CN104962991A - Quartz crucible and production method thereof - Google Patents
Quartz crucible and production method thereof Download PDFInfo
- Publication number
- CN104962991A CN104962991A CN201510274562.XA CN201510274562A CN104962991A CN 104962991 A CN104962991 A CN 104962991A CN 201510274562 A CN201510274562 A CN 201510274562A CN 104962991 A CN104962991 A CN 104962991A
- Authority
- CN
- China
- Prior art keywords
- silicon
- quartz crucible
- silicon nitride
- silicon carbide
- coat
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 239000010453 quartz Substances 0.000 title claims abstract description 82
- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 91
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 91
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 89
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 84
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 32
- 239000010703 silicon Substances 0.000 claims abstract description 32
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims description 91
- 238000000576 coating method Methods 0.000 claims description 41
- 239000011248 coating agent Substances 0.000 claims description 39
- 239000006255 coating slurry Substances 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 19
- 229960001866 silicon dioxide Drugs 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 239000003085 diluting agent Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 10
- 239000010410 layer Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000011247 coating layer Substances 0.000 abstract 8
- 238000005507 spraying Methods 0.000 description 20
- 235000011194 food seasoning agent Nutrition 0.000 description 14
- 238000005266 casting Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 239000002210 silicon-based material Substances 0.000 description 9
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000012634 fragment Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005457 optimization Methods 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000002153 concerted effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 238000007569 slipcasting Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 102220043159 rs587780996 Human genes 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Crucibles And Fluidized-Bed Furnaces (AREA)
Abstract
The invention provides a quartz crucible and a production method thereof. The quartz crucible comprises a quartz crucible body, and a silicon carbide coating layer and a silicon nitride coating layer which are sequentially coated on the inner wall of the quartz crucible body; the silicon carbide coating layer comprises silicon carbide and silica; and the silicon nitride coating layer comprises silicon nitride and silica. Compared with the prior art, the method is characterized in that the inner wall of the quartz crucible body is coated with the silicon carbide coating layer, silicon carbide is close to the silicon nitride coating layer in thermal conductivity, expansion coefficient, density and high temperature compressive strength, has strong binding force with the quartz crucible body, and can form a compact protection layer on the inner wall of the crucible; and the silicon carbide coating layer is coated with the silicon nitride coating layer, so the quartz crucible can effectively prevent pollution of crucible impurities to silicon ingots, and has a good demolding effect.
Description
Technical field
The invention belongs to crucible preparing technical field, particularly relate to a kind of quartz crucible and preparation method thereof.
Background technology
Quartz crucible also can be described as " fused silica crucible ", " quartz glass crucibles ", " quartz ceramic crucible ", with features such as its good thermal shock resistance, less thermal expansivity, resistance to chemical attack, be widely used in holding the material needing at high temperature melting, decomposition or conversion.In order to ensure the purity and the production efficiency thereof that are received material, the internal surface of quartz crucible and material generation physics accommodated therein or chemical reaction need be prevented.
At present, polycrystalline silicon ingot casting process crucible used is quartz crucible, silicon material melt and growth tens hours in, crucible generally remains on 1450 DEG C ~ 1550 DEG C, traditional quartz crucible directly contacts with silicon liquid, in such a situa-tion, first, the one-tenth branch of crucible invades polysilicon, silicon ingot periphery is made to be polluted and scrap, and also make its overall quality decline, secondly, crucible meeting and polycrystalline silicon material react, generate silicon monoxide (SiO), both silicon liquid had been polluted, again reduce the intensity of crucible, increase the risk of breaking, and in the above conditions, very easily combine closely with quartz crucible after polycrystalline silicon ingot casting, be difficult to separately, add production cost and difficulty.
For above problem, people have invented some crucible internal layer coating methods, namely at crucible internal walls coating last layer material, in order to stop the mutual erosion between quartz crucible and silicon material.
The patent No. be US5980629 U.S. patents disclose a kind of surperficial treated crucible, barium carbonate coating is all coated with at the inner and outer wall of crucible, in crystal growing process, crucible internal walls and outer wall all form the cristobalite layer of one deck dense uniform, the cristobalite layer of inwall can reduce crystal quartz particle and discharge in the semiconductor material of melting, the cristobalite layer of crucible outer wall can reinforce the body of described quartz crucible, increases its intensity and work-ing life.This technology was once used in small size monocrystalline silicon cast ingot, but the sticking power of barium carbonate coating is too little, be easy to peel off under external force, easily be scratched in transport and dress silicon material process, and it has the effect promoting crystallization, for the large size of polysilicon crucible, is not a good thing, also can bring impurity into, therefore be eliminated in quartz crucible for casting polycrystalline silicon ingot.
Publication number is that the Chinese patent of CN202116689U discloses a kind of compound quartz crucible, it adopts the mode at crucible internal walls plating carbon film, suppress the effusion of bubble in crucible body, stop the generation of silicon single-crystal microdefect, stop quartz crucible by the silicon corrosion of high temperature simultaneously.But this coating technique cost is too high, cannot drop into actual production.
Publication number is method and the silicon nitride coating that the Chinese patent of CN103506263A discloses that oven dry is exempted from polysilicon crucible spraying, this patent is by silicon nitride, deionized water, Mag solution is formed after silicon sol mixing mixing, the solution mixed is after atomization, spray on the inwall of crucible, form the mixing solutions film of one deck silicon nitride, after seasoning, at crucible surface formation silicon nitride coating, it is the main coating process of current crucible used for polycrystalline silicon ingot casting, itself and silicon ingot have good non-infiltration, the silicon ingot demoulding can be helped, but still there is the shortcomings such as the not enough and coating of coating and substrate caking power is fine and close not in the method.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of quartz crucible and preparation method thereof, and this quartz crucible coating bonding force is comparatively strong and compactness is better.
The invention provides a kind of quartz crucible, comprising: quartz crucible body, the coat of silicon carbide being coated in quartz crucible inner body wall successively and silicon nitride coating;
Described coat of silicon carbide comprises silicon carbide and silicon-dioxide;
Described silicon nitride coating comprises silicon nitride and silicon-dioxide.
Preferably, the thickness of described coat of silicon carbide is 0.05 ~ 2mm.
Preferably, the thickness of described silicon nitride coating is 0.05 ~ 2mm.
Preferably, the total thickness of described coat of silicon carbide and silicon nitride coating is 0.1 ~ 2mm.
Present invention also offers a kind of preparation method of quartz crucible, comprising:
A) by silicon carbide and silicon carbide mixing diluents, coat of silicon carbide slurry is obtained;
By silicon nitride and silicon nitride mixing diluents, obtain silicon nitride coating slurry;
Described silicon carbide thinner and silicon nitride thinner are silicon sol independently of one another;
B) described coat of silicon carbide slurry is coated on the inwall of quartz crucible body, dry, then apply described silicon nitride coating slurry, dry, obtain quartz crucible.
Preferably, the quality of described silicon carbide is 40% ~ 80% of coat of silicon carbide stock quality.
Preferably, the particle diameter of described silicon carbide is D50≤100 μm.
Preferably, in described silicon carbide thinner and silicon nitride thinner, the mass concentration of silicon-dioxide is 15% ~ 50% independently of one another.
Preferably, the quality of described silicon nitride is 40% ~ 80% of silicon nitride coating stock quality.
Preferably, the particle diameter of described silicon nitride is D50≤100 μm.
The invention provides a kind of quartz crucible and preparation method thereof, this quartz crucible comprises: quartz crucible body, the coat of silicon carbide being coated in quartz crucible inner body wall successively and silicon nitride coating; Described coat of silicon carbide comprises silicon carbide and silicon-dioxide; Described silicon nitride coating comprises silicon nitride and silicon-dioxide.Compared with prior art, the present invention first applies one deck coat of silicon carbide in quartz crucible inner body wall, silicon carbide is close with silicon nitride coating in thermal conductivity, the coefficient of expansion, density, crushing strength under high temperature etc., make a concerted effort comparatively strong with quartz crucible bulk junction, and it can form fine and close protective layer at crucible internal walls; On coat of silicon carbide, apply one deck silicon nitride coating simultaneously, make quartz crucible both can effectively stop crucible impurity to the pollution of silicon ingot, there is again good demoulding effect.
Accompanying drawing explanation
Fig. 1 is the structural representation of quartz crucible of the present invention.
Embodiment
Below in conjunction with the accompanying drawing of the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of quartz crucible, comprising: quartz crucible body, the coat of silicon carbide being coated in quartz crucible inner body wall successively and silicon nitride coating;
Described coat of silicon carbide comprises silicon carbide and silicon-dioxide;
Described silicon nitride coating comprises silicon nitride and silicon-dioxide.
As shown in Figure 1, wherein 1 is quartz crucible body to the structural representation of this quartz crucible, and 2 is coat of silicon carbide, and 3 is silicon nitride coating.
Described quartz crucible body is uncoated quartz crucible well known to those skilled in the art, special restriction to its shape and structure, the quartz crucible that the present invention preferably adopts slip casting or Inject & congeal shaping method to produce.
The thickness of described coat of silicon carbide is preferably 0.05 ~ 2mm, is more preferably 0.1 ~ 1.5mm, then is preferably 0.1 ~ 1mm.Described coat of silicon carbide comprises silicon carbide and silicon-dioxide, and the mass ratio of described silicon carbide and silicon-dioxide is preferably (40 ~ 80): (3 ~ 30), are more preferably (40 ~ 60): (5 ~ 20).
The thickness of described silicon nitride coating is preferably 0.05 ~ 2mm, is more preferably 0.1 ~ 1.5mm, then is preferably 0.1 ~ 1mm.Described silicon nitride coating comprises silicon nitride and silicon-dioxide, and the mass ratio of described silicon nitride and silicon-dioxide is preferably (40 ~ 80): (3 ~ 30), are more preferably (40 ~ 60): (5 ~ 20).
The total thickness of described coat of silicon carbide and silicon nitride coating is preferably 0.05 ~ 2mm, is more preferably 0.1 ~ 2mm, then is preferably 0.5 ~ 1.5mm.
The present invention first applies one deck coat of silicon carbide in quartz crucible inner body wall, silicon carbide is close with silicon nitride coating in thermal conductivity, the coefficient of expansion, density, crushing strength under high temperature etc., make a concerted effort stronger with quartz crucible bulk junction, and it can form fine and close protective layer at crucible internal walls, fine and close coating also prevents silicon liquid for the erosion of crucible, decreases the risk that crucible breaks; On coat of silicon carbide, apply one deck silicon nitride coating simultaneously, make quartz crucible both can effectively stop crucible impurity to the pollution of silicon ingot, there is again good demoulding effect.
Present invention also offers a kind of preparation method of above-mentioned quartz crucible, comprising: A) by silicon carbide and silicon carbide mixing diluents, obtain coat of silicon carbide slurry; By silicon nitride and silicon nitride mixing diluents, obtain silicon nitride coating slurry; B) described coat of silicon carbide slurry is coated on the inwall of quartz crucible body, dry, then apply described silicon nitride coating slurry, dry, obtain quartz crucible; Described silicon carbide thinner and silicon nitride thinner are silicon sol independently of one another.
By silicon carbide and silicon carbide mixing diluents, obtain coat of silicon carbide slurry.Wherein, the particle diameter of described silicon carbide is preferably D50≤100 μm, is more preferably D50≤50 μm, then is preferably D50≤10 μm; The quality optimization of described silicon carbide is 40% ~ 80% of coat of silicon carbide slurry, is more preferably 40% ~ 70%, then is preferably 40% ~ 60%; Described silicon carbide thinner is silicon sol well known to those skilled in the art, there is no special restriction, the present invention is preferably the silicon sol that dioxide-containing silica is 15wt% ~ 50wt%, be more preferably the silicon sol that dioxide-containing silica is 15wt% ~ 40wt%, then be preferably 15wt% ~ 30wt%; Described silicon-dioxide is preferably nanometer grade silica; The quality optimization of described silicon carbide thinner is 20% ~ 60% of coat of silicon carbide slurry, is more preferably 30% ~ 60%, then is preferably 40% ~ 60%.Silicon carbide is preferably mixed 5 ~ 30min with silicon carbide thinner, more preferably mixes 10 ~ 20min, coat of silicon carbide slurry can be obtained.
By silicon nitride and silicon nitride mixing diluents, obtain silicon nitride coating slurry.Wherein, the particle diameter of described silicon nitride is preferably D50≤100 μm, is more preferably D50≤50 μm, then is preferably D50≤10 μm; The quality optimization of described silicon nitride is 40% ~ 80% of silicon nitride coating slurry, is more preferably 40% ~ 70%, then is preferably 40% ~ 60%; Described silicon nitride thinner is silicon sol well known to those skilled in the art, there is no special restriction, the present invention is preferably the silicon sol that dioxide-containing silica is 15wt% ~ 50wt%, be more preferably the silicon sol that dioxide-containing silica is 15wt% ~ 40wt%, then be preferably 15wt% ~ 30wt%; Described silicon-dioxide is preferably nanometer grade silica; The quality optimization of described silicon nitride thinner is 20% ~ 60% of silicon nitride coating slurry, is more preferably 30% ~ 60%, then is preferably 40% ~ 60%.Silicon nitride is preferably mixed 5 ~ 30min with silicon nitride thinner, more preferably mixes 10 ~ 20min, silicon nitride coating slurry can be obtained.
Described coat of silicon carbide slurry is coated on the inwall of quartz crucible body, the method of described coating is method well known to those skilled in the art, there is no special restriction, the present invention preferably adopts the mode of spraying to apply, and can form coat of silicon carbide after drying; Described drying is preferably seasoning, is more preferably seasoning 3 ~ 7h, then is preferably 5 ~ 7h.
Then apply described silicon nitride coating slurry, can silicon nitride coating be formed after drying, obtain quartz crucible.Described drying is preferably seasoning, is more preferably seasoning 3 ~ 7h, then is preferably 5 ~ 7h; The temperature of described seasoning preferably >=25 DEG C.
The preparation method of quartz crucible of the present invention is simple, and cost is lower.
In order to further illustrate the present invention, below in conjunction with embodiment, a kind of quartz crucible provided by the invention and preparation method thereof is described in detail.
Reagent used in following examples is commercially available, and described crucible is Yangzhong City of place of production Jiangsu Province, and the life size adopting slip casting method to produce is the crucible of G6; Described carborundum powder is purchased from Fuyang City of Zhejiang Province, and wherein the content of silicon carbide is greater than 99.9%, D50=7 μm; Described silicon nitride powder is purchased from AlzChem AG company, and wherein the content of silicon nitride is greater than 99.99%, D50≤10 μm; The concentration of silicon sol is 15wt%, and total impurities is less than 5ppm, and silicon-dioxide is nano level.
Embodiment 1
Carborundum powder mixes with the ratio of mass ratio 1:1 with silicon sol by 1.1 at normal temperatures, stirs 15min, obtains coat of silicon carbide slurry.
Silicon nitride powder mixes with the ratio of mass ratio 1:1 with silicon sol by 1.2 at normal temperatures, stirs 15min, obtains silicon nitride coating slurry.
The 1.3 coat of silicon carbide slurries obtained in crucible internal walls spraying machine spraying 1.1, room temp >=25 DEG C during spraying, coat-thickness is 0.1mm, after seasoning 5h, spray the silicon nitride coating slurry obtained in 1.2 again, room temp >=25 DEG C during spraying, coat-thickness is 0.1mm, after seasoning 5h, obtain quartz crucible.
Place silicon material fragment in the quartz crucible obtained in 1.3, be then placed in sintering oven, under 1500 DEG C of vacuum conditions, be incubated 10h.Experimental result shows: after experience high temperature ingot casting condition, this quartz crucible surface silicon nitride coating is discrete particle shape, and internal layer coat of silicon carbide then possesses fabulous compactness.
Embodiment 2
Carborundum powder mixes with the ratio of mass ratio 2:3 with silicon sol by 2.1 at normal temperatures, stirs 15min, obtains coat of silicon carbide slurry.
Silicon nitride powder mixes with the ratio of mass ratio 2:3 with silicon sol by 2.2 at normal temperatures, stirs 15min, obtains silicon nitride coating slurry.
The 2.3 coat of silicon carbide slurries obtained in crucible internal walls spraying machine spraying 2.1, room temp >=25 DEG C during spraying, coat-thickness is 0.5mm, after seasoning 5h, spray the silicon nitride coating slurry obtained in 2.2 again, room temp >=25 DEG C during spraying, coat-thickness is 0.1mm, after seasoning 5h, obtain quartz crucible.
Place silicon material fragment in the quartz crucible obtained in 2.3, be then placed in sintering oven, under 1500 DEG C of vacuum conditions, be incubated 10h.Experimental result shows: after experience high temperature ingot casting condition, this quartz crucible surface silicon nitride coating is discrete particle shape, and internal layer coat of silicon carbide then possesses fabulous compactness.
Embodiment 3
Carborundum powder mixes with the ratio of mass ratio 3:2 with silicon sol by 3.1 at normal temperatures, stirs 15min, obtains coat of silicon carbide slurry.
Silicon nitride powder mixes with the ratio of mass ratio 3:2 with silicon sol by 3.2 at normal temperatures, stirs 15min, obtains silicon nitride coating slurry.
The 3.3 coat of silicon carbide slurries obtained in crucible internal walls spraying machine spraying 3.1, room temp >=25 DEG C during spraying, coat-thickness is 0.1mm, after seasoning 5h, spray the silicon nitride coating slurry obtained in 3.2 again, room temp >=25 DEG C during spraying, coat-thickness is 0.5mm, after seasoning 5h, obtain quartz crucible.
Place silicon material fragment in the quartz crucible obtained in 1.3, be then placed in sintering oven, under 1500 DEG C of vacuum conditions, be incubated 10h.Experimental result shows: after experience high temperature ingot casting condition, this quartz crucible surface silicon nitride coating is discrete particle shape, and internal layer coat of silicon carbide then possesses fabulous compactness.
Comparative example 1
Carborundum powder mixes with the ratio of mass ratio 1:1 with silicon sol by 1.1 at normal temperatures, stirs 15min, obtains coat of silicon carbide slurry.
The 1.2 coat of silicon carbide slurries obtained in crucible internal walls spraying machine spraying 1.1, room temp >=25 DEG C during spraying, coat-thickness is 0.1mm, after seasoning 5h, obtains quartz crucible.
Place silicon material fragment in the quartz crucible obtained in 1.2, be then placed in sintering oven, under 1500 DEG C of vacuum conditions, be incubated 10h.Experimental result shows: after experience high temperature ingot casting condition, this quartz crucible surface coat of silicon carbide is extremely fine and close, very strong with crucible base bonding force, visual inspection is less than crack, be difficult to leave cut with steel cross cut test device, also firmly more solid than substrate, also finer and close.
Comparative example 2
Silicon nitride powder mixes with the ratio of mass ratio 1:1 with silicon sol by 2.1 at normal temperatures, stirs 15min, obtains silicon nitride coating slurry.
The 2.2 silicon nitride coating slurries obtained in crucible internal walls spraying machine spraying 2.1, room temp >=25 DEG C during spraying, coat-thickness is 0.1mm, after seasoning 5h, obtains quartz crucible.
Place silicon material fragment in the quartz crucible obtained in 2.2, be then placed in sintering oven, under 1500 DEG C of vacuum conditions, be incubated 10h.Experimental result shows: after experience high temperature ingot casting condition, this quartz crucible surface silicon nitride coating is discrete particle shape, and all very poor with substrate caking power, self compactness, one scrapes namely to fall, and overall integrity is fair.
Through to embodiment 1 ~ 3 and ratio compared with 1 ~ 2 in the foreign matter content of silicon ingot fragment after high temperature ingot casting detect, the quartz crucible that embodiment 1 ~ 3 obtains is compared with the quartz crucible only containing silicon nitride coating in comparative example 2, there is better isolated from contaminants effect, in silicon ingot fragment, usual impurities constituent content have dropped 10% ~ 30%, also remains original demoulding effect simultaneously.
Claims (10)
1. a quartz crucible, is characterized in that, comprising: quartz crucible body, the coat of silicon carbide being coated in quartz crucible inner body wall successively and silicon nitride coating;
Described coat of silicon carbide comprises silicon carbide and silicon-dioxide;
Described silicon nitride coating comprises silicon nitride and silicon-dioxide.
2. quartz crucible according to claim 1, is characterized in that, the thickness of described coat of silicon carbide is 0.05 ~ 2mm.
3. quartz crucible according to claim 1, is characterized in that, the thickness of described silicon nitride coating is 0.05 ~ 2mm.
4. quartz crucible according to claim 1, is characterized in that, the total thickness of described coat of silicon carbide and silicon nitride coating is 0.1 ~ 2mm.
5. a preparation method for quartz crucible, is characterized in that, comprising:
A) by silicon carbide and silicon carbide mixing diluents, coat of silicon carbide slurry is obtained;
By silicon nitride and silicon nitride mixing diluents, obtain silicon nitride coating slurry;
Described silicon carbide thinner and silicon nitride thinner are silicon sol independently of one another;
B) described coat of silicon carbide slurry is coated on the inwall of quartz crucible body, dry, then apply described silicon nitride coating slurry, dry, obtain quartz crucible.
6. preparation method according to claim 5, is characterized in that, the quality of described silicon carbide is 40% ~ 80% of coat of silicon carbide stock quality.
7. preparation method according to claim 5, is characterized in that, the particle diameter of described silicon carbide is D50≤100 μm.
8. preparation method according to claim 5, is characterized in that, in described silicon carbide thinner and silicon nitride thinner, the mass concentration of silicon-dioxide is 15% ~ 50% independently of one another.
9. preparation method according to claim 5, is characterized in that, the quality of described silicon nitride is 40% ~ 80% of silicon nitride coating stock quality.
10. preparation method according to claim 5, is characterized in that, the particle diameter of described silicon nitride is D50≤100 μm.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510274562.XA CN104962991B (en) | 2015-05-26 | 2015-05-26 | A kind of silica crucible and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510274562.XA CN104962991B (en) | 2015-05-26 | 2015-05-26 | A kind of silica crucible and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN104962991A true CN104962991A (en) | 2015-10-07 |
CN104962991B CN104962991B (en) | 2018-04-17 |
Family
ID=54217069
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201510274562.XA Expired - Fee Related CN104962991B (en) | 2015-05-26 | 2015-05-26 | A kind of silica crucible and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN104962991B (en) |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105256370A (en) * | 2015-10-27 | 2016-01-20 | 镇江环太硅科技有限公司 | Method for preparing high-purity crucible provided with smooth inner surface |
CN105568372A (en) * | 2015-12-30 | 2016-05-11 | 佛山市业丰赛尔陶瓷科技有限公司 | Coating composition for graphite equipment of polycrystalline silicon ingot furnace |
CN106012005A (en) * | 2016-07-13 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Measuring quartz rod |
CN107779950A (en) * | 2017-11-29 | 2018-03-09 | 镇江市高等专科学校 | A kind of fire protection flame retarding device for solar energy quartz crucible |
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 |
CN109627050A (en) * | 2018-12-25 | 2019-04-16 | 宁波宝斯达坩埚保温制品有限公司 | A kind of quartz crucible inner surface coating and preparation method thereof |
CN111020695A (en) * | 2019-12-24 | 2020-04-17 | 江苏润弛太阳能材料科技有限公司 | Preparation method of low-oxygen quartz crucible |
CN112850713A (en) * | 2020-06-09 | 2021-05-28 | 北京世纪金光半导体有限公司 | Synthesis and treatment method of silicon carbide powder |
CN113716878A (en) * | 2021-09-10 | 2021-11-30 | 湖南倍晶新材料科技有限公司 | Quartz surface composite coating and preparation method thereof |
CN115109439A (en) * | 2021-03-23 | 2022-09-27 | 新沂市中鑫光电科技有限公司 | High-density combined coating material for quartz crucible and preparation method thereof |
CN116535245A (en) * | 2023-05-08 | 2023-08-04 | 徐州协鑫太阳能材料有限公司 | Preparation method of high-purity coating of compact quartz crucible |
CN116768653A (en) * | 2023-06-15 | 2023-09-19 | 湖南世鑫新材料有限公司 | Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN87206316U (en) * | 1987-04-16 | 1987-12-30 | 清华大学 | Crucible with si3n4 coating |
CN201842894U (en) * | 2010-09-16 | 2011-05-25 | 扬州华尔光电子材料有限公司 | Composite coating quartz crucible for polycrystalline silicon ingot preparation |
CN102221293A (en) * | 2011-06-08 | 2011-10-19 | 大连理工大学 | Preparation method of coating for melting crucible |
JP4815003B2 (en) * | 2010-03-09 | 2011-11-16 | 佑吉 堀岡 | Crucible for silicon crystal growth, crucible manufacturing method for silicon crystal growth, and silicon crystal growth method |
CN202164381U (en) * | 2011-06-30 | 2012-03-14 | 常州天合光能有限公司 | Reusable crucible for ingoting |
CN103102170A (en) * | 2011-11-11 | 2013-05-15 | 浙江昱辉阳光能源有限公司 | Crucible and preparation method thereof |
CN103320854A (en) * | 2013-06-07 | 2013-09-25 | 英利集团有限公司 | Coating structure for crucible, preparation method thereof, and crucible with coating structure |
CN103553711A (en) * | 2013-09-27 | 2014-02-05 | 西安超码科技有限公司 | Composite coating carbon/carbon composite material crucible and preparation method thereof |
CN203487280U (en) * | 2013-08-08 | 2014-03-19 | 徐州协鑫太阳能材料有限公司 | Quartz crucible |
CN104109902A (en) * | 2014-05-16 | 2014-10-22 | 江西赛维Ldk太阳能高科技有限公司 | Crucible for polysilicon ingot casting, coating structure of crucible and coating preparation method |
CN204022994U (en) * | 2014-07-21 | 2014-12-17 | 常州旷达阳光能源有限公司 | The crucible of efficient polycrystal silicon ingot for casting |
-
2015
- 2015-05-26 CN CN201510274562.XA patent/CN104962991B/en not_active Expired - Fee Related
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN87206316U (en) * | 1987-04-16 | 1987-12-30 | 清华大学 | Crucible with si3n4 coating |
JP4815003B2 (en) * | 2010-03-09 | 2011-11-16 | 佑吉 堀岡 | Crucible for silicon crystal growth, crucible manufacturing method for silicon crystal growth, and silicon crystal growth method |
CN201842894U (en) * | 2010-09-16 | 2011-05-25 | 扬州华尔光电子材料有限公司 | Composite coating quartz crucible for polycrystalline silicon ingot preparation |
CN102221293A (en) * | 2011-06-08 | 2011-10-19 | 大连理工大学 | Preparation method of coating for melting crucible |
CN202164381U (en) * | 2011-06-30 | 2012-03-14 | 常州天合光能有限公司 | Reusable crucible for ingoting |
CN103102170A (en) * | 2011-11-11 | 2013-05-15 | 浙江昱辉阳光能源有限公司 | Crucible and preparation method thereof |
CN103320854A (en) * | 2013-06-07 | 2013-09-25 | 英利集团有限公司 | Coating structure for crucible, preparation method thereof, and crucible with coating structure |
CN203487280U (en) * | 2013-08-08 | 2014-03-19 | 徐州协鑫太阳能材料有限公司 | Quartz crucible |
CN103553711A (en) * | 2013-09-27 | 2014-02-05 | 西安超码科技有限公司 | Composite coating carbon/carbon composite material crucible and preparation method thereof |
CN104109902A (en) * | 2014-05-16 | 2014-10-22 | 江西赛维Ldk太阳能高科技有限公司 | Crucible for polysilicon ingot casting, coating structure of crucible and coating preparation method |
CN204022994U (en) * | 2014-07-21 | 2014-12-17 | 常州旷达阳光能源有限公司 | The crucible of efficient polycrystal silicon ingot for casting |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105256370A (en) * | 2015-10-27 | 2016-01-20 | 镇江环太硅科技有限公司 | Method for preparing high-purity crucible provided with smooth inner surface |
CN105568372A (en) * | 2015-12-30 | 2016-05-11 | 佛山市业丰赛尔陶瓷科技有限公司 | Coating composition for graphite equipment of polycrystalline silicon ingot furnace |
CN106012005A (en) * | 2016-07-13 | 2016-10-12 | 江苏协鑫硅材料科技发展有限公司 | Measuring quartz rod |
CN107779950A (en) * | 2017-11-29 | 2018-03-09 | 镇江市高等专科学校 | A kind of fire protection flame retarding device for solar energy quartz crucible |
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 |
CN109627050A (en) * | 2018-12-25 | 2019-04-16 | 宁波宝斯达坩埚保温制品有限公司 | A kind of quartz crucible inner surface coating and preparation method thereof |
CN111020695A (en) * | 2019-12-24 | 2020-04-17 | 江苏润弛太阳能材料科技有限公司 | Preparation method of low-oxygen quartz crucible |
CN112850713A (en) * | 2020-06-09 | 2021-05-28 | 北京世纪金光半导体有限公司 | Synthesis and treatment method of silicon carbide powder |
CN115109439A (en) * | 2021-03-23 | 2022-09-27 | 新沂市中鑫光电科技有限公司 | High-density combined coating material for quartz crucible and preparation method thereof |
CN113716878A (en) * | 2021-09-10 | 2021-11-30 | 湖南倍晶新材料科技有限公司 | Quartz surface composite coating and preparation method thereof |
CN116535245A (en) * | 2023-05-08 | 2023-08-04 | 徐州协鑫太阳能材料有限公司 | Preparation method of high-purity coating of compact quartz crucible |
CN116768653A (en) * | 2023-06-15 | 2023-09-19 | 湖南世鑫新材料有限公司 | Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof |
CN116768653B (en) * | 2023-06-15 | 2024-04-02 | 湖南世鑫新材料有限公司 | Carbon-carbon thermal field crucible containing composite ceramic coating and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN104962991B (en) | 2018-04-17 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN104962991A (en) | Quartz crucible and production method thereof | |
CN112144115B (en) | Quartz crucible with long service life and low deformation rate and preparation method thereof | |
CN102453955B (en) | Crucible coating for purification and ingot casting of solar grade polysilicon and preparation method thereof as well as crucible | |
TWI423937B (en) | Composite crucible, method of manufacturing the same, and method of manufacturing silicon crystal | |
CN101348324A (en) | Non-transparent quartz crucible for polysilicon crystallization and manufacturing method thereof | |
CN104651931A (en) | Quartz crucible capable of controlling nucleation and impurity diffusion and used for polycrystal cast ingot and preparation method of quartz crucible | |
EP0949358A2 (en) | Mold for producing silicon ingot and method for fabricating the same | |
EP1570117A1 (en) | Vessel for holding silicon and method of producing the same | |
JP2004131317A (en) | Process for strengthening quartz glass member and strengthening-treated quartz glass crucible | |
CN201857440U (en) | Crucible for purification and ingot casting of solar-grade polysilicon | |
CN109704782B (en) | Si for photovoltaic polycrystalline silicon production2N2Preparation method of O ceramic powder | |
NO178463B (en) | Resistant materials to metal and salt melts, their manufacture and use | |
KR101779267B1 (en) | Polycrystalline silicon ingot, method for producing the same, and crucible | |
JP2001198648A (en) | Casting mold for casting silicon ingot and method for manufacturing the same | |
JP5072936B2 (en) | Composite crucible and manufacturing method thereof | |
JP3250149B2 (en) | Silicon ingot casting mold and method of manufacturing the same | |
CN107400922A (en) | A kind of quartz crucible coating and its production and use | |
CN105621866A (en) | Production method of high-quality and high-purity melted quartz blocks | |
CN2884103Y (en) | Quartz crucible for vertical pulling method for prodn. of monocrystalline silicon | |
JP2011088775A (en) | Composite crucible and method for manufacturing the same | |
CN103003209A (en) | Vitreous silica crucible having a polygonal opening, and method for manufacturing same | |
CN103112862A (en) | Method for producing fused obtuse quartz sand from quartz crucibles | |
CN208501149U (en) | A kind of crucible | |
CN103014834A (en) | Method for improving casting quality of polycrystalline silicon ingot | |
JP2013095652A (en) | Silica sintered body crucible |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180417 |