CN104846435A - P type gallium-doped crystalline silicon and preparation method thereof - Google Patents
P type gallium-doped crystalline silicon and preparation method thereof Download PDFInfo
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- CN104846435A CN104846435A CN201510295978.XA CN201510295978A CN104846435A CN 104846435 A CN104846435 A CN 104846435A CN 201510295978 A CN201510295978 A CN 201510295978A CN 104846435 A CN104846435 A CN 104846435A
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Abstract
The invention relates to a preparation method of P type gallium-doped crystalline silicon. The preparation method comprises the following steps: feeding a silicon material containing a gallium dopant into a crucible, wherein the inner side of the sidewall of the crucible is coated with a circle of N type compensation agent doped coating and the position of the N type compensation agent doped coating is located within the range of the height difference between the silicon liquid surface after the fed silicon material containing the gallium dopant is melted and the crystal silicon formed from the silicon liquid; and melting the silicon material, and performing directional solidification so that the silicon liquid containing the gallium dopant can be formed into the P type gallium-doped crystalline silicon. According to the preparation method of the P type gallium-doped crystalline silicon, doping compensation can be realized in the crystal growth direction, and therefore, the problem of overlarge electrical resistivity distribution range of the P type gallium-doped crystalline silicon in the crystal growth direction can be solved and the electrical resistivity of the whole P type gallium-doped crystalline silicon can be accurately controlled. In addition, the invention also provides P type gallium-doped crystalline silicon produced by use of the method.
Description
Technical field
The present invention relates to solar energy photovoltaic material preparation field, be specifically related to a kind of P type and mix gallium crystalline silicon and preparation method thereof.
Background technology
Current casting polycrystalline silicon sheet is based on P type polycrystalline, and doping agent is mainly boron, because the segregation coefficient of boron is close to 1, so resistivity distribution is comparatively even, and cycle stock easily processes use.But boron-doping silicon chip due to the existence of boron oxygen complex body can produce photo attenuation in the follow-up use of cell piece.
For P-type silicon sheet, mix gallium silicon chip to be proved to be and to there is no light decay, but because the segregation coefficient of gallium in silicon is extremely low, be only 0.008, in actual production, normal method mixes the silicon ingot resistivity distribution of gallium between 0.1-5 Ω cm, distribution range is excessive, meets the qualified part of resistivity between 0.8-3 Ω cm usual less than 50%, cannot carry out production and promote.
Some uniform methods of controlling resistance rate mentioned in improving one's methods, mix altogether based on doping compensation element and boron gallium substantially at present.But it is serious that this method can cause silicon chip to compensate, and in cycle stock, impurity component is very complicated, and the existence that boron gallium is mixed altogether due to boron in addition can not solve light decay problem completely, it is the major cause that in actual production, inconvenience is promoted.
Summary of the invention
Based on this, be necessary to provide one can accurately controlling resistance rate, make the uniform P type of resistivity distribution mix the preparation method of gallium crystalline silicon.
A preparation method for gallium crystalline silicon mixed by P type, comprises the following steps:
The silicon material containing gallium doping agent is dropped in crucible, a circle N-type doping compensation agent coating is coated with, within the scope of the difference of altitude of the crystalline silicon that the silicon liquid surface after the input fusing of the silicon material containing gallium doping agent, the position of described N-type doping compensation agent coating generates with silicon liquid inside wherein said crucible wall;
Silicon material melts, directional freeze, makes the silicon liquid containing gallium doping agent generate P type and mixes gallium crystalline silicon.
Aforementioned p-type is mixed in the preparation method of gallium crystalline silicon, in long brilliant process, because the density of the density ratio liquid silicon of solid silicon is large, therefore along with silicon crystal grow, silicon liquid surface can raise gradually, silicon liquid contacts with the N-type doping compensation agent on crucible wall, from crucible wall, constantly liquid is dissolved in along with increasing N-type doping compensation agent duration of contact, along with the increase of silicon ingot height, compensator mixes more, therefore the preparation method of aforementioned p-type crystalline silicon can carry out doping compensation on crystal growth direction, thus solve P type and mix gallium crystalline silicon ingot and generate at crystal the problem that resistivity distribution range is excessive on direction, the resistivity of gallium crystalline silicon ingot mixed by accurate control P type.
Wherein in an embodiment, before the step dropping into the silicon material containing gallium doping agent in crucible, further comprising the steps of:
The quality of silicon material containing gallium doping agent according to input and the internal diameter of crucible, calculate the height on the silicon liquid surface after the fusing of silicon material and the height of the crystalline silicon generated;
The crucible wall of difference of altitude scope being positioned at the crystalline silicon that silicon liquid surface generates with silicon liquid applies N-type doping compensation agent coating.
Wherein in an embodiment, all regions first on crucible internal walls apply one deck silicon nitride coating, then on the crucible wall of difference of altitude scope being positioned at the crystalline silicon that silicon liquid surface generates with silicon liquid, apply N-type doping compensation agent coating, this coating is at inner surface of crucible or on silicon nitride coating.
Wherein in an embodiment, described N-type doping compensation agent coating is coated on crucible wall by the mode spraying or brush.
Wherein in an embodiment, described gallium doping agent is silicon-gallium mother alloy or pure gallium.
Wherein in an embodiment, described N-type doping compensation agent is N-type mother alloy or N-type semiconductor element.
Wherein in an embodiment, described N-type mother alloy is silicon-phosphorus, silicon-arsenic or silicon-antimony mother alloy; Described N-type semiconductor element is phosphorus, arsenic or antimony.
In addition, additionally provide a kind of P type obtained by aforesaid method and mix gallium crystalline silicon.
Gallium crystalline silicon mixed by the P type obtained by aforesaid method, in long brilliant process, crystal growth direction obtains doping compensation, therefore the resistivity of the crystalline silicon ingot of major part height can by the scope of accurate control 0.8-3 Ω cm, decrease the intercepting height at silicon ingot top, improve the utilization ratio of silicon ingot.
Accompanying drawing explanation
Fig. 1 is the schema that the preparation method of gallium crystalline silicon mixed by P type;
Fig. 2 is the position view that the N-type doping compensation agent coating in the preparation method of gallium crystalline silicon on crucible wall mixed by P type;
Fig. 3 is that P type is mixed in gallium crystalline silicon preparation method process, the position relationship schematic diagram of silicon liquid surface, solid-liquid surface and N-type doping compensation agent coating.
Embodiment
Please refer to Fig. 1, disclose the preparation method that gallium crystalline silicon mixed by a kind of P type, comprise the following steps:
S110, to drop in crucible containing the silicon material of gallium doping agent, a circle N-type doping compensation agent coating is coated with, within the scope of the difference of altitude of the crystalline silicon that the silicon liquid surface after the input fusing of the silicon material containing N-type doping agent, the position of described N-type doping compensation agent coating generates with silicon liquid inside wherein said crucible wall.
Please refer to Fig. 2, the height of the silicon liquid surface distance crucible bottom after the silicon material containing gallium doping agent melts in crucible is L1, the height of the crystalline silicon that silicon liquid generates is L2, the position of N-type doping compensation agent coating 110 is between L1 ~ L2, and wherein the solid surface of crystal that formed of the height of crystalline silicon and silicon liquid is to the height of crucible bottom.
When gallium crystalline silicon mixed by preparation P type, first at all region coatings in whole crucible internal walls surface last layer silicon nitride layer, form N-type doping compensation agent coating in the certain area then on crucible inner side-wall, use this crucible to produce crystalline silicon by directional solidification method.
Silicon nitride coating can prevent silicon ingot from gluing pot.The position of N-type doping compensation agent coating on crucible wall is by calculating.Please refer to Fig. 2, according to the quality of the silicon material containing gallium doping agent preparing to drop into and the internal diameter of the crucible used, calculate the height L1 on the silicon liquid surface after the fusing of silicon material and the height L2 of the crystalline silicon generated respectively, then the position of N-type doping compensation agent coating 110 is determined within the scope of the difference of altitude of L1 and L2.The position of N-type doping compensation agent coating is coated on crucible wall by the mode spraying or brush after determining.
Gallium doping agent can be silicon-gallium mother alloy or gallium element.N-type doping compensation agent is N-type mother alloy or N-type semiconductor element, and N-type mother alloy is silicon-phosphorus, silicon-arsenic or silicon-antimony mother alloy; Described N-type semiconductor element is phosphorus, arsenic or antimony.N-type doping compensation agent coating can obtain as follows: add appropriate binding agent by after N-type doping compensation agent, silica flour, silica powder dilute with water; On this basis, silicon nitride can also be added, silicon oxide powder.
In production process, can in advance by calculating the crucible with N-type doping compensation agent coating of obtained different size, like this, when gallium crystalline silicon mixed by preparation P type as stated above, directly to the silicon material containing gallium doping agent putting into certain mass in the crucible with N-type doping compensation agent coating, can enhance productivity.
S120, silicon material melt, directional freeze, make the silicon liquid containing gallium doping agent generate P type and mix gallium crystalline silicon.Please refer to Fig. 3, in long brilliant process, because the density of the density ratio liquid silicon of solid silicon is large, therefore along with the growth of silicon crystal, , silicon liquid surface raises gradually, N-type doping compensation agent on silicon liquid and crucible wall comes in contact, along with duration of contact increases, N-type doping compensation agent constantly dissolves in liquid from crucible wall, along with the increase of silicon ingot height, compensator mixes more, therefore on crystal growth direction, constantly doping compensation can be carried out to crystal, thus solve P type and mix gallium crystalline silicon and generate at crystal the problem that resistivity distribution range is excessive on direction, the resistivity of gallium crystalline silicon mixed by the whole P type of accurate control, the electrical resistivity range making the P type of major part height mix gallium crystalline silicon controls between 0.8-3 Ω cm.
The preparation method of above-mentioned crystalline silicon is simple to operate, is easy to produce promote, and resistivity control effects P type being mixed to gallium crystalline silicon ingot is remarkable, decreases the intercepting height at silicon ingot top, reduces production cost, improve the utilization ratio of silicon ingot.
Below in conjunction with embodiment, the implementation process how preparation method of gallium crystalline silicon mixed by P type is described.
Embodiment one,
1, choose appropriate P powder or silicon phosphorus alloy as N-type compensator, add appropriate binding agent, as the raw material making coating with after silica flour, silica powder dilution.
2, normal spraying silicon nitride coating on crucible internal walls.
3, then coating location is determined by calculating, the raw material prepared is coated in the position range of calculating by the mode spraying or brush, form one deck coating, the wherein ingot casting of charge amount 480kg, crucible internal diameter 840mm, calculate the height on fusing its silicon liquid surface rear at 268mm, it is 292mm that long crystalline substance terminates rear crystal height, then can determine that coating location is between distance crucible bottom 268-292mm.
4, the mixture of the polycrystalline silicon material of 480kg and pure gallium is loaded crucible, wherein the doping content of gallium is 25000ppbw.
5, heat fused, directional freeze, makes silicon liquid generate crystalline silicon.
In long brilliant process, because the segregation coefficient of gallium is very little, gallium can be distributed to upper part of silicon ingot by the fractional condensation overwhelming majority, and the doping content of gallium increases gradually from bottom to top.Because the density of the density ratio liquid silicon of solid silicon is large, therefore along with silicon crystal grow, silicon liquid surface can raise gradually, and silicon liquid contacts with the P powder on crucible wall or silicon phosphorus alloy, along with duration of contact increases, phosphorus constantly dissolves in liquid from crucible wall, along with the increase of silicon ingot height, mix more, more to the doping compensation of silicon ingot, thus the resistivity of silicon ingot head is controlled, the resistivity distribution of whole silicon ingot.
In addition, because the resistivity of silicon ingot head can be controlled by doping compensation, in polycrystalline silicon material, the doping content of gallium can promote further, and the gallium doping content bottom silicon ingot is promoted, and the resistivity bottom silicon ingot also can be controlled within 3 Ω cm.
After silicon ingot evolution, measured the distribution of crystal resistivity by four probe method, find that the resistivity of the silicon ingot within 85% height is all within the scope of 1.5-2.5 Ω cm; The resistivity of the silicon ingot within 95% height is all within the scope of 0.8-3 Ω cm.As can be seen here, the preparation method that aforementioned p-type mixes gallium crystalline silicon precisely can control the resistivity of crystalline silicon ingot, the resistivity of the silicon ingot within 95% height, all within the scope of 0.8-3 Ω cm, intercepting height because this reducing silicon ingot top, improve the utilization ratio of silicon ingot.
Embodiment two,
1, choose appropriate antimony powder or silicon-antimony alloy, add appropriate binding agent, as the raw material making coating with after silica flour, silica powder dilution.
2, coating location is determined by calculating, the coating material prepared is fixed on the position range determined by the mode spraying or brush, form the coating that one deck has compensation ability, the wherein ingot casting of charge amount 800kg, crucible internal diameter is 1000mm, after having melted, the height on its silicon liquid surface is at 314mm, and it is 343mm that long crystalline substance terminates rear crystal height, then coating location is determined between distance crucible bottom 314-343mm.
3, then continue crucible internal walls spraying silicon nitride coating.
4, the mixture of the polysilicon of 800kg and pure gallium is loaded crucible.
5, directional freeze, makes virgin polycrystalline silicon material melt and form crystalline silicon.
In long brilliant process, because the segregation coefficient of gallium is very little, gallium can be distributed to upper part of silicon ingot by the fractional condensation overwhelming majority, and the doping content of gallium increases gradually from bottom to top.Because the density of the density ratio liquid silicon of solid silicon is large, therefore along with silicon crystal grow, silicon liquid surface can raise gradually, the antimony powder on silicon liquid and crucible wall or silicon-antimony alloy, along with duration of contact increases, antimony constantly dissolves in liquid from crucible wall, along with the increase of silicon ingot height, mix more, more to the doping compensation of silicon ingot, thus the resistivity of silicon ingot head is controlled, the resistivity distribution of whole silicon ingot.
In addition, because the resistivity of silicon ingot head can be controlled by doping compensation, in polycrystalline silicon material, the doping content of gallium can promote further, and the gallium doping content bottom silicon ingot is promoted, and the resistivity bottom silicon ingot also can be controlled within 3 Ω cm.
After silicon ingot evolution, measured the distribution of crystal resistivity by four probe method, find that the resistivity of the silicon ingot within 85% height is all within the scope of 1.5-2.5 Ω cm; The resistivity of the silicon ingot within 95% height is all within the scope of 0.8-3 Ω cm.As can be seen here, the preparation method that aforementioned p-type mixes gallium crystalline silicon precisely can control the resistivity of crystalline silicon ingot, the resistivity of the silicon ingot within 95% height, all within the scope of 0.8-3 Ω cm, intercepting height because this reducing silicon ingot top, improve the utilization ratio of silicon ingot.
Each technical characteristic of the above embodiment can combine arbitrarily, for making description succinct, the all possible combination of each technical characteristic in above-described embodiment is not all described, but, as long as the combination of these technical characteristics does not exist contradiction, be all considered to be the scope that this specification sheets is recorded.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. a preparation method for gallium crystalline silicon mixed by P type, it is characterized in that, comprises the following steps:
The silicon material containing gallium doping agent is dropped in crucible, a circle N-type doping compensation agent coating is coated with, within the scope of the difference of altitude of the crystalline silicon that the silicon liquid surface after the input fusing of the silicon material containing gallium doping agent, the position of described N-type doping compensation agent coating generates with silicon liquid inside wherein said crucible wall;
Silicon material melts, directional freeze, makes the silicon liquid containing gallium doping agent generate P type and mixes gallium crystalline silicon.
2. the preparation method of gallium crystalline silicon mixed by P type according to claim 1, it is characterized in that, before the step dropping into the silicon material containing gallium doping agent in crucible, further comprising the steps of:
The quality of silicon material containing gallium doping agent according to input and the internal diameter of crucible, calculate the height on the silicon liquid surface after the fusing of silicon material and the height of the crystalline silicon generated;
The crucible wall of difference of altitude scope being positioned at the crystalline silicon that silicon liquid surface generates with silicon liquid applies N-type doping compensation agent coating.
3. the preparation method of gallium crystalline silicon mixed by P type according to claim 2, it is characterized in that, the crucible wall of difference of altitude scope being positioned at the crystalline silicon that silicon liquid surface generates with silicon liquid applies N-type doping compensation agent coating, and this coating is at inner surface of crucible or on silicon nitride coating.
4. the preparation method of gallium crystalline silicon mixed by P type according to claim 1, it is characterized in that, described N-type doping compensation agent coating is coated on crucible wall by the mode spraying or brush.
5. the preparation method of gallium crystalline silicon mixed by P type according to claim 1, it is characterized in that, described gallium doping agent is silicon-gallium mother alloy or pure gallium.
6. the preparation method of gallium crystalline silicon mixed by P type according to claim 1, it is characterized in that, described N-type doping compensation agent is N-type mother alloy or N-type semiconductor element.
7. the preparation method of gallium crystalline silicon mixed by P type according to claim 6, it is characterized in that, described N-type mother alloy is silicon-phosphorus, silicon-arsenic or silicon-antimony mother alloy; Described N-type semiconductor element is phosphorus, arsenic or antimony.
8. a gallium crystalline silicon mixed by P type, it is characterized in that, described P type is mixed the method for gallium crystalline silicon according to any one of claim 1 to 7 and obtained.
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Application publication date: 20150819 |