Summary of the invention
The technical problem to be solved by the present invention is providing a kind of detection method and device of monocrystalline silicon defect area, the party
Method is able to detect the distribution of the defect area of monocrystalline silicon, simple and quick, can be used for feeding back in silicon ingot growth technique to produce nothing
Defect monocrystalline silicon.
The present invention provides a kind of detection methods of monocrystalline silicon defect area, comprising the following steps:
Obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value;
The sample silicon wafer is heat-treated, precipitates interstitial oxygen concentration in vacancy-like defects region forming core;
Obtain heat treatment after sample silicon wafer diametrically on the multiple test site the second interstitial oxygen concentration
Value;The difference of each test site the second interstitial oxygen concentration value and the first interstitial oxygen concentration value is calculated;
The defect area shape appearance figure of sample silicon chip surface after obtaining heat treatment;
The difference for comparing the interstitial oxygen concentration of the defect area shape appearance figure and the test site, determines the sample silicon
The vacancy-like defects region of piece and the distribution of clearance type defect area.
Preferably, it is described obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value packet
It includes:
Diametrical direction using infrared spectrometer along sample silicon wafer is scanned, obtain sample silicon wafer diametrically on
First interstitial oxygen concentration value of multiple test sites.
Preferably, it is described obtain heat treatment after sample silicon wafer diametrically on the multiple test site second
Interstitial oxygen concentration value includes:
Diametrical direction using infrared spectrometer along sample silicon wafer is scanned, and the sample silicon wafer after obtaining heat treatment is along straight
Second interstitial oxygen concentration value of the multiple test site on diameter direction.
Preferably, it is described to the sample silicon wafer carry out heat treatment include:
The sample silicon wafer is successively handled 4~6 hours under the conditions of 700~900 DEG C, under the conditions of 1000~1050 DEG C
Processing 10~17 hours.Preferably, it is described to the sample silicon wafer carry out heat treatment include:
The time that the sample silicon wafer is successively handled under the conditions of 1000~1050 DEG C is 4~6 hours, 700~900
DEG C condition is handled 4~6 hours, is handled 10~17 hours under the conditions of 1000~1050 DEG C.
Preferably, it is described to the sample silicon wafer carry out heat treatment include: by the sample silicon wafer successively 700~900
DEG C condition is handled 4~6 hours, and the time handled under the conditions of 1000~1050 DEG C is 4~6 hours, in 700~900 DEG C of conditions
Processing 4~6 hours, is handled 4~6 hours under the conditions of 1000~1050 DEG C.
Preferably, the defect area shape appearance figure for obtaining the sample silicon chip surface after heat treatment includes:
The defect area shape appearance figure of the sample silicon chip surface after heat treatment is obtained using X-ray scanning.
Preferably, the sample silicon wafer is made by slicing silicon ingots.
Preferably, the interstitial oxygen concentration difference of the defect area shape appearance figure and the test site determines
The vacancy-like defects region of the sample silicon wafer and the distribution of clearance type defect area, specifically include:
According to the sample defect area shape appearance figure, the defect area distribution situation of the sample silicon chip surface is determined;
Compare the interstitial oxygen concentration difference of each test site, the big test site of the difference of interstitial oxygen concentration is concentrated
Region be vacancy-like defects region, the region that the small test site of the difference of interstitial oxygen concentration is concentrated is clearance type defect area
Domain.
The present invention provides a kind of detection devices of monocrystalline defect silicon, comprising:
First module, for obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value
And the second interstitial oxygen concentration value;
Second module, for obtaining the defect area pattern of sample silicon chip surface;
Third module, for comparing the defect area of silicon chip surface and the interstitial oxygen concentration difference of the test site, really
Determine the distribution in vacancy-like defects region Yu clearance type defect area.
Compared with prior art, the present invention obtains the first interstitial oxygen concentration value of test site first, then carries out hot place
Reason, obtains the second interstitial oxygen concentration value of each test site.Since gap oxygen atom occurs in sky by diffusion and precipitating
Bit-type defect area, and the presence of clearance type defect area oxygen atom very close to each other, therefore after heat treatment, each test position
The growth degree of the interstitial oxygen concentration of point is different.Finally, utilizing the position of the different test site of interstitial oxygen concentration growth degree
With the shape appearance figure check analysis of defect area, so that it is determined that the vacancy-like defects region of sample silicon wafer and clearance type defect area
Distribution.Detection method of the present invention does not damage silicon wafer property, the distribution of simple and quick detection monocrystalline silicon defect area.
It can be used for feeding back in silicon ingot growth technique to produce zero defect monocrystalline silicon.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
It finds after study, crystal growth condition can have an impact to the grown-in defects of crystal, and lack to the primary of crystal
It falls into influential parameter to include at least: the axial-temperature gradient (G) of pulling rate (V) and solid liquid interface.The two above parameters
Ratio V/G can determine the distribution of defect.
Referring to Fig. 1, when V/G is larger, the mainly vacancy-like defects region (the hereinafter referred to as area V) 11 of vacancy dominant,
When V/G is gradually reduced, oxidation induced stacking faults (Oxidation Induced Stacking Fault, OSF) 12 is formed,
It is understood that can be shown after carrying out certain thermal oxidation to silicon wafer with OSF ring, followed by vacancy-like defects size compared with
Small micro- area V 13.When V/G reaches near preset critical, it will form and promote the area Yang Xi (Pv) 14 and inhibit oxygen that area is precipitated
(Pi) 15, grown-in defects are nearly no detectable in the area Pv 14 and the area Pi 15.When V/G is smaller, mainly gap silicon is accounted for leading
Clearance type defect area (the hereinafter referred to as area I) 16.The area Pv 14 and the area Pi 15 are wherein referred to as no crystal defect region (COP-free
Area).
Embodiment of the invention discloses a kind of detection methods of monocrystalline silicon defect area, include the following steps, specific to join
See Fig. 2:
Obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value [Oi]0;
The sample silicon wafer is heat-treated, precipitates interstitial oxygen concentration in vacancy-like defects region forming core;
Obtain heat treatment after sample silicon wafer diametrically on the multiple test site the second interstitial oxygen concentration
It is worth [Oi]1;The difference △ of each test site the second interstitial oxygen concentration value and the first interstitial oxygen concentration value is calculated
[Oi];
The defect area shape appearance figure of sample silicon chip surface after obtaining heat treatment;
The difference for comparing the interstitial oxygen concentration of the defect area shape appearance figure and the test site, determines the sample silicon
The vacancy-like defects region of piece and the distribution of clearance type defect area.
Below referring to Fig. 3, the detection method of monocrystalline silicon defect area is illustrated.
Step S1: obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value.
Preferably, the sample silicon wafer is made by slicing silicon ingots.The diameter of the sample silicon wafer can be 300 millimeters or more
Large-sized silicon wafers, or diameter is lower than 300 millimeters of silicon wafer.
In order to avoid the method for obtaining interstitial oxygen concentration causes to damage to sample silicon wafer, it is preferable that the acquisition sample silicon
Piece diametrically on the first interstitial oxygen concentration value of multiple test sites include: using infrared spectrometer along sample silicon wafer
Diametrical direction is scanned, obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value
[Oi]0。
Oxygen in silicon is mostly in interstitial site, and interstitial oxygen concentration is that have infrared-active, and concentration can be by room temperature Fu
1107cm in leaf infrared light (FTIR) spectrum-1Absorption peak indicates.The method that FTIR measures oxygen in silicon wafer is not only directly simple and right
Sample nondestructive is bad.
Step S2: being heat-treated the sample silicon wafer, precipitates interstitial oxygen concentration in vacancy-like defects region forming core.
It finds after study, the diffusion of interstitial oxygen concentration and precipitating all occur in primarily in vacancy-like defects area, clearance type defect area
Substantially the presence of oxygen very close to each other.Therefore, the present invention has selected heat-treating methods, makes interstitial oxygen concentration in vacancy-like defects region shape
Core precipitating.
Preferably, carrying out heat treatment to the sample silicon wafer includes:
The sample silicon wafer is successively handled 4~6 hours under the conditions of 700~900 DEG C, under the conditions of 1000~1050 DEG C
Processing 10~17 hours.
Processing under the conditions of 700~900 DEG C is used for the growth of oxygen precipitation.
Processing under the conditions of 1000~1050 DEG C for defect nucleation and becomes large-sized.
In order to make oxygen atom whole forming core, to improve the accuracy of detection, it is preferable that carry out hot place to the sample silicon wafer
Reason includes:
The time that the sample silicon wafer is successively handled under the conditions of 1000~1050 DEG C is 4~6 hours, 700~900
DEG C condition is handled 4~6 hours, is handled 10~17 hours under the conditions of 1000~1050 DEG C.
Or
The sample silicon wafer is successively handled 4~6 hours in 700~900 DEG C of conditions, under the conditions of 1000~1050 DEG C at
The time of reason is 4~6 hours, handles 4~6 hours in 700~900 DEG C of conditions, 4~6 are handled under the conditions of 1000~1050 DEG C
Hour.
By the heat treatment of above three stage or four-stage, gap oxygen atom is complete in vacancy-like defects region
Forming core precipitating.
Step S3: obtain heat treatment after sample silicon wafer diametrically on the multiple test site the second gap
Oxygen concentration value [Oi]1;The difference of each test site the second interstitial oxygen concentration value and the first interstitial oxygen concentration value is calculated
Value △ [Oi].
Preferably, it is described obtain the sample silicon wafer diametrically on the multiple test site the second interstitial oxygen concentration
Concentration value includes: that the diametrical direction using infrared spectrometer along sample silicon wafer is scanned, and obtains the sample silicon wafer diametrically
Second interstitial oxygen concentration value of the multiple test site on direction.
Test site in this step is identical as the test site in step S1.Second interstitial oxygen concentration of each test site is dense
Angle value subtracts the first interstitial oxygen concentration value, for the difference of the interstitial oxygen concentration of the test site.
Step S4: the defect area shape appearance figure of the sample silicon chip surface after obtaining heat treatment.
Preferably, the defect area shape appearance figure for obtaining the sample silicon chip surface after heat treatment includes: to be swept using X-ray
Retouch the defect area shape appearance figure of the sample silicon chip surface after obtaining heat treatment.
Sample silicon wafer after X-ray scanning heat treatment, only can determine that the region of silicon wafer existing defects, but not can determine that
The type of defect area.Therefore, interstitial oxygen concentration changing rule is obtained defect area pattern with X-ray scanning and mutually tied by the present invention
It closes, to determine the distribution of different type defect area.
Step S5: the difference of the interstitial oxygen concentration of the defect area shape appearance figure and the test site determines institute
State the vacancy-like defects region of sample silicon wafer and the distribution of clearance type defect area.
Preferably, it specifically includes:
According to the defect area shape appearance figure, the defect area distribution situation of the sample silicon chip surface after determining heat treatment;
Compare the interstitial oxygen concentration difference of each test site, the big test site of interstitial oxygen concentration difference is concentrated
Region is vacancy-like defects region, and the region that the small test site of interstitial oxygen concentration difference is concentrated is clearance type defect area.
In the present invention, occur in vacancy-like defects region due to gap oxygen atom by diffusion and precipitating, and gap
The presence of type defect area oxygen atom very close to each other, therefore after heat treatment, the increasing of the interstitial oxygen concentration of each test site
Long degree is different.Between test site the second interstitial oxygen concentration value and the first interstitial oxygen concentration value in vacancy-like defects region
Difference is greater than the difference between test site the second interstitial oxygen concentration value and the first interstitial oxygen concentration value in clearance type defect area
Value.Behind the major defect region for determining sample silicon wafer using the shape appearance figure of defect area, by the interstitial oxygen concentration of test site
Difference check analysis therewith, so that it is determined that the distribution in the vacancy-like defects region of sample silicon wafer and clearance type defect area.This hair
The bright detection method does not damage silicon wafer property, the distribution of simple and quick detection monocrystalline silicon defect area.It can be used for anti-
It presents in silicon ingot growth technique to produce zero defect monocrystalline silicon.
Test proves that the detection method used time of the invention is in 1~3 hour, accuracy in detection reaches 90% or more.
The embodiment of the present invention also discloses a kind of detection device of monocrystalline defect silicon, comprising:
First module, for obtain sample silicon wafer diametrically on multiple test sites the first interstitial oxygen concentration value
And the second interstitial oxygen concentration value;
Second module, for obtaining the defect area pattern of sample silicon chip surface;
Third module, for comparing the defect area of silicon chip surface and the interstitial oxygen concentration difference of the test site, really
Determine the distribution in vacancy-like defects region Yu clearance type defect area.
It preferably, further include that sample silicon wafer obtains module.
Optionally, first module includes:
First acquisition unit, for obtaining test site the first interstitial oxygen concentration value;
Second acquisition unit, for obtaining test site the second interstitial oxygen concentration value.
First module is preferably infrared scanning equipment.
Second module, preferably X-ray scanning equipment.
In the embodiment of the present invention, the detection device of the monocrystalline defect silicon can detect rapidly the defects of monocrystalline silicon piece point
Cloth region, promotes defect analysis efficiency, and defect distribution in simple and quick analysis silicon wafer preferably controls and avoid product not
It is good.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.