CN102061515B - Quartz glass crucible and preparation method thereof - Google Patents
Quartz glass crucible and preparation method thereof Download PDFInfo
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- CN102061515B CN102061515B CN 201110001348 CN201110001348A CN102061515B CN 102061515 B CN102061515 B CN 102061515B CN 201110001348 CN201110001348 CN 201110001348 CN 201110001348 A CN201110001348 A CN 201110001348A CN 102061515 B CN102061515 B CN 102061515B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
- C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
Abstract
The invention discloses a quartz glass crucible which comprises a crucible basic body, wherein outer surfaces are covered outside the crucible basic body; the outer surfaces are outer surface layers of wall parts of the crucible basic body or all outer surface layers of the crucible basic body; the theoretical thickness of the wall part outer surface layers or the all outer surface layers is 0.2-0.3mm, and the layers are obtained by melting natural quartz sand doped with aluminum elements coming from aluminum hydroxide and/or an aluminum salt; the mass of the aluminum elements is calculated according to aluminum oxide which can be generated; and the mass content of the aluminum elements in the natural quartz sand doped with the aluminum elements is 100-1,000ppm. The quartz glass crucible is difficult to deform in a use process of pulling monocrystalline silicon, has longer service life, can be used for meeting the requirement for long-time use of a crucible with a larger diameter and can obtain a more stable crystal pulling progress.
Description
(1) technical field
The present invention relates to a kind of quartz glass crucibles, the quartz glass crucibles that particularly in crystal pulling method manufacture order crystal silicon, uses, and the preparation method of said quartz glass crucibles.
(2) background technology
The CZ method is widely used in the production process of silicon single crystal; Quartz crucible is generally adopted as the container that holds polycrystalline silicon material in the CZ method high temperature production silicon single crystal process; Therefore quartz crucible conduct and the object that the raw material of manufacture order crystal silicon directly contacts determined the key factor that can silicon single crystal be produced smoothly.
The process of CZ method manufacture order crystal silicon is to put into quartz crucible to many silicon wafers of raw material piece, and heating and melting in single crystal growing furnace is immersed in a bar-shaped crystal seed (title seed crystal) in the fused silicon liquid again.Under suitable temperature, the Siliciumatom in the molten silicon liquid can become single crystal along the crystallization of Siliciumatom arrangement architecture formation rule on the solid-liquid interface of crystal seed.The fusing point of silicon is about 1420 ℃, and whole C Z method produce single crystal process remains in the environment of high temperature negative pressure carries out.Therefore, quartz crucible behavior such as be prone to deform forces the crystal pulling process to be interrupted, and the crystal pulling process is caused disadvantageous effect, when serious even accident such as fused silicon liquid leakage can take place, causes heavy losses.Simultaneously, the continuous increase that requires along with the silicon chip diameter, to the also constantly increase thereupon of requirement of polycrystalline silicon raw material tonburden in the size of quartz crucible and the quartz crucible, this just further improves the non-deformability of quartz crucible and the requirement in work-ing life.
Usually solve quartz crucible non-deformability and the method that increases the service life; The purity that improve quartz crucible that adopt to improve quartz crucible viscosity at high temperature, are improved the non-deformability of quartz crucible more; For example Chinese patent CN 1671891 adopts the synthetic sand of based on very high purity to form the way of transparent internal layer at quartz crucible inner surface; Prolong quartz crucible duration of service at high temperature, but this method causes product cost higher because of a large amount of very expensive synthetic sands of prices that use; Technology is complicated simultaneously, is difficult to satisfy production requirement.
(3) summary of the invention
The purpose of this invention is to provide a kind of quartz glass crucibles, this crucible has stronger non-deformability, can prolong its work-ing life, and the present invention simultaneously also provides the preparation method of said quartz glass crucibles.
The technical scheme that the present invention adopts is:
A kind of quartz glass crucibles; Said quartz glass crucibles comprises crucible base, and described crucible base is coated with outside surface, and described outside surface is the wall portion outer surface layer of crucible base or whole outer surface layers of crucible base; The theoretic throat of said wall portion's outer surface layer or whole outer surface layers is 0.2～3.0mm; The natural siliceous sand fusion that is contained aluminium element by doping prepares, and said aluminium element comes from white lake and/or aluminium salt, and the quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate; The mass content that said doping contains aluminium element in the natural siliceous sand of aluminium element is 100～1000ppm, preferred 300～600ppm.
Further; Said quartz glass crucibles obtains by following method: the natural siliceous sand that doping is contained aluminium element is put into the crucible die of rotation; Said doping contains the outer or whole matrixes skins of wall portion matrix of the natural siliceous sand formation crucible shape of aluminium element under centrifugal action, adds natural siliceous sand then, and said natural siliceous sand forms the base layer of crucible shape on the outer or whole outer field surfaces of matrix of wall portion matrix under action of centrifugal force; Electrode to the crucible die top feeds the electric arc that strong current forms the condition of high temperature more than 2000 ℃ then; Silica sand is slowly melted, wall portion matrix outer or all outer corresponding wall portion's outer surface layer of formation of matrix or all outer surface layer, base layer forms crucible base; After treating that the silica sand fusion is accomplished; Take out the cooling back, promptly makes said quartz glass crucibles, and described aluminium element comes from white lake and/or aluminium salt.
Said aluminium salt is preferably the mixing of any one or two kinds in aluminum nitrate or the aluminum chloride, most preferably is aluminum nitrate.
The natural siliceous sand that said doping contains aluminium element can obtain by following method: white lake and/or aluminium salt are soluble in water; Be made into the solution that quality percentage mark is 0.1～30% (preferred 5%～15%); Join in the natural siliceous sand; Fully mix back following dry 20～500 minutes at 50～800 ℃; Obtain mixing and contain the natural siliceous sand of aluminium element, making the mass content of aluminium element in natural siliceous sand is 100～1000ppm, and the quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate.
Comparatively concrete, quartz glass crucibles of the present invention prepares by following method:
(1) any one or two or more mixing of white lake, aluminum nitrate, aluminum chloride are soluble in water; Be made into the quality percentage composition and be 0.1～30% solution; Join in the natural siliceous sand, fully mix the back 50～800 ℃ dry 20～500 minutes down, obtain mixing and contain the natural siliceous sand of aluminium element; Making the mass content of aluminium element in natural siliceous sand is 100～1000ppm, and the quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate;
(2) natural siliceous sand that the doping that step (1) is obtained contains aluminium element is put into the crucible die of rotation; Said doping contains the outer or whole matrixes skins of wall portion matrix of the natural siliceous sand formation crucible shape of aluminium element under centrifugal action; Add natural siliceous sand then, said natural siliceous sand forms the base layer of crucible shape on the outer or whole outer field surfaces of matrix of wall portion matrix under action of centrifugal force, and the electrode to the crucible die top feeds the electric arc that strong current forms the condition of high temperature more than 2000 ℃ then; Silica sand is slowly melted; Outer or whole outer corresponding wall portion's outer surface layer or the whole outer surface layers of forming of matrixes of wall portion matrix, base layer forms crucible base, treat that the silica sand fusion is accomplished after; Take out the cooling back, promptly makes said quartz glass crucibles; Said doping contains the quality consumption m1 of the natural siliceous sand of aluminium element; Estimate the thickness b1 and the area S1 that estimates wall portion's outer surface layer or whole outer surface layers of wall portion's outer surface layer or whole outer surface layers; Calculate according to formula m1=K1 * S1 * b1 * ρ 1; Wherein K1 is a different size diameter crucible experience factor, K1=1.2～1.8, the density of the natural siliceous sand that ρ 1 contains aluminium element for mixing; The density that described doping contains the natural siliceous sand of aluminium element is come in the density of natural siliceous sand, said expectation wall portion's outer surface layer or all the thickness b1 of outer surface layers be 0.2～3.0mm.
The normal density of natural siliceous sand before high-temperature fusion that ρ 1 according to the invention contains aluminium element for mixing; Doping contains the natural siliceous sand of aluminium element after fusion; Density can increase usually; For thickness that makes the outer surface layer that actual fusion obtains and the consistency of thickness of estimating outer surface layer; When calculating the quality consumption m1 of the natural siliceous sand that required doping contains aluminium element, the natural siliceous sand that contains aluminium element of mixing after the fusion contains the multiple that the density of the natural siliceous sand of aluminium element increases than the doping before the fusion, be also embodied among the COEFFICIENT K 1.
Can also be coated with theoretic throat on the internal surface of the crucible base of quartz glass crucibles according to the invention is the internal layer Clear coating of 0.5～1.5mm; Said internal layer Clear coating is to prepare through the fusion natural siliceous sand 2 contain aluminium element that mixes; Said aluminium element comes from white lake and/or aluminium salt; The quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate; The mass content that said doping contains aluminium element in the natural siliceous sand 2 of aluminium element is 50～500ppm, and preferred 100～300ppm, said internal surface are meant the bottom interior surface of crucible base, the wall portion internal surface of crucible base or whole internal surfaces of crucible base.
It is in order to distinguish mutually with the natural siliceous sand that doping that being used to before prepares outer surface layer contains aluminium element that said doping contains 2 in the natural siliceous sand 2 of aluminium element, not other implication.
The quartz glass crucibles that is coated with the internal layer Clear coating on the internal surface of said crucible base can prepare by following method:
The natural siliceous sand that doping is contained aluminium element is put into the crucible die of rotation; Said doping contains the outer or whole matrixes skins of wall portion matrix of the natural siliceous sand formation crucible shape of aluminium element under centrifugal action; Add natural siliceous sand then; Said natural siliceous sand forms the base layer of crucible shape on the outer or whole outer field surfaces of matrix of wall portion matrix under action of centrifugal force, and the electrode to the crucible die top feeds the electric arc that strong current forms the condition of high temperature more than 2000 ℃ then, and silica sand is slowly melted; Wall portion matrix outer or all outer corresponding wall portion's outer surface layer of formation of matrix or all outer surface layer; Base layer forms crucible base, treat that the silica sand fusion is accomplished after, the natural siliceous sand 2 that doping is contained aluminium element is put into the internal surface of crucible base uniformly; Said internal surface is the bottom interior surface of crucible base, the wall portion internal surface of crucible base or whole internal surfaces of crucible base; Feed intake after end and the fusion completion, the taking-up of cooling back promptly makes said quartz glass crucibles.
More specifically, be coated with on the internal surface of said crucible base the internal layer Clear coating quartz glass crucibles prepare by following method:
(1) any one in white lake, aluminum nitrate, the aluminum chloride or two or more mixing are soluble in water; Be made into the solution that quality percentage mark is 0.1～30% (preferred 5%～15%); Join in the natural siliceous sand, fully mix the back 50～800 ℃ dry 20～500 minutes down, obtain mixing and contain the natural siliceous sand of aluminium element; Making the mass content of aluminium element in natural siliceous sand is 100～1000ppm, and the quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate;
(2) any one in white lake, aluminum nitrate, the aluminum chloride or two or more mixing are soluble in water; Be made into the solution that quality percentage mark is 0.1～30% (preferred 5%～15%); Join in the natural siliceous sand, fully mix afterwards and descended the natural siliceous sand 2 that obtains mixing and contain aluminium element dry 20～500 minutes at 50～800 ℃; Making the mass content of aluminium element in natural siliceous sand is 50～500ppm, and the quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate;
(3) natural siliceous sand that the doping that step (1) is obtained contains aluminium element is put into the crucible die of rotation; Said doping contains the outer or whole matrixes skins of wall portion matrix of the natural siliceous sand formation crucible shape of aluminium element under centrifugal action; Add natural siliceous sand then, said natural siliceous sand forms the base layer of crucible shape on the outer or whole outer field surfaces of matrix of wall portion matrix under action of centrifugal force, and the electrode to the crucible die top feeds the electric arc that strong current forms the condition of high temperature more than 2000 ℃ then; Silica sand is slowly melted; Outer or whole outer corresponding wall portion's outer surface layer or the whole outer surface layers of forming of matrixes of wall portion matrix, base layer forms crucible base, treat that the silica sand fusion is accomplished after; The doping that step (2) is obtained contains the natural siliceous sand 2 of aluminium element; Put into the internal surface of crucible base uniformly with 50～100g/ minute speed, said internal surface is the bottom interior surface of crucible base, the wall portion internal surface of crucible base or whole internal surfaces of crucible base, feeds intake to finish and after fusion accomplishes; Take out the cooling back, promptly makes said quartz glass crucibles;
Said doping contain aluminium element natural siliceous sand quality consumption m1 with estimate wall portion's outer surface layer or all outer surface layers thickness b1 with estimate wall portion's outer surface layer or whole area S1 of outer surface layers; Calculate according to formula m1=K1 * S1 * b1 * ρ 1; Wherein K1 is a different size diameter crucible experience factor; K1=1.2～1.8; The density that the density of the natural siliceous sand that ρ 1 contains aluminium element for mixing, described doping contain the natural siliceous sand of aluminium element is come in the density of natural siliceous sand, said expectation wall portion's outer surface layer or all the thickness b1 of outer surface layers be 0.2～3mm;
Said doping contains the quality consumption m2 of natural siliceous sand 2 of aluminium element with the area S2 of thickness b2 that estimates the internal layer Clear coating and the internal surface of estimating to apply; Calculate according to formula m2=K2 * S2 * b2 * ρ 2; Wherein K2 is a different size diameter crucible experience factor; K2=1.2～1.8; The density that the density of the natural siliceous sand 2 that ρ 2 contains aluminium element for mixing, described doping contain the natural siliceous sand 2 of aluminium element is come in the density of natural siliceous sand, and the thickness b2 of said expectation internal layer Clear coating is 0.5～1.5mm.
The normal density of natural siliceous sand 2 before high-temperature fusion that ρ 2 according to the invention contains aluminium element for mixing; Doping contains the natural siliceous sand 2 of aluminium element after fusion; Density can increase usually; For thickness that makes the internal layer Clear coating that actual fusion obtains and the consistency of thickness of estimating the internal layer Clear coating; When calculating the quality consumption m2 of the natural siliceous sand 2 that required doping contains aluminium element, the natural siliceous sand 2 that contains aluminium element of mixing after the fusion contains the multiple that the density of the natural siliceous sand 2 of aluminium element increases than the doping before the fusion, be also embodied among the COEFFICIENT K 2.
Quartz glass crucibles provided by the invention is difficult for deforming in the use of pulling silicon single crystal, and pot life is longer, can satisfy than the long-time requirement of using of major diameter crucible, can obtain more stable crystal pulling process.
(4) description of drawings
Fig. 1 is the transversal profile synoptic diagram that is coated with the quartz glass crucibles of internal layer Clear coating on whole internal surfaces of whole outer surface layers of comprising crucible base, crucible base, crucible base;
Fig. 2 is the enlarged diagram of the part of A shown in Fig. 1, and among Fig. 2,1 is depicted as the internal layer Clear coating; 2 are depicted as crucible base; 3 are depicted as outer surface layer.
(5) embodiment
Below in conjunction with specific embodiment the present invention is further described, but protection scope of the present invention is not limited in this:
Doping contains the compound method of the silica sand of aluminium element: the white lake and/or the aluminium salt that take by weighing certain mass; The solution that is mixed with soluble in water; Then this solution is added in the natural siliceous sand, fully mixes after drying, can make mixes contains the silica sand of aluminium element.
Preparation is mixed and is contained the silica sand of aluminium element, concrete white lake and/or reaction conditions such as following tables 1 such as aluminium salt consumption, strength of solution according to the method described above:
Table 1
The natural siliceous sand 833g of the doped with Al element of model b (is estimated thickness b1=1.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Natural siliceous sand is poured in the quartz crucible mould again, under action of centrifugal force, formed the base layer of crucible shape, the electrode to mould top feeds strong current formation electric arc then; And then in mould moment form＞2000 ℃ the condition of high temperature silica sand slowly melted; Wall portion matrix outer fusion formation wall portion outer surface layer, base layer forms crucible base, treat that the silica sand fusion is accomplished after; Take out in mould the cooling back, promptly can make outer the doping and contain the quartz crucible of Al element.
The natural siliceous sand 1666g of the doped with Al element of model c (is estimated thickness b1=2.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Natural siliceous sand is poured in the quartz crucible mould again, under action of centrifugal force, formed the base layer of crucible shape, the electrode to mould top feeds strong current formation electric arc then; And then in mould moment form＞2000 ℃ the condition of high temperature silica sand slowly melted; Wall portion matrix outer fusion formation wall portion outer surface layer, base layer forms crucible base, treat that the silica sand fusion is accomplished after; Take out in mould the cooling back, promptly can make outer the doping and contain the quartz crucible of Al element.
The natural siliceous sand 2499g of the doped with Al element of model d (is estimated thickness b1=3.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Natural siliceous sand is poured in the quartz crucible mould again, under action of centrifugal force, formed the base layer of crucible shape, the electrode to mould top feeds strong current formation electric arc then; And then in mould moment form＞2000 ℃ the condition of high temperature silica sand slowly melted; Wall portion matrix outer fusion formation wall portion outer surface layer, base layer forms crucible base, treat that the silica sand fusion is accomplished after; Take out in mould the cooling back, promptly can make outer the doping and contain the quartz crucible of Al element.
Embodiment 4
The natural siliceous sand 1666g of the doped with Al element of model e (is estimated thickness b1=1.0mm, estimates the outer field area s1=7000cm of whole matrixes
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the whole matrixes that constitute the quartz crucible matrix are outer.Natural siliceous sand is poured in the quartz crucible mould again, under action of centrifugal force, formed the base layer of crucible shape, the electrode to mould top feeds strong current formation electric arc then; And then in mould moment form＞2000 ℃ the condition of high temperature silica sand slowly melted; Wall portion matrix outer fusion formation wall portion outer surface layer, base layer forms crucible base, treat that the silica sand fusion is accomplished after; Take out in mould the cooling back, promptly can make outer the doping and contain the quartz crucible of Al element.
Embodiment 5
The natural siliceous sand 833g of the doped with Al element of model f (is estimated thickness b1=1.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Again natural siliceous sand is poured in the quartz crucible mould; Under action of centrifugal force, form the base layer of crucible shape; Then the electrode on mould top is fed strong current and forms electric arc, so in mould moment form＞2000 ℃ the condition of high temperature and silica sand slowly melted wall portion matrix outer fusion formation wall portion outer surface layer; Base layer forms crucible base; After treating the silica sand melt molding, the natural siliceous sand 416.5g that the doping of model a is contained the doped with Al element (estimates thickness b=0.5mm, estimates the internal surface area s=3500cm of wall portion that applies
2, density p=1.4g/cm
3, get COEFFICIENT K=1.7), evenly put into the wall portion internal surface of quartz glass crucible base body with 100g/ minute speed, wait to feed intake and finish and after fusion accomplishes, after the cooling crucible is taken out, promptly can make inside and outside layer and mix and contain the quartz crucible of Al element.
Embodiment 6
The natural siliceous sand 833g of the doped with Al element of model f (is estimated thickness b1=1.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Again the 25Kg natural siliceous sand is poured in the quartz crucible mould; Under action of centrifugal force, form the base layer of crucible shape; Then the electrode on mould top is fed strong current and forms electric arc, so in mould moment form＞2000 ℃ the condition of high temperature and silica sand slowly melted wall portion matrix outer fusion formation wall portion outer surface layer; Base layer forms crucible base; After treating the silica sand melt molding, the natural siliceous sand 416.5g that the doping of model a is contained the doped with Al element (estimates thickness b=0.5mm, estimates the long-pending s=3500cm of the bottom interior surface that applies
2, density p=1.4g/cm
3, get COEFFICIENT K=1.7), evenly put into the bottom interior surface of quartz glass crucible base body with 100g/ minute speed, wait to feed intake and finish and after fusion accomplishes, after the cooling crucible is taken out, promptly can make inside and outside layer and mix and contain the quartz crucible of Al element.
Embodiment 7
The natural siliceous sand 833g of the doped with Al element of model f (is estimated thickness b1=1.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Again the 25Kg natural siliceous sand is poured in the quartz crucible mould; Under action of centrifugal force, form the base layer of crucible shape; Then the electrode on mould top is fed strong current and forms electric arc, so in mould moment form＞2000 ℃ the condition of high temperature and silica sand slowly melted wall portion matrix outer fusion formation wall portion outer surface layer; Base layer forms crucible base; After treating the silica sand melt molding, the natural siliceous sand 2499g that the doping of model c is contained the doped with Al element (estimates thickness b=1.5mm, estimates the whole internal surface area s=7000cm that apply
2, density p=1.4g/cm
3, get COEFFICIENT K=1.7), evenly put into whole internal surfaces of quartz glass crucible base body with 100g/ minute speed, wait to feed intake and finish and after fusion accomplishes, after the cooling crucible is taken out, promptly can make inside and outside layer and mix and contain the quartz crucible of Al element.
Embodiment 8
The natural siliceous sand 833g of the doped with Al element of model f (is estimated thickness b1=1.0mm, estimates the outer field area s1=3500cm of wall portion's matrix
2, density p 1=1.4g/cm
3, get COEFFICIENT K=1.7), put into 20 inches quartz crucible moulds of diameter of rotation, through centrifugal action this silica sand is evenly distributed on the rotating mold, the wall portion matrix that constitutes the quartz crucible matrix is outer.Again the 25Kg natural siliceous sand is poured in the quartz crucible mould; Under action of centrifugal force, form the base layer of crucible shape; Then the electrode on mould top is fed strong current and forms electric arc, so in mould moment form＞2000 ℃ the condition of high temperature and silica sand slowly melted wall portion matrix outer fusion formation wall portion outer surface layer; Base layer forms crucible base; After treating the silica sand melt molding, the natural siliceous sand 1249.5g that the doping of model d is contained the doped with Al element (estimates thickness b=1.5mm, estimates the internal surface area s=3500cm of wall portion that applies
2, density p=1.4g/cm
3, get COEFFICIENT K=1.7), evenly put into the wall portion internal surface of quartz glass crucible base body with 100g/ minute speed, wait to feed intake and finish and after fusion accomplishes, after the cooling crucible is taken out, promptly can make inside and outside layer and mix and contain the quartz crucible of Al element.
Comparative example 1:
The natural siliceous sand of 25Kg is put in 20 inches crucible dies of rotation; Through centrifugal action this natural siliceous sand is formed the quartz crucible shape; Electrode to mould top feeds strong current then, so in mould moment form the electric arc of＞2000 ℃ the condition of high temperature, slowly silica sand is melted into quartz crucible; Take out the cooling back, and obtaining inside and outside surface does not all have the common quartz crucible of mixing Al.
Through automatic control crystal pulling environmental testing test; Test-results shows: mix inside and outside layer that the quartz crucible that contains the Al element and embodiment 5～8 make of outside surface that embodiment 1～4 makes mixes and contains the quartz crucible of Al element; Tear stove open after in the brilliant environment of Cz farad, continuing 160 hours, crucible does not all deform etc. and to be unfavorable for the behavior of crystal pulling; And the quartz crucible that the Comparative Examples 1 of not carrying out admixture Al element makes continues 100 hours in the brilliant environment of Cz farad after; The crucible port deforms; Find that the embedding behavior in three lobe pot bearings of quartz crucible matrix is arranged after tearing stove open, cause the crucible distortion, this will have a strong impact on carrying out smoothly of crystal pulling.
Claims (4)
1. the preparation method of a quartz glass crucibles; Said quartz glass crucibles comprises crucible base; Described crucible base is coated with outside surface, and described outside surface is the wall portion outer surface layer of crucible base or whole outer surface layers of crucible base, and the theoretic throat of said wall portion's outer surface layer or whole outer surface layers is 0.2～3.0mm; The natural siliceous sand fusion that is contained aluminium element by doping prepares; Said aluminium element comes from white lake and/or aluminium salt, and the quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate, and the mass content that said doping contains aluminium element in the natural siliceous sand of aluminium element is 100～1000ppm; It is characterized in that: the natural siliceous sand that doping is contained aluminium element is put into the crucible die of rotation; Said doping contains the outer or whole matrixes skins of wall portion matrix of the natural siliceous sand formation crucible shape of aluminium element under centrifugal action, adds natural siliceous sand then, and said natural siliceous sand forms the base layer of crucible shape on the outer or whole outer field surfaces of matrix of wall portion matrix under action of centrifugal force; Electrode to the crucible die top feeds the electric arc that strong current forms the condition of high temperature more than 2000 ℃ then; Silica sand is slowly melted, wall portion matrix outer or all outer corresponding wall portion's outer surface layer of formation of matrix or all outer surface layer, base layer forms crucible base; After treating that the silica sand fusion is accomplished, take out the cooling back.
2. preparation method as claimed in claim 1; It is characterized in that; After treating that the silica sand fusion is accomplished, the natural siliceous sand 2 that doping is contained aluminium element is put into the internal surface of crucible base uniformly, and said aluminium element comes from white lake and/or aluminium salt; The quality of said aluminium element is with the Mass Calculation of the aluminum oxide that can generate; The mass content that said doping contains aluminium element in the natural siliceous sand 2 of aluminium element is 50～500ppm, and said internal surface is the bottom interior surface of crucible base, the wall portion internal surface of crucible base or whole internal surfaces of crucible base, feeds intake to finish and after fusion accomplishes; Take out the cooling back, is the internal layer Clear coating of 0.5～1.5mm thereby on the internal surface of crucible base, form theoretic throat.
3. preparation method as claimed in claim 2; It is characterized in that; Natural siliceous sand and natural siliceous sand 2 that said doping contains aluminium element obtain by following method: white lake and/or aluminium salt are soluble in water; Be made into quality percentage mark and be 0.1～30% solution, join in the natural siliceous sand, fully mix the back 50～800 ℃ dry 20～500 minutes down.
4. like each described preparation method among the claim 1-3, it is characterized in that said aluminium salt is the mixing of any one or two kinds in aluminum nitrate or the aluminum chloride.
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| KR102253602B1 (en) * | 2016-09-13 | 2021-05-18 | 가부시키가이샤 사무코 | Quartz glass crucible |
| CN106927802A (en) * | 2017-03-17 | 2017-07-07 | 邹亚静 | A kind of manufacture method for noting solidification forming fused silica crucible |
| CN109467306B (en) * | 2018-11-08 | 2021-10-19 | 锦州佑鑫石英科技有限公司 | Processing method of high-strength quartz crucible for monocrystalline silicon production |
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| CN101570391A (en) * | 2009-06-10 | 2009-11-04 | 黄洁 | Process for producing arc quartz crucible by vacuum plus coating, equipment, product thereof |
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Effective date of registration: 20170117 Address after: 750299 Yinchuan economic and Technological Development Zone, Guangming West Road, No. 23, No. Patentee after: Ferrotec (Ningxia) Advanced Quartz Material Co., Ltd. Address before: 310053 Binjiang District, Zhejiang Province, Hangzhou Road, No. 668 Patentee before: Advanced Quartz Material (Hangzhou) Co., Ltd. |
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Address after: 750299 No. 23, Guangming West Road, economic and Technological Development Zone, Yinchuan City, Ningxia Hui Autonomous Region Patentee after: Ningxia dunyuan poly core semiconductor technology Co.,Ltd. Address before: 750299 No. 23, Guangming West Road, economic and Technological Development Zone, Yinchuan City, Ningxia Hui Autonomous Region Patentee before: FERROTEC (NINGXIA) ADVANCED QUARTZ MATERIAL Co.,Ltd. |