CN103074672A - Gas phase epitaxial growth method of single crystal silicon - Google Patents
Gas phase epitaxial growth method of single crystal silicon Download PDFInfo
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- CN103074672A CN103074672A CN2013100021747A CN201310002174A CN103074672A CN 103074672 A CN103074672 A CN 103074672A CN 2013100021747 A CN2013100021747 A CN 2013100021747A CN 201310002174 A CN201310002174 A CN 201310002174A CN 103074672 A CN103074672 A CN 103074672A
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- 238000000034 method Methods 0.000 title claims abstract description 51
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 56
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 44
- 239000010703 silicon Substances 0.000 claims abstract description 44
- 238000003860 storage Methods 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims description 40
- 239000012808 vapor phase Substances 0.000 claims description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 12
- 238000000151 deposition Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 230000002950 deficient Effects 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 abstract 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 150000002500 ions Chemical group 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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Abstract
The invention discloses a gas phase epitaxial growth method of single crystal silicon and belongs to the semiconductor manufacturing field. The method can effectively solve problems that the single crystal silicon manufacturing process is complicated and the energy consumption is high. The method comprises steps: a, providing a substrate available for treatment; b, cleaning the substrate; c, providing a cavity for the epitaxial growth of the single crystal silicon, wherein a substrate storage device is arranged in the cavity, and the substrate is arranged on the substrate storage device; d, feeding reducing gas into the cavity, and adjusting the pressure and temperature in the cavity to be the needed pressure and temperature; e, feeding a gaseous silicon source into the cavity, and generating a sacrificial layer with a preset thickness on the substrate surface; f, forming a single crystalline silicon layer on the sacrificial layer; and g, separating the connection body of the single crystalline silicon layer and the sacrificial layer from the substrate. According to the gas phase epitaxial growth method of single crystal silicon, energy consumption and the complexity are reduced, the operation process is easily controlled, the production cost is reduced, and the method is suitable for large scale production.
Description
Technical field
The present invention relates to field of semiconductor manufacture, especially a kind of vapor phase epitaxial growth method of silicon single crystal.
Background technology
In recent years, Chinese photovoltaic cell output annual growth rate be 1-3 doubly, the ratio that photovoltaic cell output accounts for global output also by rose in 2002 1.07% 2008 nearly 15%.The efficient of the commercialization crystal silicon solar energy battery also 13%-14% before 3 years is brought up to 16%-17%.All in all, the international market share of Chinese solar cell and technological competitiveness significantly improve.Solar energy power generating can occupy the important seat of world energy sources consumption in the near future, not only wants the Substitute For Partial conventional energy resources, and will become the main body of world energy supplies.
In solar energy power generating, assembly mainly is comprised of solar cell, and silicon single crystal is the important raw and processed materials of making solar cell.At present, the method for making silicon single crystal mainly contains vertical pulling method and zone melting method, and what two kinds of methods were made all is silicon single crystal ingot usually, before making solar cell, also needs silicon single crystal ingot is cut, and this process has increased the energy consumption of equipment virtually.In general, the preparation process of two kinds of methods is wayward, and energy consumption and complexity are larger, and preparation technology falls behind, and cost is higher, is not suitable for scale operation.
Summary of the invention
Technical assignment of the present invention is the vapor phase epitaxial growth method that a kind of silicon single crystal is provided for above-mentioned deficiency of the prior art, and this kind vapor phase epitaxial growth method can effectively solve silicon single crystal complex manufacturing process and the higher problem of energy consumption.
The technical solution adopted for the present invention to solve the technical problems is: the vapor phase epitaxial growth method of this kind silicon single crystal may further comprise the steps: a, provide and can supply pretreated substrate; B, cleaning; C, provide and to supply the epitaxially grown cavity of silicon single crystal, be provided with the substrate storage apparatus in the cavity, substrate is positioned on the substrate storage apparatus; D, in cavity, pass into reducing gas, and pressure in the cavity and temperature are transferred to required pressure and temperature; E, in cavity, pass into gaseous state silicon source, and generate the sacrifice layer of preset thickness by gas-phase deposition at substrate surface; Described sacrifice layer is the defective silicon single crystal of lattice that tentatively generates at substrate surface, and namely some room is not filled up in the crystal; F, above sacrifice layer, form monocrystalline silicon layer; G, with putting into deionized water after substrate, sacrifice layer and the monocrystalline silicon layer cooling, separate with substrate by the linker of ultrasonic vibration with monocrystalline silicon layer and sacrifice layer.
In the vapor phase epitaxial growth method of described silicon single crystal, in step a, described is the monocrystalline silicon piece of structural integrity for pretreated substrate.
In the vapor phase epitaxial growth method of described silicon single crystal, in step b, the hydrogen peroxide system in the matting is adopted in described cleaning.
In the vapor phase epitaxial growth method of described silicon single crystal, in step c, described substrate storage apparatus is a monocrystalline silicon piece carrying disk, and it can effectively be separated substrate and cavity, is convenient to simultaneously substrate is processed.
In the vapor phase epitaxial growth method of described silicon single crystal, in steps d, described reducing gas is hydrogen, its role is to, and it can remove the silicon oxide of substrate surface; Pressure is 2 to 3 kPas in the described cavity; Temperature is 950 to 1200 degrees centigrade in the described cavity.
In the vapor phase epitaxial growth method of described silicon single crystal, in step e, described gaseous state silicon source is silane; Described chemical vapor deposition method is rpcvd technique, and temperature range is 600 to 700 degrees centigrade, and deposition pressure is 11 to 14 kPas; The preset thickness of sacrifice layer is 1 to 3 micron; This step silane flow rate is 13.1～17.5sccm, and the time is 30～50 seconds.
In the vapor phase epitaxial growth method of described silicon single crystal, in step f, this step silane flow rate is 7.0～7.88sccm, and temperature is 800-1000 degree centigrade, and pressure is 11 to 14 kPas.
The present invention has following outstanding beneficial effect:
1, owing in cavity, passing into gaseous state silicon source, and by the sacrifice layer of gas-phase deposition in substrate surface generation preset thickness, so it can effectively be kept apart monocrystalline silicon layer and substrate, because sacrifice layer is the preliminary defective silicon single crystal of lattice that generates at substrate surface, be that some room is not filled up in the crystal, therefore its structural instability also is convenient in the subsequent technique separation to monocrystalline silicon layer.
2, because this technique is carried out matting to substrate first, in subsequent technique, in body, pass into reducing gas again, and pressure in the cavity and temperature transferred to required pressure and temperature, so it can effectively remove the silicon oxide of substrate surface, get ready for next step technique simultaneously, and remove silicon oxide with physical method and compare, reduced cost and energy consumption.
3, owing to will put into deionized water after substrate, sacrifice layer and the monocrystalline silicon layer cooling, then separate with substrate by the linker of ultrasonic wave utilization stress wherein with sacrifice layer and monocrystalline silicon layer, so it is convenient and swift in the sepn process of silicon single crystal rod, easy to operate, reduce cost, be fit to scale operation.
Description of drawings
Accompanying drawing 1 is the schema of the vapor phase epitaxial growth method of silicon single crystal of the present invention;
Accompanying drawing 2 is preparation schematic diagram of the vapor phase epitaxial growth method of silicon single crystal of the present invention;
Accompanying drawing 3 is cross-sectional view of monocrystalline silicon layer of the present invention, sacrifice layer and substrate one;
Accompanying drawing 4 is cross-sectional view that the linker of monocrystalline silicon layer of the present invention and sacrifice layer separates with substrate;
Description of reference numerals: 1 cavity, 2 substrates, 3 substrate storage apparatus, 4 sacrifice layers, 5 monocrystalline silicon layers, 6 ultrasonic containers, 7 deionized waters.
Embodiment
Such as Fig. 1, Fig. 2, shown in Figure 3, the vapor phase epitaxial growth method of this kind silicon single crystal is at first carried out step S1, provides to supply pretreated substrate 2, and described substrate 2 is the monocrystalline silicon piece of structural integrity.
Then continue step S2, clean, the hydrogen peroxide system in the matting is adopted in described cleaning, concrete operation step is, be sulfuric acid with the composition ratio first with monocrystalline silicon piece: the Acidic Liquid of hydrogen peroxide=5: 1 or 4: 1 cleans, then wash with ultrapure water, be water with the composition ratio again: hydrogen peroxide: the alkaline cleaning fluid of ammoniacal liquor=5: 2: 1 or 5: 1: 1 or 7: 2: 1 cleans, it is water-soluble because the oxygenizement of hydrogen peroxide and the complexing action of ammoniacal liquor, many metal ions form stable soluble complexes; Then use composition than being water: hydrogen peroxide: the acidic cleaning solution of hydrochloric acid=7: 2: 1 or 5: 2: 1, because the oxygenizement of hydrogen peroxide and the dissolving of hydrochloric acid, and the complexing of chlorion, many metals generate water-soluble complex ion, thereby have reached the purpose of cleaning.
Then continue step S3, provide to supply the epitaxially grown cavity 1 of silicon single crystal, be provided with substrate storage apparatus 3 in the cavity 1, substrate 2 is positioned on the substrate storage apparatus 3; Described substrate storage apparatus 3 is a monocrystalline silicon piece carrying disk, and it can effectively be separated substrate 2 and cavity 1, is convenient to simultaneously substrate 2 is processed.
Then continue step S4, in cavity 1, pass into reducing gas, and cavity 1 interior pressure and temperature are transferred to required pressure and temperature; Described cavity 1 interior pressure is 2 to 3 kPas; Described cavity 1 interior temperature is 950 to 1200 degrees centigrade.In the present embodiment, described cavity 1 interior pressure is 2.565 kPas, and described cavity 1 interior temperature is 1170 degrees centigrade.
Then continue step S5, in cavity 1, pass into gaseous state silicon source, and by the sacrifice layer 4 of gas-phase deposition in substrate 2 Surface Creation preset thickness; Described sacrifice layer 4 is the defective silicon single crystal of lattice that tentatively generates at substrate surface, and namely some room is not filled up in the crystal.Described gaseous state silicon source is silane; Silane flow rate induces greatly, initially that the time is short, and then the monocrystalline silicon strip is wide, and a little less than polysilicon laterally spreads, but epitaxial layer quality is relatively poor, therefore can do sacrifice layer 4, and it helps separating of monocrystalline silicon layer 5 and substrate 2 in the subsequent technique; This step silane flow rate is 13.1～17.5sccm, and the time is 30～50 seconds; Silane flow rate is 14.1sccm in the present embodiment, and the time is 40 seconds.The temperature range of described chemical vapor deposition method is 600 to 700 degrees centigrade, deposition pressure is 11 to 14 kPas, and in the present embodiment, the temperature of chemical vapor deposition method is 690 degrees centigrade, deposition pressure is 13.227 kPas, and the preset thickness of described sacrifice layer 4 is 2 microns.
Then continue step S6, form monocrystalline silicon layer 5 above sacrifice layer 4, more excellent condition is: silane flow rate is 7.0～7.88sccm, and temperature is 800-1000 degree centigrade, and pressure is 11 to 14 kPas; In the present embodiment, silane flow rate is 7.5sccm, and temperature is 980 degrees centigrade, and pressure is 13.266 kPas, under this kind preparation condition, understands formation monocrystalline silicon layer 5 faster above sacrifice layer 4.
Then continue step S7, substrate 2, sacrifice layer 4 and monocrystalline silicon layer 5 are carried out naturally cooling, put into afterwards the ultrasonic container 6 that fills deionized water 7, by ultrasonic wave utilization stress wherein monocrystalline silicon layer 5 is separated, this kind method velocity of separation is fast, and effect is more satisfactory.
The vapor phase epitaxial growth method of silicon single crystal of the present invention, the preparation technology in cavity 1 are the stopping property operation.
The vapor phase epitaxial growth method of silicon single crystal of the present invention has reduced energy consumption and complexity, and operating process is easy to control, and has reduced process costs, is fit to scale operation.
The above is preferred embodiment of the present invention only, is not that the present invention is done any pro forma restriction.Any those of ordinary skill in the art are not breaking away from the technical solution of the present invention scope situation, all can utilize technology contents described above that technical solution of the present invention is made many possible changes and modification, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical solution of the present invention to any change modification, equivalent variations and modification that above embodiment makes, all belongs to the protection domain of the technical program according to technology of the present invention.
Claims (7)
1. the vapor phase epitaxial growth method of a silicon single crystal, it is characterized in that, may further comprise the steps: a, provide and to supply pretreated substrate b, clean c, provide and to supply the epitaxially grown cavity of silicon single crystal, be provided with the substrate storage apparatus in the cavity, and substrate is positioned on the substrate storage apparatus; D, in cavity, pass into reducing gas, and pressure in the cavity and temperature transferred to required pressure and temperature e, passes into gaseous state silicon source in cavity, and by gas-phase deposition substrate surface generate preset thickness sacrifice layer f, above sacrifice layer, form monocrystalline silicon layer; G, with putting into deionized water after substrate, sacrifice layer and the monocrystalline silicon layer cooling, separate with substrate by the linker of ultrasonic vibration with monocrystalline silicon layer and sacrifice layer;
Described sacrifice layer is the defective silicon single crystal of lattice that tentatively generates at substrate surface, and namely some room is not filled up in the crystal.
2. the vapor phase epitaxial growth method of a kind of silicon single crystal according to claim 1 is characterized in that, in step a, described is the monocrystalline silicon piece of structural integrity for pretreated substrate.
3. the vapor phase epitaxial growth method of a kind of silicon single crystal according to claim 1 is characterized in that, in step b, the hydrogen peroxide system in the matting is adopted in described cleaning.
4. the vapor phase epitaxial growth method of a kind of silicon single crystal according to claim 1, it is characterized in that, in step c, described substrate storage apparatus is a monocrystalline silicon piece carrying disk, it can effectively be separated substrate and cavity, is convenient to simultaneously substrate is processed.
5. the vapor phase epitaxial growth method of a kind of silicon single crystal according to claim 1 is characterized in that, in steps d, described reducing gas is hydrogen, and it can remove the silicon oxide of substrate surface; Pressure is 2 to 3 kPas in the described cavity; Temperature is 950 to 1200 degrees centigrade in the described cavity.
6. the vapor phase epitaxial growth method of a kind of silicon single crystal according to claim 1 is characterized in that, in step e, described gaseous state silicon source is silane; Described chemical vapor deposition method is rpcvd technique, and temperature range is 600 to 700 degrees centigrade, and deposition pressure is 11 to 14 kPas; The preset thickness of sacrifice layer is 1 to 3 micron; This step silane flow rate is 13.1～17.5sccm, and the time is 30～50 seconds.
7. the vapor phase epitaxial growth method of a kind of silicon single crystal according to claim 1 is characterized in that, in step f, this step silane flow rate is 7.0～7.88sccm, and temperature is 800-1000 degree centigrade, and pressure is 11 to 14 kPas.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109790642A (en) * | 2016-08-02 | 2019-05-21 | Qmat股份有限公司 | The seed chip that GaN is thickened is used for using gas phase or liquid phase epitaxy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1826434A (en) * | 2003-07-24 | 2006-08-30 | S.O.I.Tec绝缘体上硅技术公司 | Method of fabricating an epitaxially grown layer |
| CN1918697A (en) * | 2004-01-15 | 2007-02-21 | 独立行政法人科学技术振兴机构 | Process for producing monocrystal thin film and monocrystal thin film device |
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- 2013-01-06 CN CN2013100021747A patent/CN103074672A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1826434A (en) * | 2003-07-24 | 2006-08-30 | S.O.I.Tec绝缘体上硅技术公司 | Method of fabricating an epitaxially grown layer |
| CN1918697A (en) * | 2004-01-15 | 2007-02-21 | 独立行政法人科学技术振兴机构 | Process for producing monocrystal thin film and monocrystal thin film device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109790642A (en) * | 2016-08-02 | 2019-05-21 | Qmat股份有限公司 | The seed chip that GaN is thickened is used for using gas phase or liquid phase epitaxy |
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