TW536562B - Low defect density, vacancy dominated silicon - Google Patents

Abstract

The present invention relates to single crystal silicon, in ingot or wafer form, which contains an axially symmetric region in which vacancies are the predominant intrinsic point defect and which is substantially free of agglomerated vacancy intrinsic point defects wherein the first axially symmetric region comprises the central axis or has a width of at least about 15 mm and a process for the preparation thereof.

Description

536562 Printed by A7 of the Central Laboratories of the Ministry of Economic Affairs, Cooperating Consumers Co., Ltd. V. Description of the invention (tgg background The present invention is roughly based on the preparation of semiconductor-grade single-crystal rhenium, which is used in the electronics group = manufacturing: especially the present invention is about single-crystal silicon Blocks and wafers, which have θ lattice stations as king materials (axially symmetric regions, without condensed intrinsic point defects, and methods for their preparation. 〃 一 'Precious spar is one of the most important semiconductor electronic component manufacturing processes. The starting material j is usually prepared by the commonly known Chralski (ez) method. In this method, polycrystalline stone is used to melt and melt the material. And the growth. After the generation of a neck is completed, the diameter of the printed body is enlarged by slowing the rate of pulling the single crystal and / or the melting temperature until the required or mesh diameter is known. The cylindrical body of the crystal is then grown by controlling the rate of single crystal growth and the melting temperature, and supplemented by: reducing the degree of melting. Close to the end of the growth process, but before the crucible 7 is used up, the crystal diameter needs to be gradually reduced to form End cone, = cone is usually formed by increasing the pulling rate of single crystal and the heat supplied to the crucible. When the diameter becomes small enough, the crystal will leave the molten state. In recent years, many defects in single crystal silicon are known to The crystals are formed in the day-limb growth chamber after solidification and cooling. Part of this defect is caused by the existence of internal point defects in excess (that is, the concentration is above the limit of dissolution). This is the conventional lattice vacancy and row filling. Silicon crystals grown in a state of matter are generally grown with an excess of one or other intrinsic point defects, that is, crystal lattice-shaped crystal vacancies (v) or interstitial filling (I). It is recommended that the types of point defects in silicon and The initial concentration is judged at the curing time. If the concentration reaches a critical supersaturation in the system and the mobility of point defects is quite high, a reaction or a condensation phenomenon will be easy (please read the precautions on the back before filling this page) }

、 1T -4- 536562 A7 B7 printed by the Goods and Consumers Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (2) The condensed internal point defect in the second occurred in the manufacturing of complex and high-integrity circuits. Production volume.

Lattice vacancy type defects are generally recognized as the origin of visible crystal defects, such as D-shaped defects, streamlined defects (FPDs), gate oxide (G0I) defects, crystal original particle (cop) defects, and crystal original light spot defects ( LPIH) 'is a large-scale defect of a specific grade that can be observed by infrared scattering technology, such as using a scanning infrared microscope and laser scanning photography. Nucleiform defects are also present in the region of excessive lattice vacancies, becoming epoxidation stacking errors (〇ISF). It is speculated that this particular defect is the coagulation of high-temperature nucleated oxygen catalyzed by the presence of excessive lattice vacancies. The defects related to inter-row charging are rarely studied. It is usually regarded as the density of inter-row charging dislocation rings or networks. This defect is not related to gate oxide failure, which is an important criterion for wafer performance, but it is widely recognized It is the cause of the failure of other devices, and it is generally about the leakage problem. This desire exists in CzochralSk; the lattice vacancies in the L silicon and the desire for filling condensation defects between the rows generally range from about 1 * l03 / cm3 to iMOVcm3. This is a rapid increase, and in fact has now become a production limiting factor in the device manufacturing process. At present, there are mainly three ways to deal with the problem of condensed intrinsic point defects. The tenth formula includes a method for pulling single crystal technology to reduce the density of condensed intrinsic point defects in ingots. This method can be further subdivided into several methods, namely the method with single crystal pulling condition, which causes the generation of lattice vacancies as the main material, and the method with single crystal pulling condition, which results in the generation of interstellar filling as the main material. For example, the density of coagulation defects can be reduced by the following methods after suggestion. -5- This paper size applies Chinese National Standard (CNS) Λ4 specification (210X 297 mm) (Please read the precautions on the back before filling this page) t Γ 536562 Printed by the Central Bureau of Standards, Ministry of Economic Affairs, Consumers' Cooperatives ¾ A7 B7 V. Description of Invention (3) — Low: (i) Control V / G. In order to grow a crystal, the lattice-shaped lattice vacancies are mainly intrinsic point defects, and (ii) by changing (usually slowing down) the cooling rate of the silicon block from about 11001 to 1050 ^ during the single crystal pulling process, In order to change the nucleation rate of coagulation defects. Although this method can reduce the density of condensation defects, it cannot be avoided due to the requirements of device manufacturers. The more stringent, the existence of flaws will continue to be a major problem. Other methods also suggest slowing down the pulling rate of single crystal to below 0.4mm / min during the growth of the crystal body. However, this suggestion is not suitable, because the slow pulling of single crystal rate will lead to the reduction of various crystal pulling machines. The more important thing is that This pulling single crystal rate will result in the formation of single crystal silicon with a constant concentration of interstitial interstitials, and therefore the high concentration will cause the generation of condensation interstitial interstitial defects and all the problems associated with this defect. The second way to deal with the problem of condensed intrinsic point defects includes the method of dissolving or eliminating the condensed intrinsic point defects after generation. Generally speaking, it is achieved by heat treatment at the south temperature of the wafer-like seconds. For example, Fusegawa et al. As shown in European Patent Application No. 50381 / A1, silicon blocks are grown at a growth rate exceeding 0 8 mm / min, and wafers cut from the ingots at a temperature range of U5 (TC to 1280 ° C) are heat-treated to reduce access The density of defects in thin areas on the wafer surface. The specific treatment required is based on the concentration and location of the condensed spots in the wafer. Different wafers cut from a crystal have no uniform #directional defect concentration, Therefore, different post-growth processing conditions are required. In addition, the wafer heat treatment is relatively expensive, which may allow metal contaminants to enter the silicon wafer, and has no applicable effect on all crystal defects. The third method is inherent in the treatment of condensation The problem of point defects is made of single crystals. -6- This paper size applies the Chinese National Standard (CNS) Λ4 specification (2I0X29? Mm) (Please read the precautions on the back before filling this page)

Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives 536562 A7 ---: __ ___ B7 V. Description of the Invention ~~~~ '~' — Epitaxial deposition of thin stone crystalline layers on the wafer surface. This method provides The monocrystalline stone has a surface that is substantially free of condensed internal spots. However, epitaxial deposition increases the cost of the wafer. From the perspective of developments, it is necessary to use a method for preparing single crystal silicon to prevent the formation of intrinsic point defects in condensation, which is formed by inhibiting the condensation reaction at the time of production. It does not simply limit the formation rate of this defect or Only try to eliminate some blemishes after they are formed. The method of inhibiting the coagulation reaction can produce a silicon substrate which is approximately the typical intrinsic point of coagulation. This method also provides single crystal wafers with increased yield, which uses several integrated circuits required per wafer. Yes, without the high costs associated with epitaxial processes. SUMMARY OF THE INVENTION The object of the present invention is to provide an ingot-shaped or wafer-shaped single crystal silicon which has an axially symmetrical region with a substantially radial width, and does not substantially have lattice vacancies or silicon interstitial condensation. Generated flaws; and a method for preparing single crystal hard blocks, in which the concentration of lattice vacancies and interstitial filling is controlled to prevent intrinsic point flaws on one axis of the fixed diameter section of the ingot when the key block cools from the Guhua temperature Condensing into a symmetrical segment. Therefore, in short, the present invention refers to a single crystal silicon wafer having a center line, a front side and a back side, all of which are substantially perpendicular to the central axis, a ring side edge, and an extending from the central axis of the wafer to Measure the radius of the edge. The wafer contains a first axially symmetric region, in which the main wife of the lack of lattice vacancies is an intrinsic point defect and the crystal lattice S site is substantially defective. The first axially symmetric region includes a central axis or has a At least about 5 legs wide. The present invention also refers to a monocrystalline stone block, which has a central axis and a seed cone. 7- This paper size is applicable to the Chinese National Cricket (CNS) Λ4 specification (210X 297 mm) " ^ (Please read the back first (Notes for filling in this page)

536562 A7 B7 ------- ------------------------------ 5. Description of the invention (5), one end cone And a fixed diameter section between the seed cone and the end cone. The fixed diameter section has a ring side edge and a radius extending from the central axis to the ring side edge. The single crystal silicon block is characterized in that when the ingot grows and After cooling at the solidification temperature, the fixed-diameter section contains a first axially symmetric region, in which the lattice vacancies are mainly intrinsic point defects and are substantially free of condensed crystal lattice holes: intrinsic force point defects, where the first axial direction The symmetry zone includes the central axis or has a width of at least about 15 cm and has a length measured along the central axis of at least about 20% of the length of the fixed diameter section of the ingot. The invention also refers to a method for growing a single crystal fragment, wherein the key block includes a central axis, a seed cone, an end cone, and a fixed diameter section between the seed cone and the end cone. The fixed diameter section has A ring side edge and a radius extending from the centerline to the ring side edge. The ingot is grown from molten silicon and cooled at a self-curing temperature according to the Czochral method, which includes self-curing to not low during the growth of a fixed crystal. Control a growth rate v and an average axial temperature gradient G0 over a temperature range of about 1325 ° C to cause a first axially symmetric segment to generate Z. Where the ingot cools at the solidification temperature, the lattice vacancies are Is a major intrinsic point defect and is substantially free of condensation intrinsic point defects where the first axially symmetric region extends with a width of at least about 15 mils or contains a central axis. Other objects and features of the present invention will be made clear and specified later. Brief description of diagrams. Figure 1 is a chart showing examples of how the initial concentration ⑴ and [V] of row filling and lattice vacancies change as the ratio V / G0 increases. V is the growth rate and G is the average. Axial temperature gradient. (Please read the notes on the back before filling this page)

, 1T Printed by the Beijin Consumers Cooperative of the Central Bureau of Standards of the Ministry of Lijing-8-

536562 Central Bureau of Standards, Ministry of Economic Affairs ^: Printed by the Industrial and Consumer Cooperatives A7 B7 V. Description of the Invention (6) ^ Figure 2 is a chart that reveals the change in the free energy required to generate the defects between the lines of charging. Example of changing the initial concentration τ temperature τ Figure 3 is a chart that reveals the initial concentration 行 of interstitial charge and lattice vacancies, how to go along an ingot-block when v / G〇 値 decreases due to increase in G〇 値-Or 'Circle radius changes. It should be noted that at the V / I boundary, a transition phenomenon occurs from the lattice vacancy as the main material to the interspace charge as the main material. FIG. 4 is a top view of a single crystal silicon block or wafer, revealing that the lattice vacancy region V and the row interstitial region I are the main materials and the V / I boundary existing therebetween. Fig. 5 is a longitudinal cross-sectional view of a single crystal silicon block, showing in detail an axially symmetric region of a fixed diameter section of an ingot. … Figure 6 is a series of images of a small number of carriers #scanned by scanning a key block axially after heat treatment of a series of milks. It shows a roughly cylindrical lattice space as the main material area, and a generally circular row of interstitials. An axially symmetric region of the main material, a V / I boundary existing therebetween, and a condensed line defect region. Figure 7 is a graph of twisted single crystal rate (ie, seed crystal rise) as a function of crystal length, revealing how the pulled single crystal rate decreases linearly over a length of crystal. Fig. 8 is an image generated by scanning the axial life of a few ingots of a small number of carriers after a series of oxygen precipitation heat treatments, as described in Example 1. Figure 9 is a graph of the individual crystal length functions of a Simu single crystal silicon block with a pull single crystal rate. Table ′ silicon blocks are labeled 1-4 respectively to generate a curve v * (z), as described in the example. Figure 10 is the average axial temperature gradient (} at the melt / solid state 'interface. As a function of coincidence position, it is used for two different examples described in Example 2. -9- This paper scale applies China National Standard (CNS) Α4 specification (210X297 mm) (Please read the precautions on the back before filling this page} • —- ##.

、 1T Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives 1i 536562 A7 __________ V. Description of the Invention (7) Figure 11 is a graph of the initial concentration [V], [I] of the lattice vacancies or interrow filling as a function of the radial position For two different examples described in Example 2. Figure 12 is a graph using temperature as a function of axial position, revealing the axial temperature profile in an ingot used in Example 3 households and two different examples. FIG. 13 is a graph showing the intercharge density of A in detail, which is generated by the two cooling conditions shown in FIG. Fig. 14 is an image generated by scanning the whole ingot axial slice after a series of oxygen precipitation heat treatments, and the life of a few carriers, as described in Example 4. Figure 15 illustrates the position of the V / I boundary as a function of the length of the monocrystalline silicon block in a chart, as described in Example 5. Figure 16a: Scanning after a series of heat treatments in a series of "Oxygen" > A section of an ingot with a small distance from the shoulder of the key block about 100 to 250 legs is axially sliced from the life of a few carriers, as described in Example 6. . Fig. 16b is an image generated by scanning a small section of an ingot axially sliced from a small section of the ingot about 250 to 400 legs away from the ingot shoulder after a series of oxygen precipitation heat treatments, as shown in Example 6. Fig. 17 is an axial temperature gradient G. The graphs at different axial positions of an ingot are as described in Example 7. Fig. 18 is a graph of radial changes in the average axial temperature gradient at different positions of an ingot, as described in Example 7. FIG. 19 is a diagram illustrating the relationship between the width of the axial coupling region and the cooling rate, as described in Example 7. Fig. 20 is a series of copper ornaments and flaws. After the etching, a small section of the ingot is sliced axially from the shoulder of the ingot about 23 5 to 350 legs, as shown in Example 7. -10- This paper size applies to the Chinese National Standard (CNS) A4 specification (2 丨 0χ 297 mm) (Please read the precautions on the back before filling in this page j

536562 In the Ministry of Economic Affairs, the Bureau of Industry and Trade Cooperatives of the Panpan Bureau printed and cracked A7 B7. V. Description of the invention (8) Figure 21 series of copper ornaments and flaws after etching, one of the range from 305 to 460 legs from the shoulder of the ingot A photograph of axial sectioning of small ingots, as described in Example 7. Fig. 22 is a series of copper ornaments and flaws. After etching, a small section of the ingot is sliced axially from about 14 to 275 legs away from the ingot shoulder, as shown in Example 7. Fig. 23 is a series of copper ornaments and flaws. After etching, a small section of the ingot is axially sliced from 600 to 730 legs away from the shoulder of the ingot, as described in Example 7. FIG. 24 is a graph illustrating the radial change in the average axial temperature gradient, G0, which can occur in hot zones of different structures. Figure 25 graphically illustrates the axial temperature profile of an ingot in four different hot zone structures. Detailed description of the best example —— According to the experimental evidence, it is known that the type and initial concentration of intrinsic point defects are determined in advance, and the ingot self-curing temperature (ie, about 141.0%) is cooled to 1300. Above the temperature (ie at least about 1325. (:, at least about 135.0. 0 or even at least about 1375 ° C)), that is, the type and initial concentration of the defects are controlled by the v / G. Ratio, v is growing Speed · degree and G. It is the average axial temperature gradient in this temperature range. Refer to Figure 1. In order to increase v / Gg 一, a transition occurs from reducing row interstitial growth to increasing lattice vacancy mainly growth. Close to a critical 値 WG0, according to known data, it is approximately 2.1 valence ^^ Han, g is determined under the condition that the axial temperature gradient is constant within the above temperature range. At this critical ，, the internal The concentration of dot defects is in equilibrium. When v / GQ 値 exceeds the critical value, the concentration of lattice vacancies increases. Similarly, when V / G. 値 falls below the critical value, the concentration of row filling increases. -11 -This paper size applies to Chinese National Standard (CNS) Λ4 specification (210X297 mm) (Please read the precautions on the back before filling this page)

536562 A7 V. Description of the invention (9) Right / Chen reached the system (a critical degree of supersaturation, and if the mobility of spot cancer is quite high, a reaction or coagulation phenomenon should occur easily, and Shi Xizhong The condensed intrinsic point defect will seriously impact the material drop in the manufacture of complex and high-integration circuits. According to the present invention, it is found that the lattice voids in the broken matrix (reaction: reactions that produce defects in the condensed crystal lattice vacancies and silicon The reaction of row-to-row interstitial reaction in the matrix, which can cause coagulation and interstitial defect, can be suppressed. It is believed that the concentration of lattice vacancies and row-to-row interstitials can be applied during the growth and cooling of the crystal block in the process of the present invention, without being limited to any specific principle. Control so that the change in the free energy of the system does not exceed a critical threshold, which is the time when condensation reactions occur naturally and condensate lattice vacancies or interstitial defects are generated. In general, the reaction can be driven to cause condensate lattice vacancy defects Lattice vacancy point defects are formed or condensed interstitial defects are changed in the free energy of the system formed by interstitial atoms in single crystal silicon. AGv / I = kT ln (JV ^ L ⑴ [V / I〆

XI where △ Gv / I is the change in the free energy required to form a crystal lattice vacancy defect reaction or to form an interstitial defect response, k is the Boltzmann constant, T is the temperature, and the unit is K. '[V / I] is the concentration of available lattice vacancies or interstitial spaces at a point in space and time in single crystal silicon, and' [V / I] eq is the available lattice vacancies or interstitial spaces occurring [ V / I] and temperature T-like 12- (Please read the precautions on the back before filling this page) • Ji 1-J— · \ Printed by the Central Standards Bureau of the Ministry of Industry π Beigong Consumer Cooperatives? The standard of woody paper is applicable to Chinese national standard (<:] ^) 8 4 specifications (2) 0 '/ 297 mm) Printed by the Industrial and Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 536 562 A7 ________ B7 V. Description of the invention (ι〇 Γ " Equilibrium concentration at the same point in space and time in the state. According to this formula, in terms of a certain lattice vacancy concentration [V], the temperature reduction amount T is due to the sharp drop of [V;] eq with temperature. Δ Gv is generally increased. Similarly, in the case of a row of interstitial concentration [I], the temperature reduction amount T is roughly caused by [I] eq as the temperature drops sharply. — 一 'Figure 2 is a brief illustration △ h and concentration change of Shiyuki line filling for an ingot cooled at a solidification temperature without using some devices to suppress the concentration of Shiyake line filling. When the ingot is cooled, △ q is due to [I] Increasing supersaturation and increasing according to the formula (1), and the energy barrier used to condense the formation of interstitial defect is close to reaching, and when the cooling continues, this energy barrier is actually excessive, at this point it is A reaction occurs, which results in the formation of filling defects between coagulation lines and the accompanying decrease in △ Gz The supersaturation system is in the release state, that is, when the [I] concentration is reduced. Similarly, when an ingot is cooled at the self-solidification temperature and some devices are not used to suppress the lattice vacancy concentration, △ Gv is due to [V] The increased supersaturation increases according to formula (1), and the energy barrier used for the formation of crystal lattice vacancy defects is close to being achieved, and when the cooling continues, this energy barrier is actually excessive, and at this point it is A reaction occurs, which results in the formation of condensed crystal lattice vacancy defects and the accompanying reduction of △ Gv, and the supersaturated system is in a released state. The condensation of the lattice 2 and the interspace filling can be mainly based on the lattice vacancy and the interspace filling, respectively. It is avoided in the material area, and this selective bond block is cooled by the self-curing temperature, and it is achieved by keeping the free energy of the lattice 2 position system and the interstitial system to be less than that at the time of the condensation reaction. In other words, the system can Controlled so as not to cause critical supersaturation in lattice vacancies or inter-row charging. This can be achieved by -13-this paper wave scale applies Chinese National Standard (CNS) A4 specification (2 丨 0X29 * 7 mm) (please first Read the back (Please fill in this page again)

536562 A7 B7 Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Nuxi V. Description of the invention (U) ~ ^ The initial concentration of the crystalline lattice vacancies and the filling between rows was achieved (using v (Γ) control later in the article) to make It is quite low without reaching critical supersaturation. However, this concentration is difficult to achieve across the entire crystal radius during implementation. Therefore, the generally dangerous supersaturation phenomenon can be avoided by suppressing the initial lattice vacancies after the crystal is solidified; After establishing the initial concentration determined by v⑴. Surprisingly, it has been found that due to the large inter-row charge mobility and small lattice vacancy move rate of about 1 (Hcm 2 / sec), it can achieve the suppression of lattice vacancies and inter-row charge over a large distance. , I.e., a distance of about 5 to 1011 or more, the radial diffusion can be used to suppress the interstitial charge and the vacancy in the crystal as the main area. Lattice station < song degree, but it is necessary to assume that there is sufficient time to allow the m point of the internal point defect to diffuse to the ground. Generally, the 'diffusion time' depends on the radial change in the initial concentration of row filling and lattice vacancies. A smaller radial change requires a shorter diffusion time. The average axial temperature 埽 degree G is increased as a function of the radius of the single crystal silicon, which grows according to the Czochralski method, which means v / g〇 値 is not unitary when it crosses the radius of an ingot. The result is that the result is an intrinsic point ~ G, Γ :: degrees are not constant. If the WI boundary shown in Figures 3 and 4 When the boundary indicated by 2 reaches certain points along the ingot radius 4, the material is in full position by the crystal lattice. Mainly changed to interstitial charge ^. In addition, the ingot will contain interstitial charge Mawangzu material 6 feet and one car from Xiangpansen r / Jishan% 5 (The initial concentration of silicon interstitial atoms is to increase the radius Correspondence materials f ?, ^ and increase ^ means that the material department is mainly around the lattice vacancies-roughly cylindrical area; Ί .------ (Please read the precautions on the back before filling this page) Order The initial concentration of J0, I! -I · U in Japan and Japan is -14-

536562 Consumption Cooperation by Employees of the Central Bureau of Standards, Ministry of Economic Affairs, printed A7 B7 V. Description of Invention (12) Increased as a function of radius). When the ingot containing a V / I boundary cools down at the solidification temperature, the radial diffusion of interstitial atoms and lattice vacancies is caused by the reorganization of row interstitials and lattice vacancies, which causes the control direction in the V / I boundary to change inward. . In addition, the radial diffusion between the rows and the surface of the crystal will occur as the crystal cools. The watch guard of the crystal can maintain the defect concentration near the equilibrium point when the crystal cools. The radial diffusion of point defects easily reduces the V / I boundary. The interstitial concentration on the outer row and the lattice vacancy concentration on the inner side of the V / I boundary. Therefore, if there is sufficient time for diffusion, the concentration of lattice vacancies and interstitial spaces anywhere can be Δ Gv and Δ GI less than the critical thresholds at which the lattice vacancy condensation reaction and interstitial condensation reaction occur. — Please refer to FIG. 5. A single crystal silicon block 10 is grown according to the Czochralski method in the first example of the method of the present invention. The stone block includes a central axis 12, a seed cone 14, an end cone 16, and a The fixed diameter # 18 between the seed cone and the end cone. The diameter of the fixed foot has a ring side edge 20 and a radius 4 extending from the central axis n to the ring side edge 20. Solar growth conditions including growth rate v, horizontal and average axial temperature gradient G (), and cooling rate are best controlled to facilitate the formation of a line of interstitial axially symmetrical regions 6 and A lattice vacancy containing an axially symmetrical region 9 of a condensed intrinsic point flawless material is a substantially cylindrical region 8 of the main material. The axially symmetric region 9 has a width measured along a radius extending from the V / I boundary 2 to the axis 12. In one example of the present invention, it is at least about 15 mm in width, and the width is at least ingot fixed. The diameter section has a radius of 75%, preferably at least about 15%, more preferably at least about 25%, and most preferably at least about 50%. In a preferred example, the axially symmetric region 9 includes the ingot axis 12, which is the axial pair -15- (Please read the precautions on the back before filling this page}

Paper Λ4 Specifications Staff of the Central Bureau of Standards, Ministry of Economic Affairs, Consumer Cooperatives, sworn 536562 A7 _ _B7____ _ V. Description of the invention (13) The area 9 is consistent with the roughly cylindrical area 8 series. In other words, the ingot 10 includes a lattice space The substantially cylindrical region 8 of the main material, at least a part of which is free of condensation defects. In addition, the axially symmetric region 9 extends over at least about 20% of the length of the fixed diameter section of the ingot, preferably at least about 40%, more preferably at least about 60%, and most preferably at least about 80%. < A Λ axial symmetry zone 6 (if present) has approximately a width, measured from the ring side edge 20 toward the center axis 12 radially inward, and is at least about 30 of the radius of the fixed diameter section of the ingot %, In some examples at least about 40%, at least about 60%, or even at least about 80%. In addition, the axially symmetric region extends approximately at least about 20% of the length of the fixed diameter section of the ingot, preferably at least about 40%, more preferably at least about 60%, and most preferably at least about 80/0. The width of the axially symmetric regions 6, 9 may have some variations along the length of the central axis 12. Therefore, for an axially symmetric region of a given length, the width of the axially symmetric region 6 is determined by measuring the ingot 10 rings. The side edge 20 is determined to be the distance at a point farthest from the center axis. In other words, the measured width can determine the minimum distance within the predetermined length of the axially symmetric region 6. Similarly, the width of the axially symmetric region 9 is determined by measuring the distance at a point where the ν / Ι boundary 2 radially moves farthest from the center axis. In other words, the measured width can make the axially symmetric region 9 The minimum distance within a given length is determined. The growth rate ν and the average axial temperature gradient (as previously defined) are controlled such that the V / Gg ratio 値 ranges from approximately -0.5 to 25 times v / G. Critical 値 (that is, according to v / G. The critical 値 data obtained is about 丨 χ 1〇_5cm2 / sK ^ 5x 1〇-5cm2 / sK), and the v / GQ ratio 値 is preferably about 0.6 to 15 times V / G. Critical volume (that is, about 1.3 × 10-5cm2 / sKS3x 1〇-5cm2 / sK obtained from the critical volume data), -16-This paper size applies Chinese National Standard (CNS) 8 4 ^^ 210 > < 297 Mm ----- ~~ ·.; --- r ----- (Please read the notes on the back before filling this page)

1T 536562 Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the invention (14) The optimal I v / Gg ratio 値 ranges from about 75 to 25 times V / G. Critical 値 (i.e., about 16 > < 10-5 cmVsK to 2.1 x 10 · 5αη 2 / sK obtained from v / Gg critical 値 data). In a particularly preferred embodiment, v / G within the generally cylindrical region 8. It is at the v / Gq threshold and 1.1 times V / G. Critical 値. When the width of the axially symmetric region 9 is to be maximized, it is best to cool the solidification temperature of the block to more than about 1050X: for a period of time, that is, at least 5 hours, preferably at least about 10 hours, and more preferably At least about 5 hours, for silicon crystals with a nominal diameter of 150mm, (丨 丨) at least about 5 hours, preferably at least about 10 hours, more preferably at least about 20 hours, and more preferably at least about 25 hours, Most preferably at least about 30 hours, for use in crushed crystals with a nominal diameter of 200 mm, and (iii) at least about 20 hours, more preferably at least about 40 hours, more preferably at least about 60 hours, and most preferably At least about 75 hours' for silicon crystals with a nominal diameter of more than 200 legs. Cooling rate control can be achieved using a variety of conventional techniques to reduce heat transfer, including the use of insulators, heaters, heat shields, and magnetic fields. The control of the average axial temperature gradient can be achieved through the "hot zone" design of the crystal pulling single crystal machine, which is made of graphite (or other materials) such as heaters, heat insulators, heat and radiation hoods, and other objects. It depends on the production and model of the crystal pulling single crystal machine, and it is generally G. It can still be controlled by any device known in the art for controlling heat transfer between the molten / solid interface, including reflectors, heat sinks, wash tubes, light tubes, and heaters. Generally speaking, the radial change in 'can be greatly reduced by positioning this device within about a crystal diameter above the molten / solid interface, and G0 can also be controlled by adjusting the position of the device relative to the dissolved substance and the crystal. This is because the adjustment device is -17- This paper size is applicable to the Chinese National Standard (CNS) M specification (2 Euro M? Public Chu) (Please read the precautions on the back before filling this page)

536562 Printed by the Central Bureau of Standards, Ministry of Economic Affairs, Co-operative Society. A7 V. Description of Invention (15) ~ Position in the hot zone or adjust the position of the molten surface in the hot zone. In addition, when a heater is used, G0 can also be controlled by adjusting the supply of the moon to the heater. Any or all of the methods can be used during a batch of CzochralsKi process, where the volume of molten material It is completely discharged during the process. For some examples of the present invention, the average axial temperature gradient is preferably relatively constant and is a function of the ingot diameter. However, it should be noted that due to the improvements in the design of the hot zone, G0 can be changed the least. Therefore, it is related to a fixed birth rate: The mechanical item is gradually increasing as an important factor. This is because the growth process is becoming extremely sensitive to any change in the pull single crystal rate, and then directly affects the growth rate V. By process control, it means that the significant difference in the difference between the half position of the ingot and the ingot will result in a larger concentration between the rows that generally increase toward the edge of the wafer, thereby increasing the difficulty to avoid condensation. The generation of dot defects. From the previous perspective, the control involves reducing the radial change in G0 and achieving favorable process control conditions in the winter equilibrium. Therefore, after a crystal length of about one diameter, the pull single crystal rate range is about 0 2 To 〇8111111 / 111111, the pulling single crystal rate is preferably from 0.25 to 0.6 mm / min, and is desirably about 0.3 to 0.5 mm / mm. It should be noted that the pulling rate depends on both the crystal diameter and the crystal pulling rate. The foregoing range is generally used for 200-diameter crystals. Generally speaking, the pulling rate of single crystal will decrease due to the increase of crystal diameter. However, the single crystal pulling machine can be designed to allow the pulling single crystal rate to exceed the previous one. Therefore, it is best to design the crystal carrying single crystal machine so that The faster the single crystal rate is, the better, while still allowing an axially symmetric region to be generated according to the present invention. -18- The paper size is off --- ^ --- Γ --- II (Please read the notes on the back before filling this page), 11 Printed by the Central Standards Bureau of the Ministry of Economic Affairs, Industrial and Commercial Consumer Cooperatives 536562 A7 ____ B7 V. Description of the invention (16) The amount of inter-row interstitial diffusion is the temperature at which the ingot is cooled from the solidification temperature (approximately 1410r) to the temperature at which the inter-row interstitial method is moved. The precision is controlled by controlling the cooling rate. Silicon has more mobility at the curing temperature, which is about 1410 ° F. However, this mobility will decrease as the temperature of the single crystal silicon block decreases. Generally speaking, the diffusion between banks is slow to a considerable range-degree, making it impossible to move the general implementation time below 700 ° C, and even at 80 (Γ (:, 900 ° C, i〇〇). This is also true for 〇 ° C or i050 ° C. It should also be noted that, although the temperature at which the inter-row charge condensation reaction occurs can theoretically vary over a wide range of temperatures, in practice this range is for general czochralski-type growth. Silicon is narrower, which is due to the narrower initial row interstitial concentration range obtained in the second growth time of Czochchski method. Therefore, the intersegment condensation reaction can generally occur at about i 10 (In the temperature range from rc to 800 c, it is generally about 1050 ° C. In the temperature range where the row charge appears to be mobile, and depends on the temperature in the hot zone, the cooling rate is usually about 0lX: / min To 3.0 / min, the cooling rate is preferably about 0.1 c / min to / min, more preferably about 0 / min to 1 C / min 'and most preferably about O.rC / min to 0.5QC / min By controlling the cooling rate of the ingots within the temperature range that makes the inter-bank charge appear to be mobile, the inter-bank charge can get more It mainly diffuses to the grooves on the surface of the crystal, or to the lattice vacancies that make it extinct. Therefore, the concentration of interstitial I in this row can be suppressed to prevent the occurrence of condensation. It is used by controlling the cooling rate. The diffusion rate of line charging can relax the strict v / G0 requirement, which is necessary to take the axially symmetric region of the condensate defect. In other words, the cooling rate can be controlled in fact for the line charging There is a lot of time diffusion, relatively -19- Zhang scale is applicable (CNS) 7 ^^ 〇-χ 297 礼 礼 -----— (Please read the precautions on the back before filling this page)

Printed by the Central Standards of the Ministry of Economic Affairs, Consumers, and Cooperatives, printed by 536562 A7 --- ______B7 V. Description of Invention (17).-In the critical range of v / G〇, it can be accepted and used for acquisition-no condensation Axial symmetry area of the defect. In order to obtain this cooling rate at a considerable length of the fixed diameter section of the crystal, it is also necessary to consider the growth process of the end cone of the ingot, and the &lt; treatment when the ingot is grown. Generally, once the growth of the fixed diameter section of the ingot is completed, the single crystal pulling rate will increase and the taper required to form the end cone will begin. However, this increase in single crystal pulling rate will cause the bottom section of the fixed diameter section to Faster cooling within the temperature range where the intercharging can be fully moved. As a result, there is not enough time for the inter-row charging to spread to the trough to be extinct, that is, the concentration in this bottom section cannot be suppressed to a considerable degree 'and the condensation of inter-row filling defects may occur. In order to prevent this defect from being generated in the bottom section of the ingot, it is best that the fixed diameter section of the ingot has an average sentence thermal history according to the Czochralski method. _ The uniform thermal history can be used at a relatively constant rate. Obtained from a single crystal block, not only during the growth of the fixed diameter section, but also during the end cone growth of the crystal and possibly the subsequent end cone growth. A more solid enough rate can be obtained, for example, by reducing the crucible and crystal rotation rate during the growth of the end cone with respect to the crucible and crystal growth period during the growth of the fixed diameter section of the crystal, and / or (ii) increasing the heating during the end cone growth The energy supplied by the disintegrated heater is relative to the general energy supplied during the growth of the end cone. Other adjustments to process variables can occur individually or in combination. At the beginning of the growth of the anise 'cone, the pull single crystal rate of the terminal iridium is established, so that the temperature still exceeds about 1 050X: any small section of the fixed diameter section of the ingot can experience axial symmetry including one of the intrinsic point defects And the same thermal history of other small sections of the fixed diameter section of the ingot below. -20- This paper size applies to the Chinese National Standard (CNS) Λ4 specification (210X29 ^ 7gongchu) &quot; --- (Please read the precautions on the back before filling out this page}, 11 536562 He Gongxiao, Central Standards Bureau of the Ministry of Economic Affairs, printed A7 Cooperative Fifth, Invention Description (18): — ~~-As previously mentioned It shows that the lattice vacancies are the main area-the minimum radius is to suppress the condensed spots between condensation lines. The minimum radius 値 depends on ⑽r) and the cooling rate. Because the design of the crystal pulling single crystal machine and the hot zone will change, Therefore, the range for the WG. ⑴, the single crystal pulling rate, and the cooling rate will also change. Similarly, the conditions may also change along the length of the _growth crystal, and a change S is shown above, without condensing interline. The width of the main area should be as large as Large, so it is necessary to keep the completeness of this area as close as possible and not exceed the crystal radius and the difference between the minimum radius of the main area of the TO lattice vacancies along the length of the growing crystal in the existing crystal pulling single crystal machine. Directional symmetry zone 6, ideal width and required ideal crystal pulling single crystal rate profile used for known crystal pulling single crystal machine hot zone design can be determined by experiments, generally. This experimental method is about the axial temperature profile first. Obtain radial available data for ingots grown in a specific crystal pulling single crystal machine, and obtain radial changes in average axial temperature gradient for ingots grown in the same pulling single crystal machine In short, this data is used to pull single crystals-or polymorph single crystal silicon blocks, but it is like analyzing the existence of condensing interstitial defects. Based on this, an ideal pull single crystal rate profile can be determined. Figure 6 After a series of oxygen precipitation heat treatments to find the defect distribution pattern, scanning the axial life of a 200 mm diameter ingot with a section of a small number of carrier lifetimes, it illustrates a range, one of which is a nearly ideal pull single crystal rate The profile is used for the design of a known hot zone of a crystal pulling single crystal machine. In this example, the _ transition phenomenon occurs when v / G〇 (r) 値 (which causes condensation between rows) Generation of defect-filled area 28) to an ideal v / G with the largest width in an axially symmetric area. ⑴ 値. -21- This paper size applies to China National Standard (CNS) A4 (210X 297 mm) (Please read first Note on the back, please fill in this page again.) P * 衣 ·-口 536562 A7 V. Description of the invention (I9) In addition to increasing the radial change of G0 in the radius of the ingot, v / G0 also It can change in the axial direction due to the change of v, or the natural change of gg due to the process. In a standard Czochralski process, v is changed as the single crystal pulling rate is adjusted in the growth cycle to maintain the bond block. For a fixed diameter, various adjustments or changes in the pull single crystal rate are made _ and then ~~ is changed over the length of the fixed diameter section of the ingot. According to the process of the present invention, the single crystal pulling rate can be controlled to increase the width of the fixed diameter section of the ingot. However, the result is a change in the radius of the ingot. In order to ensure that the resulting ingot has a fixed diameter, it is best to grow the ingot to a length larger than the required long diameter. The ingot is then subjected to a standard process to remove excess material from the surface, thereby giving the key block a fixed diameter segment . In general, when the radial change of the axial temperature gradient Gg⑴ is minimized, it is easier to make the lattice vacancies free of condensation defects in the main material; see the figure for the description of the axial direction for four separate hot zone structures Temperature profile; Figure 24 presents the axial temperature gradient of 2 from the center of the crystal to half the radius of the crystal. Changes in the middle Printed by the Central Standards Bureau of the Ministry of Economic Affairs S <Industrial and Consumer Cooperatives, which is obtained by averaging the gradient from the curing temperature to the temperature shown on the X axis. When the crystal is pulled into a single crystal in the hot regions Ver 丨 and Ver 4, these two hot regions have a large radial change in G0⑴, and it cannot obtain the crystal from the center of any axial length to the edge. Lattice vacancies without condensation spots are the main material. However, when the crystal is pulled into a single crystal in the hot regions Ver 2 and Ver 3, the two fluorene regions: with less radial-change in G "r), it can obtain the crystal and has some axial directions in the crystal Lattice vacancies with no condensation flaws or rings from the center to the edge in length are the main material. For an ingot prepared according to the process of the present invention and having a -V / I boundary,

536562 A7 B7 V. Description of the invention (2G) is an ingot with lattice vacancies as the main material. According to experience, materials with low oxygen content are better, that is, less than about 13 PPMA (according to ASTM standard F-121-83). The weight per million atoms), it is preferred that the single crystal silicon contains oxygen below 12 PPMA, more preferably below 11 PPMA, and most preferably below 10 ppma. This is because in wafers with medium to high oxygen content In the case of 14H pp g A, the generation of stacking errors and the enhancement of oxygen clustering bands inside the V / I boundary become increasingly important. They are each a potential source of problems in known integrated circuit manufacturing processes. The effect of the enhanced oxygen cluster can be further reduced by various methods, which can be used alone or in combination. For example, the oxygen precipitation core generally forms silicon with an annealing temperature of about 350 C to 750 ° C. Therefore, for some applications, Preferably, the crystal is a "short" crystal, that is, a crystal has been grown in the CzochralsKi process until the seed end has cooled from the melting point of silicon (about 141.0%) to about 750 ° C, after which the ingot is Cools quickly. In this way, the time spent in the temperature range that is important for core generation is kept to a minimum, and the core of the oxygen sink has unsuitable time to form in the crystal pulling single crystal machine. Printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Health (please read the notes on the back before filling this page). However, the oxygen precipitation core formed during the single crystal growth period is best dissolved by annealing single crystal crushing, assuming it The core of the oxygen sink can be annealed by rapidly heating the silicon to a temperature of at least about 875x without performing a stable heat treatment, and the temperature is preferably continuously increased to at least 100 (rc, at least; no (rC, or more) High. Before silicon reaches i00〇r, almost all (for example, more than 99%) of these defects have been annealed, it is important that the wafer system is fast and heated to the temperature, that is, the temperature rise rate is at least about every minute 10: (: and preferably at least about 5 (rc) per minute, otherwise the knife or all oxygen precipitation cores will be stabilized by heat treatment. The equilibrium seems to reach within a short period of time, that is, about 60 seconds or less, Based on this, Shan-23- the official bid winning rate (CNS) eighty four secrets (210 χ29ϋ ^ &quot;-the work of the Central Standards Bureau of the Ministry of Economic Affairs Consumer Cooperatives printed 536562 A7 ____ __ B7 V. Description of the invention (21) The core of oxygen precipitation in Shi Xi can be annealed At least about 875 ° C and dissolving, preferably at least about 950 ° C, and ideally at least about 1100 ° C, with a period of at least about 5 seconds, and ideally at least about 10 minutes. Dissolution can be in a general oven or Implemented in a rapid thermal annealing (RTA) system, rapid thermal annealing of silicon can be performed in a variety of general rapid thermal annealing (RrA) furnaces, where the wafers are individually heated using a row of high-power lamps The RTA oven can quickly heat a silicon wafer. For example, it can heat a wafer from the chamber to 1200 C in a few seconds. One of the RTA ovens is a Model 610 oven from the AG Association (Scenic Mountain, California). In addition, The dissolution can be performed on a silicon block or a silicon wafer, and is preferably a wafer. In one example of the process of the present invention, the initial concentration of silicon row interstitial atoms is controlled in the axially symmetrical row interstitial of the ingot 10 as the main region. Within 6, refer to Figure 1. In general, the initial concentration of silicon interstitial atoms is achieved by controlling the crystal growth rate v and the average axial temperature gradient gq, so that the v / Gg ratio 値 is closer to the critical threshold 値, Where the ν / ι boundary occurs. In addition, the average axial The degree gradient can build jl, so that the change of Gg and G.⑴ (and V / G.⑴) become a variation of G. (that is, v / G.) 'Which becomes a function of the ingot radius and is also controlled. In another example of the present invention, v / Go is also controlled so that at least a part of the length of the ingot does not have a V / I boundary along the radius. In this length, the silicon system has a lattice from the center to the edge of the ring side. Vacancy is the main one, and the defect of condensed crystal lattice is to control v / G0 to avoid grams in an axially symmetrical area extending radially inward from the side edge of the ingot ring, that is, the growth conditions are controlled. In order to make WGg have a threshold between v / Gg and 乂 乂 times. Critical 値. It should be noted that the wafers prepared in accordance with the present invention are suitable as its ---; -------- (Please read the precautions on the back before filling this page)

、 1T —24- Working and Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs, Yinfan 536562 A7 r ----- B7 V. Description of Invention (22) — '~~ &quot;' 一-Available for accumulation on the upper surface The surface layer deposition can be performed using conventional techniques.

〃 In addition, it should also be noted that the wafer prepared according to the present invention is suitable for the junction hydrogen or argon annealing treatment, as shown in the European Patent Application No. 503816 A1. Visual inspection of condensing defects 彳 彳 2 Condensing defects can be detected using a variety of different techniques, such as streamline defects or D-shaped defects are usually used to etch single crystal silicon samples in Secc0 etching solution for about 30 minutes, And then let the sample be inspected by microscopy (see, for example, H. Yamagishi et al., 1992. Semic 0nd% τ_η〇ι 7 A135 works), although the detection of crystal lattice defects is a Standard, this method can also be used to detect condensate filling defects. When using this technique, if there is such a defect, it will appear as a large hole on the surface of the sample. Condensation defects can also be detected using laser scattering technology. Compared with other etching techniques, laser scattering X-ray tomography has a detection limit of low defect density. In addition, the condensed intrinsic point defects can be visually detected by decorating the defects with a metal. It is measured that the metal can diffuse into the single crystal silicon matrix when heated. Especially for single crystal silicon samples, such as wafers, crystal wafers or slow-moving rings, if there is a flaw, the sample can be coated with a metal-containing composition first. table While doing a visual inspection, 'the metal can decorate various flaws' and the composition can be, for example, a concentrated copper schistate solution; the coated sample is then heated to approximately 900 ° C and 100 ° C (TC It lasts about 5 to 15 minutes to facilitate the diffusion of metal into the sample; the heat-treated sample is cooled to room temperature again to allow the metal to gradually reach supersaturation and sink in the sample matrix containing the flaw. _2 5_ degree Applicable to China National Standard (CNS) A4 specification (210X297 mm) '': ~ (Please read the notes on the back before filling this page), 11 Printed by the Central Standards Bureau of the Ministry of Economic Affairs, Fong Cooperative Cooperative 536562 A7 __________B7 V. Description of the invention (23) After cooling, the sample is first subjected to a flawless drawing and etching to remove the surface leftovers and sunken objects. It is about 8 to 12 knife clocks for processing the sample with _Fengliang money carving solution, typically Hair shell etchant contains approximately 55% nitric acid (70% solution weight ratio), approximately 20% hydrofluoric acid (49% solution weight ratio), and approximately 25% hydrochloric acid (concentrated solution). The sample is then deionized Water washing and utilization. Immerse or treat the sample with a SeCC0 or Wrigh The etching solution is about 35 to 55 minutes, and the second etching step is performed. Usually, the sample is etched with Secc0 etching solution, which contains a ratio of 0.15 mole of potassium dichromate to hydrofluoric acid (49% solution weight ratio). This etching step is used to find or depict possible condensation defects. In general, the row filling for condensation defects and the material area dominated by lattice vacancies can be distinguished from each other, and the above-mentioned copper decoration technology is used to distinguish them from condensation. Defective materials, non-defective interstitial filling is the main material area and does not contain the coating characteristics present in the etching, while the non-defective lattice vacancy-dominated material area (prior to the high-temperature oxygen nucleation dissolution treatment) is due to the copper decoration of the oxygen nucleus. Contains small pits. Definition. The following wording or phrase used in this article has the intended meaning: "condensation intrinsic point defect" means that the defect comes from the condensing of the ⑴ lattice vacancies, resulting in 0-shaped defects, streamline defects, gate oxide accumulation defects, crystal original particles Defects, Ei m original: ICR light spot defects, and other such lattice vacancy-related defects, or (ii) interstitial condensation caused by dislocation rings and networks, and other continuations Defect response; "Condensation between rows of defects" refers to the reaction of the intrinsic point defect of condensation from Shi Xixing's interstitial atomic condensation; "Condensation and warrior P Gurugui" refers to the vacancy of the condensed crystal lattice. Condensing the opposite: fm tmtmmt tamml fm im 11 &gt; 1 «νϋϋ ϋ—l mi« m. (Please read the notes on the back and fill in this page first) Order-26- 536562 Printed by Zhengong Consumer Cooperative, Standards Bureau, Ministry of Economic Affairs System A7 B7 V. Description of the invention (24) ~-Produced, "half branch" refers to the% ^ distance measured from the center axis of a wafer or ingot to the side edge of a ring; "roughly no condensation &amp; "Pain" means-less than the limits of flaw detection The concentration of condensation defects is about 103 defects / cm 3; "V / I boundary" means that the material along the radius of an ingot or wafer changes from lattice vacancies to interstitial filling; And "Jingjing = King" and "mainly interstitial" mean that the internal point defects are mainly lattice vacancies or interstitials. '' For example, as shown in the following I example, the present invention provides a method for preparing a single silicon crystal block. When the ingot is cooled at the self-curing temperature according to the dovhtsldki method, the condensation of intrinsic point defects can be avoided for cutting. The axially symmetrical region of the fixed diameter section of the ingots forming the wafer. The following example sets out a set of conditions that can be used to achieve the desired result. There are several other methods that can be used to determine the ideal single crystal rate profile of an existing crystal pulling single crystal machine. In the series of ingots, a single to body can be grown using a pull single crystal rate that increases or decreases along the length of the crystal. In this way, '&amp; knots are filled with defects in the single crystal, which will appear and disappear multiple times over a long period of time, and then the best pull single crystal rate can be determined at a number of different crystal positions' based on this' The following examples are not self-limiting. Example 1 Optimal procedure for a single crystal pulling machine with a preset chirped area design-The first 200 mm single crystal chopping block is grown under the following conditions, that is, the single crystal pulling rate is from about 0.75 mm / Min is oblique to 〇35 mm / min, -27- This paper size applies to Chinese National Standard (CNS) A4 (210X 297 mm) (Please read the precautions on the back before filling this page) Order 536562 A7 B7 V. Description of the invention (25) FIG. 7 reveals that the pulling single crystal is a function of crystal length. Please consider the pre-established axial temperature profile and average axial temperature gradient G of a 200 mm ingot grown in a pulling single crystal machine. The radial change in the medium, that is, the axial temperature gradient at the capacitive / solid interface, and the pull single crystal rate are selected to ensure that one end of the ingot is mainly dominated by lattice vacancies from its center to the edge. On the ingot's block / another end a, the material is mainly filled from the center to the edge. The generated ingots are cut longitudinally and analyzed to determine where the condensed line defects begin to form. Figure 8 is an image produced by scanning the life of a small number of carriers in the axial section of a segment approximately 635 mm to 760 mm from the shoulder after a series of oxygen precipitation heat treatments to find the defect distribution pattern; one of approximately 680 mm At the crystal position, a band-shaped condensed interstitial filling defect 28 can be seen. This position is equivalent to a critical pulling single crystal rate of V * (680 mm) = 0.3 3 mm / min. At this point, the width of the axially symmetric region 6 (this region is filled with the main material region, but without condensation between the row filled defects) is at its maximum, and the lattice vacancy is the width of the main region 8 Rv * (680 ) Is about 35 mm, and the width of the axially symmetric region 1 ^ * (680) is about 65 mm. Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives (please read the precautions on the back before filling out this page). A row of Simu's monocrystalline silicon blocks was subsequently grown at a stable pull single crystal rate. Single crystal pulling rate at the maximum width of the axially symmetric region of the first 200 mm key block. Figure 9 reveals the crystal length function of each crystal with a single crystal rate of 1-4. The four crystals are then analyzed to determine the axial position where the condensing interstitial defects appear or disappear first (and the corresponding single crystal). Crystal rate), the points obtained by the four animal husbandry experiments (indicated by the * mark) are shown in FIG. 9, a curve is generated by inserting between the points and extrapolating from the points, which is marked as v * in FIG. 9 (Z), this curve represents a first approximation, that is, the pull single crystal rate of a 200 mm crystal as a function of the length in a single crystal machine. At this time, the axial symmetry region is at its maximum width -28- The scale is applicable to the Chinese National Standard (CNS) A4 specification (210X 297 mm). It is printed by the Central Standards Bureau of the Ministry of Economic Affairs and printed by the Consumer Cooperative. 536562 5. Description of the invention (2δ) The growth of other crystals with different single crystal rates and the growth of these crystals Further analysis can further delineate the experimental definition of ν * (Z). Example G0 (r) Reduction of Radial Change --- 'Figures 10 and 11 illustrate the improvement of quality, which is achieved by reducing the radial change G0 (r) in the axial temperature gradient of the molten / solid interface. The initial concentration of the lattice vacancies and the interspace charge (approximately at the distance of 1 cm from the molten / solid interface) are different according to two different examples. G⑺: ⑴G0 (r) = 2.65 + 5 X l0-V / (K / mm) and ⑵ G0 (〇 = 2.65 + 5 X 10-5rV (K / mm), the pull single crystal rate of each example can be adjusted to make the silicon with lattice vacancies and The boundary between silicon is a radius of 3 cm. The pull single crystal rates used in Example 2 are 〇04 and 〇35mm / min. It can be clearly seen in Figure 11 that the initial concentration of row filling in the crystal-rich row filling section varies with As the radial change in the initial axial temperature gradient decreases, the dramatic decrease in Λ leads to an improvement in material quality, because it is easier to avoid the formation of interstitial defect groups due to the supersaturation of interstitial charging. Example 3 Increasing the diffusion time of interstitial charging Figure 13 Λ Brightness (improved 'It can be achieved by increasing the interstitial charge and diffusion when the interstitial degree is different. There are two different examples of the crystal to the temperature wheel. dT / dz, the axial temperature gradient energy at the dissolved state: / solid interface can be the same. Therefore, the initial concentration of row charging (approximate distance from the melting point: solid interface w) is the same for both examples. In this example The pull single ^ can be adjusted so that the entire crystal is rich in row charge. The pull single crystal rate is the same in both cases (please read the precautions on the back before filling this page)

----____ _29- 536562 A7 B7 V. Description of the invention (27) The sample is 0.32 mm / min. The longer outward diffusion time of the row charge in Example 2 will cause the overall decrease in the charge amount of the row charge, which leads to the quality of the material. The improvement is because it is easier to avoid the generation of inter-row filling defect groups due to super-saturation of inter-row filling. Example 4 A crystal system with a length of 700 mm and a diameter of 150 mm grows at a rate of varying single crystal growth rate. The single crystal growth rate is almost linear from the shoulder at 1.2 mm / min to a distance of 430 mm from the shoulder. 0.4 mm / min, and then returned in a nearly straight line to 0.65 mm / min from the shoulder 700 mm. Under this condition, in this particular single crystal pulling machine, the entire radius is rich in the length of the crystal. The condition is about 320 to 525 mm from the shoulder of the crystal. Referring to FIG. 14, at an axial position of about 525 mm and a pull single crystal rate of about 0.47 mm / min, the crystal has no condensed intrinsic point defect group across the entire diameter. In other words, there is a small section of In the crystal, the width of the axially symmetric region is equal to the radius of the ingot, that is, a region free of condensation defects. Example 5: Printed by the Central Standards Bureau of the Ministry of Economic Affairs and Consumer Cooperatives (please read the precautions on the back before filling out this page). As shown in Example 1, a row of shore crystal second blocks are grown at a variable pull single crystal rate and then analyzed to Determine the axial position (and the corresponding pull single crystal rate) at which the filling line defects appear first or disappear, and insert and extrapolate from the points to plot the single crystal rate v, axial direction A curve is generated on the position chart, which represents the first approximation, that is, the pulling single crystal rate of a 200 mm crystal as a function of the length in the pulling single crystal machine. At this time, the axis &gt; symmetry region is at its maximum width. Other crystals are grown at different pull rates, and further analysis of the crystals can be used to determine the optimal pull single crystal rate profile for this experimental determination. Using this information and following this best single crystal rate profile, a paper size of approximately 1000-30- applies to the Chinese National Standard (CNS) Λ4 specification (210X 297 mm) 536562 mm Cooperatives print A7 B7 V. Description of the invention (28) Crystals with a length of 200 mm in diameter can grow, and the growing crystal slices obtained from different axial positions are then analyzed using the oxygen precipitation method standard in this technology to facilitate It is judged whether there is a condensed line defect, (ii) the position of the V / I boundary is determined as a function of the slice radius. Based on this, the existence of an axially symmetric region and the width of this region as a function of the crystal length or potential coverage ~ function + can be determined. The results obtained from the axial position of the ingot shoulder in the range of approximately 200 mm to 950 mm are shown in the graph of Fig. 15. The results show that a single crystal rate profile can be determined for the growth of a single crystal silicon block. , So that the fixed diameter section of the ingot can include an axially symmetric region with a width measured from the side edge of the ring radially toward the central axis of the ingot, at least about 40% of the radius of the fixed diameter section. In addition, the results show that this axially symmetric region may have a length, measured along the central axis of the ingot, which is approximately 75% of the length of the fixed straight section of the ingot. Example 6 A single crystal silicon block having a length of about 1100 miQ and a diameter of 15 mm is grown at a reduced pull rate of about 0 mm. The pull single crystal rate at the shoulder of a fixed diameter section of an ingot is about 1 mm / min. The single crystal rate decreases exponentially to about 0.4 mm / nun, which is equivalent to the axial position at about 200111111 from the shoulder. The single crystal rate then decreases linearly until about 0.33 The rate reaches near the end of the fixed diameter section of the ingot.

Under these process conditions, the specific structure and the structure of the ingot, the resulting ingot contains a region, where the axially symmetric region has a width approximately equal to the radius of the ingot. Please refer to Fig. 10a and Mb, which are the following. _ BA You after the _ oxygen precipitation heat treatment-31- ^ Zhang Zhang scale I for China i? I ^ CNS) (Please read the precautions on the back before filling this page }

536562 A7 B7 V. Description of the invention (29) Scanning the image of the life of a small number of carriers of the axial section of an ingot, the continuous segmentation of the key block is presented, and its range is about 100 mm to 250 mm and 250 In the axial position from mm to 400 mm, it can be seen from the figure that an area exists in the key block, and the range is in the axial position about 170 to 290 mm from the shoulder, which does not condense over the entire diameter. Intrinsic point defects, in other words, a region exists in the ingot, and the width of the axially symmetric region, that is, a region substantially free of condensation and interstitial defects, is approximately equal to the radius of the ingot. In addition, in a range of axial positions ranging from approximately 125 mm to 170 mm and approximately from 290 mm to 400 mm or more, there are a number of non-condensing intrinsic point defects between the rows filled with the axial symmetry zone of the main material. The lattice vacancies of the non-condensing intrinsic dot defect are roughly cylindrical cores as one of the main materials. Finally, in an area within an axial position range of approximately 100 mm to 125 mm, there is an axially symmetric region of the main material filled with non-condensing defects that surrounds the substantially cylindrical core of the main material. In the material where the lattice vacancies are dominant, an axially symmetric region without condensation defects surrounds a core containing the crystal lattice vacancy defects. Example 7 Cooling rate and location of the V / I boundary Printed by the Consumers Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling this page) A series of single crystal seconds blocks (150 and 200 mm rated diameters) are based on The growth of the Czochralski method makes different hot zone structures designed by ordinary techniques to affect the residual silicon content at temperatures exceeding about 1050 ° C. The pull single crystal rate profile of each ingot changes along the length of the ingot. The transition from the defect area of the coagulation crystal lattice vacancy point to the filling defect area between the condensation rows. Once grown, the ingot is made along the central axis parallel to the growth direction. -32- This paper size applies the Chinese National Standard (CNS) A4 specification (210X 297 mm) 536562 A7 ^ ---________ B7 V. Invention Note (30): ^ Longitudinal cutting, and further divided into several sections with a thickness of about 2 mm each. When using the copper decoration technique, a set of this longitudinal section is added and intentionally copper For cold decoration, the heating conditions are suitable for high concentration dissolution of a copper row. After this heat treatment, the sample was rapidly cooled, during which the copper spots spread outward or precipitated where there were defects in oxide groups or condensation between rows— After the a-standard and defect-delineation etching, the sample was visually inspected for the presence of precipitated stains, and those areas without precipitated stains corresponded to the areas without condensation and filled with defects. Carved = a series of longitudinal sections are subjected to a series of oxygen precipitation heat treatment to facilitate the moon load and can be caused to form the core and growth of new oxide groups before the chart. The comparison band in the life chart is used to judge and measure the instant melt / solid interface shape at different axial positions in each ingot, and then use the data on the melt / solid interface shape as described below to evaluate the average axis The temperature gradient &lt; absolute chirp and radial change, this data is also used in conjunction with the pull single crystal rate to evaluate the radial change in v / Gq. Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs. In order to further examine the role of growth conditions in the quality of a monocrystalline silicon block, according to existing experiments, it is believed that there are a variety of assumptions that can be used for judgment. First of all, in order to simplify the processing of thermal history by cooling the time it takes to reach the condensation temperature of inter-row filling defects, it is assumed that approximately 105 (rc is a reasonable approximation of the temperature at which silicon inter-row filling condensation occurs). This temperature seems to be consistent with the use Changes in density of interstitial filling defects observed during the experiment with different cooling rates. As mentioned above, although condensation occurs or not-it is also a factor of interstitial concentration, but the phase condensate will not occur at 105. The temperature above ° C, because of the row intercalation concentration in the Czochralski-type growth process, it can reasonably be assumed that the system does not become critical supersaturation of the intercharging when it is above this temperature. In other words-33- This paper scale applies Chinese national standards (CNS) Λ4 specification (210X297 mm) 536562 A7 B7 V. Description of the invention (31) In terms of the typical row interstitial concentration of the Czochralski-type growth process, it can be reasonably false and the system is not inconsistent, and it becomes a critical supersaturation, and therefore Above 丨 no condensation will occur. The second assumption is to change the growth conditions on the quality of single crystal silicon into a variable and rely on the interstitial diffusion of silicon. The temperature is omitted and easy. In other words, it assumes that the interstellar charge is diffused at the same rate at all temperatures between about 140 ° C and 1050 ° F. It should be understood that about 1050X: can be considered as condensation Temperature &lt; A reasonable approximation 値, the basic point of this assumption is that the cooling tunes 'spring,' and 'field part' from the melting point are not important, and the diffusion distance depends only on the total time spent cooling from the melting point to about 1050 ° C. When using the axial temperature profile data to design in each hot zone and the profile of single solid crystal rate in a special foot ingot, the total cooling time from about 140 ° C to 105 ° C can be calculated. Note that the temperature change rate of each hot zone is quite uniform. The uniformity of the dagger uniformity is used to select the core molding temperature for condensing defects. Arbitrary error, such as about 1050 °, will only result in the success of calculating the cooling time. Proportional error. In order to determine the radial range of the main area of the lattice vacancies of the key block (R lattice vacancies), printed by He Gong Consumer Cooperative, Central Standards Bureau of the Ministry of Economic Affairs ---------------__ ( (Please read the precautions on the back and fill in this page) The width of the axially symmetric region is further assumed to be determined by the life graph. The main grid radius is equal to v / G0 = v / G〇. The width of the axially symmetric region is approximately equal to the critical solidification point. It is assumed to be based on the IV / I boundary position after cooling to room temperature. As mentioned earlier, this is because when the ingot is cooled, the reorganization of the lattice level and the interstellar filling can occur. When the reorganization does occur, V / The I boundary is the inward position, which is the inward direction of the ingot, which is the final position referred to herein.

(匸 奶) / \ 4 specifications (210 \ 297 mm) 536562 Printed by the Baker Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the invention (32) To simplify the average axial temperature gradient G of the crystal in the curing time. The melting / solid interface shape is assumed to be the melting point isotherm. The surface temperature of the crystal is calculated using finite vane molding (FEA) technology and hot zone design details. The entire range / degree range in the crystal and G are calculated correctly. The boundary conditions are solved by the Lapiace formula, that is, the melting point along the melting / solid interface and the surface temperature I FEA along the crystal-body / axis a. The different axial positions of the ingots prepared and evaluated from one of them The results obtained on the premises are shown in Figure 丨 7. To estimate G. When the effect of the mid-radial change on the initial row charge density is a radial position R, that is, the position halfway between the V / I boundary and the crystal surface, it can be assumed that a silicon row charge distance is a slot in the ingot. The furthest point of the groove, and the groove is in the main zone of the w-lattice station or on the crystal surface. Calculate v / G by using the growth rate and G0 in the above ingots at the position and. The difference from v / Gg at the ν / ι boundary (ie, critical v / G〇 値) provides an indication of the radial change in the initial row interstitial concentration and its ability to be used to interstitially reach the crystal surface or The lattice vacancy is a groove in the main region. For this particular material, tantalum seems to be at v / G. There is no systematic dependence on the crystal quality in the radial change within. As seen in Figure 18, the axial dependence in the ingot is the smallest in this sample. The growth conditions involved in this experimental series represent the G0 diameter. One of the changes is quite narrow. As a result, this data set is too narrow to resolve the discernable dependencies on radial changes in Gq (ie, the presence or absence of a condensed intrinsic point defect band)-. · As mentioned above, the prepared ingot samples are obtained at different axial positions when the condensing line is full of flaws or not. Q is set for each checked axial t and the sample quality is symmetrical with the axial direction. Compare the width of the zones (please read the precautions on the back before filling this page)

536562 A7 ---------- B7 V. Description of the invention (33) Relevance. Please refer to Figure 19, a graph can be made, “λ α ν Existing sample quality ratio Γ μ At the axial position, the self-curing temperature is cooled to delete. When ^, please read the back φ precautions before filling in this page R ΠΓ : Wanter, this chart shows the width of the axially symmetric region (ie. Crystal Xieshan has a strong dependence on the cooling history of the samples in this particular temperature range. To make the axially symmetric region wide, one of the Trend: It is necessary for me to increase the diffusion time or slow down the cooling rate. According to the information in this chart, we can calculate 笪 屮 σ T f out of the ^ distribution line, which represents the "gen" (ie, flawless disease) ) To "bad" (i.e. a flawed change transition, which is a function of the cooling temperature allowed in a given temperature range in a specific temperature range, the approximate relationship between the axial symmetry region and the cooling rate: :… (R crystal-R transition) 2 = Deff * t105 (rc where the radius of the R crystal heterogeneous ingot, the R transition is at an axial position in the sample, and the line filling occurs in the main material from flawless to Radius of the axially symmetric region of the defective transition, or vice versa j Printed by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs

Deff system-constant, about 9.3,-"], represents the average time and temperature of interstitial charge diffusivity, and ^ 1050. (: The sample's predetermined axial position is cooled from solidification to about 1050 ° The time required.-Refer to Figure 19 again, it can be seen that for a given key block diameter, a cooling time can be estimated to obtain an axially symmetric region of the required diameter. Example I For a 150 mm diameter key block, — with a width approximately equal to the ingot — 36-

536562 A7 &quot; ~~ '~' ~~ ---_ Β7 V. Description of the Invention (34) &quot; ~: 1 '----- When the axially symmetric area of the block radius is available, This part of the block between the T temperature ranges should be able to cool for about 15 hours. Similarly, for a key block of about 200 mm diameter, if this particular part of the key block can be cooled for about 25 to 35 hours in this temperature range, an axially symmetric region having a width of approximately equal reading block radius can be obtained. "If the line advances-extrapolation, it may take about 65 to 75 hours to cool down in order to obtain a 4-way symmetry zone 'and its width is approximately equal to the radius of the ingot with a diameter of approximately 鸠Note that when the diameter of the ingot is increased, the increase in distance causes the inter-row charge to diffuse to reach the surface of the key block or the slot of the lattice vacancy, so additional cooling time is required. Please refer to Figure 20, 21, 22, 23 / The effect of increasing the cooling time of different key blocks can be seen. Each figure illustrates a part of an ingot with a nominal diameter of 200 mm. The cooling time is from the solidification temperature to 1050τ, in order from Figure 2. Increase to Figure 23. Printed by He Gong Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs, see Figure 20, which reveals that the ingots in the axial position range of about 235 to 35 mm from the shoulder are in the axial direction of about 255 mm. At the location, there is no condensation between lines The width of the axially symmetric region is at the maximum, which is about 45% of the half of the ingot. Outside of this position, a transition occurs from an area without this defect to an area with this defect. Please That is, refer to FIG. 21 'It reveals the key block shaofen within a range of about 305 to 460 mm away from the shoulder' at a large: about 360 mm in the axial position, the width of the axially symmetric region without condensing defects between lines. At the maximum, it is about 65% of the radius of the key block. Beyond this position, defects are generated. Refer to Figure 22, which reveals the axial position about 140 to 275 mm from the shoulder. Applicable to Chinese National Standard (〇 奶) 6.4 specifications (210 '乂 29 ^ cent)' One = 536562 A7 B7 V. Description of the invention (35) The key block within the range is in the axial position of about 2 0mm Where the width of the axially symmetric region is approximately equal to the ingot radius, that is, a small part of the ingot within this range has no condensed intrinsic point defects. Please refer to FIG. 23 ', which reveals that the distance from the shoulder is about 600mm to The ingot portion within the 730 mm axial position range is from about 64 mm to 5 m ^. In the axial position, the width of the axially symmetric region is approximately equal to the ingot radius. In addition, the length of the ingot segments with the width of the axially symmetric region approximately equal to the ingot radius is greater than the observation of the ingot in Fig. 22. Therefore, when merged When viewed, Figures 20, 21, 22, and 23 illustrate the cooling of the% area t width and length in the axial direction of the defect-free area to 1050. Generally, the effect is that the area containing condensed lines is filled with defects. The result of the initial decrease of the single crystal rate caused by the continuous reduction of the crystal single crystal rate is too large to reduce the crystal portion and the cooling time. The larger length of the axially symmetric region means that a larger range of single crystal rate can be obtained (That is, the initial row filling density) The increased cooling time used for the growth of this flawless material allows higher initial row filling density because sufficient time for radial diffusion can be obtained to suppress the concentration of flaw filling between the rows: Below the required critical concentration. In other words, for longer cooling times, printed by the Consumers' Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs. Slightly lower (pulling single crystal rate (and higher initial row interstitial concentration) will still result in the largest axially symmetric region 6. Therefore, a longer cooling time results in an increase in the allowable early crystallization rate change, which is roughly the core condition required for the diameter of the largest axially symmetric region, and loosens process control restrictions. As a result, the key block has a large length. The process of forming an axially symmetric region becomes easier. : Refer to: Figure 23, at about 665 to 73 ° from the shoulder of the crystal, the U-direction position of non-condensing mosquitoes _ lattice vacancies dominate -38- 536562 A7 B7 V. Description of the invention (36) The width of the area is equal to the radius of the ingot. From the above data, it can be seen that, by controlling the cooling rate, "interstitial charging allows more time for interstitial charging to diffuse to where it can disappear. ^^^ As a result, condensed interstitial charging defects can be prevented in monocrystalline stones. The main part of the evening block: it happens from the inside. ^ From the top view, it can be seen that many items of the present invention can be achieved. Because a variety of changes can still be achieved in the above composition and process without departing from the scope of the present invention, Therefore, all the matters in the foregoing should be regarded as illustrations, and not meant to have restrictions.-The printed paper size of the Zhongjia Standard Bureau of the Ministry of Economic Affairs and Consumer Cooperatives is printed in accordance with the Chinese National Standard (CNS) A4 (210X 297) Mm)

Claims (1)

Scope of patent application 536562 Patent No. 87105351 Chinese patent application scope_ 1 · An early-crystal silicon wafer with a central axis, a front side and a back side, all of which are approximately perpendicular to the central axis, a ring side edge, and a self-wafer center The axis extends to the radius of the side edge of the ring. The wafer includes a first axially symmetric region, in which the lattice vacancies are mainly intrinsic point defects and there are substantially no condensed crystal lattice vacancies. The first axially symmetric region includes The central axis may have a width of at least 15 mm. 2. As for the wafer in the first item of the patent application scope, wherein the wafer includes a second axially symmetric region, wherein the silicon row interstitial atomic system is mainly an intrinsic point defect and is substantially free of condensed silicon row interstitial intrinsic point defect. 3. If the wafer of the first patent application scope, the width of the first axially symmetric region is at least 15% of the radius. — 4. The wafer as claimed in item 3 of the patent application scope, wherein the wafer includes a second axially symmetric region, wherein the silicon row interstitial atomic system is mainly an intrinsic point defect and is substantially free of condensed silicon row interstitial intrinsic point defect. 5. If the wafer of the first patent application scope, the width of the first axially symmetric region is at least 25% of the radius. 6. The wafer according to item 5 of the patent application scope, wherein the wafer includes a second axially symmetric region, wherein the silicon row interstitial atomic system is mainly an intrinsic point defect and is substantially free of condensed silicon row interstitial intrinsic point defect. 7. If the wafer of the first patent application scope, the width of the first axially symmetric region is at least 50% of the radius. 8. The wafer according to item 7 of the patent application scope, wherein the wafer includes a second axially symmetric region, wherein the silicon row interstitial atomic system is mainly an intrinsic point defect and is substantially free of condensed silicon row interstitial intrinsic point defect. (Please read the precautions on the back before filling out this page), 1T Printed by the Consumer Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs 536562 A8 B8 C8 D8 Patent application scope Printed by the Consumer Cooperatives of the Central Bureau of Standards of the Ministry of Economic Affairs 9 · If the patent application scope of the first wafer, the first axial symmetry area contains the central axis. 10. The wafer of item 9 in the scope of patent application, wherein the wafer includes a second axially opposite% region, in which the silicon row interstitial atomic system is mainly an intrinsic point defect and is substantially free of condensed silicon row interstitial intrinsic point defect. 11. Oxygen content of wafer PPMA such as the first item in the scope of patent application. 12. Oxygen content of wafer PPMA such as the first item in the scope of patent application. 13. The core of the wafer as in the first patent application. — 14 · A monocrystalline silicon block having a central axis, a seed cone, an end cone, and a fixed diameter section between the seed cone and the end cone, the fixed diameter section has a ring side edge and a self-center axis Extending to the radius of the ring side edge, the single crystal silicon block is characterized in that when the ingot is grown and the self-solidification temperature is cooled, the fixed diameter section contains a first axially symmetric region, wherein the lattice vacancies are mainly intrinsic point defects. And there are substantially no point defects in the crystal lattice vacancies, in which the first axially symmetric region includes the center axis or has a width of at least 15 mm and has a length of 'at least 20% of the length along the fixed diameter section of the ingot Axis. _ 15. The monocrystalline silicon block according to item 14 of the application, wherein the ingot contains a second axially symmetric region that is concentric with the first axially symmetric region, and the second axially symmetric region contains interstitial atoms. As the main intrinsic point defect, and there is almost no intrinsic point defect of the condensed silicon row. Wherein the wafer has less than about 13 where the wafer has less than about 11 where the wafer has an anaerobic precipitation-2- This paper size is applicable to Chinese National Standard (CNS) A4 (210X297 mm) (please read the back first) (Notes for filling in this page) 536562 A8 B8 C8. ___ D8 6. Scope of patent application 16. If the monocrystalline silicon block of item 14 of the patent application scope, the length of the axial symmetry area is at least 400 / 〇 of the length of the fixed diameter section of the ingot. 17. The monocrystalline silicon block according to item 16 of the patent application, wherein the ingot contains a second axially symmetric region that is concentric with the first axially symmetric region, and the second axially symmetric region contains interstitial atoms. It is the main intrinsic point defect, and there is almost no intrinsic point defect of the condensed silicon row. 18. The single crystal silicon block according to item 16 of the application, wherein the width of the first axially symmetric region is at least 5% of the radius. 19. The single crystal silicon block according to item 16 of the application, wherein the width of the first axially symmetric region is at least 25% of the radius. 20. The single crystal silicon block according to item 16 of the patent application scope, wherein the length and width of the first axially symmetric region is at least 60/0 of the length of the fixed diameter section of the ingot. 21 · —A method for growing a single crystal silicon block, wherein the ingot includes a central axis, a seed cone, an end cone, and a fixed diameter section between the seed cone and the end cone. A ring side edge and a radius' ingot that extends from the central axis to the ring side edge are ingots grown in a molten state and cooled at a solidification temperature according to the Czochrai method, which includes printing by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economy ( Please read the precautions on the back before filling in this page} During the growth of the fixed diameter section of the crystal, self-curing to a temperature range not lower than about 325 ° C, control a growth rate v and an average axial temperature gradient G0 'to cause A first axially symmetric segment is generated, wherein when the ingot is cooled at the solidification temperature, the lattice vacancies are the main intrinsic point defects and there are substantially no condensation intrinsic point defects, wherein the first axially symmetric region extends with a width of at least 15 mm or including the central axis. 22. The method according to item 21 of the patent application range, wherein the length of the first axial symmetry zone is -3- This paper size applies to the family standard (CNS) (21 () &gt; & lt (297 public celebrations) &quot; 536562 The scope of patent application A8 B8 C8 D8 is at least 40% of the length of the fixed diameter section of the ingot. 23 If by, • The method of item 12 of the patent scope, where the first axis is symmetrical The length of the zone is at least 60/0 of the length of the fixed diameter section of the ingot. • 17 The method of applying for item 11 of the patent scope, wherein the first axially symmetric zone has a width 'is at least the radius of the fixed diameter section of the ingot. 60 // 25. If you use the method described in item 22 of the patent, wherein the first axially symmetric region /, has a width 'the width is at least 25% of the radius of the fixed diameter portion of the ingot &Amp; '26 The method according to item 22 of the scope of patent application, wherein the ingot includes a second axially symmetric region that is concentric with the first axially symmetric region, and the second axially symmetric region contains interstitial atoms As the main intrinsic point defect, and there is substantially no 'incorporated point defect' of the incinerated silicon row. 7 'The method of item 23 in the patent scope, wherein the first axially symmetric region has a width, and the width is at least Is the solid of the ingot 15% of the half of the fixed diameter portion. 28. The method according to item 23 of the scope of patent application, wherein the first axially symmetric region has a width that is at least half the size of the fixed diameter portion of the ingot. 25%. &Amp; Printed by the Consumers' Cooperative of the Central Government Bureau of the Ministry of Economic Affairs (please read the precautions on the back before filling out this page), 11 29 · ^ The method of claim 23 in the patent scope, where the ingot includes _ The _ # direction symmetry region is concentric with the first axial-symmetric region, and the second axial symmetry region contains interstitial atoms as the main intrinsic point defect, and there are substantially no condensed silicon interstitial region interstitial defects. 30. The method of claim 21, wherein the first axially symmetric region includes a central axis. -4- This paper size applies to Chinese National Standard (CNS) A4 specification (210X297 mm) A8 Βδ C8 '^ D8, scope of patent application (please read the notes on the back before filling this page) 31 · &amp; scope of patent application The method of item 21, wherein the ingot includes a second axially symmetric region that is concentric with the first axially symmetric region, and the second axially symmetric region contains interstitial atoms as the main intrinsic point defect, and There are virtually no pitfalls in the interstitial charge. • The method of item 21 of the u patent application, in which the growth rate V and the instantaneous axial temperature gradient gg are controlled so that the ratio v / Gq is 0.6 to 1.5 times the critical ratio v / c ^. 33. The method of claim 21, wherein the growth rate v and the instantaneous axial temperature gradient Gq are controlled so that the ratio v / Gq is 0.775 to 1.25 times the critical ratio v / G0. 34. The method of claim 21, wherein the growth rate V and the instantaneous axial temperature gradient Gg are controlled so that the ratio V / Gq is 1 to 1.1 times the critical ratio V / G0. 35. The method of claim 21, wherein the crystal has a diameter of 15 mm, wherein the method further includes controlling the cooling rate of the crystal so that the crystal is cooled from the solidification temperature for at least 10 hours. To 1050c. Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs 36. If the method of applying for the scope of the patent No. 21, wherein the crystal has a diameter of 150mm ', where the method further includes controlling the cooling rate of the crystal so that the crystal is at least 15 During the hour, the solidification temperature was cooled to 1050. 〇. 37. The method of claim 21, wherein the crystal has a diameter of 200 mm, and the method further includes controlling the cooling rate of the crystal so that the crystal is cooled from the solidification temperature to 1 within a period of at least 10 hours. 5 (rc. 38. The method according to item 21 of the patent application, wherein the crystal has a diameter of 200 mm, and the method further includes controlling the cooling rate of the crystal so that this paper ϋ applies Chinese national standards (CNS) A4 specifications (210 ^^^ ---- * 536562 A8 B8 C8 D8 VI. Patent application scope 々, .., g, within a period of at least 2G hours, cooled from the curing temperature to 1 () 50. 39. The method according to item 21 of the application, wherein the crystal has a diameter of 200 mm. The method further includes controlling the cooling rate of the crystal so that the crystal is cooled from the solidification temperature to at least 40 hours. 105 (rc. 40). The method according to the patent application No. 2 丨, wherein the crystal has a diameter of 200 mm, and the method further includes controlling the cooling rate of the crystal so that the crystal is in a period of at least 60 hours. Conggu The temperature is cooled down to 1050t. (Please read the precautions on the back before filling this page.) Printed on the paper by the Consumers' Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs. The paper size applies to the Chinese National Standard (CNS) A4 (210X 297 mm). )