CN101571502B - Method for measuring content of boron and content of phosphorus in polysilicon - Google Patents
Method for measuring content of boron and content of phosphorus in polysilicon Download PDFInfo
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Abstract
The invention discloses a method for measuring content of boron and content of phosphorus in polysilicon. The method comprises the following steps: preparing monocrystalline silicon by drawing the polysilicon in argon atmosphere; measuring resistivity and a P/N type of a preset position of the monocrystalline silicon; combining a formula of difference of the boron and the phosphorus in the monocrystalline silicon with a segregation coefficient formula of the preset position of the monocrystalline silicon to establish a system of linear equations with two unknowns by taking the content of the boron and the content of the phosphorus in the monocrystalline silicon as the unknowns; and obtaining the content of the boron and the content of the phosphorus in the polysilicon according to the system of linear equations with two unknowns. Compared with the prior art, the method can help calculate the content of the boron and the content of the phosphorus in the monocrystalline silicon which is also the content of the boron and the content of the phosphorus in the polysilicon according to the measured resistivity, the P/N type and the existing formulae after measuring the resistivity and theP/N type of the preset position of the monocrystalline silicon. Calculation according to the formulae after measuring data in the method helps save much time; in addition, the method is realized with out using a low-temperature Fourier transform infrared spectrometer or a low-temperature Fourier transform photo-luminometer, thus reducing cost.
Description
Technical field
The present invention relates to technical field of semiconductors, more particularly, relate to a kind of method of measuring boron in the polysilicon, phosphorus content.
Background technology
Along with the develop rapidly of infotech and solar energy industry, the whole world is swift and violent to the demand growth of polysilicon, and supply falls short of demand in market.In the decades in future, also not having other materials can the substituted for silicon material and become electronics and photovoltaic industry main raw material(s).Polysilicon has semiconductor property, is very important defect semiconductor material, is widely used in the basic material of making transistor radio, sound-track engraving apparatus, refrigerator, colour TV, video recorder, robot calculator etc. in the electronics industry.Polysilicon is a primary raw material of producing solar cell, can produce the solar battery group of different model, is conversion of solar energy electric energy.
In industry, need to measure the content of boron, phosphorus in the polysilicon, in the prior art; At first under argon gas atmosphere, polysilicon is drawn into monocrystalline silicon with zone melting furnace; The monocrystalline silicon disk of about 2mm is cut in the place that utilizes boron phosphorus segregation coefficient calculated single crystal silicon and polysilicon boron phosphorus content to equate then, at last with the polishing both surfaces of monocrystalline silicon disk; Measure with low temperature FTIS or low temperature Fourier transform photoluminescence appearance, promptly obtain the content of boron in the polysilicon, phosphorus.
Though can measure the content of boron in the polysilicon, phosphorus in the prior art, in whole measuring process, require a great deal of time; In addition, it is very expensive to use low temperature FTIS or low temperature Fourier transform photoluminescence appearance in the prior art, and use and maintenance cost is also very high.
Summary of the invention
In view of this, the invention provides a kind of method of measuring boron in the polysilicon, phosphorus content and solve the problem that Measuring Time is oversize and equipment is very expensive.
The present invention is achieved in that
A kind of method of measuring boron in the polysilicon, phosphorus content comprises:
In argon gas atmosphere, polysilicon is drawn into monocrystalline silicon;
Measure resistivity and the P/N type of monocrystalline silicon predeterminated position, said predeterminated position is specially measurement monocrystalline silicon head and apart from position, at least 5 times of melting zones of head;
The segregation coefficient formula of residual quantity formula between boron, the phosphorus and monocrystalline silicon predeterminated position in the monocrystalline silicon is combined, as unknown number, set up the linear equation in two unknowns group with boron content and phosphorus content in the monocrystalline silicon;
Obtain the content of boron in the polysilicon and the content of phosphorus according to said linear equation in two unknowns group.
Preferably; In the said determination polysilicon in the method for boron, phosphorus content; The resistivity of said measurement monocrystalline silicon predeterminated position and the concrete steps of P/N type are: measure the resistivity and the P/N type of the head of monocrystalline silicon, and test monocrystalline silicon is apart from the resistivity and the P/N type of position, at least 5 times of melting zones of head.
Preferably, in the said determination polysilicon in the method for boron, phosphorus content, when the conduction type of measuring the monocrystalline silicon head is the N type, and when also being the N type apart from the conduction type of position, at least 5 times of melting zones of head, the first party formula of then said linear equation in two unknowns group is:
10^((LOG(R1)-4.87815)/-0.96262)＝0.35*X-0.8*Y；
The second party formula of said linear equation in two unknowns group is:
10^((LOG(R2)-4.87815)/-0.96262)＝X-Y；
R1 is the resistivity of monocrystalline silicon head, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is the total content of phosphorus, and Y is the total content of boron.
Preferably, in the said determination polysilicon in the method for boron, phosphorus content, when the conduction type of measuring the monocrystalline silicon head is the P type, and when being the N type apart from the conduction type of position, at least 5 times of melting zones of head, the first party formula of then said linear equation in two unknowns group is:
10^((LOG(R1)-5.38454)/-0.97857)＝0.8*Y-0.35*X；
The second party formula of said linear equation in two unknowns group is:
10^((LOG(R2)-4.87815)/-0.96262)＝X-Y；
R1 is the resistivity of monocrystalline silicon head, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is the total content of phosphorus, and Y is the total content of boron.
Preferably, in the said determination polysilicon in the method for boron, phosphorus content, when the conduction type of measuring the monocrystalline silicon head is the P type, and when also being the P type apart from the conduction type of position, at least 5 times of melting zones of head, the first party formula of then said linear equation in two unknowns group is:
10^((LOG(R1)-5.38454)/-0.97857)＝0.8*Y-0.35*X；
The second party formula of said linear equation in two unknowns group is:
10^((LOG(R2)-5.38454)/-0.97857)＝Y-X；
R1 is the resistivity of monocrystalline silicon head, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is the total content of phosphorus, and Y is the total content of boron.
Compared with prior art, the technical scheme that provides of the embodiment of the invention has the following advantages and characteristics:
A kind of method of measuring boron in the polysilicon, phosphorus content provided by the invention; The monocrystal rod head that measurement zone melts and apart from the resistivity and the PN type of position, at least 5 times of melting zones of head; And judge that according to the data surveyed this monocrystalline silicon belongs to any of three kinds of situation, confirmed after the type can to calculate the total amount of boron, phosphorus through computing formula.Because the present invention adopts computing method of formula, so in measuring process, the used time is very short, for enterprise has practiced thrift great amount of time.Simultaneously, need not to use low temperature FTIS or low temperature Fourier transform photoluminescence appearance, therefore provide cost savings.
Description of drawings
In order to be illustrated more clearly in the present invention or technical scheme of the prior art; To do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the process flow diagram of the method for boron, phosphorus content in the mensuration polysilicon provided by the present invention.
Embodiment
To combine the accompanying drawing in the embodiment of the invention below, the technical scheme in the embodiment of the invention is carried out clear, intactly description, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills are not making the every other embodiment that is obtained under the creative work prerequisite, all belong to the scope of the present invention's protection.
The present invention is a kind of method of measuring boron in the polysilicon, phosphorus content.This method at first is drawn into monocrystalline silicon with polysilicon in argon gas atmosphere; Then made monocrystalline silicon is measured, measured the monocrystalline silicon head and apart from the resistivity and the P/N type of position, at least 5 times of melting zones of head; At last according to 2 resistivity and P/N type on the monocrystalline silicon of surveying; The segregation coefficient formula of residual quantity formula between boron, the phosphorus and monocrystalline silicon predeterminated position in the monocrystalline silicon is combined; Boron content and phosphorus content are as unknown number in the monocrystalline silicon; Set up the linear equation in two unknowns group, solve the linear equation in two unknowns group, obtain the content of boron in the polysilicon and the content of phosphorus.Because the present invention adopts to measure on the monocrystalline silicon resistivity and P/N type earlier at 2; Combine formula to calculate according to resistivity on the survey monocrystalline silicon and P/N type then; So the entire method step is simple, whole measuring process only needs tens minutes, can practice thrift great amount of time.
See also Fig. 1, workflow of the present invention may further comprise the steps:
Step 101: in argon gas atmosphere, polysilicon is drawn into monocrystalline silicon.
Step 102: resistivity R and the P/N type of measuring the predeterminated position of monocrystalline silicon.
Wherein, when the impurity in the monocrystalline silicon had only boron and phosphorus, the resistance type of monocrystalline silicon and resistivity depended on the impurity that content is many.So when phosphorus content during greater than boron content, single crystal silicon material is a N type resistivity; When boron content during greater than phosphorus, single crystal silicon material is a P type resistivity.Resistivity is to weigh the easy degree of electric current through silicon materials.
This analysis method is measured 4 data, measures resistivity and two data of P/N type of monocrystalline silicon head earlier, again two data of the resistivity of position, at least 5 times of melting zones of measuring distance head and P/N type.The most accurate for measurement data, the distance between testing at 2 generally is made as 15cm.
Step 103: whether the conduction type of judging the monocrystalline silicon head is the N type, if then get into step 104; If, then do not get into step 105.
Step 104: the segregation coefficient formula of residual quantity formula between predeterminated position boron, the phosphorus content and monocrystalline silicon predeterminated position in the monocrystalline silicon is combined, set up the first linear equation in two unknowns group.
Wherein, Because monocrystalline silicon head conduction type is a kind of situation of having only of N type; The conduction type that is head is the N type and also is the N type apart from the conduction type of position, at least 5 times of melting zones of head, is the N type and is the situation of P type apart from the conduction type of position, at least 5 times of melting zones of head so need not to consider the monocrystalline silicon head resistivity.
Wherein, if when the content of predeterminated position phosphorus is greater than the content of boron in the monocrystalline silicon, the residual quantity formula of phosphorus and boron is P=10^ ((LOG (R)-4.87815)/-0.96262), and R is the resistivity of predeterminated position; If when the content of predeterminated position boron was greater than the content of phosphorus in the monocrystalline silicon, the residual quantity formula of boron and phosphorus was B=10^ ((LOG (R)-5.38454)/-0.97857), R is the resistivity of predeterminated position.
Wherein, the segregation coefficient of phosphorus content is 0.35 in the monocrystalline silicon, apart from position, at least 5 times of melting zones of head phosphorus content with polysilicon in phosphorus content equate; The segregation coefficient of boron content is 0.8 in the monocrystalline silicon, apart from position, at least 5 times of melting zones of head boron content with polysilicon in boron content equate.
Wherein, the residual quantity formula of boron, phosphorus is combined with the segregation coefficient formula, and, set up the first linear equation in two unknowns group according to resistivity and the P/N type of measuring at 2.Head is that the residual quantity equation of N type resistivity is 10^ ((LOG (R1)-4.87815)/-0.96262)=0.35*X-0.8*Y, and R1 is the resistivity of head, and X is a phosphorus content, and Y is a boron content.Apart from position, at least 5 times of melting zones of head is that the residual quantity equation of N type resistivity is 10^ ((LOG (R2)-4.87815)/-0.96262)=X-Y, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is a phosphorus content, and Y is a boron content.Separate for two that can solve the first linear equation in two unknowns group thus, can obtain phosphorus content and boron content.
Step 105: judge whether monocrystalline silicon is the P type apart from the conduction type of position, at least 5 times of melting zones of head, if then get into step 106; Otherwise, get into step 107.
Step 106: the segregation coefficient formula of residual quantity formula between predeterminated position boron, the phosphorus content and monocrystalline silicon predeterminated position in the monocrystalline silicon is combined, set up the second linear equation in two unknowns group.
Wherein, the residual quantity formula of boron, phosphorus is combined with the segregation coefficient formula, and, set up the second linear equation in two unknowns group according to resistivity and the P/N type of measuring at 2.Head is that the residual quantity equation of P type resistivity is 10^ ((LOG (R1)-5.38454)/-0.97857)=0.8*Y-0.35*X, and R1 is the resistivity of head, and X is a phosphorus content, and Y is a boron content.Apart from position, at least 5 times of melting zones of head is that the residual quantity equation of P type resistivity is 10^ ((LOG (R2)-5.38454)/-0.97857)=Y-X, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is a phosphorus content, and Y is a boron content.Separate for two that can solve the second linear equation in two unknowns group thus, can obtain phosphorus content and boron content.
Step 107: the segregation coefficient formula of residual quantity formula between predeterminated position boron, the phosphorus content and monocrystalline silicon predeterminated position in the monocrystalline silicon is combined, set up the 3rd linear equation in two unknowns group.
Wherein, the residual quantity formula of boron, phosphorus is combined with the segregation coefficient formula, and, set up the 3rd linear equation in two unknowns group according to resistivity and the P/N type of measuring at 2.Head is that the residual quantity equation of P type resistivity is 10^ ((LOG (R1)-5.38454)/-0.97857)=0.8*Y-0.35*X, and R1 is the resistivity of head, and X is a phosphorus content, and Y is a boron content.Apart from position, at least 5 times of melting zones of head is that the residual quantity equation of N type resistivity is 10^ ((LOG (R2)-4.87815)/-0.96262)=X-Y, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is a phosphorus content, and Y is a boron content.Separate for two that can solve the 3rd linear equation in two unknowns group thus, can obtain phosphorus content and boron content.
In sum; The present invention has utilized resistivity, P/N type and the fractional condensation principle of study on floating zone silicon dexterously; Set up the linear equation in two unknowns group in conjunction with above-mentioned formula or principle; Try to achieve the content of phosphorus and the content of boron through separating the linear equation in two unknowns group, solved thus and measured boron, phosphorus content long problem consuming time in the polysilicon in the prior art; Need not to use low temperature FTIS or low temperature Fourier transform photoluminescence appearance in addition, therefore provide cost savings.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (5)
1. a method of measuring boron in the polysilicon, phosphorus content is characterized in that, comprising:
In argon gas atmosphere, polysilicon is drawn into monocrystalline silicon;
Measure resistivity and the P/N type of monocrystalline silicon predeterminated position, said predeterminated position is specially measurement monocrystalline silicon head and apart from position, at least 5 times of melting zones of head;
The segregation coefficient formula of residual quantity formula between boron, the phosphorus and monocrystalline silicon predeterminated position in the monocrystalline silicon is combined, as unknown number, set up the linear equation in two unknowns group with boron content and phosphorus content in the monocrystalline silicon;
Obtain the content of boron in the polysilicon and the content of phosphorus according to said linear equation in two unknowns group.
2. the method for boron, phosphorus content in the mensuration polysilicon according to claim 1; It is characterized in that; The resistivity of said measurement monocrystalline silicon predeterminated position and the concrete steps of P/N type are: measure the resistivity and the P/N type of the head of monocrystalline silicon, and test monocrystalline silicon is apart from the resistivity and the P/N type of position, at least 5 times of melting zones of head.
3. the method for boron, phosphorus content in the mensuration polysilicon according to claim 2; It is characterized in that; When the conduction type of measuring the monocrystalline silicon head is the N type, and when also being the N type apart from the conduction type of position, at least 5 times of melting zones of head, the first party formula of then said linear equation in two unknowns group is:
10^((LOG(R1)-4.87815)/-0.96262)＝0.35*X-0.8*Y；
The second party formula of said linear equation in two unknowns group is:
10^((LOG(R2)-4.87815)/-0.96262)＝X-Y；
R1 is the resistivity of monocrystalline silicon head, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is the total content of phosphorus, and Y is the total content of boron.
4. the method for boron, phosphorus content in the mensuration polysilicon according to claim 2; It is characterized in that; When the conduction type of measuring the monocrystalline silicon head is the P type, and when being the N type apart from the conduction type of position, at least 5 times of melting zones of head, the first party formula of then said linear equation in two unknowns group is:
10^((LOG(R1)-5.38454)/-0.97857)＝0.8*Y-0.35*X；
The second party formula of said linear equation in two unknowns group is:
10^((LOG(R2)-4.87815)/-0.96262)＝X-Y；
R1 is the resistivity of monocrystalline silicon head, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is the total content of phosphorus, and Y is the total content of boron.
5. the method for boron, phosphorus content in the mensuration polysilicon according to claim 2; It is characterized in that; When the conduction type of measuring the monocrystalline silicon head is the P type, and when also being the P type apart from the conduction type of position, at least 5 times of melting zones of head, the first party formula of then said linear equation in two unknowns group is:
10^((LOG(R1)-5.38454)/-0.97857)＝0.8*Y-0.35*X；
The second party formula of said linear equation in two unknowns group is:
10^((LOG(R2)-5.38454)/-0.97857)＝Y-X；
R1 is the resistivity of monocrystalline silicon head, and R2 is the resistivity apart from position, at least 5 times of melting zones of head, and X is the total content of phosphorus, and Y is the total content of boron.
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Application publication date: 20091104 Assignee: Xinjiang Daqo New Energy Co.,Ltd. Assignor: Chongqing Daqo New Energy Co., Ltd. Contract record no.: 2013990000750 Denomination of invention: Method for measuring content of boron and content of phosphorus in polysilicon Granted publication date: 20120613 License type: Exclusive License Record date: 20131108 |
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