CN201527173U - Composite-layer quartz crucible - Google Patents

Composite-layer quartz crucible Download PDF

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Publication number
CN201527173U
CN201527173U CN2009201586611U CN200920158661U CN201527173U CN 201527173 U CN201527173 U CN 201527173U CN 2009201586611 U CN2009201586611 U CN 2009201586611U CN 200920158661 U CN200920158661 U CN 200920158661U CN 201527173 U CN201527173 U CN 201527173U
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layer
silica
crucible
transparent glass
thickness
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Expired - Lifetime
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CN2009201586611U
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Chinese (zh)
Inventor
黄乃军
黄洁
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Yuyao Qiming quartz Co., Ltd.
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Yuyao Jingying Crucible Co Ltd
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Abstract

The utility model discloses a composite-layer quartz crucible which pertains to the technical field of a crucible furnace. The composite-layer quartz crucible comprises an outer derivation layer, a silica body layer, a transparent glass layer, a high-temperature settled layer and a normal-temperature coating, wherein the outer derivation layer is at the outmost layer, and the silica body layer, the transparent glass layer, the high-temperature settled layer and the normal-temperature coating are arranged in sequence from outside to inside; the silica body layer is a high-purity natural quartz sand layer which contains 99.99 percent of silica, and the thickness thereof is 6 to 8 MM; the transparent glass layer is a high-purity natural quartz sand layer which contains 99.99 percent of silica without gas, and the thickness thereof is 2 to 6 MM; the high-temperature settled layer is an ultra-high-purity natural quartz sand layer which contains more than 99.999 percent of silica, and the thickness thereof is 0.7 to 2.0 MM; the outer derivation layer is a crystallization accelerator layer, and the thickness thereof is 0.2 to 0.4 MM; and the normal-temperature coating is a crystallization layer combining silicic acid with silicon nitride mixture, and the thickness thereof is 0.01 to 0.03 MM. The composite-layer quartz crucible has the benefits of well solving the problem of strength of the quartz crucible in environment with high temperature for a long time, meeting the requirement of purity on the inner surface of the crucible in crystal pulling process, reducing the oxygen content of a silicon single crystal rod, and improving the crystallization rate of single crystal.

Description

A kind of composite bed silica crucible
Technical field
The utility model relates to a kind of silica crucible, particularly relates to a kind of composite bed silica crucible, belongs to the crucible furnace technical field.
Background technology
Along with the progress of science and technology, there is a day by day strict demand in market to the quality requirements of monocrystalline silicon.And the crystal pulling industry specifically refine on the quality requirements to silicon chip, is absorbed in " crystal forming rate " " oxygen content ", the raising of " conversion ratio " and " service life " these indexs.For the container that must use---the intensity and the purity of silica crucible have proposed harsher requirement.As raw material---the monocrystalline silicon that most of solar energy and semi-conductor electricity sub-element are made, must in monocrystal growing furnace, refine and form.The method that this refinement draws high is referred to as Czochralski technique (being called for short the CZ method).Polysilicon is dropped into silica crucible, by near being warmed to 1450 degree of silica crucible, melt that polysilicon in the silica crucible is solid-state to contact molten silicon with crystal seed then to liquid state, by the pull monocrystal rod of growing.Lift in the process this, silica crucible must stand long vacuum environment, high mechanochemistry stress and hot environment, and tangible distortion do not occur, and cracking, and the serious crystallization of crucible entity do not occur and come off.The quality quality of silica crucible directly has influence on the quality of the monocrystal rod of being grown.
The silica crucible of making on the domestic market is mainly common silica crucible, transparent glass layer (vacuum layer) silica crucible, high temperature deposition layer silica crucible, normal temperature coating quartz crucible.Common silica crucible produces a lot of gases because silica at high temperature melts, and gas can not be discharged when founding crucible completely; The whole sidewall of crucible of being made under ultramicroscopic observation has a lot of micro-bubbles, because the bubble of sidewall of crucible is a lot, the situation therapeutic method to keep the adverse qi flowing downward that temperature is very high when the pulling monocrystal generation swelling fracture of steeping oneself-meeting, cause gas and impurity after the crucible bubble breaks to sneak into just in the pulled crystal rod, make monocrystalline oxygen content height, density contrast, purity is affected, final result is that monocrystalline silicon piece is not long service life, and conversion ratio is not up to standard; In addition, tangible plastic deformation appears in crucible insufficient strength easily when the high temperature crystal pulling, and this method can only be used a kind of quartz sand, so the purity of inner surface of crucible does not reach instructions for use.Transparent glass layer (vacuum layer) silica crucible, the purity requirement that can not solve inner surface of crucible; High temperature deposition layer silica crucible can not reach in the pulling monocrystal process fully because bubble-free layer is thin, silica crucible at high temperature, the Capability Requirement of resistance to deformation for a long time; The normal temperature coating quartz crucible, the normal temperature coating is very thin, can not satisfy the requirement to intensity when pulling monocrystal of heavy caliber crucible fully.
The utility model content
The purpose of this utility model is the defective at above-mentioned prior art, a kind of composite bed silica crucible is provided, the resistance to deformation of silica crucible, anti-sagging ability have been increased, reduced the oxygen content of silicon single crystal rod, when having improved crystal forming rate, improve the purity of calorific intensity and inner surface, satisfied the needs of CZ method pulling monocrystal.
The technical scheme taked of the utility model is to achieve these goals: a kind of composite bed silica crucible, comprise body layer, body layer is the high-purity natural quartz sand layer that contains silica 99.99%, and thickness is 6-8MM, also comprises transparent glass layer, high temperature deposition layer; Outermost layer is the silica body layer, inwardly is transparent glass layer, high temperature deposition layer successively.
Described transparent glass layer is not for to contain high-purity natural quartz sand layer gas, that contain silica 99.99%, and the thickness of transparent glass layer is 2-6MM.
Described high temperature deposition layer is that to contain silica be ultra-pure natural quartz layer of sand more than 99.999%, and the thickness of high temperature deposition layer is 0.7-2.0MM.
Described a kind of composite bed silica crucible also comprises the outer layer that spreads out, and outermost layer is the outer layer that spreads out, and inwardly is the silica body layer successively, transparent glass layer, high temperature deposition layer.
The described outer layer that spreads out is crystallization promoter layer, and crystallization promoter layer is AL 2O 3With the mixture layer of glass sand, thickness is 0.2-0.4MM.
Described a kind of composite bed silica crucible also comprises the normal temperature coating, and outermost layer is the outer layer that spreads out, and inwardly is the silica body layer successively, transparent glass layer, high temperature deposition layer, normal temperature coating.
Described normal temperature coating is the crystallization layer of silicate compound and silicon nitride mixture, and the thickness of normal temperature coating is 0.01-0.03MM.Main component is the mixture of silicate compound and silicon nitride, magnesium silicate for example, calcium silicates, barium silicate, the level that any one of silicic acid germanium and silicon nitride cooperate the back to make by diffusion method according to 1: 1 ratio.
Compared with prior art, the beneficial effects of the utility model are:
Transparent glass layer increases temperature sedimentary deposit, well solved the strength problem of silica crucible under high-temperature, long state, resistance to deformation, anti-sagging ability improve greatly, the high-purity transparent coating has solved in the crystal pulling process purity requirement to inner surface of crucible, and the crystal forming rate of monocrystalline is greatly improved; Transparent glass layer increases temperature sedimentary deposit and adds the normal temperature coating again, the normal temperature coating is the crystallization layer of silicate compound and silicon nitride mixture, at high temperature generate the material of cristobalite with the reaction of silica crucible wall, it is a lot of that the fusing point of cristobalite is about 1720 ℃ of 1420 ℃ high of fusing points than polysilicon.Cristobalite has blocked as the armor with transparent glass layer that polysilicon has also been blocked silica dioxide granule to the erosion of quartz glass and impurity is dissolved in the polysilicon when the high temperature crystal pulling, silicon single crystal rod " oxygen content " wherein of pulling out with this silica crucible is lower than conventional common silica crucible and transparent glass layer (vacuum layer) silica crucible, " crystal forming rate " is higher than common silica crucible and transparent glass layer (vacuum layer) silica crucible, so this silica crucible, not only increased the resistance to deformation of silica crucible, anti-sagging ability, reduced the oxygen content of silicon single crystal rod, improved crystal forming rate, and the purity of calorific intensity and inner surface is better than common silica crucible and transparent glass layer (vacuum layer) silica crucible again.Can reach silica crucible in long vacuum, indeformable under the condition of high temperature, do not come off.Reducing silica crucible has side effects to crystal-pulling.
Layer main component of spreading out outward is aluminium compound, milky.Because environment when silica crucible is being used must reach near 1450 degree, and quartzy softening point is also near this, and silica crucible is easy to generate softening and is out of shape.Because the protection of external coating is arranged, and one deck of aluminium compound is commonly called as is " corundum " AL2O3.Have stronger high temperature resistance and high mechanical hardness, whole crucible is played a supporting role, make crucible high temperature indeformable.
Description of drawings
Accompanying drawing 1: silica body layer, transparent glass layer increase temperature sedimentary deposit silica crucible structure chart;
Accompanying drawing 2: the layer that spreads out outward, silica body layer, transparent glass layer increase temperature sedimentary deposit silica crucible structure chart.
Accompanying drawing 3: the layer that spreads out outward, silica body layer, transparent glass layer, high temperature deposition layer add normal temperature coating quartz crucible structure chart.
Description of reference numerals: the 1. layer 5. normal temperature coating of spreading out outside the silica body layer 2. transparent glass layers 3. high temperature deposition layers 4.
The specific embodiment
The utility model is described in further detail below in conjunction with the drawings and specific embodiments, but not as to qualification of the present utility model.
Embodiment 1:
As shown in Figure 1, a kind of composite bed silica crucible (3 layers) comprises silica body layer 1, also comprises transparent glass layer 2, high temperature deposition layer 3.Outermost layer is a silica body layer 1, inwardly is transparent glass layer 2, high temperature deposition layer 3 successively.Silica body layer 1 is the high-purity natural quartz sand layer of silica 99.99%, and thickness is 7MM, has constituted the physical form of silica crucible.Transparent glass layer is not for containing high-purity natural quartz sand layer gas, that contain silica 99.99%, the thickness of transparent glass layer 2 is 2MM, transparent glass layer 2 is at high temperature formed with the gas that vacuum method sucking-off silica produces by silica body layer 1 inboard, owing under vacuum environment, generate, the gas that SIO2 produces under melting state is detached, present on the color and luster near transparent, can obviously with the naked eye distinguish level.The main effect of this layer is, can cause the layer OH-base near inner of whole silica crucible to reduce, and has reduced the probability that crucible at high temperature is out of shape.After above-mentioned high-temperature vacuum legal system is got silica crucible, again above-mentioned silica crucible being carried out the high temperature deposition method handles, at high temperature, the highly purified silica of gasification, through vapor deposition repeatedly, finally after cooling, form at quartz crucible inner surface (just at transparent glass layer 2 inner surfaces) and to generate high temperature deposition layer 3, high temperature deposition layer 3 is for to contain the ultra-pure natural quartz layer of sand of silica more than 99.999%, and the thickness of high temperature deposition layer is 1MM.Owing to be that the glass sand that melts is in layer deposited the method for covering,, finally cause this layer bright for colourless full impregnated so do not contain any bubble.The effect of this layer is owing to be not contain bubble, so this layer can not produce thermal expansion under hot environment, avoided the molecule of quartzy composition to come off in the absence of thermal expansion (quartz particles comes off and incorporates in the silicon liquid and can produce great quality influence to the monocrystalline that draws out).
Embodiment 2:
As shown in Figure 2, a kind of composite bed silica crucible (4 layers) comprises silica body layer 1, also comprise transparent glass layer 2, high temperature deposition layer 3, the layer 4 that spreads out outward, outermost layer is the outer layer 4 that spreads out, and inwardly is silica body layer 1 successively, transparent glass layer 2, high temperature deposition layer 3.Silica body layer 1, transparent glass layer 2, high temperature deposition layer 3 are with embodiment 1.The layer 4 that spreads out outward is crystallization promoter layer, and crystallization promoter layer is AL 2O 3With the mixture layer of glass sand, thickness is 0.2MM, because environment when silica crucible is being used must reach near 1450 degree, and quartzy softening point is also near this, and silica crucible is easy to generate softening and is out of shape.Because the protection of external coating 4 is arranged, have stronger high temperature resistance and high mechanical hardness, whole crucible is played a supporting role, make crucible high temperature indeformable.
Embodiment 3:
As shown in Figure 3, a kind of composite bed silica crucible (5 layers), comprise silica body layer 1, also comprise transparent glass layer 2, high temperature deposition layer 3, the layer 4 that spreads out outward, normal temperature coating 5, outermost layer are the outer layers 4 that spreads out, and inwardly are silica body layer 1 successively, transparent glass layer 2, high temperature deposition layer 3, normal temperature coating 5.Layer 4, silica body layer 1, transparent glass layer 2, high temperature deposition layer 3 spread out outward with embodiment 2.Normal temperature coating 5 main components are the mixture of barium silicate and silicon nitride, and barium silicate and silicon nitride cooperate the level of back by the diffusion method manufacturing according to 1: 1 ratio, and the thickness of normal temperature coating 5 is 0.01MM.At high temperature; when silica crucible uses; can allow crucible surface be converted into cristobalite; can form the protective layer of hard cristobalite on the surface; this layer is near Transparent color; the effect of this layer is; at high temperature; silicate compound and silicon nitride and silicon liquid and the reduction of quartz (SIO2) association response generate a kind of high oxide; we are referred to as crystallization DIVITRIFICATION, and this layer firmly sticks at inner surface of crucible, cut off other levels of crucible; make the composition of crucible and the impurity particle that contains not be shed in the silicon liquid, do not influence the growth of monocrystalline.
Above-described embodiment, the utility model three kinds of the specific embodiment more preferably just, the common variation that those skilled in the art carries out in the technical solutions of the utility model scope and replacing all should be included in the protection domain of the present utility model.

Claims (7)

1. a composite bed silica crucible comprises body layer, and body layer is the high-purity natural quartz sand layer, and thickness is 6-8MM, it is characterized in that: also comprise transparent glass layer, high temperature deposition layer; Outermost layer is the silica body layer, inwardly is transparent glass layer, high temperature deposition layer successively.
2. a kind of composite bed silica crucible according to claim 1 is characterized in that: described transparent glass layer is the high-purity natural quartz sand layer, and the thickness of transparent glass layer is 2-6MM.
3. a kind of composite bed silica crucible according to claim 1 is characterized in that: described high temperature deposition layer is ultra-pure natural quartz layer of sand, and the thickness of high temperature deposition layer is 0.7-2.0MM.
4. a kind of composite bed silica crucible according to claim 1 is characterized in that: also comprise the outer layer that spreads out, outermost layer is the outer layer that spreads out, and inwardly is the silica body layer successively, transparent glass layer, high temperature deposition layer.
5. a kind of composite bed silica crucible according to claim 4 is characterized in that: the described outer layer that spreads out is crystallization promoter layer, and thickness is 0.2-0.4MM.
6. a kind of composite bed silica crucible according to claim 4 is characterized in that: also comprise the normal temperature coating, outermost layer is the outer layer that spreads out, and inwardly is the silica body layer successively, transparent glass layer, high temperature deposition layer, normal temperature coating.
7. a kind of composite bed silica crucible according to claim 6 is characterized in that: described normal temperature coating is the crystallization layer of silicate compound and silicon nitride mixture, and the thickness of normal temperature coating is 0.01-0.03MM.
CN2009201586611U 2009-06-10 2009-06-10 Composite-layer quartz crucible Expired - Lifetime CN201527173U (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102061515A (en) * 2011-01-06 2011-05-18 杭州先进石英材料有限公司 Quartz glass crucible and preparation method thereof
CN102586856A (en) * 2012-02-01 2012-07-18 江西赛维Ldk太阳能高科技有限公司 Crucible capable of improving utilization rate of silicon ingot and using frequency of seed crystal and preparation method of crucible
CN102732948A (en) * 2012-06-20 2012-10-17 常州天合光能有限公司 Method for improving ingot-casting monocrystaline silicon yield
CN103201226A (en) * 2010-11-05 2013-07-10 信越半导体股份有限公司 Quartz glass crucible, method for producing same, and method for producing monocrystalline silicon
CN107299392A (en) * 2017-07-12 2017-10-27 晶科能源有限公司 A kind of high fine and close silica crucible barrier layer preparation method and polycrystalline ingot furnace
CN109111102A (en) * 2018-11-02 2019-01-01 宁夏富乐德石英材料有限公司 A kind of semiconductor grade silica crucible and its manufacturing method
TWI651283B (en) * 2017-04-28 2019-02-21 友達晶材股份有限公司 Crucible structure and manufacturing method thereof and silicon crystal structure and manufacturing method thereof
TWI651439B (en) * 2016-09-13 2019-02-21 日商勝高股份有限公司 Quartz glass crucible and its manufacturing method
CN110302854A (en) * 2018-03-27 2019-10-08 连云港科拓信息科技有限公司 A kind of silica crucible that heat insulation effect is excellent
CN110670121A (en) * 2019-11-20 2020-01-10 宁夏富乐德石英材料有限公司 Local coating quartz crucible and manufacturing method thereof
CN115724598A (en) * 2021-08-31 2023-03-03 内蒙古中环协鑫光伏材料有限公司 Quartz crucible pretreatment method for improving first grain crystallization rate

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103201226A (en) * 2010-11-05 2013-07-10 信越半导体股份有限公司 Quartz glass crucible, method for producing same, and method for producing monocrystalline silicon
CN103201226B (en) * 2010-11-05 2015-08-05 信越半导体股份有限公司 The manufacture method of quartz glass crucibles and manufacture method and silicon single crystal
US9376336B2 (en) 2010-11-05 2016-06-28 Shin-Etsu Handotai Co., Ltd. Quartz glass crucible, method for producing the same, and method for producing silicon single crystal
CN102061515B (en) * 2011-01-06 2012-10-10 杭州先进石英材料有限公司 Quartz glass crucible and preparation method thereof
CN102061515A (en) * 2011-01-06 2011-05-18 杭州先进石英材料有限公司 Quartz glass crucible and preparation method thereof
CN102586856A (en) * 2012-02-01 2012-07-18 江西赛维Ldk太阳能高科技有限公司 Crucible capable of improving utilization rate of silicon ingot and using frequency of seed crystal and preparation method of crucible
CN102586856B (en) * 2012-02-01 2015-03-11 江西赛维Ldk太阳能高科技有限公司 Crucible capable of improving utilization rate of silicon ingot and using frequency of seed crystal and preparation method of crucible
CN102732948A (en) * 2012-06-20 2012-10-17 常州天合光能有限公司 Method for improving ingot-casting monocrystaline silicon yield
TWI651439B (en) * 2016-09-13 2019-02-21 日商勝高股份有限公司 Quartz glass crucible and its manufacturing method
TWI651283B (en) * 2017-04-28 2019-02-21 友達晶材股份有限公司 Crucible structure and manufacturing method thereof and silicon crystal structure and manufacturing method thereof
CN107299392A (en) * 2017-07-12 2017-10-27 晶科能源有限公司 A kind of high fine and close silica crucible barrier layer preparation method and polycrystalline ingot furnace
CN110302854A (en) * 2018-03-27 2019-10-08 连云港科拓信息科技有限公司 A kind of silica crucible that heat insulation effect is excellent
CN109111102A (en) * 2018-11-02 2019-01-01 宁夏富乐德石英材料有限公司 A kind of semiconductor grade silica crucible and its manufacturing method
CN110670121A (en) * 2019-11-20 2020-01-10 宁夏富乐德石英材料有限公司 Local coating quartz crucible and manufacturing method thereof
CN110670121B (en) * 2019-11-20 2024-04-12 宁夏盾源聚芯半导体科技股份有限公司 Locally coated quartz crucible and manufacturing method thereof
CN115724598A (en) * 2021-08-31 2023-03-03 内蒙古中环协鑫光伏材料有限公司 Quartz crucible pretreatment method for improving first grain crystallization rate

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Owner name: YUYAO QIMING QUARTZ CO., LTD.

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Effective date: 20130502

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Address after: 315450, No. 98, Dong Zhen Road, Ma Ma, Yuyao, Zhejiang

Patentee after: Yuyao Qiming quartz Co., Ltd.

Address before: 315450, No. 98, Dong Zhen Road, Ma Ma, Yuyao, Zhejiang

Patentee before: YuYao JingYing Crucible Co., Ltd.

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Granted publication date: 20100714