CN101445955A - Device for space-modulating atomic layer chemical vapour deposition epitaxial growth and method thereof - Google Patents
Device for space-modulating atomic layer chemical vapour deposition epitaxial growth and method thereof Download PDFInfo
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- CN101445955A CN101445955A CNA2007101782824A CN200710178282A CN101445955A CN 101445955 A CN101445955 A CN 101445955A CN A2007101782824 A CNA2007101782824 A CN A2007101782824A CN 200710178282 A CN200710178282 A CN 200710178282A CN 101445955 A CN101445955 A CN 101445955A
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Abstract
The invention relates to a device for space-modulating atomic layer chemical vapor deposition epitaxial growth. The device is characterized by comprising an air-intake shower and a base wherein, the air-intake shower is barrel-shaped and the interior of the air-intake shower is divided into a plurality of regions, and each region is an air-intake nozzle of feed gas; the base is a column and is provided with a plurality of circular grooves thereon, the circular grooves are used for placing a substrate; the diameter of the base is less than or equal to the diameter of the air-intake shower and the base can rotate; wherein, the air-intake shower is positioned at the side of base, the surface of which is provided with the circular groove; a certain distance exists between the air-intake shower and the base; one end of the air-intake shower, which is close to the base, is an air outlet; and the other end, which is far from the basement, is an air outlet.
Description
Technical field
The present invention relates to a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth method, being specifically related to a kind of diffuser by particular design spatially keeps apart various different types of unstripped gass mutually, spatial " spatial modulation " method that the substrate of epitaxial material is covered in succession by methods such as rotation or translations by the different sorts unstripped gas realizes then, can avoid taking place between the unstripped gas parasitic reaction, unstripped gas utilising efficiency height, (especially the III-nitride material comprises AlN to the high preparation semiconductor epitaxial material of growth velocity, GaN and InN and their alloy cpd) the atomic layer chemical vapour deposition epitaxial growth method.
Background technology
Chemical vapour deposition technique (Chemical Vapor phaseDeposition is called for short CVD) is a kind of important epitaxial growth of semiconductor material growth deposition technique, its principle be will sedimentary metal or nonmetallic volatile compound on the substrate of heating, decompose or reduction, thereby on the surface of substrate precipitating metal, metal and compound semiconductor etc.The development of CVD and production answer the needs of low dimension semiconductor device architecture material epitaxy growth to grow up.It is mainly by being conveyed into approach that reaction chamber carries out angry phase chemistry reaction of hybrid concurrency and the surface reaction solid film material of growing to the source of volatile compound and other component (mainly being hydride) on substrate.
Molecular beam epitaxy (Molecular Beam Epitaxy is called for short MBE) is the technology of the preparation single or multiple lift monocrystal thin films as thin as a wafer that grows up on the basis of vacuum-evaporation.The principle of MBE is under UHV condition, constitutes each component of crystalline and foreign atom (molecule) with certain heat movement speed, be ejected on the substrate surface of heat and carry out crystal epitaxy according to a certain percentage.The characteristics of MBE are that the speed of growth slow (approximate 1 micron/hour), growth temperature are low.Utilize the MBE method can arbitrarily change the component and the doping of epitaxial film, not only can in atomic scale, accurately control the thickness of epitaxial film, can also be in atomic scale inner control heterojunction boundary planeness and dopant profiles.The advantage of the maximum of MBE is that it has multiple detection means on the throne, can be in the process of growth the process of growth of original position research epitaxial surface, and can do various surface analyses such as high energy electron diffraction, low-energy electron diffraction, four-electrode spectrum.
Atomic layer epitaxy (Atomic Layer Epitaxy is called for short ALE) and two kinds of technology of migration enhanced epitaxy (Migration Enhanced Epitaxy is called for short MEE) are deriving technologies of MBE.The principle of these two kinds of epitaxy methods all is alternately to throw to the substrate pulse participating in epitaxially grown atom (molecule) bundle, (perhaps not having) certain time interval is arranged between two pulses, make extension can be strictly connect the growth of one deck ground by growth rhythm one deck of monoatomic layer or unimolecular layer.Therefore, the planeness on ALE and the easier control epitaxial material of MEE method surface.
(Metal organic chemicalvapor phase deposition MOCVD) is a kind of novel vapour phase epitaxial growth technology that grows up to the Organometallic chemical vapor deposition on the basis of CVD.It adopts III family, the organic compound of II family element and the hydride of V group element etc. as the crystal growth raw material, on substrate, carry out vapour phase epitaxy in the pyrolysis mode, the thin film layer monocrystal material of grow various III-V family, II-VI compound semiconductor and their multivariate solid solution.General MOCVD equipment all is made of source supply system, gas transport and flow control system, reaction chamber and temperature controlling system, vent gas treatment and safety precaution and GA gas alarm system.Compare with the CVD of routine, MOCVD has series of advantages.Extensive such as the scope of application, almost can grow all compounds and alloy semiconductor; Various heterogeneous structure materials are very suitable for growing; Can the grow ultra-thin epitaxial film, and can obtain very steep interface structure; Growth is easy to control; The material with very high purity of can growing; The epitaxial film large-area uniformity is good; Can carry out scale operation.
Compare with MBE, MOCVD not only has the superthin layer that MBE can carry out, the epitaxially grown ability in steep interface, but also have equipment simple, easy to operate, be convenient to characteristics such as scale operation, thereby have bigger practical value than MBE.
The development trend of MOCVD is by the supply mode that changes source gas or the suspension and the rotation of substrate, realizes the computer control production of big area, in enormous quantities, high uniformity and precipitous transition interface layer.
Nineteen sixty-eight, the years such as H.M.Manasevit of U.S. Rockwell International have at first proposed a kind of method for preparing compound semiconductor thin layer single crystal film, i.e. the MOCVD method.MOCVD has nearly 30 years applicating history, and its performance has been updated and be perfect.The greatest advance that MOCVD obtains in recent years is that the hydromechanical principle of utilization realizes the substrate rotation in the process of growth, thereby has improved the homogeneity of growth greatly.Mainly be with reference to halogenide, hydride vapor-phase epitaxy Study on Technology achievement, epitaxy be controlled at the mass transport condition get off to carry out that the control air-flow is a laminar flow, keeps stable frictional belt.Adopted technology such as high flow rate, low pressure, pedestal rotation for this reason, and the structure of reaction chamber and pedestal has been improved.
The people such as Suchtelen of Holland Nijmegen university have designed a kind of efficient, high uniformity, action of low-voltage pulse MOCVD reactor.It is made up of configuration quick electromagnetic valve and vacuum pump on the conventional MOCVD equipment.The characteristics of this system are that source gas is periodically introduced reaction chamber.After gas entered reaction chamber, the pressure of reaction chamber can increase suddenly, a spike occurs, and this is a kind of temperature equilibrium phenomenon.The process in each cycle is: at first gas mixing chamber is vacuumized, and simultaneously reaction chamber is vacuumized by source gas arsine (AsH3), trimethyl-gallium (TMG) etc., open switch, mixed gas is entered, through reaction back combustion gas, growth cycle finishes.In each cycle, chemical composition can be chosen arbitrarily, and growth thickness is adjusted arbitrarily from 1～30 atomic shell.Because in process of growth, the source gas molecule only arrives substrate surface by diffusion, not relative substrate flow.So overcome the gas " depletion effect " that produces in traditional flow reactor.The advantage of this reactor is to have improved the homogeneity of epitaxial film component and thickness; Use source gas expeditiously; The atom level of growing abrupt interface epitaxial film; Whole process available computers control is produced in batches.
In addition, the P.M.Frijlink of French Applied Physics electronic experiment chamber has designed a kind of multi-functional large-sized MOCVD reactor, can make big area, chemical component in enormous quantities and thickness utmost point homogeneous high purity epitaxial film.The feature of this reactor is, utilizes hydrogen stream that main substrate holder and 7 sub-substrate holder are suspended and rotates new technology, and 72 inches substrates on the substrate holder are rotated, and avoided any physics contact between substrate and the epitaxial system.This reactor is ignored fringing effect, and 2 inches GaAs epitaxy layer thickness and uniform doping＜± 1% have been realized the even epitaxy of high two-dimensional electron gas mobility, and 1.5K can obtain the mobility of 720000cm2/V.s down.
The CVD equipment that is used for thin film epitaxy mainly contains horizontal and rectilinear two big classes.If the parasitic reaction between the raw material is more serious, then should adopt rectilinear reactor.Rectilinear reactor mainly partly is made up of the fluffy head of air inlet, substrate bracket, rotation system, heating unit, vacuum system etc.In the prior art, even for guaranteeing film thickness, on the fluffy head of air inlet, evenly be furnished with many several jet sieve apertures usually, the different material gas phase is interlocked mutually, is fed in the reaction chamber simultaneously, makes substrate top gaseous component as far as possible evenly, thorough mixing before arriving substrate.But there is defective in the diffuser of this structure, because unstripped gas promptly mixes in course of conveying mutually, each other gas-phase chemical reaction can take place, thereby the parasitic reaction situation between the unstripped gas is very serious.The consequence of parasitic reaction is that raw material availability is low, film quality is poor.
In order to suppress the generation of parasitic reaction, the method that can adopt mainly contains: (1) strengthens the revolution of substrate bracket, shorten the time of flow of feed gas to the high temperature substrate holder, reduce the radiation heated time of unstripped gas in transport process, but it is stable that the increase revolution can influence mass transfer, the heat transfer boundary layer of deposition reaction, form eddy current, be unfavorable for film growth.(2) adopt intermittently air inlet, strengthen MOCVD (MEMOCVD) as pulse atomic layer epitaxy (PALE) and migration, by the valve switching different material gas is intermittently fed, unstripped gas staggers in time like this, near substrate the time, do not mix, suppressed the generation of parasitic reaction.The problem that this method exists is, because pipe resistance, portion gas remains in a standstill, and that part of unstripped gas of hysteresis still parasitic reaction can take place; For addressing this problem, there is the people between unstripped gas switches, to introduce carrier gas and purges, just reduced film deposition rate but do like this, reduced plant factor.
Summary of the invention
The device and method that the purpose of this invention is to provide a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth, it is the advantage of having concentrated MOCVD equipment and MBE equipment, realize by " spatial modulation " technology, can avoid taking place between the unstripped gas that parasitic reaction, unstripped gas utilising efficiency height, growth velocity are big, the atomic layer chemical vapour deposition epitaxial growth method of preparation semiconductor epitaxial material (especially the III-nitride material comprises AlN, GaN and InN and their alloy cpd).Adopt this method can in the MOCVD system just as the thickness of in the MBE system, in atomic scale, accurately controlling epitaxial film, control heterojunction boundary planeness and dopant profiles, can also improve film quality and growth velocity effectively, have the potentiality of scale operation.
The device of a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth of the present invention is characterized in that, comprising:
The fluffy head of one air inlet, the fluffy head of this air inlet is barrel-shaped, is divided into a plurality of districts in the fluffy head of this air inlet, each district all is the inlet nozzle of unstripped gas;
One pedestal, this pedestal is a column, is manufactured with a plurality of circular grooves above this pedestal, and this circular groove is in order to place substrate, and the diameter of this pedestal is less than or equal to the diameter of the fluffy head of air inlet, and this pedestal can rotate;
Wherein the fluffy head of air inlet is positioned at the side that pedestal has the surface of circular groove, is separated with a distance mutually between the fluffy head of this air inlet and the pedestal, and an end of the nearly pedestal of the fluffy head rest of this air inlet is a pneumatic outlet, is the gas inlet away from the other end of pedestal.
The a plurality of districts that are divided in the fluffy head of wherein said air inlet are 2-10 districts.
The distance of being separated by between fluffy head of wherein said air inlet and the pedestal is 0.1-20 centimetres.
The number of the circular groove of making above of wherein said pedestal is more than or equal to 1.
The speed of rotation of wherein said pedestal is 0-3000 rpm.
Each district of the fluffy head of wherein said air inlet is the inlet nozzle of unstripped gas, and the shape of spout is circular, tetragon or fan-shaped;
Wherein said each spout is subdivided into a plurality of holes as required, is used for uniform distribution unstripped gas in limited spatial dimension.
The fluffy head of wherein said air inlet feeds the unstripped gas of difference or identical type, the time independent control of the size of its flow, break-make respectively at synchronization.
The method of a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth of the present invention, this growth method are to adopt the described device of claim 1, it is characterized in that, comprising following steps:
Step 1: the substrate of epitaxial material that will be to be grown is placed in the circular groove above the pedestal;
Step 2: pedestal is heated to the material epitaxy needed temperature of growing;
Step 3: the speed according to setting that rotating basis, this rotating basis drive in the groove that is placed on pedestal is rotated around central shaft;
Step 4: feed different or identical reactant gases in a plurality of districts in the fluffy head of air inlet;
Step 5: be placed on substrate in the groove of pedestal under the drive of pedestal through the zone that gas covered that the subregion of the fluffy head of the air inlet of associating feeds, deposit growth one deck subregion feeds on substrate pairing atom of gas or molecule;
Step 6: repeating step 4,5, till satisfying predetermined material growth requirement.
The present invention is a kind of atomic layer chemical vapour deposition epitaxial growth method that realizes by " spatial modulation " technology.One of two main gordian techniquies that realize this method are the fluffy heads of reaction chamber air inlet in a plurality of districts of branch, and each district of the fluffy head of air inlet all is provided with tuyere, are separate, equivalent equivalence on function.The fluffy head of this sectional air inlet is the key of implementation space modulation atomic layer chemical vapour deposition; To be substrate enter the zone that the different material gas of reaction chamber covers respectively through each independent partitions of the fluffy head of the air inlet of associating by rotation to the another one technology successively, thereby different types of atom (molecule) is deposited on substrate last layer one deck ground by the precedence that configures, realize the growth on substrate material of thin-film material.
Description of drawings
For further specifying concrete technology contents of the present invention, below in conjunction with embodiment and accompanying drawing describes in detail as after, wherein:
Fig. 1 is a structural representation of the present invention.
Embodiment
See also shown in Figure 1ly, the device of a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth of the present invention is characterized in that, comprising:
Fluffy 11 of one air inlet, fluffy 11 of this air inlet is barrel-shaped, be divided into a plurality of districts 14-17 (showing 4 districts among the figure) in fluffy 11 of this air inlet, each district all is the inlet nozzle of unstripped gas, the shape of this spout is circular, tetragon or fan-shaped, wherein said each spout is subdivided into a plurality of holes (figure do not show) as required, is used for uniform distribution unstripped gas in limited spatial dimension, and a plurality of districts in fluffy 11 of this air inlet are 2-10 districts;
One pedestal 21, this pedestal 21 is a column, be manufactured with a plurality of circular groove 22-24 (showing among the figure that circular groove is 3) above this pedestal 21, the number of this circular groove is more than or equal to 1, this circular groove 22-24 is in order to place substrate, the diameter of this pedestal 21 is less than or equal to the diameter of fluffy 11 of air inlet, and this pedestal 21 can rotate, and speed of rotation is 0-3000 rpm;
Wherein fluffy 11 of air inlet is positioned at the side that pedestal 21 has the surface of circular groove 22-24, be separated with a distance mutually between fluffy 11 of this air inlet and the pedestal 21, this distance is 0.1-20 centimetres, fluffy 11 of this air inlet is pneumatic outlet near an end of pedestal 21, is the gas inlet away from the other end of pedestal 21.
Fluffy 11 of wherein said air inlet feeds the unstripped gas of difference or identical type, the time independent control of the size of its flow, break-make respectively at synchronization.
Please again in conjunction with consulting Fig. 1, the method for a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth of the present invention, this growth method are to adopt the described device of claim 1, it is characterized in that, comprising following steps:
Step 1: the substrate of epitaxial material that will be to be grown is placed in the circular groove 22-24 above the pedestal 21;
Step 2: pedestal 21 is heated to the material epitaxy needed temperature of growing;
Step 3: rotating basis 21, this rotating basis 21 drives rotating around central shaft 31 according to the speed of setting among the groove 22-24 that is placed on pedestal 21;
Step 4: feed different or identical reactant gases among a plurality of district 14-17 in fluffy 11 of air inlet;
Step 5: be placed on substrate in the groove 22 of pedestal 21 under the drive of pedestal 21 through the zone that gas covered that the subregion 14-17 of fluffy 11 of the air inlet of associating feeds, deposit growth one deck subregion 14-17 feeds on substrate pairing atom of gas or molecule;
Step 6: repeating step 4,5, till satisfying predetermined material growth requirement.
Example
Different with the fluffy head of traditional air inlet, the fluffy head of sectional air inlet mainly is made up of the barrel-shaped parts 11 of a hollow.The barrel-shaped district 14,15,16 and 17 that is divided into four separate, equivalent equivalences of being cut apart by two dividing plates 12 and 13.The function in each district in these four districts is all identical with fluffy of traditional air inlet.That is to say the needed various unstripped gas of can transfer material from each district growing.And, feed identical unstripped gas simultaneously in four subregions, perhaps feed the unstripped gas that has nothing in common with each other simultaneously.
With the very serious aluminium nitride (AlN) of growth parasitic reaction is example.In the process of growth, fluffy 11 of air inlet shown in Figure 1 can followingly distribute.Subregion 14 logical trimethyl aluminiums (TMAl), subregion 16 logical ammonia (NH
3), subregion 15 and subregion 17 all lead to carrier gas (hydrogen H
2Perhaps nitrogen N
2).The TMAl and the NH that import of subregion 14 and subregion 16 wherein
3Be the unstripped gas of the indispensability of growing AIN, and the H that subregion 15 and subregion 17 import
2Perhaps N
2Major function be to be used for spatially the NH of the TMAl of subregion 14 and subregion 16
3Separately, avoid the two before arriving substrate, to react, and then avoid the generation of parasitic reaction, improve the utilising efficiency of unstripped gas, improve the quality of the material of growth with regard to mutual mixing.
Because TMAl and NH
3Spatially separate, the chance that does not react each other carries out introducing another technology so material is grown, i.e. the substrate rotation technique smoothly.Pedestal 21 is a kind of pedestals that can put three substrates simultaneously among Fig. 1.Pedestal 21 is made up of the main body of a tubbiness, has dug three groove 22-24 that are used for laying substrate slice on the top of main body.Pedestal 21 is positioned at air outlet one side of fluffy 11 of the air inlet that is divided into a plurality of districts as shown in Figure 1 in reaction chamber.Can maintain a certain distance between fluffy 11 of air inlet and the pedestal 21, be beneficial to improve the homogeneity of growth.Fluffy 11 of air inlet is actionless in process of growth, and pedestal 21 rotates.The rotation 21 carrying be placed in groove 22,23 and 24 substrate slice rotate with certain speed along its axle center 31.
The growth of material is to carry out with the principle of a kind of ALE of being similar to or MEE method.Detailed process is such: at first reaction chamber is stabilized in material earlier and grows under the needed temperature and pressure condition; Then, the pedestal 21 of rotation is carrying TMAl, the H that the substrate that is placed in groove 22,23 and 24 can be successively imports respectively by the subregion 14,15,16 and 17 from fluffy 11 of sectional air inlet
2, NH
3, H
2The area of space that covers or be full of.When leading to the subregion 14 of TMAl, the process of the substrate in the groove 22 can deposit one deck Al.Then the substrate in the groove 22 can be through logical H
2Subregion 15, the Al atom can fully move at substrate surface in this process; Can be with the substrate in the rearward recess 22 through logical NH
3The space that covered of subregion 16.In this process, previous sedimentary Al atomic shell and N+ ion can react and generate AlN on the substrate.At last, the substrate of 22 kinds of grooves will be through logical H
2Subregion 17.This process can make the N+ ion fully move at substrate surface.Meanwhile, the substrate in groove 23 and the groove 24 is the process that substrate lived through in repeating groove 22 also, and making also can the same last layer AlN that grows with the substrate in the groove 22 above the substrate in these two grooves.Such process is gone round and begun again, and constantly repeats, and final AlN material just can realize that one deck Al atom, one deck N are grown in above the substrate slice of being laid among the pedestal 21 groove 22-24 atomically.
Substrate among the pedestal 21 groove 22-24 recited above is successively through each zone that 14-17 covered, district of fluffy 11 of divisional air admission, realizes that differing molecular (or atom) is exactly foregoing " space-modulating atomic layer chemical vapour deposition " growth technology by the method that both definite sequences is grown in above the substrate layer by layer.Adopt after this spatial modulation growth technology, can in the CVD system, as in the MBE system, realize atomic shell (perhaps migration strengthens) the deposit growth of material.
Because the technique scheme utilization, the advantage that the space-modulating atomic layer chemical vapour deposition growth method compared with prior art has is:
1, compares with traditional atomic layer epitaxy (perhaps migration enhanced epitaxy) growth method, the space-modulating atomic layer epitaxy is spatially isolated containing not the unstripped gas of homoatomic (molecule), good in different spatial distributions in advance, allow then the pedestal 21 of substrate by rotation by both definite sequences successively through containing each space of different material gas, thereby realize that not homoatomic or molecule grow respectively on substrate last layer one deck ground.In whole growth process, unstripped gas can be in opening state always.Traditional atomic shell (migration strengthens) extension then is to realize successively growing of monoatomic layer by synthetic method of time.Just adopt the mode of pulse, in first time period, first kind of unstripped gas opened, import reaction chamber.Reach after the given time, first kind of unstripped gas closed, reaction chamber carries out emptying, and first kind of unstripped gas rinsed well.Then, second kind of unstripped gas opened, imported reaction chamber.After reaching given time, again second kind of unstripped gas closed, the emptying reaction chamber is opened first kind of unstripped gas again.So go round and begin again, realize the growth of material.So, traditional atomic shell (migration strengthens) epitaxy is by staggering around time first kind and second kind unstripped gas importing reaction chamber, the mode that makes them enter reaction chamber in the different time periods realizes, also can be described as by " time modulation " technology and realizes.The shortcoming of this " time modulation " technology is will ceaselessly switch between the unstripped gas, and reaction chamber is also wanted emptying and flushing, thereby the growth velocity of material is very low." spatial modulation " atomic layer epitaxial growth technique does not then have between the unstripped gas frequent the switching and process that the continuous emptying of reaction chamber is washed, thereby can shorten the time that material epitaxy is grown to a great extent, increase work efficiency greatly, improve the growth velocity of material.
2, because fluffy 11 of the air inlet of " spatial modulation " atomic-layer epitaxial growth system is divided into several relatively independent regional 14-17, form separate air inlet unit, different types of unstripped gas is spatially isolated, thereby avoided unstripped gas mixing each other, eliminate parasitic reaction, improved film quality; On the other hand, because each unstripped gas independently participates in reaction separately, can conveniently realize film modulation doping technology;
3, owing to adopt the aforementioned techniques scheme, parasitic reaction between the unstripped gas is suppressed, make the speed of rotation of substrate pedestal 21 freely to regulate and control, utilize rotating speed to adjust the time length of substrate certain unstripped gas of contact in certain zone, thereby realize the deposition of monoatomic layer or polyatom layer film, film surface is difficult for forming cluster or big island.Film dislocation and room be can reduce like this, film crystal quality and mobility improved;
4, because fluffy 11 of air inlet is divided into several relatively independent zones, unstripped gas feeds in the reaction chamber from each subregion of fluffy head, thereby can in the subregion between two kinds of unstripped gass, feed carrier gas, be used for isolating two kinds of unstripped gass that parasitic reaction may take place, to guarantee to avoid the generation of parasitic reaction between the unstripped gas.Simultaneously, by the kind and the flow of control carrier gas, the desorption rate of control film in different zones can improve the film surface reaction conditions, improves thin film surface planeness, the superthin layer that acquisition has abrupt interface, control growth for Thin Film speed.
Core of the present invention is a material outgrowth device and growth method.This device comprises fluffy 11 of an air inlet.Fluffy 11 of this reaction chamber air inlet is divided into a plurality of districts, and each district all is the inlet nozzle of unstripped gas; Be incorporated into the design of air pipe, under meter, switch valve, each subregion is separate, equivalent equivalence on function.The time that is to say size, the ventilation of air inlet kind, the gas flow in each district all is the independent control that requires according to the material growth; This device also comprises a substrate pedestal 21 in addition.Pedestal 21 is used for carrying the substrate that growth material is used, and has rotation and heating function simultaneously.Under the drive of rotating basis 21, substrate passes through successively according to sequencing below the inlet nozzle of fluffy 11 each independent subregion 14-17 of air inlet.In addition, this device also comprises a cavity that can hold fluffy 11 of rotating basis 21 and air inlet.This cavity is from the pedestal 21 of fluffy 11 reactant gases of coming in of air inlet, rotation with place substrate base and air outside on the pedestal 21 to keep apart.
The growth method of material comprises the steps:
Pedestal in the reaction chamber 21 is heated to the temperature of material growth needs, makes the speed rotation of pedestal 21 simultaneously to set;
Open air intake valve, make reactant gases enter reaction chamber, the state that each district all is in opening state always or switches for continuous switch through each independent partitions 14-17 of fluffy 11 of air inlet;
Feed the used various unstripped gass of growth material, wherein, the unstripped gas that feeds among fluffy 11 each district 14-17 of air inlet has nothing in common with each other or is identical;
Substrate under the drive of rotating basis 21 below first subregion 14 of fluffy 11 of air inlet the time, the unstripped gas that subregion 14 feeds decomposes at substrate surface, absorption or reaction, deposits contained atom or the molecule of one deck this kind unstripped gas at substrate surface;
Substrate can in the time of below sectional through 15,16,17, deposit pairing atom of unstripped gas or the molecule that is feeding in last 15,16,17 subregions successively successively through districts such as 15,16,17 subregions on the substrate;
In a manner mentioned above, substrate again and again under the drive of rotating basis 21 below fluffy 11 of the air inlet of multi-division process.In this process, substrate passes through corresponding atom of following and deposition growing or the molecular layer of a plurality of subregion 14-17 of fluffy 11 of air inlet successively, finally realizes the atomic-layer epitaxial growth of material film.
Embodiment one: shown in accompanying drawing 1, and the reaction chamber structure synoptic diagram of a kind of space-modulating atomic layer chemical vapour deposition system.Fluffy 11 of the air inlet and one that comprises a multi-division 14,15,16 and 17 can rotate, above dig the pedestal 21 that fluted 22-24 can place substrate, and one hold rotating basis and the fluffy head of air inlet, the cavity of reactant gases and air insulated.
Make use-case one: the reaction chamber structure that adopts embodiment one, when the thin film deposition of preparation high-crystal quality zinc oxide (ZnO), a kind of unstripped gas zinc ethyl enters through subregion 14 from inlet pipe, another kind of unstripped gas oxygen enters through subregion 16 from inlet pipe, and the carrier gas argon gas enters through subregion 15 and 17 from inlet pipe.Unstripped gas zinc ethyl and oxygen independently transport near the substrate process separately like this, do not mix, even be heated also can not react each other (parasitic reaction).(the zinc ethyl quadrant is meant the zone below the subregion 14 when each regional quadrant of substrate rotation process unstripped gas, the oxygen quadrant is meant the zone below the subregion 16), single raw material only participates in substrate surface film growth reaction, remaining raw material will be taken away by the carrier gas of next quadrant, can not enter next unstripped gas quadrant, the parasitic reaction that so can suppress the substrate top greatly improves the zinc-oxide film crystal mass.
Make use-case two: adopt embodiment one reaction chamber structure, when the thin film deposition of preparation high-crystal quality aluminium nitride (AlN), unstripped gas trimethyl aluminium (or triethyl aluminum) enters through subregion 14 from inlet pipe, the unstripped gas ammonia enters through subregion 16 from inlet pipe, and carrier gas hydrogen enters through subregion 15 and 17 from inlet pipe.Unstripped gas trimethyl aluminium and ammonia independently transport near the substrate process separately, do not mix each other before arriving substrate, and parasitic reaction ([Al (CH does not take place when being heated
3)
2: NH
2] the n polyreaction); In addition, film surface contacts different material gas successively, has improved the surface mobility of aluminium atom, and the dislocation desity in the film reduces greatly, and the aluminium nitride film crystal mass that obtains can be than higher, and X-ray diffraction half-breadth (102 face) can be less than 300 seconds.
Make use-case three: adopt embodiment one reaction chamber structure, when the thin film deposition of preparation high mobility gan (GaN), unstripped gas trimethyl-gallium (or triethyl-gallium) enters through subregion 14 from inlet pipe, the unstripped gas ammonia enters through subregion 16 from inlet pipe, and carrier gas hydrogen enters through subregion 15 and district 17 from inlet pipe.Unstripped gas trimethyl-gallium and ammonia independently transport near the substrate process separately, and parasitic reaction does not take place when being heated, and parasitic reaction product or intermediate product can not introduced film.Therefore, the defect concentration of film can reduce greatly, and the gallium nitride film mobility that obtains can be greater than 1000cm
2/ VS.
Make use-case four: the reaction chamber structure that adopts embodiment one, when aluminium indium gallium nitrogen (AlInGaN) the quaternary component membrane structure of preparation thickness and the accurate control of component, unstripped gas trimethyl indium, trimethyl aluminium and trimethyl-gallium enter from subregion 14, carrier gas hydrogen enters through subregion 15 and 17 from inlet pipe, and the unstripped gas ammonia enters through subregion 16 from inlet pipe.Easily the unstripped gas trimethyl aluminium that parasitic reaction takes place does not mix with the unstripped gas ammonia in transport process, parasitic reaction can not take place, and can improve aluminium indium gallium nitrogen (AlInGaN) film crystal quality greatly.
Make use-case five: the reaction chamber structure that adopts embodiment one, when preparation has indium gallium nitrogen/gan (InGaN/GaN) multiple quantum trap deposition at steep interface, unstripped gas trimethyl-gallium and trimethyl indium enter through subregion 14 from inlet pipe, the unstripped gas ammonia enters through subregion 16 from inlet pipe, and carrier gas nitrogen enters through subregion 15 and 17 from inlet pipe.Unstripped gas trimethyl-gallium (or trimethyl indium) does not mix with ammonia in transport process, parasitic reaction can not take place; Because the superthin layer deposition is after the overload air-blowing is swept, desorption can take place in film under the carrier gas atmosphere, has suppressed the segregation of indium component, and the indium gallium nitrogen luminescent quantum dot component that obtains is even, size is little, forms multiple quantum trap (InGaN/GaNMQWs) active layer at steep interface.
The invention discloses a kind of space-modulating atomic layer chemical vapour deposition epitaxial growth method.The realization of this method mainly relies on the employing of two kinds of technology.First kind is fluffy 11 of the air inlet of multi-division, can spatially keep apart different types of unstripped gas, avoids the reaction between the unstripped gas; Second kind is the substrate pedestal 21 of rotation.Substrate pedestal 21 can carry substrate and together rotate, and makes the substrate area of space by different material gas place successively, thus on substrate by a graded needed material of growing layer by layer.The combination of these two kinds of technology can realize the high growth rates atomic-layer epitaxial growth in the CVD system.The inventive method is passed through separately independently air inlet subregion realization to the inhibition of unstripped gas parasitic reaction, thereby improves the quality and the growth velocity of film.
Claims (9)
1, a kind of device of space-modulating atomic layer chemical vapour deposition epitaxial growth is characterized in that, comprising:
The fluffy head of one air inlet, the fluffy head of this air inlet is barrel-shaped, is divided into a plurality of districts in the fluffy head of this air inlet, each district all is the inlet nozzle of unstripped gas;
One pedestal, this pedestal is a column, is manufactured with a plurality of circular grooves above this pedestal, and this circular groove is in order to place substrate, and the diameter of this pedestal is less than or equal to the diameter of the fluffy head of air inlet, and this pedestal can rotate;
Wherein the fluffy head of air inlet is positioned at the side that pedestal has the surface of circular groove, is separated with a distance mutually between the fluffy head of this air inlet and the pedestal, and an end of the nearly pedestal of the fluffy head rest of this air inlet is a pneumatic outlet, is the gas inlet away from the other end of pedestal.
2, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 1 is characterized in that, a plurality of districts that are divided in the fluffy head of wherein said air inlet are 2-10 districts.
3, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 1 is characterized in that, the distance of being separated by between fluffy head of wherein said air inlet and the pedestal is 0.1-20 centimetres.
4, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 1 is characterized in that, the number of the circular groove of making above of wherein said pedestal is more than or equal to 1.
5, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 1 is characterized in that, the speed of rotation of wherein said pedestal is 0-3000 rpm.
6, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 1 is characterized in that, each district of the fluffy head of wherein said air inlet is the inlet nozzle of unstripped gas, and the shape of spout is circular, tetragon or fan-shaped;
7, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 6 is characterized in that, wherein said each spout is subdivided into a plurality of holes as required, is used for uniform distribution unstripped gas in limited spatial dimension.
8, the device of space-modulating atomic layer chemical vapour deposition epitaxial growth according to claim 1, it is characterized in that, the fluffy head of wherein said air inlet feeds the unstripped gas of difference or identical type, the time independent control of the size of its flow, break-make respectively at synchronization.
9, a kind of method of space-modulating atomic layer chemical vapour deposition epitaxial growth, this growth method are to adopt the described device of claim 1, it is characterized in that, comprising following steps:
Step 1: the substrate of epitaxial material that will be to be grown is placed in the circular groove above the pedestal;
Step 2: pedestal is heated to the material epitaxy needed temperature of growing;
Step 3: the speed according to setting that rotating basis, this rotating basis drive in the groove that is placed on pedestal is rotated around central shaft;
Step 4: feed different or identical reactant gases in a plurality of districts in the fluffy head of air inlet;
Step 5: be placed on substrate in the groove of pedestal under the drive of pedestal through the zone that gas covered that the subregion of the fluffy head of the air inlet of associating feeds, deposit growth one deck subregion feeds on substrate pairing atom of gas or molecule;
Step 6: repeating step 4,5, till satisfying predetermined material growth requirement.
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| CNA2007101782824A CN101445955A (en) | 2007-11-28 | 2007-11-28 | Device for space-modulating atomic layer chemical vapour deposition epitaxial growth and method thereof |
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| CNA2007101782824A CN101445955A (en) | 2007-11-28 | 2007-11-28 | Device for space-modulating atomic layer chemical vapour deposition epitaxial growth and method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205733A (en) * | 2013-04-27 | 2013-07-17 | 南昌黄绿照明有限公司 | Vertical airflow type MOCVD (Metal-organic Chemical Vapor Deposition) spray head device with multiple gas mixing chambers |
| CN104280280A (en) * | 2014-10-13 | 2015-01-14 | 赵烨梁 | Device for preparing unimolecular sample by microleakage sample injection method |
| CN108362721A (en) * | 2018-01-16 | 2018-08-03 | 长春理工大学 | A kind of device and method of in-situ monitoring ALD deposition thin-film material quality |
| CN109576784A (en) * | 2017-09-29 | 2019-04-05 | 上海新昇半导体科技有限公司 | A kind of preparation method and device of SiC epitaxial layer |
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2007
- 2007-11-28 CN CNA2007101782824A patent/CN101445955A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205733A (en) * | 2013-04-27 | 2013-07-17 | 南昌黄绿照明有限公司 | Vertical airflow type MOCVD (Metal-organic Chemical Vapor Deposition) spray head device with multiple gas mixing chambers |
| CN104280280A (en) * | 2014-10-13 | 2015-01-14 | 赵烨梁 | Device for preparing unimolecular sample by microleakage sample injection method |
| CN109576784A (en) * | 2017-09-29 | 2019-04-05 | 上海新昇半导体科技有限公司 | A kind of preparation method and device of SiC epitaxial layer |
| CN108362721A (en) * | 2018-01-16 | 2018-08-03 | 长春理工大学 | A kind of device and method of in-situ monitoring ALD deposition thin-film material quality |
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Open date: 20090603 |