CN101017864A - Silicon base covariant underlay with the ultrathin carbon silicon middle layer and its preparing method - Google Patents
Silicon base covariant underlay with the ultrathin carbon silicon middle layer and its preparing method Download PDFInfo
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Abstract
The silicon-base coviant substrate with ultrathin SiC intermediate layer comprises: from bottom to top, a silicon substrate for support, a ultrathin 3C-SiC intermediate layer for mismatch strain coordination, and an extension layer with much lattice mismatch with the substrate.
Description
Technical field
The present invention relates to technical field of semiconductors, refer in particular to a kind of silicon based compliant substrate that utilizes the preparation of ion beam epitaxy equipment with ultra-thin carborundum intermediate layer.
Background technology
Quality better, price are low except that having for silicon (Si), large scale, device technology is ripe and can be integrated etc. the advantage, also have good heat conduction, conductive characteristic, the substrate that therefore often is used as big mismatch heterogeneous structure material zinc oxide (ZnO), gallium nitride (GaN) and the growth of aluminium nitride (AlN) homepitaxy uses.Owing to there is the influence of big lattice mismatch and thermal expansion coefficient difference and surface chemistry problem, direct growth is difficult to achieve satisfactory results.Adopting the substrate preparation technology is the main means that solve big mismatch epitaxial problem, promptly make substrate be more suitable for heteroepitaxial growth by crystal structure, physics and the chemical property that changes substrate surface, but as conventional buffer layer technology, routine covariant (flexibility) substrate technology and graph substrate technology etc.Though carried out many trials, yet existing various substrate preparation technology is difficult to fundamentally to solve the big mismatch problems of above-mentioned important wide bandgap compound semiconductors material, causes its commercial applications and popularization to be subjected to greatly restriction and influence always.Therefore, continuing the new substrate preparation technology of development remains big mismatch heterogeneous structure material and prepares important topic in the increment study.
In recent years the conventional buffer layer technology and based on " no support substrates " but but but developed a kind of new covariant substrate technology that is called as ultra-thin intermediate layer covariant substrate on the basis of the routine covariant substrate technology of model again.Promptly introduce the ultra-thin intermediate layer of satisfying certain condition between substrate in a certain mismatch epitaxial system and the epitaxial loayer, but and just call ultra-thin intermediate layer covariant substrate comprising substrate with the ultra-thin intermediate layer of misfit strain coordinative role strong bonding.Roll up in the 9th phase scientific paper of 1740 pages by " semiconductor journal " the 26th being published in 2005 for people such as Chen Yonghai, utilize " the ultra-thin intermediate layer substrate " model that is proposed that the misfit strain mechanism of action of the mismatch epitaxial system in the ultra-thin intermediate layer of introducing strong bonding has been carried out systematically theoretic discussion and analysis, but and provided the primary condition that the ultra-thin intermediate layer of ideal covariant should be satisfied: the lattice mismatch opposite in sign between (1) and support substrates and the epitaxial loayer, promptly one positive one is negative or one negative one just, and with support substrates and epitaxial loayer better lattice match relation is arranged all as far as possible; (2) thin as far as possible, preferably less than the minimum critical thickness between itself and substrate and the epitaxial loayer, and smooth surface is smooth.In addition, consider actual epitaxial growth situation, also should meet following condition as far as possible: (3) have good heat, chemical stability.Be difficult for substrate and epitaxial loayer between generation interfacial chemical reaction or have the chemical composition counterdiffusion, cause the misfit strain coordinative role in intermediate layer to weaken or lose; (4) with the material of conventional semiconductor technical compatibility; (5) preparation technology is simple, low-cost.But this both provided basic theoretical foundation and guidance for the selection and the preparation in the ultra-thin intermediate layer of covariant, also some experimental results of utilizing ultra-thin intermediate layer to solve big mismatch epitaxial problem had been given to explain.Such as, the calendar year 2001 breadboard researcher of U.S. Motorola is to have the thick ultra-thin SrTiO of 12nm of mismatch (3.2%) greatly with the GaAs epitaxial loayer
3For the preparation growth on the Si substrate of intermediate layer success obtains large scale GaAs thin-film material near zero dislocations density, and before this, many people attempt with the GaAs epitaxial loayer the ultra-thin Ge or the Ge of better matching relationship (0.1%) to be arranged
xSi
1-xFor but all preparing growth on the Si substrate, the intermediate layer do not obtain gratifying GaAs thin-film material.This is because SrTiO
3The lattice mismatch of intermediate layer and Si substrate and GaAs epitaxial loayer is respectively-1.6% and 3.2%, and symbol one negative just and only has 12nm thick, but meets the primary condition in the ultra-thin intermediate layer of covariant, and Ge or Ge
xSi
1-xFor the lattice mismatch of intermediate layer and Si substrate and GaAs epitaxial loayer is respectively-4.0% and-0.1%, symbol all is negative, but does not meet the primary condition in the ultra-thin intermediate layer of covariant, therefore is difficult to obtain very desired result.As seen, but how selecting to meet the ultra-thin intermediate layer of the ultra-thin intermediate layer of covariant primary condition, is the important prerequisite that realizes the big mismatch epitaxial floor height mass growth on the Si substrate.Compare original various based on " no support substrates " but the routine covariant substrate of theoretical model, but the preparation technology of the ultra-thin intermediate layer of this class covariant substrate is simple, good reproducibility and low cost, but only just can obtain the covariant layer that crystalline quality is good and smooth surface is smooth by simple superthin layer growth, inject chemical reduction technology with nanoscale and need not complicated bonding techniques or energetic ion, also may avoid introducing contaminating impurity in the secondary epitaxy process.
For wide bandgap compound semiconductors material ZnO, GaN and AlN that preparation growth on the Si substrate has approximate lattice constant, but the ultra-thin intermediate layer of the 3C-SiC with cubic structure meets the primary condition in covariant intermediate layer, promptly the mismatch degree with the Si substrate is 3.68%, be respectively-5.40% ,-3.44% and-0.95% with the mismatch degree of ZnO, GaN and AlN epitaxial loayer, and the ultra-thin intermediate layer of 3C-SiC has good heat, chemical stability and thermal conduction characteristic, in addition, also with the Si based semiconductor device process compatible of maturation.Yet, present existing conventional SiC film preparation growth technique, as chemical vapor deposition (CVD), magnetron sputtering and plasma ion assisted deposition etc., all be difficult to realize the 3C-SiC film in the high-purity high-quality growth of the low temperature on the Si substrate (below 1000 ℃) ultra-thin (a few to tens of nanometers), but thereby the ultra-thin 3C-SiC of the Si base intermediate layer covariant substrate that can't obtain to have very high crystalline quality and smooth planar surface.Therefore, but the Si base covariant substrate preparation technology that develops new ultra-thin 3C-SiC intermediate layer has important Research Significance and practical value.
Summary of the invention
The objective of the invention is to, but provide a kind of covariant substrate, be meant a kind of silicon based compliant substrate that utilizes the preparation of ion beam epitaxy equipment especially with ultra-thin carborundum intermediate layer, utilize ion beam epitaxy equipment to realize the high-quality growth of ultra-thin 3C-SiC thin-film material on Si (111) substrate, for the epitaxial growth of big mismatch heterogeneous structure material zinc oxide, gallium nitride and aluminium nitride etc. provides a kind of silicon based compliant substrate with ultra-thin carborundum intermediate layer, and lay the foundation for developing novel opto-electronic device.
The technical scheme that technical solution problem of the present invention is adopted is:
A kind of silicon based compliant substrate with ultra-thin carborundum intermediate layer of the present invention is characterized in that, comprises following a few part:
One silicon substrate, this silicon substrate plays support;
One ultra-thin 3C-SiC intermediate layer, this ultra-thin 3C-SiC intermediate layer preparation plays misfit strain and coordinates, and constitute the silicon based compliant substrate with silicon substrate on silicon substrate;
One epitaxial loayer, this epitaxial loayer prepares on ultra-thin 3C-SiC intermediate layer, and has than Macrolattice mismatch with the bottom silicon substrate.
The thickness in wherein ultra-thin 3C-SiC intermediate layer is 5-30nm, and material is monocrystalline and polycrystal carborundum thin-film material.
The lattice mismatch opposite in sign of the lattice mismatch symbol between epitaxial loayer and the ultra-thin 3C-SiC intermediate layer and middle ultra-thin 3C-SiC intermediate layer and silicon substrate wherein, promptly one negative one just, and the lattice mismatch numerical value in epitaxial loayer and ultra-thin 3C-SiC intermediate layer is 0-10%.
Wherein the material of epitaxial loayer is: zinc oxide, gallium nitride, aluminium nitride and carborundum films material, those materials are to adopt magnetron sputtering, metal organic chemical vapor deposition, chemical vapour deposition (CVD), pulsed laser deposition, molecular beam epitaxy and the preparation of ion beam epitaxy method.
A kind of preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer of the present invention is characterized in that the preparation method comprises following steps:
Get a silicon substrate;
Adopt the method for ion beam epitaxy, the ultra-thin 3C-SiC of preparation intermediate layer on silicon substrate;
Adopt the method for magnetron sputtering, preparation one epitaxial loayer on ultra-thin 3C-SiC intermediate layer.
The preparation process in wherein ultra-thin 3C-SiC intermediate layer is as follows:
Step 1: select for use the not high argon gas of purity requirement to produce the ar-ion beam raw material that are used for substrate surface dry method sputter clean as low energy double-ion beam epitaxial device I beam ion source;
Step 2: select for use the not high CO (carbon monoxide converter) gas of purity requirement to produce the carbon ion beam raw material that are used for carborundum films preparation growth as low energy double-ion beam epitaxial device II beam ion source;
Step 3: Si (111) substrate is inserted low energy double-ion beam epitaxial device growth room;
Step 4: the vacuum of taking out low energy double-ion beam epitaxial device whole system;
Step 5: two ion sources are toasted degas;
Step 6: the silicon substrate in the growth room toasted degas and surperficial high temperature deoxidation treatment;
Step 7: the isotopically pure low energy ion beam bundle bombardment sputter dry method of utilizing low energy double-ion beam epitaxial device I bundle to produce is cleaned surface of silicon;
Step 8: the ar-ion beam of closing low energy double-ion beam epitaxial device I bundle;
Step 9: the isotopically pure low energy carbon ion beam that utilizes low energy double-ion beam epitaxial device II bundle to produce carries out the high-purity growth of low temperature in ultra-thin 3C-SiC intermediate layer 2 on Si (111) substrate.
Wherein toast the interior vacuum degree of preceding two ion sources that degas in the step 5 and reach 5-9 * 10
-4Pa, the temperature of baking heating is 120-300 ℃.
Wherein in the step 6 silicon substrate baking degas and surperficial high temperature deoxidation before the indoor vacuum degree of growth should reach 1-5 * 10
-5Pa, heating-up temperature is 750-850 ℃, time 20-30 minute.
The beam current density that wherein is used for the isotopically pure low energy ion beam bundle of surface of silicon bombardment sputter dry method cleaning in the step 7 should be 50-100 μ A/cm
2, the argon ion energy is 200-300eV, the dry method scavenging period is 2-5 minute.
The isotopically pure low energy carbon ion beam that wherein obtains in the step 9 is that the magnetic quadrupole lens device by adjusting the II bundle is controlled low energy carbon ion beam bundle shape of spot and the size that is deposited on the substrate with the magnetic field of auxiliary magnetic steering device and the electric field of electrostatic deflection electrodes device, and the scanning swing is with the uniformity that improves prepared carborundum films with increase to membrane area about the additional substrate low-angle.
Wherein the isotopically pure low energy carbon ion beam beam current density in the step 9 should be 50-100 μ A/cm
2, energy should be 20-100eV, and dosage should be 1-8 * 10
17Dose, growth temperature should be 700-800 ℃.
Wherein when preparation epitaxial loayer zinc-oxide film, should adopt 60-100W to exchange radio frequency sputtering power sputter purity is 99.99%-99.999% zinc oxide target, working gas argon gas and assisted reaction gas oxygen throughput proportioning should be 4: 1-9: 1, total work air pressure should be 0.2-1.0Pa, growth temperature should be 450 ℃-550 ℃, the pre-growth time of no assisted reaction gas oxygen should be 1-5 minute, has the growth time of assisted reaction gas oxygen to should be 120-240 minute.
The present invention compared with prior art has following beneficial effect:
Compare existing conventional SiC film preparation growth technique, as chemical vapor deposition (CVD), magnetron sputtering and plasma ion assisted deposition etc., the present invention adopts the ion beam epitaxy method can realize on the Si substrate that the 3C-SiC film is in the ultra-thin high-purity high-quality growth of the low temperature below 1000 ℃, a few to tens of nanometer thickness films have single 3C-SiC (111) orientation of high crystalline quality, and surface also smoother is smooth, but thereby has obtained to have the Si base covariant substrate in high-quality ultra-thin 3C-SiC intermediate layer.
Compare existing various based on " no support substrates " but the routine covariant substrate of theoretical model, but the preparation technology of the ultra-thin 3C-SiC of Si of the present invention base intermediate layer covariant substrate is simple, good reproducibility and low cost.Only just can realize by the high-purity growth of simple ion beam epitaxy superthin layer low temperature, but the crystalline quality of covariant layer is good, smooth surface is smooth, inject chemical reduction technology with nanoscale and need not complicated bonding techniques or energetic ion, can also avoid the contaminating impurity problem.
Compare common silicon substrate and existing various conventional buffer layer technology, but the ultra-thin 3C-SiC of Si base of the present invention intermediate layer covariant substrate has better misfit strain coordinative role, big mismatch epitaxial layer zinc oxide material growth quality of prepared growth improves on it, and tensile residual stresses reduces.This substrate also is applicable to the epitaxial growth of big mismatch heterogeneous structure material gallium nitride and aluminium nitride simultaneously.Therefore for realizing that these important wide bandgap compound semiconductors materials with superior photoelectric properties are with ripe Si base microelectronic component technology perfect adaptation with develop novel opto-electronic device and lay the foundation.
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:
But Fig. 1, have the Si base covariant substrat structure schematic diagram in ultra-thin 3C-SiC intermediate layer: wherein 21 are bottom Si (111) substrate; 22 is ultra-thin 3C-SiC intermediate layer, preparation on 21, but and constitute Si base covariant substrate with 1; 23 is big mismatch epitaxial layer, and preparation and 21 has than Macrolattice mismatch on 22, and constitutes big mismatch heterogeneous structure material with 21,22.
The low energy double-ion beam epitaxial device schematic diagram in Fig. 2, the ultra-thin 3C-SiC of preparation intermediate layer: wherein the I bundle produces the isotopically pure low energy ion beam bundle that is used for dry method sputter clean surface of silicon, the II bundle produces the isotopically pure low energy carbon ion beam that is used for the ultra-thin 3C-SiC of silicon carbide substrates surface epitaxial growth intermediate layer, 1 is ion source, 2 is ion source line regulation device, 3 is the magnetic analyzer device, and 4.1 is argon ion (Ar
+) bundle, 4.2 is carbon ion (C
+) bundle, 5.1 is the electric quadrupole lens devices, and 5.2 is the magnetic quadrupole lens device, and 6 is the electrostatic deflection electrodes device, and 7 is the retarding lens device, and 8 is substrate, and 9 is ion beam line monitoring device, and 10 is the ultra high vacuum growth room.
The ultra-thin 3C-SiC intermediate layer Measurement results that adopts the ion beam epitaxy method to prepare on Fig. 3, Si (111) substrate: a is X-ray diffraction test (XRD) for atomic force surface topography test (AFM), b, and c is Auger spectroscopy depth analysis (AES).
Fig. 4, at common Si (111) substrate (a) but and have on the Si base covariant substrate (b) in ultra-thin 3C-SiC intermediate layer, adopt atomic force surface topography (AFM) Measurement results of the ZnO film sample that identical magnetron sputtering growth technique prepares.
Fig. 5, at common Si (111) substrate (a) but and have on the Si base covariant substrate (b) in ultra-thin 3C-SiC intermediate layer, adopt X-ray diffraction (XRD) Measurement results of the ZnO film sample that identical magnetron sputtering growth technique prepares.
Embodiment
See also shown in Figure 1ly, a kind of silicon based compliant substrate with ultra-thin carborundum intermediate layer of the present invention is characterized in that, comprises following a few part:
One silicon substrate 21, this silicon substrate 21 plays support;
One ultra-thin 3C-SiC intermediate layer 22, these ultra-thin 3C-SiC intermediate layer 22 preparations play misfit strain and coordinate, and constitute the silicon based compliant substrate with silicon substrate 21 on silicon substrate 21; The thickness in wherein ultra-thin 3C-SiC intermediate layer 2 is 5-30nm, and material is monocrystalline and polycrystal carborundum thin-film material;
One epitaxial loayer 23, this epitaxial loayer prepares on ultra-thin 3C-SiC intermediate layer 22, and has than Macrolattice mismatch with bottom silicon substrate 21; The lattice mismatch opposite in sign of the lattice mismatch symbol between this epitaxial loayer 23 and the ultra-thin 3C-SiC intermediate layer 22 and middle ultra-thin 3C-SiC intermediate layer 22 and silicon substrate 21, promptly one negative one just, and the lattice mismatch numerical value in epitaxial loayer 3 and ultra-thin 3C-SiC intermediate layer 22 is 0-10%; The material of this epitaxial loayer 23 is: zinc oxide, gallium nitride, aluminium nitride and carborundum films material, those materials are to adopt magnetron sputtering, metal organic chemical vapor deposition, chemical vapour deposition (CVD), pulsed laser deposition, molecular beam epitaxy and the preparation of ion beam epitaxy method.
Please consult Fig. 1 again, a kind of preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer of the present invention is characterized in that the preparation method comprises following steps:
Get a silicon substrate 21;
Adopt the method for ion beam epitaxy, the ultra-thin 3C-SiC of preparation intermediate layer 22 on silicon substrate 21;
Adopt the method for magnetron sputtering, preparation one epitaxial loayer 23 on ultra-thin 3C-SiC intermediate layer 22.
The preparation process in this ultra-thin 3C-SiC intermediate layer 22 is as follows:
Step 1: select for use the not high argon gas of purity requirement to produce the ar-ion beam raw material that are used for substrate surface dry method sputter clean as low energy double-ion beam epitaxial device I beam ion source;
Step 2: select for use the not high CO (carbon monoxide converter) gas of purity requirement to produce the carbon ion beam raw material that are used for carborundum films preparation growth as low energy double-ion beam epitaxial device II beam ion source;
Step 3: Si (111) substrate is inserted low energy double-ion beam epitaxial device growth room;
Step 4: the vacuum of taking out low energy double-ion beam epitaxial device whole system;
Step 5: two ion sources are toasted degas, this baking is degassed, and vacuum degree reaches 5-9 * 10 in preceding two ion sources
-4Pa, the temperature of baking heating is 120-300 ℃;
Step 6: the silicon substrate in the growth room toasted degass and surperficial high temperature deoxidation treatment, this silicon substrate baking degas and surperficial high temperature deoxidation before the indoor vacuum degree of growth should reach 1-5 * 10
-5Pa, heating-up temperature is 750-850 ℃, time 20-30 minute;
Step 7: the isotopically pure low energy ion beam bundle bombardment sputter dry method of utilizing low energy double-ion beam epitaxial device I bundle to produce is cleaned surface of silicon, and this beam current density that is used for the isotopically pure low energy ion beam bundle of surface of silicon bombardment sputter dry method cleaning should be 50-100 μ A/cm
2, the argon ion energy is 200-300eV, the dry method scavenging period is 2-5 minute;
Step 8: the ar-ion beam of closing low energy double-ion beam epitaxial device I bundle;
Step 9: the isotopically pure low energy carbon ion beam that utilizes low energy double-ion beam epitaxial device II bundle to produce carries out the high-purity growth of low temperature in ultra-thin 3C-SiC intermediate layer 22 on Si (111) substrate, the isotopically pure low energy carbon ion beam that obtains is to control low energy carbon ion beam bundle shape of spot and the size that is deposited on the substrate by the magnetic quadrupole lens device of adjusting the II bundle with the magnetic field of the magnetic steering device of assisting and the electric field of electrostatic deflection electrodes device, scanning swing is with the uniformity that improves prepared carborundum films with increase to membrane area about the additional substrate low-angle, and this isotopically pure low energy carbon ion beam beam current density should be 50-100 μ A/cm
2, energy should be 20-100eV, and dosage should be 1-8 * 10
17Dose, growth temperature should be 700-800 ℃.
Wherein when preparation epitaxial loayer zinc-oxide film, should adopt 60-100W to exchange radio frequency sputtering power sputter purity is 99.99%-99.999% zinc oxide target, working gas argon gas and assisted reaction gas oxygen throughput proportioning should be 4: 1-9: 1, total work air pressure should be 0.2-1.0Pa, growth temperature should be 450 ℃-550 ℃, the pre-growth time of no assisted reaction gas oxygen should be 1-5 minute, has the growth time of assisted reaction gas oxygen to should be 120-240 minute.
Realize the best way of invention:
1. realize the capital equipment of invention:
Semiconductor film film preparation equipment (as ion beam epitaxy (IBE) system, outer (MBE) system of molecular beam, magnetron sputtering (MS) equipment, pulsed laser deposition (PLD) system, metal organic chemical vapor deposition (MOCVD) system and chemical vapor deposition (CVD) system etc.);
Vacuum equipment (as oil-sealed rotary pump, turbomolecular pump, cryo pump, ionic pump, sublimation pump etc.);
The cleaning equipment of semiconductor substrate materials.
2. according to the functional characteristics and the concrete condition of growth apparatus, the growing technology route of ultra-thin 3C-SiC intermediate layer and big mismatch epitaxial layer is adjusted.
3. utilize outer (IBE) system of ion beam to carry out the preparation growth in ultra-thin 3C-SiC intermediate layer, utilize equipment such as magnetron sputtering (MS) equipment, outer (MBE) system of molecular beam, pulsed laser deposition (PLD) system, metal organic chemical vapor deposition (MOCVD) system and chemical vapor deposition (CVD) system to carry out the preparation growth of big mismatch epitaxial layer.
4. for the device parameter of semiconductor film preparing system, be determined on a case-by-case basis.
Embodiment
The structure of silicon based compliant substrate with ultra-thin carborundum intermediate layer is referring to Fig. 1, and its major technology parameter sees Table 1.
Table 1: important technological parameters with ultra-thin carborundum intermediate layer silicon based compliant substrate
| |
Material | Silicon (Si) |
| Thickness (μ m) | 300-500 | |
| Crystal mass | Monocrystalline | |
| But covariant |
Material | Cubic silicon carbide (3C-SiC) |
| Thickness (nm) | 5-30 | |
| Crystal mass | Monocrystalline or polycrystalline | |
| |
Lattice mismatch with |
Be not less than 10% |
| But lattice mismatch with covariant |
Be not more than 10% | |
| Crystal mass | Monocrystalline or polycrystalline |
But with reference to the Si base covariant substrate schematic diagram among Fig. 1 and low energy double-ion beam extension (IBE) the equipment schematic diagram among Fig. 2 and experiment parameter in the table 2 and examination analysis result, but narration has ion beam epitaxy (IBE) the method preparation process of the Si base covariant substrate in ultra-thin 3C-SiC intermediate layer 22, specifically comprises following steps:
Step 1: select for use argon gas to produce ar-ion beam 4.1 raw material that are used for substrate 21 surperficial dry method sputter clean as low energy double-ion beam epitaxial device I beam ion source 2;
Step 2: select for use CO (carbon monoxide converter) gas to produce carbon ion beam 4.2 raw material that are used for carborundum films preparation growth as low energy double-ion beam epitaxial device II beam ion source 2;
Step 3: silicon substrate 21 is inserted ion beam epitaxy equipment growth room 10;
Step 4: the vacuum of taking out whole ion beam epitaxy device systems;
Step 5: two ion sources are toasted degas;
Step 6: the silicon substrates 21 in the growth room 10 are toasted degas and surperficial high temperature deoxidation treatment;
Step 7: the isotopically pure low energy ion beam bundle 4.1 bombardment sputter dry method of utilizing low energy double-ion beam epitaxial device I bundle to produce are cleaned the surface of silicon substrate 21;
Step 8: the ar-ion beam 4.1 of closing low energy double-ion beam epitaxial device I bundle;
Step 9: the isotopically pure low energy carbon ion beam 4.2 that utilizes low energy double-ion beam epitaxial device II bundle to produce carries out the high-purity growth of low temperature in ultra-thin 3C-SiC intermediate layer 22 on substrate 21.
Step 10: atomic force surface topography (AFM), X-ray diffraction (XRD) and Auger spectroscopy (AES) test analysis are carried out in the ultra-thin 3C-SiC intermediate layer 22 to preparation.
Table 2: the ion beam epitaxy method prepares the experiment parameter and the test result in ultra-thin 3C-SiC intermediate layer
Utilize and exchange radio frequency magnetron sputtering method, but on prepared Si base covariant substrate, carry out the preparation growth experiment of big mismatch epitaxial layer zinc oxide material 23 with ultra-thin 3C-SiC intermediate layer 22, and with common Si (111) substrate on the result compare, main experiment parameter is referring to table 3, and the test result of zinc oxide epitaxial layer sample is referring to Fig. 4 and Fig. 5.
Table 3: exchange the main experiment parameter that radio frequency magnetron sputtering method prepares the zinc oxide epitaxial layer
| The sputtering target parameter | Target material | Purity is not less than 99.99% zinc oxide |
| Range | 6-9cm | |
| Main growth room base vacuum degree | Be not more than 1 * 10 -5Pa | |
| The pre-sputtering parameter of zinc oxide target | Exchange radio frequency sputtering power | 80-120W |
| Working gas | Argon gas (Ar) | |
| Operating air pressure | 0.5-1.5Pa | |
| Sputtering time | 30-60 minute | |
| The pre-growth parameter(s) of zinc oxide epitaxial layer | Exchange radio frequency sputtering power | 60-100W |
| Working gas | Argon gas (Ar) | |
| Operating air pressure | 0.2-1.0Pa | |
| Sputtering time | 1-5 minute | |
| Growth temperature | 450-550℃ | |
| Zinc oxide epitaxial layer growth parameter | Exchange radio frequency sputtering power | 60-100W |
| Working gas and proportioning | Argon gas (Ar) and oxygen, proportioning 4: 1-9: 1 | |
| Operating air pressure | 0.2-1.0Pa | |
| Sputtering time | 120-180 minute | |
| Growth temperature | 450-550℃ |
Provide the two-dimensional surface roughness (RMS) of two ZnO film samples of a, b in 5 * 5 μ m yardsticks by atomic force surface topography (AFM) Measurement results of Fig. 4 and be respectively 6.4nm and 3.9nm.Show that but the ZnO film sample a surface on the Si base covariant substrate with the thin intermediate layer of 3C-SiC is Paint Gloss smooth.The surface topography of ZnO film sample b on common Si (111) substrate compares relatively poor, and explanation is the bigger stress of rete inner accumulated.From X-ray diffraction (XRD) test result of Fig. 5 as can be seen, ZnO sample a on common Si (111) substrate does not realize the single preferred orientation growth of C axle, in the XRD spectrum except observing 72.537 ° of 34.403 ° more intense of C axle oriented ZnO (002) diffraction maximums and ZnO (004) diffraction maximums, also observe 31.743 ° of ZnO (100) diffraction maximums of more weak non-C axle orientation, 62.840 ° of 36.232 ° of ZnO (101) diffraction maximums and ZnO (103) diffraction maximums, and the halfwidth (FWHM) at ZnO (002) diffraction maximum 2 θ angles is 0.418 °, calculating ZnO (002) face interplanar distance d value is 2.6047 , and standard value d
0Be 2.6033 , the crystallite dimension that calculates (D) is 19.7nm, shows that the crystalline quality of this sample is poor, and the bigger compression of rete inner accumulated.
Comparatively speaking, but the ZnO sample b that has on the Si base covariant substrate in ultra-thin 3C-SiC intermediate layer has realized the single preferred orientation growth of C axle, only observe 72.642 ° of 34.450 ° very strong of C axle oriented ZnO (002) diffraction maximums and ZnO (004) diffraction maximums in the XRD spectrum, and also smaller 0.351 ° of 2 θ angle halfwidths (FWHM) of ZnO (002) diffraction maximum value, the d value of the ZnO that calculates (002) interplanar distance is 2.6014 , and crystallite dimension (D) is 23.4nm.Show that this sample has reasonable crystalline quality, and remnant tensile stress only.But the Si base covariant substrate that above-mentioned experimental result explanation has ultra-thin 3C-SiC intermediate layer has reasonable misfit strain coordinative role, adopt the raising of crystalloid amount, the surface topography of the big mismatch epitaxial layer ZnO material that exchanges radio frequency magnetron sputtering method preparation growth to improve significantly on it, and residual stress reduce in the rete.So be a kind of New Si base substrate that improves ZnO film material growth quality, and also can be used for the preparation growth of GaN and AlN epitaxial loayer.
Claims (12)
1. the silicon based compliant substrate with ultra-thin carborundum intermediate layer is characterized in that, comprises following a few part:
One silicon substrate, this silicon substrate plays support;
One ultra-thin 3C-SiC intermediate layer, this ultra-thin 3C-SiC intermediate layer preparation plays misfit strain and coordinates, and constitute the silicon based compliant substrate with silicon substrate on silicon substrate;
One epitaxial loayer, this epitaxial loayer prepares on ultra-thin 3C-SiC intermediate layer, and has than Macrolattice mismatch with the bottom silicon substrate.
2. the described silicon based compliant substrate with ultra-thin carborundum intermediate layer of claim 1 is characterized in that the thickness in wherein ultra-thin 3C-SiC intermediate layer is 5-30nm, and material is monocrystalline and polycrystal carborundum thin-film material.
3. the described silicon based compliant substrate of claim 1 with ultra-thin carborundum intermediate layer, it is characterized in that, the lattice mismatch opposite in sign of the lattice mismatch symbol between epitaxial loayer and the ultra-thin 3C-SiC intermediate layer and middle ultra-thin 3C-SiC intermediate layer 2 and silicon substrate wherein, promptly one negative one just, and the lattice mismatch numerical value in epitaxial loayer and ultra-thin 3C-SiC intermediate layer is 0-10%.
4. claim 1,3 described silicon based compliant substrates with ultra-thin carborundum intermediate layer, it is characterized in that, wherein the material of epitaxial loayer is: zinc oxide, gallium nitride, aluminium nitride and carborundum films material, those materials are to adopt magnetron sputtering, metal organic chemical vapor deposition, chemical vapour deposition (CVD), pulsed laser deposition, molecular beam epitaxy and the preparation of ion beam epitaxy method.
5. preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer is characterized in that the preparation method comprises following steps:
Get a silicon substrate;
Adopt the method for ion beam epitaxy, the ultra-thin 3C-SiC of preparation intermediate layer on silicon substrate;
Adopt the method for magnetron sputtering, preparation one epitaxial loayer on ultra-thin 3C-SiC intermediate layer.
6. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 5 is characterized in that, the preparation process in wherein ultra-thin 3C-SiC intermediate layer is as follows:
Step 1: select for use the not high argon gas of purity requirement to produce the ar-ion beam raw material that are used for substrate surface dry method sputter clean as low energy double-ion beam epitaxial device I beam ion source;
Step 2: select for use the not high CO (carbon monoxide converter) gas of purity requirement to produce the carbon ion beam raw material that are used for carborundum films preparation growth as low energy double-ion beam epitaxial device II beam ion source;
Step 3: Si (111) substrate is inserted low energy double-ion beam epitaxial device growth room;
Step 4: the vacuum of taking out low energy double-ion beam epitaxial device whole system;
Step 5: two ion sources are toasted degas;
Step 6: the silicon substrate in the growth room toasted degas and surperficial high temperature deoxidation treatment;
Step 7: the isotopically pure low energy ion beam bundle bombardment sputter dry method of utilizing low energy double-ion beam epitaxial device I bundle to produce is cleaned surface of silicon;
Step 8: the ar-ion beam of closing low energy double-ion beam epitaxial device I bundle;
Step 9: the isotopically pure low energy carbon ion beam that utilizes low energy double-ion beam epitaxial device II bundle to produce carries out the high-purity growth of low temperature in ultra-thin 3C-SiC intermediate layer on Si (111) substrate.
7. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 6 is characterized in that, wherein toasts the interior vacuum degree of preceding two ion sources that degas in the step 5 and reaches 5-9 * 10
-4Pa, the temperature of baking heating is 120-300 ℃.
8. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 6 is characterized in that, wherein in the step 6 silicon substrate baking degas and surperficial high temperature deoxidation before the indoor vacuum degree of growth should reach 1-5 * 10
-6Pa, heating-up temperature is 750-850 ℃, time 20-30 minute.
9. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 6, it is characterized in that the beam current density that wherein is used for the isotopically pure low energy ion beam bundle of surface of silicon bombardment sputter dry method cleaning in the step 7 should be 50-100 μ A/cm
2, the argon ion energy is 200-300eV, the dry method scavenging period is 2-5 minute.
10. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 6, it is characterized in that, the isotopically pure low energy carbon ion beam that wherein obtains in the step 9 is that the magnetic quadrupole lens device by adjusting the II bundle is controlled low energy carbon ion beam bundle shape of spot and the size that is deposited on the substrate with the magnetic field of auxiliary magnetic steering device and the electric field of electrostatic deflection electrodes device, and the scanning swing is with the uniformity that improves prepared carborundum films with increase to membrane area about the additional substrate low-angle.
11. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 6 is characterized in that, wherein the isotopically pure low energy carbon ion beam beam current density in the step 9 should be 50-100 μ A/cm
2, energy should be 20-100eV, and dosage should be 1-8 * 10
17Dose, growth temperature should be 700-800 ℃.
12. the preparation method with the silicon based compliant substrate in ultra-thin carborundum intermediate layer according to claim 5, it is characterized in that, wherein when preparation epitaxial loayer zinc-oxide film, should adopt 60-100W to exchange radio frequency sputtering power sputter purity is 99.99%-99.999% zinc oxide target, working gas argon gas and assisted reaction gas oxygen throughput proportioning should be 4: 1-9: 1, total work air pressure should be 0.2-1.0Pa, growth temperature should be 450 ℃-550 ℃, the pre-growth time of no assisted reaction gas oxygen should be 1-5 minute, has the growth time of assisted reaction gas oxygen to should be 120-240 minute.
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