CN106987899A - Use Material growth device, growing method and the detection means of gas phase transmission - Google Patents
Use Material growth device, growing method and the detection means of gas phase transmission Download PDFInfo
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- CN106987899A CN106987899A CN201610929270.XA CN201610929270A CN106987899A CN 106987899 A CN106987899 A CN 106987899A CN 201610929270 A CN201610929270 A CN 201610929270A CN 106987899 A CN106987899 A CN 106987899A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/08—Reaction chambers; Selection of materials therefor
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/32—Carbides
- C23C16/325—Silicon carbide
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/14—Feed and outlet means for the gases; Modifying the flow of the reactive gases
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/16—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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Abstract
The invention discloses a kind of Material growth device of use gas phase transmission, including vacuum chamber and growth room, growth room is placed in vacuum chamber, and growth room includes gas off-take and at least two inner surfaces, and two inner surfaces are respectively used to shelve required growth source material and substrate;Growth source material at least include upper surface and and lower surface, the upper surface of growth source material and substrate with respect to and lower surface is then contacted with growth room;Substrate at least includes aufwuchsplate and the back side, and the back side of substrate is contacted with growth room and aufwuchsplate is relative with growth source material, and growth chamber is formed between the upper surface of growth source material and the aufwuchsplate of substrate;It is characterized in that:It is parallel with the aufwuchsplate of substrate when the upper surface of growth source material, the aufwuchsplate of substrate, growth room and gas off-take are arranged so that the air-flow produced by growth source material flows on the aufwuchsplate of substrate.Also disclose the detection means of the method and material growth course using grower formation material.
Description
Technical field
The present invention relates to a kind of Material growth device of use gas phase transmission, use the side of grower formation material
The detection means of method and growth course.
Background technology
The renewable sources of energy technology and cleaning electric motor car of 21st century needs the transistor device of a new generation to be used as switch
Device, the circuit for having important use for two classes.One class is commutator transformer (converter):It is low direct current buckling
Into high-voltage dc voltage, so that the electric current in circuit is reduced, to reduce heating loss, so as to apply in solar electricity generation field and electricity
To improve their operating voltage in motivation car.Another kind of is inverter (inverter):It can be the DC current of motor
Become three-phase alternating current, so that motor or the DC current that solar electricity generation field is produced, become alternating current,
So as among electrical energy transportation to existing power network.Therefore, such transistor must have the characteristics that:1) low energy consumption, so
The farther or solar electricity generation field that electric automobile can be run is more effective;2) high operating voltage, at least above 600V more has choosing
Higher than 1200V;3) internal resistance is small;4) it is easy to use in changeable environment;5) speed of switch is fast;5) to have well
Heat sinking function, device performance is just stable.
Existing device respectively has advantage and disadvantage.Very widely used today Si insulation Gate bipolar transistors (IGBT), cost is low,
Manufacturing technology is ripe.But, 20-30% energy losses can be caused.This makes due to the hysteresis effect of minority carrier among Si
Into the background current of closed mode.So, in recent years, broadband semiconductor SiC, GaN and AlN become more important.Particularly
FET (the double-diffusion metal oxide field for the double-diffused metal oxide semiconductor that SiC makes
Effect transistor, DMOSFET), there is very strong competitiveness at present.Because their pressure-resistant performance is high, switch resistance
It is low, low and thermal conductance is lost and feels better to favor.In recent years, SiC single crystal growing technology achieved long-range progress, 4 " substrate lists
Growth techniques are ripe, and 6 " substrates have begun to put on market expensive.But related growth technology is also not
Needs can be met, and make device fabrication processes complicated.
Very widely used today vapour deposition (chemical vapour deposition, CVD) growth SiC, growth speed
Rate is relatively low, it is necessary to which 10-20 hour can just form the electronics drift layer close to assertive evidence SiC (or n-SiC).In addition, this
The temperature of method growth is not also enough height, and surface is easily roughened, and this will reduce the performance of device.(U.S. is special by Vodakov etc.
Profit is 4,147,572) and Syvajarvi etc. (United States Patent (USP) 7,918,937B2) proposes close-spaced sublimation method (close space
Sublimation, CSS) growth SiC.Although the growth rate of these methods is high, these methods can not control doping dense
Degree.Jiang uses CSS, and growth chamber (pad expects the gap that surface is formed with source) is placed directly within vacuum chamber, CdTe is realized
Quick epitaxial growth (Journal of ELECTRONIC MATERIALS 38 (2009) 1548).But, due to lacking one
Individual growth room, is surrounded growth chamber, cannot control the atmosphere of growth chamber;Also, at high temperature, radially temperature ladder is too big, raw
Length is in uneven thickness.Further, since lacking the appropriate growing technology in terms of SiC multilayer knot materials are grown, so having to
Using particle injection technique, so as to cause lattice damage, reduce the electron mobility of DMOSFET conductive channels, device performance and
Reliability decrease.
The content of the invention
First technical problem to be solved by this invention is in view of the above-mentioned problems of the prior art, providing one kind just
In Controlling Growth Rate, adjustment doping concentration and Optimal Growing condition, Material growth device using gas phase transmission.
Second technical problem to be solved by this invention is to provide a kind of side using above-mentioned grower formation material
Method.
3rd technical problem to be solved by this invention is to provide a kind of detection means, for being filled using above-mentioned growth
When putting, the growth course of material is detected.
The present invention solve technical scheme that above-mentioned first technical problem used for:A kind of material of use gas phase transmission
Grower, including vacuum chamber and growth room, the growth room are placed in the vacuum chamber, the growth room include gas off-take and
At least two inner surfaces, two inner surfaces are respectively used to shelve required growth source material and substrate;The growth source material is at least wrapped
Include upper surface and and lower surface, the upper surface of the growth source material is relative with substrate and lower surface is then contacted with growth room;It is described
Substrate at least includes aufwuchsplate and the back side, and the back side of the substrate is contacted with growth room and aufwuchsplate is relative with growth source material, institute
State and form growth chamber between the upper surface of growth source material and the aufwuchsplate of substrate;It is characterized in that:The upper table of the growth source material
Face, the aufwuchsplate of substrate, growth room and gas off-take are arranged so that the air-flow produced by the growth source material in the substrate
It is parallel with the aufwuchsplate of the substrate when being flowed on aufwuchsplate.
Further, the growth chamber or growth room are connected with air intake duct, thus can adjust growth chamber by air intake duct
Component and doping concentration.
It is preferred that, growth source material be realized by sensing heating it is heated, be provided with the vacuum chamber sensing heating dress
Put.
To ensure that airflow direction is parallel with substrate surface, increase atom or ion are in the movement of substrate surface, the growth
The upper surface of source material, be smaller than substrate growth face diameter 1/5 with the aufwuchsplate of substrate.
It is preferred that, the gross area of the gas off-take is not more than 1/2 with the ratio of growth chamber lateralarea.
According to currently preferred, at least one inner surface of the growth room, including llowing group of materials one kind or
It is a variety of:W, Mo, Ta, Nb, graphite, diamond, BN, WC, MoC, TaC and NbC.So as to prevent used in impurity from the growth room
Material, into described growth chamber.
According to currently preferred, the growth source material includes one kind of llowing group of materials:SiC、GaN、Cd1-xZnxTe(0≤
X≤1) and AlN.
The present invention solve technical scheme that above-mentioned second technical problem used for:One kind is used and used as described above
The method of the grower formation material of gas phase transmission, it is characterised in that:Comprise the following steps:1) growth source needed for providing
Material, the growth source material at least includes upper and lower surface;2) substrate needed for providing, the substrate at least includes aufwuchsplate
And the back side, the upper surface of the growth source material and the aufwuchsplate of substrate are relative;3) the growth source material and substrate are placed so that institute
State and form growth chamber between the upper surface of growth source material and the aufwuchsplate of substrate;4) when the growth source material is heated, there is provided height
Pure gas, is injected into the growth chamber, and grown material is formed on the aufwuchsplate of substrate.
For the saturation degree needed for meeting Material growth, the spacing of the upper surface of the growth source material and the aufwuchsplate of substrate is small
In the 1/5 of substrate growth face diameter.
The present invention solve technical scheme that above-mentioned 3rd technical problem used for:A kind of material of use gas phase transmission
The detection means of growth, the growth course for detecting material using grower as described above, it is characterised in that:Bag
It is the substrate and thermal conductor of twin polishing and for the optical channel by detection light to include, and the substrate at least includes life
Long face and the back side, the aufwuchsplate of the substrate are used for the growth of material;The thermal conductor is placed in the back side of the substrate;It is described
Detection light out of optical channel by rear, through the thermal conductor, substrate and the material of growth after return.
Compared with prior art, the advantage of the invention is that:Semi-enclosed grower is used, i.e., including gas off-take
And/or air intake duct, it is easily controlled growth rate, adjustment doping concentration and Optimal Growing condition:
1. due to having used semiclosed growing system, so that accumulation of the impurity in growth room (chamber) is avoided, for control
Doping concentration provides possibility.
2. due to having used semiclosed growing system, so as to avoid component that some are unsuitable for Material growth in growth room
Accumulation in (chamber), possibility is provided for control more reasonably growth atmosphere.
3. due to using air intake duct, high-purity gas can be passed through, such as high-purity hydrogen, can be with so as to reduce background doped
Grow the epitaxial layer closely with intrinsic semiconductor.
4. due to using air intake duct, it can be passed through for different impurity gas, so that multilayer knot material is formed, so that simple
Change the manufacturing process of device.
5. because growing system includes the device that vapor phase growth is detected, so as to monitoring growth rate or/and temperature in real time
Degree, realizes the control to growth course.
Brief description of the drawings
Fig. 1 is the structural section schematic diagram of grower proposed by the present invention, example;
Fig. 2 is growth room's cap surface structural representation of the grower of the present invention.
Fig. 3 uses an example of the present invention, in material deposition process, detects the demonstration song that light intensity is changed over time
Line.
Fig. 4 is growth room's schematic cross-section of the example of the multiple substrates of use of the present invention.
Fig. 5 is proposed by the present invention, example growth cell configuration schematic cross-section.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Referring to Fig. 1 and Fig. 2, a Material growth device section typical, using sensing heating, using gas phase transmission
With the schematic diagram of the upper surface of growth chamber cap.
Include vacuum chamber 101 and the growth room 102 of metal, whole growth room using the Material growth device of gas phase transmission
102 are placed among vacuum chamber 101, and growth room 102 is arranged on by mounting bracket 113 on the bottom surface of vacuum chamber 101, mounting bracket
113 using insulation, relatively adiabatic material, and growth room 102 includes growth chamber cap 107.Vacuum chamber 101 passes through interface 114
A vavuum pump is connected to, vacuum chamber 101 is additionally provided with vacuum chamber breather pipe 122.
There are at least two inner surfaces in growth room 102, be respectively used to shelve required growth source material 105 and substrate 112,
Substrate 112 is arranged on the top of growth source material 105.On at least one inner surface of growth room 102, include the one of llowing group of materials
Plant or a variety of:W, Mo, Ta, Nb, graphite, diamond, BN, WC, MoC, TaC and NbC.Growth source material 105 includes at least two faces,
Such as upper and lower surface, its lower surface is contacted with growth room 102, and upper surface is relative with substrate 112.Substrate 112 is also included extremely
Few two faces, such as upper and lower surface, upper surface is the back side, contacted with growth room 102, and lower surface and growth source material 105
Relatively, it is aufwuchsplate.The upper surface of growth source material 105 and substrate 112 grow towards formation between the aufwuchsplate of growth source material 105
Chamber 117.Substrate 112 is placed in growth chamber cap 107, the graphite block that its peripheral position 109 being embedded in correspondence is separately separated, and is held
It is quick detachable.Growth source material 105 is heated at high temperature to volatilize, and forms gas and air-flow, into growth chamber 117, portion gas deposition
The material 116 of growth, gas flow sideways (as shown by arrow 106), portion gas row are formed on the aufwuchsplate of substrate 112
Go out.Because the gap between substrate 112 and growth source material 105 is small (be less than the aufwuchsplate diameter of substrate 112 1/5), therefore air-flow
Direction will be parallel to the aufwuchsplate of substrate 112.Optionally, growth source material 105 includes one kind of llowing group of materials:SiC、GaN、Cd1- xZnxTe (0≤x≤1) and AlN.
In order to detect the growth course of material, also include detection means, detection means includes being arranged on the back side of substrate 112
Thermal conductor 111 and formed growth chamber cap 107 in vertical optical channel 118.Thermal conductor 111 by heat conducting material,
As diamond is made.The position of optical channel 118 is corresponding with thermal conductor 111.It is the top of vacuum chamber 101, corresponding with optical channel 118
Position offers detection light gateway 115, and collimated light beam 110, by optical channel 118, and passes through heat and passed via light gateway 115
Aufwuchsplate and growth material 116 that material (such as diamond) 111 reaches substrate 112 are led, is then back to.Thus temperature can be measured in real time
Degree, the thickness of growth material 116 and the thick perceived noisiness on surface etc..In addition, Radiation Temperature Measurement Instrument 121 can be equipped with vacuum chamber 101, it is used for
Measurement and control temperature.The sapphire or SiC columns or bullet of twin polishing can also be embedded in optical channel 118.
Vertical gas off-take 108 is formed with growth chamber cap 107, thus in Controllable growth room 102 and growth chamber 117
Air pressure.
The induction heating apparatus 104 of water cooling is set using in vacuum chamber 101, such as high frequency coil, so that high-frequency electrical be spread
It is defeated into vacuum chamber 101.So, growth room 102 must include high-temperature electric conduction material, such as graphite, Mo, W, Ta, Pt, in high frequency
They produce heat, heat growth source material 105 and substrate 112 in electric field.Graphite is easily worked, and cost is low, should be preferred.Sensing
Also one layer of glass tube 119 can be embedded between heater 104 and growth room 102, such as quartz glass tube, for depositing by growth room
102 discharge tail gas and play insulating effect.Graphite foam 120 can be implanted between glass tube 119 and growth room 102, is risen
To heat insulating function;But, graphite foam 120 contains substantial amounts of foreign gas.In order to prevent that those gases, can as growth impurity
To form many drillings on graphite foam 120, before growth starts, using high vacuum, gas is discharged.
Grower also includes the air intake duct 103 extended into outside vacuum chamber 101 in growth room 102, and air intake duct 103 is to change
Become gas componant and control doping provides extra approach.The gas containing C and/or Si, such as C can be passed through using it3H8,
SiCl4,SiH4Deng SiC crystalline phase, surface roughness etc. can be controlled.High-purity gas, high purity can be passed through using it
1ppm to 0.01ppb, the H such as filtered via Pd nethike embranes2Deng dilution background doped, for forming quasi- intrinsic semiconductor layer.Can be with
P-type impurity gas, such as trimethyl aluminium (C are passed through using it6H18Al2), trimethyl indium (C6H18In2), trimethyl gallium (C6H18Ga2)
Deng or N-type impurity gas, such as N2, PH3Deng the semiconductor epitaxial multilayer junction structure needed for being formed.The top half of air intake duct 103
Connect with growth room 102, can be made with the tubing such as graphite, Ta, Mo, W;Its upper end can make screw, be directly anchored to growth
On room 102.TaC, MoC, WC etc. can also be deposited in the inwall of tubing, so that their impurity is reduced, into growth chamber
117.Alloy can be used in the latter half of air intake duct 103, is connected to outside vacuum chamber 101.Between which can be embedded in one section of insulation
Or heat-insulating material.
Using the method for the grower formation material of above-mentioned use gas phase transmission, comprise the following steps:
1) the growth source material 105 of purification needed for providing, growth source material 105 at least includes upper and lower surface;
2) provide needed for substrate 112, substrate 112 at least include aufwuchsplate and the back side, the upper surface of growth source material 105 and
The aufwuchsplate of substrate 112 is relative;
3) growth source material 105 and substrate 112 are placed so that the upper surface of growth source material 105 and the aufwuchsplate shape of substrate 112
Into growth chamber 117;
4) it is injected into when the growth source material 105 is heated there is provided high-purity gas in the growth chamber 117, in substrate
Growth forms growth material 116 on 112 aufwuchsplate.
, can be to the dress shown in Fig. 1 in order to better control over the air pressure of the various components in doping concentration and growth chamber 117
Put the various optimizations of progress:
1) outer layer of growth room 102 can use graphite foam as insulation material;It can discharge gas, such as N2、O2
Deng being unfavorable for realizing low background doped.It can be replaced by high-purity, highdensity graphite;But have many in these graphite
Artificial perforation, plays heat insulating function.2) generally high purity graphite also has impurity or gas;In order to prevent them from entering growth room
102 and growth chamber 117, can growth room 102 inwall, patch adds at least one thin metal layer (20 microns -2 millimeters), these
Metal is including Mo, W, Ta, Pt etc..Another method is BN, MoC, WC or TaC polycrystalline on the inner side of growth room 102, deposition
Film, the thickness of film is at 5 microns to 50 microns.3) at high temperature, growth source material 105 discharge portion gas, may with by high frequency
The material for sensing and producing heat reacts.Can be the material that heat is produced by high-frequency induction, such as graphite, Mo, Pt etc. inlay
Among more stable material, such as BN ceramic materials, it is to avoid directly contacted with those gases.
4) can be using the air pressure for changing vacuum chamber 101, and the area of gas off-take 108 is relative to the section of growth chamber 117
Ratio, adjust growth atmosphere, it is to avoid accumulated impurity atom or ion.The usual gross area of gas off-take 108 is relative to growth chamber 117
The ratio of lateralarea be not more than 1/2.Gas off-take 108 can be placed in growth chamber cap 107, or the side wall of growth room 102, or growth
The bottom surface of room 102.Gas off-take 108 is symmetric relative to growth source material 105 and substrate 112, to ensure that the material of growth is thick
Degree and the uniformity of doping.So multiple apertures of circle distribution can be formed on growth chamber cap 107, as shown in Fig. 2 conduct
Gas off-take 108.Gas off-take 108 can also make taper, below diameter it is small, upper diameter is big, prevents what is caused due to deposition
Block.
5) according to the growth material 116 formed, the growth source material 105 required for selection.Growth source material 105 is preferably piece
Shape, better than granular, because being so easily controlled vapour pressure, growth is easily repeated.The material suppressed under HTHP is more
Economy, but purity will height.In order to grow quasi- intrinsic semiconductor, high-purity monocrystalline or polycrystalline flat crystal can be used as life
Long source material 105.
6) temperature of the generally aufwuchsplate of substrate 112 is lower than the upper surface temperature of growth source material 105, that is, has growth temperature
Difference, is the power for driving Material growth.This can grow the phase of the relative induction heater 104 of (room 102) chamber 117 by adjusting
The design of position or change growth room 102 is realized, growth chamber cap 107 can also be thinned or is added on growth chamber cap 107
Heat-insulating material.In growth course, these methods are unusable, but can be to the growth ventilation body of chamber cap 107, to growth chamber cap
107 are cooled down, so as to control the growth temperature difference and growth rate.
7) generally measured in real time in optics in the thickness of epitaxial film and the device of temperature, monochromatic or polychrome directional light be from
Aufwuchsplate projection.The present invention uses monochromatic or polychrome directional light from back surface incident, therefore does not influence the air-flow of growth chamber 117.
In addition, heat conducting material has been used in Fig. 1, such as diamond (2-4mm is thick, 5 millimeters x5 millimeters).Because diamond is at 2000 DEG C
Still there is good thermal conductivity, so in the position of optical channel 118, substrate 112 is unlikely to supercooling.Therefore, the position of optical channel 118
Growing state is consistent with the growing state that substrate 112 is overall, adds the reliability of measurement.In growth course, reflected light
The luminous intensity of a wavelength change with time may be similar to such as Fig. 3.When growing beginning, the intensity of reflected light is with growth
The thickness of material 116 vibrates.But be due to 116 pairs of light of growth material absorption or surface it is roughening, oscillation amplitude has
It is a certain degree of to weaken.
Growth room 102 among Fig. 1 can change system into many substrate growth systems, as shown in figure 4, air intake duct 103 be placed in it is many
The middle part of substrate.
Whole growing system is made a general survey of, can be using various methods come Controlling Growth Rate:1) substrate 112 and source material are changed
105 spacing:Spacing is bigger, and growth rate is smaller;2) thermograde is changed:The relative induction heater of growth room 102 is moved up
Or the thickness of growth chamber cap 107 is reduced, thermograde can be increased, so as to increase growth rate;3) change via air intake duct 103
Into the flow of the high-purity gas of growth chamber 117:Flow is bigger, and growth rate is lower.So growth rate can be controlled in
Several microns are to hundreds of microns per hour.In addition, the system can be used, nearly intrinsic semiconductor is formed:I) due to usual impurity
The segregation coefficient of ion or atom is less than 1, increases the gross area of airway 108, can avoid foreign ion or atom in growth
Accumulated in chamber 117, so as to increase the purity of the material of growth;Ii) increase enters the high-purity of growth chamber 117 via air intake duct 103
The flow of gas, flow is bigger, and the purity of the material of growth is higher.
Example 1:Grow accurate intrinsic SiC epitaxial films
Using sensing heating, growing system using gas phase transmission, Fig. 5 is its section:
1) grower:Metal vacuum room 401 is made by stainless steel;Its wall can be passed through cooling water;And cut with vacuum
Pump interface 413 and light gateway 414.Internal capacity is:Diameter phi 80cm x 80cm.
The support that aluminium oxide ceramics rod (bottom) and molybdenum tube (top) insulated using 4, relatively adiabatic is made
412,15cm, diameter phi 3cm, whole growth room 402 are fixed on the bottom surface of vacuum chamber 401 altogether.And in the sensing of water cooling
Heater 404 (i.e. high frequency coil) between growth room 402, add quartz ampoule 416 and have drilling graphite foam 417 (~
2cm is thick).The former plays insulating effect, and the latter plays heat insulating function.Many 0.5mm brill is deliberately formed in graphite foam 417
Hole, is conducive to foreign gas to overflow.Because among vacuum, heat radiation loss is main thermal losses, therefore can also be in sensing
Between heater 404 and vacuum chamber 401, plus last layer Mo thin layers, play insulation effect.It is another to have cooling feed channel 419, Xiang Zhen
Gas is passed through in empty room 401, the temperature of reduction growth chamber cap 406 controls the temperature difference, so as to change growth rate.
Growth room 402 (overall diameter 32cm), including growth chamber cap 406 (thick 10cm) is made by high-purity, high-density graphite.
Their inner surface has TaC coating 420 (~10 microns), so as to prevent the impurity in graphite from entering growth chamber 422.They
Extexine thick 5cm has thickly dotted diameter 0.5mm, horizontal and vertical drilling, plays heat insulating function.The bottom of growth room 402
Thick 12cm, side thickness 10cm.Substrate 411 for twin polishing 2 ", 8 °-beveling, Si- faces 4H-SiC, leaded wastewater 3x1018cm-3, can
It is 2mm with the surface spacing of growth source material 405 using the drain as transistor.The thickness 4mm of growth source material 405, is physical vapor transport
(PVT) the 6H-SiC crystal of growth, without deliberate N doping, leaded wastewater is in 1x1017cm-3.Growth room 402 also has gas off-take
407 and air intake duct 403, directly it is connected with growth chamber 422, substrate 411 is embedded in the single graphite blocks of the correspondence of periphery 408.The latter can
For introduction to high-purity gas, so as to dilute background doped.Air intake duct 403 is made up of molybdenum tube material (top) and stainless steel, internal diameter
Substantially two millimeters, connected by one section of BN earthenware.Radiation Temperature Measurement Instrument 418 is arranged at the bottom of growth room 402, for measuring and controlling
The temperature of growth room processed.
Pass through interface 413 so that vacuum chamber 401 is connected with vavuum pump, via the vertical (diameter of gas off-take 407:1mm),
So as to control in growth room 402 and growth chamber 422 (upper surface of growth source material 405 and the aufwuchsplate formation space with substrate 411)
Air pressure.Gas off-take 407 totally 12, it is symmetrical in circle.Because substrate 411 and source expect that 405 gaps are small, airflow direction will be flat
Row is in their surface.
Growing chamber cap 406 has vertical optical channel 415 (diameter 2mm)." white light " system to Laytech is used as light intensity
With the hardware and software of spectrum analysis.White light (the wavelength of focusing:The 450-700nm) (diameter of collimated light beam 409:1mm), that is, detect
Light 409, via the light gateway 414 on vacuum chamber 401, by optical channel 415, and passes through the (diameter of thermal conductor 410:6mm、
Thickness:The aufwuchsplate and growth material of substrate 411 2mm) are reached, is then back to, thickness, table for measuring growth material in real time
The thick perceived noisiness and temperature in face etc..
2) growth course includes:
I) internal pressure of vacuum chamber 401 is dropped to~10-7MBar, and maintain half an hour.Then via air intake duct 403 and very
Empty room air inlet pipe 421 is passed through high-purity hydrogen, then drops internal pressure.It is repeated twice, so as to reduce background doped.
Ii) gas entered via air intake duct 403 is changed into high-purity gas Ar:H2=1:1 (volume ratio), vacuum chamber 401
Air pressure is gradually raised to 700mbar, and is warming up to 1700 DEG C, and constant temperature 10 minutes.Then, air pressure is reduced to 2mbar, and air-flow is kept
In 1-5SLM (standard liter/min), and it is warming up to~2000 DEG C, starts SiC of the growth like intrinsic semiconductor.And growth chamber 422
Air pressure be higher by~10-50mBar than this air pressure.Thermograde~100 DEG C of growth chamber 422/cm, this can be used
The temperature that Laytec equipment is measured, compared with the temperature that bottom Radiation Temperature Measurement Instrument 418 is measured.If growth rate is not enough, gas
Body cooling growth chamber cap 406.Growth rate is up to 0.05mm/h.So as to formation~0.15mm on the aufwuchsplate of substrate 411
Thick film, wherein N doping concentrations can be reduced to~3x1015cm-3, i.e., the SiC of approximate intrinsic semiconductor.Ar/H can be adjusted2's
Volume ratio and flow, are adjusted to doping concentration.
Example 2:Grow sandwich construction SiC epitaxial films
Using one using gas phase transmission, sensing heating growing system, Fig. 5 is its section.
Grower:Metal vacuum room 401 is made by stainless steel;Its wall can be passed through cooling water;And cut with vavuum pump
Interface 413 and light gateway 414.Internal capacity is:Diameter phi 80cm x 80cm.
Using 4 insulation, relatively adiabatic aluminium oxide ceramics rod (bottom) and molybdenum tube (top) 412,15cm altogether, directly
Footpath φ 3cm, whole growth room 402 are fixed on the bottom surface of vacuum chamber 401.And in induction heating apparatus (the i.e. high frequency of water cooling
Coil) between 404 and growth room 402, add quartz ampoule 416 and have the graphite foam 417 of drilling (~2cm is thick).The former plays
Insulating effect, the latter plays heat insulating function.Many 0.5mm drilling is deliberately formed in graphite foam, is conducive to foreign gas
Overflow.Because among vacuum, heat radiation loss is main thermal losses, therefore can also be in induction heating apparatus 404 and vacuum
Between room 401, plus last layer Mo thin layers, play insulation effect.It is another to have cooling feed channel 419, it is passed through gas into vacuum chamber 401
Body, the temperature of reduction growth chamber cap 406, controls the temperature difference, so as to change growth rate.
Growth room 402 (overall diameter 32cm), including growth chamber cap 406 (thick 10cm) is made by high-purity, high-density graphite,
Inner surface has TaC coating (~10 microns), so as to prevent the impurity in graphite from entering growth chamber 422.Their thick 5cm appearance
Layer has thickly dotted diameter 0.5mm, vertically or horizontal drilling, plays heat insulating function.The base thickness of growth room 402
12cm, side thickness 10cm.Substrate 411 for twin polishing 2 ", 8 °-beveling, Si- faces 4H-SiC, leaded wastewater 3x1018cm-3, can be with
It is 2mm with the surface spacing of growth source material 405 as the drain of transistor.The thickness 4mm of growth source material 405, is physical vapor transport
(PVT) the 6H-SiC crystal of growth, without deliberate N doping, leaded wastewater is in 1x1017cm-3.Growth room 402 also has gas off-take
407 and air intake duct 403, directly it is connected with growth chamber 422.The latter can be used for introducing high-purity gas or impurity gas.Air intake duct
403 are made up of molybdenum tube material (top) and stainless steel, and substantially two millimeters of internal diameter is connected by one section of BN earthenware.Growth room 402
Bottom have Radiation Temperature Measurement Instrument 418, the temperature for measuring and controlling growth room 402.
Pass through interface 413 so that vacuum chamber 401 is connected with vavuum pump, via the vertical (diameter of gas off-take 407:1mm),
So as to control in growth room 402 and growth chamber 422 (upper surface of growth source material 405 and the aufwuchsplate formation space with substrate 411)
Air pressure.Gas off-take 407 totally 12, it is symmetrical in circle.Because substrate 411 and source expect that 405 gaps are small, airflow direction will be flat
Row is in their surface.
Growing chamber cap 406 has vertical optical channel 415 (diameter 2mm)." white light " system to Laytech is used as light intensity
With the hardware and software of spectrum analysis.White light (the wavelength of focusing:The 450-700nm) (diameter of collimated light beam 409:1mm), that is, detect
Light 409, via the light gateway 414 on vacuum chamber 401, by vertical optical channel 415, and passes through the (diameter of thermal conductor 410:
6mm, thickness:The aufwuchsplate and growth material of substrate 411 2mm) are reached, is then back to, the thickness for measuring growth material in real time
The thick perceived noisiness and temperature on degree and surface etc..
2) growth course includes:
I) internal pressure of growth chamber is dropped to~10-7MBar, and maintain half an hour.Then via air intake duct 403 and vacuum
Room air inlet pipe 421 is passed through high-purity hydrogen, then drops internal pressure.It is repeated twice, so as to reduce background doped.
Ii) gas entered via air intake duct 403 is changed into high-purity gas Ar:H2=1:1 (volume ratio), vacuum chamber 401
Air pressure is gradually raised to 700mbar, and is warming up to 1700 DEG C, and constant temperature 10 minutes.Then, air pressure is reduced to~2mbar, and air-flow is protected
Hold in 1-5SLM (standard liter/min), and be warming up to~2000 DEG C, start SiC of the growth like intrinsic semiconductor.And growth chamber
Air pressure is higher by~10-50mBar than this air pressure.Thermograde~120 DEG C of growth chamber/cm, this can use Laytec to set
The standby temperature measured, compared with the temperature that bottom is measured.If the temperature difference is inadequate, it is possible to reduce growth room 406 cover thickness or
Chamber cap 406 is grown with gas cooling.Growth rate is reachable~0.05mm/h.So as to the thickness of formation~0.15mm on substrate 411
Film, wherein N doping concentrations can be reduced to~3x1015cm-3, i.e., the SiC of approximate intrinsic semiconductor.Ar/H can be adjusted2Body
Product ratio and flow, are adjusted to doping concentration.
Iii current-diffusion layer) is grown:In Ar/H2In gas, 1% N is mixed into2, form big to 200nm thickness, high N doping
N+-SiC, be used as Electron Extended layer.Afterwards, N is closed2, and use Ar/H2In gas, the pressure of growth chamber 422 is brought up to
500mbar;Then reduction air pressure is to~2mbar, so as to reduce the remaining N in growth chamber 4222Concentration.
Iv) the p-type SiC of growth Ga doping:1SLM H2, it is passed through trimethyl gallium (C6H18Ga2, TMGa) and bubbler (temperature
Degree:0 DEG C), then via air intake duct 403, into growth chamber 422, doping concentration reaches~2x1018cm-3, form thick 1.5 microns
Ga:SiC.Afterwards, corresponding H is closed2, and use Ar/H2The pressure of growth chamber, is brought up to 500mbar by gas;Then reduce
Air pressure is to~2mbar.So as to reduce the concentration of the remaining Ga in growth chamber 422.Ga diffusion coefficients are smaller, it is easy to thereon
It is square into low Ga electron channels.
V) growth is without the SiC electron channels deliberately adulterated, and 80nm is thick.
Such structure will simplify SiC DMOSFET manufacture crafts, and ensure electron channel electron mobility, so as to reduce
The loss of transistor.Now, the substrate that industry is generally used includes nearly intrinsic n-SiC thin layers (100 microns) and highly doped n
+ SiC growth substrates.Therefore, it is necessary to using ion beam implantation, Al or it is injected into nearly intrinsic n-SiC thin layers, forms p-
Type SiC;Damage is caused to the nearly intrinsic uppermost superficial layers of n-SiC simultaneously.Therefore, SiC DMOSFET interior resistance increase,
Loss increases simultaneously.In addition, in order to increase operating current, it is necessary to increase the voltage on grid, so as to reduce the reliability of device.
The above-mentioned sandwich construction formed using the present invention, ion beam mutation is without influenceing electron channel.Its substantially process is as follows:1) formed
One protective layer;2) first layer ion beam mutation mask is formed with photoetching and evaporation, and exposes DMOSFET interface and electronics
Source region;3) nitrogen ion beam injection electronics source region and interface;4) second layer ion beam mutation mask is formed with photoetching and evaporation, exposure
Go out interface and cover electronics source region;5) nitrogen ion beam injection interface, Ga:SiC becomes n-type material.So avoid accurately
Photoetching process, and ensure that the symmetry of DMOSFET structures.
Claims (10)
1. a kind of Material growth device of use gas phase transmission, including vacuum chamber and growth room, the growth room are placed in described true
In empty room, the growth room includes gas off-take and at least two inner surfaces, and two inner surfaces are respectively used to shelve required growth
Expect and substrate in source;The growth source material at least include upper surface and and lower surface, upper surface and the substrate phase of the growth source material
To and lower surface is then contacted with growth room;The substrate at least includes aufwuchsplate and the back side, the back side and growth room of the substrate
Contact and aufwuchsplate is relative with growth source material, form growth chamber between the upper surface of the growth source material and the aufwuchsplate of substrate;
It is characterized in that:Upper surface, the aufwuchsplate of substrate, growth room and the gas off-take of the growth source material are arranged so that by the life
It is parallel with the aufwuchsplate of the substrate when air-flow that long source material is produced flows on the aufwuchsplate of the substrate.
2. as claimed in claim 1 using the Material growth device of gas phase transmission, it is characterised in that:The growth chamber or growth room
It is connected with air intake duct.
3. as claimed in claim 1 using the Material growth device of gas phase transmission, it is characterised in that:It is provided with the vacuum chamber
Induction heating apparatus.
4. as claimed in claim 1 using the Material growth device of gas phase transmission, it is characterised in that:The upper table of the growth source material
Face, be smaller than substrate growth face diameter 1/5 with the aufwuchsplate of substrate.
5. as claimed in claim 1 using the Material growth device of gas phase transmission, it is characterised in that:The gross area of the gas off-take
It is not more than 1/2 with the ratio of growth chamber lateralarea.
6. the Material growth device of gas phase transmission is used as any one of Claims 1 to 5, it is characterised in that:Described
On at least one inner surface of growth room, include the one or more of llowing group of materials:W, Mo, Ta, Nb, graphite, diamond, BN,
WC, MoC, TaC and NbC.
7. the Material growth device of gas phase transmission is used as any one of Claims 1 to 5, it is characterised in that:The life
Long source material includes one kind of llowing group of materials:SiC、GaN、Cd1-xZnxTe (0≤x≤1) and AlN.
8. a kind of side of grower formation material using such as use gas phase transmission according to any one of claims 1 to 7
Method, it is characterised in that:Comprise the following steps:1) the growth source material of purification needed for providing, the growth source material at least includes upper table
Face and lower surface;2) substrate needed for providing, the substrate at least includes aufwuchsplate and the back side, the upper surface of the growth source material
It is relative with the aufwuchsplate of substrate;3) the growth source material and substrate are placed so that the upper surface of the growth source material and substrate
Growth chamber is formed between aufwuchsplate;4) it is injected into when the growth source material is heated there is provided high-purity gas in the growth chamber,
And grown material is formed on the aufwuchsplate of substrate.
9. the method for formation material as claimed in claim 8, using gas phase transmission, it is characterised in that:The growth source material
Upper surface and substrate aufwuchsplate be smaller than substrate growth face diameter 1/5.
10. a kind of detection means of the Material growth of use gas phase transmission, for detecting using any in such as claim 1~7
The Material growth process of grower described in, it is characterised in that:Including be twin polishing substrate and thermal conductor, with
And for the optical channel by detection light, the substrate at least includes aufwuchsplate and the back side, the aufwuchsplate of the substrate is used for material
The growth of material;The thermal conductor is placed in the back side of the substrate;The detection light out of optical channel by rear, through the heat
Returned after conducting piece, substrate and the material of growth.
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CN113088924A (en) * | 2021-04-07 | 2021-07-09 | 南京工业大学 | CVD device capable of locally and directionally depositing SiC coating and deposition method |
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