US3669757A - Method of making and using diced single crystal impurity source - Google Patents

Method of making and using diced single crystal impurity source Download PDF

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Publication number
US3669757A
US3669757A US21798A US3669757DA US3669757A US 3669757 A US3669757 A US 3669757A US 21798 A US21798 A US 21798A US 3669757D A US3669757D A US 3669757DA US 3669757 A US3669757 A US 3669757A
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Prior art keywords
crystal
resistivity
dice
diced
melt
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US21798A
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English (en)
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Morris Kaufmann
Bernard R Shultz
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International Business Machines Corp
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International Business Machines Corp
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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
    • 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
    • C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
    • C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction

Definitions

  • a method for producing homogenous dilute dopant material for use in growing semiconductor device crystals of desired resistivity from a melt which includes the dilute dopant material comprises providing the dilute dopant material in single crystal alloy form, measuring the resistivity of the crystal along its length, cutting a portion of the crystal having resistivities within a desired range, slicing said portion, polishing, dicing and cleaning the' slices, and weighing out the required amount of diced dopant material as needed for the growth of a semiconductor device crystal of desired resistivity from a melt which includes the diced dopant material.
  • the growth of semiconductor material of desired resistivity is accomplished by first providing the semiconductor material in a very pure form and then adding accurately determined amounts of an appropriate impurity to achieve the desired resistivity.
  • the accuracy with which the wanted resistivity value is obtained is dependent upon the precision achieved in the introduction of the dopant material.
  • prior art methods of preparing the impurity material and for introducing the impurity material into the host semiconductor crystal do not produce acceptably uniform end results on the manufacturing floor.
  • Impurity source material traditionally is produced in powdered form which is weighed out in appropriate amounts according to the desired resistivity of the host crystal to be grown from a melt of highly purified semiconductor material and powdered impurity source material. It has been found, however, that the powdered source material comprises particles of relatively large and variable surface area having both absorbant and adsorbant properties which render them extremely susceptable to moisture and other contamination. The extremely small quantities of the powdered impurity material required for the growth of high resistivity semiconductor material particularly aggravates the problem of precisely ascertaining the correct amount of powder to achieve reproducible resistivity values in the end product host crystal.
  • the method of the present invention produces homogeneous dilute impurity source material in diced form of uniform size which does not attract moisture and other contamination which can be etch cleaned as necessary, and which is very convenient to weigh out in appropriate amounts to achieve precisely determined resistivities of the semiconductor device crystal to be grown from a melt including the impurity material.
  • the impurity material is first grown as a single crystal alloy, characterized for resistivity and cut into portions having resistivities within respective range. At least one of the portions is sliced into wafers, polished, diced and cleaned. An amount of diced impurity material required for the growth of a given Patented June 13, 1972 ice resistivity semiconductor device crystal is weighed out and included In the melt from which the device crystal is grown.
  • dilute dopant source material is provided in single crystal form.
  • Such single crystals may be procured from commercial vendors or may be grown by the user in accordance with well known crystal growth methods.
  • the single crystal dopant source is prepared for the resistivity measurement of step 2 by grinding to yield a crystal of uniform diameter. Resistivity measuring probes are brought into contact with the crystal surface parallel to the crystal axis to determine the resistivity of the crystal as a function of position along the length of crystal. The crystal then is cut transversely with respect to its longitudinal axis into portions in accordance with the measured resistivities. Each crystal portion is characterized by resistivity values within a predetermined range of values. Depending upon the requirements of the user, one or more of the portions are subjected to further processing in accordance with the present invention.
  • each portion of interest to the user is separately subjected to the additional steps 4-7.
  • step 4 each'portion is sliced into wafers.
  • the wafers are polished, diced and cleaned in step 5 in accordance with well known techniques or, optionally, they are first treated by steps 4A and 4B.
  • Steps 4A and 4B provide for the further characterization of the wafers by measuring the resistivities of the wafers (step 4A) and then segregating the wafers into respective :batches (step 4B) in accordance with their measured resistivities.
  • the wafer resistivity measurement and wafer segregation may be required where very tight resistivity control is required of the dopant source which cannot be reproducibly achieved solely by the bulk resistivity measurement of step 2.
  • either the batch of wafers yielded directly from step 4 or one of the wafer batches yielded from step 4B is polished, diced and cleaned in step 5.
  • Each of the additional wafer batches resulting from step 4B is separately processed in the same manner.
  • step 6 the required amount of dice is taken from the mixture of dice of an appropriate batch (from step 4 or from step 4B) and is included (step 7) in the melt from which the ultimately desired semiconductor device crystal is grown.
  • step 7 the amount of dilute dopant dice taken in step 6 is determined in accordance with the impurity concentration required in the semiconductor device crystal.
  • step 6 The precision with which the required impurity concentration is achieved depends, of course, on the accuracy with which the average resistivity of the dopant dice resulting from step 6 can be ascertained. It has been established that closely reproducible average resistivity values of dopant dice are obtained provided that the number of dice selected from a given batch in step 6 exceeds a minimum statistical number .and provided that the dice are adequately mixed within their respective batch. As previously mentioned, experience has shown that the conventional polishing, dicing and cleaning operations of step 5 provide sufficient mixing for many applications of the present invention.
  • step 6 Additional deliberate mixing may be introduced between steps and 6, if necessary. With adequate mixing, closely reproducible average resistivity values are achieved when at least 25 dopant dice are taken from a respective batch in step 6. It is convenient in the dicing operation of step 5 to cut a given wafer into individual dice of the order of a hundredth of an inch. Using such sized dice, the aforementioned twenty-five dice minimum quantity is exceeded several fold in constituting the dopant charge required for even the smallest semiconductor device crystal melts used in ordinary production runs.
  • the diced impurity source provided by the method of the present invention possesses a much smaller surface to volume ratio than the individual. particles of prior art pulverized dopant source material.
  • the dice exhibit a much reduced tendency to attract moisture and to react with oxygen and other contaminants than powdered source material. Moisture, in particular, is reduced in diced dopant material in relation to powdered dopant material.
  • the minimum surface area exhibited by the diced impurity material minimizes the probability of contamination While the impurity material is being processed and before it is put to use in doping a host crystal. Such minimum surface area, however, is no deterrent to the eflicient use of the desired impurities within the diced material because it is reduced to a melt along with the host semi conductor material when it is put to use.
  • said amount of dice is used by including said amount of 5 dice in a melt from which a semiconductor device crystal is grown. 3.
  • steps comprising:
  • said amount of dice is determined by weighing out the required amount of said dice as needed for the making of said semiconductor device crystal.
  • said dice of a respective batch are mixed before being used in the making of said semiconductor device crystal. 8. The method defined in claim 3 wherein: said amount of said dice exceeds 25.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Testing Or Measuring Of Semiconductors Or The Like (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
US21798A 1970-03-23 1970-03-23 Method of making and using diced single crystal impurity source Expired - Lifetime US3669757A (en)

Applications Claiming Priority (1)

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US2179870A 1970-03-23 1970-03-23

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US3669757A true US3669757A (en) 1972-06-13

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US (1) US3669757A (OSRAM)
JP (1) JPS5233468B1 (OSRAM)
DE (1) DE2114087A1 (OSRAM)
FR (1) FR2083895A5 (OSRAM)
GB (1) GB1326139A (OSRAM)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4342616A (en) * 1981-02-17 1982-08-03 International Business Machines Corporation Technique for predicting oxygen precipitation in semiconductor wafers
US4417943A (en) * 1980-06-26 1983-11-29 International Business Machines Corporation Method for controlling the oxygen level of silicon rods pulled according to the Czochralski technique
US4952425A (en) * 1987-11-27 1990-08-28 Ethyl Corporation Method of preparing high purity dopant alloys

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4789596A (en) * 1987-11-27 1988-12-06 Ethyl Corporation Dopant coated bead-like silicon particles
FI893246A7 (fi) * 1988-07-07 1990-01-08 Nippon Kokan Kk Foerfarande och anordning foer framstaellning av kiselkristaller.

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4417943A (en) * 1980-06-26 1983-11-29 International Business Machines Corporation Method for controlling the oxygen level of silicon rods pulled according to the Czochralski technique
US4342616A (en) * 1981-02-17 1982-08-03 International Business Machines Corporation Technique for predicting oxygen precipitation in semiconductor wafers
US4952425A (en) * 1987-11-27 1990-08-28 Ethyl Corporation Method of preparing high purity dopant alloys

Also Published As

Publication number Publication date
JPS5233468B1 (OSRAM) 1977-08-29
GB1326139A (en) 1973-08-08
FR2083895A5 (OSRAM) 1971-12-17
DE2114087A1 (de) 1971-10-14

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