 2013-11-25 | 2016-06-01 | 东莞市中镓半导体科技有限公司 | A kind of Controllable precursor passage |
| CN105256369A (en) * | 2015-10-20 | 2016-01-20 | 中国电子科技集团公司第四十八研究所 | High-temperature-resistant horizontal multi-layer gas inlet device for SiC epitaxy |
| CN107855011B (en) * | 2017-11-28 | 2023-08-08 | 佛山科学技术学院 | Internal mixed structure of liquid chemical raw material pipe |
| CN110164757A (en) * | 2019-05-31 | 2019-08-23 | 中国科学院半导体研究所 | Compound semiconductor and its epitaxy method |
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