CN114134558A - Method for manufacturing standard silicon wafer - Google Patents
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- CN114134558A CN114134558A CN202111420109.7A CN202111420109A CN114134558A CN 114134558 A CN114134558 A CN 114134558A CN 202111420109 A CN202111420109 A CN 202111420109A CN 114134558 A CN114134558 A CN 114134558A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 89
- 239000010703 silicon Substances 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 44
- 239000012086 standard solution Substances 0.000 claims abstract description 42
- 238000002791 soaking Methods 0.000 claims abstract description 30
- 238000004857 zone melting Methods 0.000 claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 28
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- XWROUVVQGRRRMF-UHFFFAOYSA-N F.O[N+]([O-])=O Chemical compound F.O[N+]([O-])=O XWROUVVQGRRRMF-UHFFFAOYSA-N 0.000 claims description 13
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 12
- 229910052796 boron Inorganic materials 0.000 claims description 12
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 11
- 229910052733 gallium Inorganic materials 0.000 claims description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- 239000011574 phosphorus Substances 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052785 arsenic Inorganic materials 0.000 claims description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 5
- 229910052787 antimony Inorganic materials 0.000 claims description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 15
- 239000004065 semiconductor Substances 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 description 64
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 32
- 239000013078 crystal Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 8
- 238000004364 calculation method Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 229910052732 germanium Inorganic materials 0.000 description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000005922 Phosphane Substances 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- 235000013290 Sagittaria latifolia Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000015246 common arrowhead Nutrition 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910000064 phosphane Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Images
Classifications
-
- 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
- C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
- C30B13/08—Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone
- C30B13/10—Single-crystal growth by zone-melting; Refining by zone-melting adding crystallising materials or reactants forming it in situ to the molten zone with addition of doping materials
-
- 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
- C30B29/02—Elements
- C30B29/06—Silicon
Abstract
The invention discloses a method for manufacturing a standard silicon wafer, and relates to the technical field of semiconductor manufacturing. One embodiment of the method comprises: taking out the silicon growth layer from the silicon rod; soaking the silicon growth layer in a standard solution doped with donor-acceptor elements; and taking out the silicon growth layer from the standard solution, and manufacturing the silicon growth layer by adopting a zone melting method, thereby obtaining the standard silicon wafer. The embodiment can solve the technical problem that a method for manufacturing a standard silicon wafer which can dope donor elements and acceptor elements and is applied to low-temperature Fourier infrared detection equipment does not exist.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a manufacturing method of a standard silicon wafer.
Background
At present, in the related patent documents, a preparation method for manufacturing a low-temperature Fourier infrared standard wafer is not found, while the existing main method for manufacturing a silicon single crystal is a zone-melting gas phase doping and smearing method, in the patent document ZL 02159135.0, a phosphane gas phase is used for doping single crystal silicon manufactured by zone melting, the method mainly realizes the purposes of avoiding a middle-irradiation process and realizing the production of low-resistance single crystal, but the method has high requirements on equipment, and has single dopant and high concentration; in addition, ZL 200510014891.7 relates to a germanium doping method for zone-melting single crystal silicon by a liquid coating method, which realizes the stability of the germanium doping process, but the method has certain limitations and only realizes the doping of germanium element.
In the process of implementing the invention, the inventor finds that at least the following problems exist in the prior art:
in the prior art, a method for manufacturing a standard silicon wafer which can dope donor elements and acceptor elements simultaneously and is applied to low-temperature Fourier infrared detection equipment does not exist.
Disclosure of Invention
In view of this, embodiments of the present invention provide a method for manufacturing a standard silicon wafer, so as to solve the technical problem that there is no method for manufacturing a standard silicon wafer that can dope donor elements and is applied to a low-temperature fourier infrared detection device.
In order to achieve the above object, according to an embodiment of the present invention, a method for manufacturing a standard silicon wafer is provided, including:
taking out the silicon growth layer from the silicon rod;
soaking the silicon growth layer in a standard solution doped with donor-acceptor elements;
and taking out the silicon growth layer from the standard solution, and manufacturing the silicon growth layer by adopting a zone melting method, thereby obtaining the standard silicon wafer.
Optionally, soaking the silicon growth layer in a standard solution doped with an acceptor donor element comprises:
and soaking the silicon growth layer in a standard solution doped with donor-acceptor elements, and keeping soaking in the standard solution for 2-144 hours.
Optionally, the soaking time of the silicon growth layer in the standard solution is 6-72 hours.
Optionally, the soaking time of the silicon growth layer in the standard solution is 12-48 hours.
Optionally, the donor-acceptor element is selected from one or more of boron, phosphorus, arsenic, indium, antimony, aluminum, and gallium.
Optionally, the doping concentration of the donor and acceptor elements is 0.01-5 mg/L.
Optionally, the doping concentration of the donor and acceptor elements is 0.2-0.5 mg/L.
Optionally, the standard solution is prepared by the following method:
mixing hydrofluoric acid and nitric acid to obtain a hydrofluoric acid-nitric acid solution;
and adding the donor element into the hydrofluoric acid-nitric acid solution to obtain a standard solution doped with the donor element.
Optionally, in the hydrofluoric acid-nitric acid solution, the mass percentage of the hydrofluoric acid is 5-20%, and the mass percentage of the nitric acid is 5-20%.
Optionally, the volume ratio of the hydrofluoric acid to the nitric acid is 1:4 to 1: 1.
One embodiment of the above invention has the following advantages or benefits: according to the embodiment of the invention, donor and acceptor elements with different concentrations are attached to the primary silicon body in a soaking mode, and then monocrystalline silicon wafers with different concentrations are manufactured by a zone melting method. The monocrystalline silicon wafer can be applied to the use of a reference wafer or a standard wafer, such as a standard silicon wafer applied to a low-temperature Fourier infrared detection device.
The embodiment of the invention can be used for manufacturing various doped standard silicon wafers with different concentrations, and the method has the main advantages of low requirement on equipment, no need of doping gas, traceability of doped standard substances, simple manufacturing process and easiness in operation.
Further effects of the above-mentioned non-conventional alternatives will be described below in connection with the embodiments.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts. Wherein:
FIG. 1 is a schematic diagram of a main flow of a method for fabricating a standard silicon wafer according to an embodiment of the present invention;
fig. 2 is a schematic view of a main flow of a method for manufacturing a standard silicon wafer according to a reference embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present invention are described below with reference to the accompanying drawings, in which various details of embodiments of the invention are included to assist understanding, and which are to be considered as merely exemplary. Accordingly, those of ordinary skill in the art will recognize that various changes and modifications of the embodiments described herein can be made without departing from the scope and spirit of the invention. Also, descriptions of well-known functions and constructions are omitted in the following description for clarity and conciseness.
In order to solve the technical problems in the prior art, the embodiment of the invention provides a method for manufacturing a standard silicon wafer.
Fig. 1 is a schematic view of a main flow of a method for manufacturing a standard silicon wafer according to an embodiment of the present invention. As an embodiment of the present invention, as shown in fig. 1, a method for manufacturing the standard silicon wafer may include:
step 101, taking out the silicon growth layer from the silicon rod.
And step 102, soaking the silicon growth layer in a standard solution doped with donor-acceptor elements.
And 103, taking out the silicon growth layer from the standard solution, and manufacturing the silicon growth layer by adopting a zone melting method, thereby obtaining a standard silicon wafer.
According to the embodiment of the invention, donor and acceptor elements with different concentrations are attached to the primary silicon body in a soaking mode, and then monocrystalline silicon wafers with different concentrations are manufactured by a zone melting method. The monocrystalline silicon wafer can be applied to the use of a reference wafer or a standard wafer, such as a standard silicon wafer applied to a low-temperature Fourier infrared detection device.
The embodiment of the invention can be used for manufacturing various doped standard silicon wafers with different concentrations, and the method has the main advantages of low requirement on equipment, no need of doping gas, traceability of doped standard substances, simple manufacturing process and easiness in operation.
Optionally, step 102 may comprise: and soaking the silicon growth layer in a standard solution doped with donor-acceptor elements, and keeping soaking in the standard solution for 2-144 hours, so that a standard silicon wafer with uniform doping concentration is obtained, doping is realized by a soaking mode, the manufacturing method is simple, the process is stable, and donor-acceptor elements with different concentrations and different types can be doped. The time period during which the silicon growth layer is soaked in the standard solution doped with the donor-acceptor element is typically, but not limited to, preferably 2 hours, 5 hours, 10 hours, 14 hours, 20 hours, 50 hours, 100 hours, 135 hours, 144 hours, and the like, in which the uniformity of the doping concentration can be improved in these embodiments, if the soaking time is too short, the uniformity of the doping concentration is affected, and if the soaking time is too long, the fabrication time is wasted.
Preferably, the soaking time of the silicon growth layer in the standard solution is 6-72 hours, and the soaking time of the silicon growth layer in the standard solution is controlled within 6-72 hours, so that the uniformity of the doping concentration can be ensured, the manufacturing time of the process can be shortened, and the time can be saved. Preferably, the soaking time of the silicon growth layer in the standard solution is 12-48 hours, and the soaking time of the silicon growth layer in the standard solution is controlled within 12-48 hours, so that the uniformity of the doping concentration can be ensured, the manufacturing time of the process can be shortened, and the time can be saved.
Optionally, the donor-acceptor element is selected from one or more of boron, phosphorus, arsenic, indium, antimony, aluminum and gallium, and the donor-acceptor element may be doped into the silicon growth layer in the embodiment of the present invention, so as to manufacture the standard silicon wafer with different doping concentrations and different donor-acceptor elements.
Optionally, the doping concentration of the donor-acceptor element is 0.01-5mg/L, which is helpful for doping the donor-acceptor element into the silicon growth layer, so as to dope the standard silicon wafer with the donor-acceptor element. It should be noted that the doping concentration of each donor-acceptor element can be controlled separately, and the concentration of each donor-acceptor element is 0.01-5 mg/L. Among them, the doping concentration of the donor-acceptor element is typically, but not restrictively, preferably 0.01mg/L, 0.5mg/L, 0.8mg/L, 1.1mg/L, 1.5mg/L, 2mg/L, 3.7mg/L, 5mg/L, etc., and in these embodiments, the uniformity of the doping concentration can be improved, and if the doping concentration is too small, the uniformity of the doping concentration is affected, and if the doping concentration is too large, the reagent is wasted.
Optionally, the doping concentration of the donor-acceptor element is 0.2-0.5mg/L, which is helpful for doping the donor-acceptor element into the silicon growth layer, so as to dope the standard silicon wafer with the donor-acceptor element.
Optionally, the standard solution is prepared by the following method:
mixing hydrofluoric acid and nitric acid to obtain a hydrofluoric acid-nitric acid solution;
and adding the donor element into the hydrofluoric acid-nitric acid solution to obtain a standard solution doped with the donor element.
In the embodiment of the invention, hydrofluoric acid and nitric acid are mixed according to a certain proportion to obtain a hydrofluoric acid-nitric acid solution, and when preparing acceptor standard solutions with different doping concentrations, the hydrofluoric acid-nitric acid solution is adopted for constant volume, so that the acceptor standard solution with the target concentration is obtained.
Optionally, in the hydrofluoric acid-nitric acid solution, the mass percentage of the hydrofluoric acid is 5-20%, and the mass percentage of the nitric acid is 5-20%, so that the silicon growth layer can be effectively etched, and the donor element and the acceptor element are uniformly doped into the etched silicon growth layer. And when the silicon growth layer is soaked in the standard solution doped with the donor element, the silicon growth layer is etched while being doped with the donor element, so that the standard silicon wafer with uniform doping concentration is obtained. Wherein the hydrofluoric acid is typically but not limited to preferably 5%, 8%, 16%, 20%, etc. by mass percent, and the nitric acid is typically but not limited to preferably 5%, 7%, 9%, 15%, 20%, etc. by mass percent, in these embodiments, the hydrofluoric acid-nitric acid solution can effectively etch the silicon growth layer.
Optionally, the volume ratio of the hydrofluoric acid to the nitric acid is 1:4-1:1, and the hydrofluoric acid-nitric acid solution prepared by adopting the volume ratio can effectively etch a silicon growth layer, so that the uniformity of doping concentration of donor and acceptor elements is ensured. Among them, the volume ratio of hydrofluoric acid to nitric acid is typically, but not limited to, preferably 1:4, 1:3, 1:2, 1:1, and the like.
To aid in understanding the inventive concept, several specific standard silicon wafer fabrication processes are presented below.
Example 1
The main equipment and raw materials are as follows:
the method comprises the following steps of zone melting furnace FZ-14-1, fume hood FisherPPCL-PVC customization, fume hood with acid discharge function, CryoSAS low-temperature Fourier infrared detector, etching basket, 68% ultrapure nitric acid, 48% ultrapure hydrofluoric acid, electronic primary polycrystalline silicon rod, N-type seed crystal carbon, oxygen less than or equal to 0.02ppma, boron, phosphorus less than or equal to 0.02ppba and 99.99999% argon.
As shown in fig. 2, the specific operation steps include:
1) sleeving a silicon growth layer with the diameter of 20mm and the length of 100mm on the growing polycrystalline silicon rod according to GB/T29057;
2) wiping the silicon growth layer with methanol, performing 18M omega ultrasonic cleaning for 20min, etching for 4min (the volume ratio of nitric acid to hydrofluoric acid is 4:1), cleaning with deionized water for 5min, and soaking in a standard solution (10% HF + 10% HNO) doped with 220ng/L boron, 2.0mg/L phosphorus, 120ng/L aluminum and 200ng/L gallium3) Soaking for 48 hours; the seed crystal is subjected to the same steps of ultrasound, etching and deionized water cleaning, the silicon growth layer and the seed crystal are taken out and then placed in a nitrogen drying box at 80 ℃ for drying, and the silicon growth layer and the seed crystal are placed in a transfer box after being dried for 30min and transferred to a zone melting chamber;
3) opening the zone melting furnace, cleaning the furnace chamber, a preheater and other parts by using a cleaning cloth, taking out the silicon growth layer and the etched seed crystal from the transfer box, installing the silicon growth layer and the etched seed crystal by using a clamp, adjusting a pull-up fixing frame and a seed crystal fixing head, closing a furnace door, vacuumizing according to a preset program, and filling argon gas;
4) turning on a generator, starting a filament voltage, popping out a preheater, inserting a source rod into the preheater, exposing the lower end of the source rod for 3mm, starting an upper shaft and a lower shaft to rotate (the rotation speed of the upper shaft is 2RPM, and the rotation speed of the lower shaft is 10RPM), adjusting the power to 36W (an I mode, and the I mode is power change caused by current change), preheating the end part of the source rod to become red, quickly raising the source rod, simultaneously reducing the power to 0, rebounding the preheater, switching the power to a U mode (the U mode is power change caused by voltage change), lowering the source rod to be more than about 3mm away from the top end of a coil, slowly raising the power to about 40W, and continuously preheating until the end part of the source rod forms a teardrop-shaped molten zone;
5) and slightly immersing the seed crystal into the source rod melting zone, and forming a conical melt at the bottom after contact. Heating the seed crystal, observing the color of the seed crystal, reducing the power setting when the seed crystal turns red, starting a lower shaft to pull up (about 2mm/min), pulling up an upper shaft by a double arrow head, observing that obvious sharp corners respectively appear on four edges of the seed crystal and the width of a melting zone is not more than that of the seed crystal, narrowing the neck (the diameter of the neck is less than or equal to 3mm and the length of the neck is more than or equal to 40mm), simultaneously pulling down the upper shaft and the lower shaft (the speed of the upper shaft is 1.5mm/min and the speed of the lower shaft is gradually increased to 15mm/min), adjusting the power and the pull-down speed of the upper shaft according to the state of the melting zone, ensuring the diameter of the neck to be stable, and enabling a solid-liquid line to be in the middle position of a coil;
6) after the step of necking is finished, the power is set at 36.5W, the upper shaft pull-down speed is set to be 1.8mm/min, the lower shaft pull-down speed is adjusted to be 6.5mm/min, the process is carried out after the length is gradually 200mm, the moving direction of the source rod is adjusted to be pull-up from pull-down, the speed is increased to be 12mm/min, and the power is reduced to be 30W until the source rod end is separated from the seed crystal end. And manually turning off the rotating buttons of the upper shaft and the lower shaft, stopping pulling up and down, and adjusting the power to zero.
7) After cooling for 5min, opening the furnace door, wearing new clean gloves, taking out the monocrystalline silicon piece, cutting the monocrystalline silicon piece with the diameter of 10mm into the monocrystalline silicon piece with the thickness of 3.0mm, and grinding and polishing.
8) And (3) placing the polished monocrystalline silicon wafer on a Fourier low-temperature infrared detector for detection.
Example 2
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 230ng/L boron, 1.8mg/L phosphorus, 125ng/L aluminum, and 210ng/L gallium.
Example 3
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 200ng/L boron, 2.4mg/L phosphorus, 130ng/L aluminum and 205ng/L gallium.
Example 4
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 210ng/L boron, 2.5mg/L phosphorus, 122ng/L aluminum, and 208ng/L gallium.
Example 5
The difference from the manufacturing method of example 1 is that: in step 2), the soaking time was 50 hours.
Example 6
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 212ng/L boron, 2.0mg/L phosphorus, 126ng/L aluminum and 220ng/L gallium.
The silicon growth layer before doping is placed on a Fourier low-temperature infrared spectrum detector to detect the content of donor and acceptor elements (boron, phosphorus, aluminum, arsenic, antimony and gallium), and the detection results are shown in the following table:
| examples | B(ppta) | P(ppta) | Al(ppta) | As(ppta) | Sb(ppta) | Ga(ppta) |
| Example 1 | <10 | <10 | <10 | <10 | <10 | <10 |
| Example 2 | <10 | <10 | <10 | <10 | <10 | <10 |
| Example 3 | <10 | <10 | <10 | <10 | <10 | <10 |
| Example 4 | <10 | <10 | <10 | <10 | <10 | <10 |
| Example 5 | <10 | <10 | <10 | <10 | <10 | <10 |
| Example 6 | <10 | <10 | <10 | <10 | <10 | <10 |
The monocrystalline silicon wafer prepared in the above embodiment is placed on a fourier low-temperature infrared spectrum detector to detect the content of donor element, and the detection results are shown in the following table:
the data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafers is proved to be uniform and stable and can be used as a standard silicon wafer.
Example 7
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 150ng/L boron and 300ng/L gallium.
The monocrystalline silicon wafer prepared in this example was placed on a fourier low-temperature infrared spectrometer to detect the content of donor element, and the detection results are shown in the following table:
| examples | B(ppta) | Ga(ppta) |
| Example 7 | 115.90 | 251.03 |
The data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafer is proved to be uniform and stable and can be used as a standard silicon wafer.
Example 8
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 50ng/L boron, 190ng/L gallium and 400ng/L arsenic.
The monocrystalline silicon wafer prepared in this example was placed on a fourier low-temperature infrared spectrometer to detect the content of donor element, and the detection results are shown in the following table:
| examples | B(ppta) | Ga(ppta) | As(ppta) |
| Example 8 | 35.42 | 153.77 | 325.49 |
The data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafer is proved to be uniform and stable and can be used as a standard silicon wafer.
Example 9
The difference from the manufacturing method of example 1 is that: in step 2), the donor-acceptor concentration in the standard solution is: 500ng/L phosphorus, 50ng/L aluminum and 20ng/L gallium.
The monocrystalline silicon wafer prepared in this example was placed on a fourier low-temperature infrared spectrometer to detect the content of donor element, and the detection results are shown in the following table:
| examples | P(ppta) | Al(ppta) | Ga(ppta) |
| Example 9 | 354.75 | 32.16 | 12.27 |
The data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafer is proved to be uniform and stable and can be used as a standard silicon wafer.
Example 10
The difference from the manufacturing method of example 7 is that: in step 2), the soaking time was 20 hours.
The monocrystalline silicon wafer prepared in this example was placed on a fourier low-temperature infrared spectrometer to detect the content of donor element, and the detection results are shown in the following table:
| examples | B(ppta) | Ga(ppta) |
| Example 10 | 102.33 | 235.19 |
The data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafer is proved to be uniform and stable and can be used as a standard silicon wafer.
Example 11
The difference from the manufacturing method of example 8 is that: in step 2), the soaking time was 64 hours.
The monocrystalline silicon wafer prepared in this example was placed on a fourier low-temperature infrared spectrometer to detect the content of donor element, and the detection results are shown in the following table:
| examples | B(ppta) | Ga(ppta) | As(ppta) |
| Example 11 | 38.25 | 162.36 | 338.04 |
The data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafer is proved to be uniform and stable and can be used as a standard silicon wafer.
Example 12
The difference from the manufacturing method of example 9 is that: in step 2), the soaking time was 72 hours.
The monocrystalline silicon wafer prepared in this example was placed on a fourier low-temperature infrared spectrometer to detect the content of donor element, and the detection results are shown in the following table:
| examples | P(ppta) | Al(ppta) | Ga(ppta) |
| Example 12 | 366.21 | 34.86 | 13.67 |
The data were measured 4 times for each single crystal silicon wafer, and the results are shown in the following table:
through calculation, the RSD is less than 10 percent, and the doping concentration of the monocrystalline silicon wafer is proved to be uniform and stable and can be used as a standard silicon wafer.
Therefore, the embodiment of the invention can realize simultaneous doping of various donor elements and realize doping with different concentration gradients according to actual needs, and the monocrystalline silicon wafer manufactured by the embodiment of the invention can be used for a reference wafer or a standard wafer of low-temperature infrared or normal-temperature infrared and can also be used for establishing measurement systematic analysis of detection equipment.
The above-described embodiments should not be construed as limiting the scope of the invention. Those skilled in the art will appreciate that various modifications, combinations, sub-combinations, and substitutions can occur, depending on design requirements and other factors. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for manufacturing a standard silicon wafer is characterized by comprising the following steps:
taking out the silicon growth layer from the silicon rod;
soaking the silicon growth layer in a standard solution doped with donor-acceptor elements;
and taking out the silicon growth layer from the standard solution, and manufacturing the silicon growth layer by adopting a zone melting method, thereby obtaining the standard silicon wafer.
2. The method of claim 1, wherein immersing the silicon growth layer in a standard solution doped with an acceptor donor element comprises:
and soaking the silicon growth layer in a standard solution doped with donor-acceptor elements, and keeping soaking in the standard solution for 2-144 hours.
3. The method of claim 2, wherein the soaking time of the silicon growth layer in the standard solution is 6-72 hours.
4. The method of claim 3, wherein the soaking time of the silicon growth layer in the standard solution is 12-48 hours.
5. The method of claim 1, wherein the donor-acceptor element is selected from one or more of boron, phosphorus, arsenic, indium, antimony, aluminum, and gallium.
6. The method according to claim 5, wherein the doping concentrations of the donor-acceptor elements are each 0.01 to 5 mg/L.
7. The method according to claim 6, wherein the doping concentrations of the donor-acceptor elements are each 0.2 to 0.5 mg/L.
8. The method of claim 1, wherein the standard solution is prepared by the following method:
mixing hydrofluoric acid and nitric acid to obtain a hydrofluoric acid-nitric acid solution;
and adding the donor element into the hydrofluoric acid-nitric acid solution to obtain a standard solution doped with the donor element.
9. The method according to claim 7, wherein the hydrofluoric acid and the nitric acid are contained in the hydrofluoric acid-nitric acid solution in a mass ratio of 5 to 20% and 5 to 20% respectively.
10. The method of claim 9, wherein the volume ratio of the hydrofluoric acid to the nitric acid is 1:4 to 1: 1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1749448A (en) * | 2005-08-30 | 2006-03-22 | 河北工业大学 | Germanium blending method for zone-melting silicon monocrystal by liquid smearing method |
| JP2014156376A (en) * | 2013-02-18 | 2014-08-28 | Shin Etsu Handotai Co Ltd | Method of producing silicon single crystal and method of producing silicon single crystal wafer |
| CN104979168A (en) * | 2014-04-08 | 2015-10-14 | 无锡华润华晶微电子有限公司 | Platinum doping method in fast-recovery diode preparing technologies |
| CN104979192A (en) * | 2014-04-08 | 2015-10-14 | 无锡华润华晶微电子有限公司 | Method of preparing silicon chip material with platinum composite center |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1749448A (en) * | 2005-08-30 | 2006-03-22 | 河北工业大学 | Germanium blending method for zone-melting silicon monocrystal by liquid smearing method |
| JP2014156376A (en) * | 2013-02-18 | 2014-08-28 | Shin Etsu Handotai Co Ltd | Method of producing silicon single crystal and method of producing silicon single crystal wafer |
| CN104979168A (en) * | 2014-04-08 | 2015-10-14 | 无锡华润华晶微电子有限公司 | Platinum doping method in fast-recovery diode preparing technologies |
| CN104979192A (en) * | 2014-04-08 | 2015-10-14 | 无锡华润华晶微电子有限公司 | Method of preparing silicon chip material with platinum composite center |
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