CN104445206A - Method for cleaning silicon nitride on surface of silicon block - Google Patents
Method for cleaning silicon nitride on surface of silicon block Download PDFInfo
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- CN104445206A CN104445206A CN201410527036.5A CN201410527036A CN104445206A CN 104445206 A CN104445206 A CN 104445206A CN 201410527036 A CN201410527036 A CN 201410527036A CN 104445206 A CN104445206 A CN 104445206A
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Abstract
The invention discloses a method for cleaning silicon nitride on the surface of a silicon block. The method comprises the following steps of firstly putting the silicon block with silicon nitride into a sodium hydroxide reaction tank for carrying out alkali corrosion separation; cleaning the corroded silicon block according to a program and then drying in a drying oven. By the method, silicon nitride on the surface of the silicon block with can be effectively removed; and the method has circularity and, compared with physical and mechanical polishing and the like, has the advantages that manpower and resources are saved, the volume of the silicon material is not required, the loss of the silicon material is small and the like.
Description
Technical field
The present invention relates to a kind of silicon material cleaning technique, particularly a kind of purging method of silico briquette surface nitrogen SiClx.
Background technology
At ingot casting photovoltaic art, produce silicon chip and can relate to the operation of together silicon ingot being carried out to slicing treatment, the silicon ingot remainder that its section is left is called edge skin material, and at this, for cost and economic consideration, common way carries out recycling to edge skin material.
At this, in the course of processing of silicon ingot, for effective isolation of ingot casting quartz crucible and silicon under guarantee high temperature, traditional method is acidproof, corrosion-resistant, high temperature resistant in ingot casting crucible surface-coated one and oxidation resistant silicon nitride powder last layer, the setting of this silicon nitride powder last layer, liquid-state silicon is not reacted with quartz crucible, avoids quartz crucible fracture phenomena to occur, ensure the demoulding integrity of the rear silicon ingot of cooling simultaneously.
But find through use for many years, the setting of above silicon nitride powder last layer, the silicon nitride particle that silicon ingot surface adsorption is certain can be made, and then containing a large amount of silicon nitride particle and other oxide on surface in the edge skin material making slicing silicon ingots produce, impurity etc., for realizing the re-using of this part edge skin material, the impurity such as silicon nitride must be cleaned up.
And in reality, silicon nitride is just selected as sealing coat because it is a kind of very obstinate material, and simultaneously because this material behavior makes its removing become very difficult.If take physical mechanical to throw to it to remove, not only expend very large manpower and materials, and the loss of silicon is also very large; If take chemical reaction to remove to it, effect is also very undesirable, because of the resistance to nearly all mineral acid of silicon nitride and less than 30% caustic soda soln, just current, traditional chemical cleaning method mostly is acid system and sig water purging method, but is all difficult to the silicon nitride on silicon material surface to remove, and causes and returns the rate of washing and exceed standard, even cannot wash crystalline substance and can only do waste disposal, or use yield rate degradation when causing the growth of throwing stove reluctantly.
Summary of the invention
For the problems referred to above, the invention provides a kind of purging method of silico briquette silicon nitride, it utilizes the severe corrosive of highly basic to remove the silicon nitride inclusions of silico briquette rapidly, has time saving and energy saving, economical, feature that the silico briquette rate of recovery is high.
For achieving the above object, the present invention by the following technical solutions: a kind of purging method of silico briquette surface nitrogen SiClx, comprises the steps:
(1) caustic corrosion be separated: by have with silicon nitride silico briquette drop into massfraction be carry out in 30% ~ 60% sodium hydroxide solution corrosion separation, the temperature of sodium hydroxide solution is 50 DEG C ~ 70 DEG C; Silico briquette deionized water after corrosion being separated rinses 2 ~ 5 minutes repeatedly;
(2) hydrochloric acid soln that the silico briquette after step 1 being processed is 0.05 ~ 0.5mol/L in concentration soaks 30 ~ 60 seconds; Deionized water rinsing 30 ~ 90 seconds are used after soaking;
(3) silico briquette after step 2 being processed soaks 30 ~ 60 seconds in the mixed solution of hydrofluoric acid and hydrogen peroxide, and wherein the mass ratio of hydrofluoric acid and hydrogen peroxide is 1:0.5 ~ 3;
(4) silico briquette after step 3 being processed soaks 30 ~ 60 seconds in the mixing acid of hydrofluoric acid and nitric acid, and the mass ratio of described hydrofluoric acid and nitric acid is 1:11 ~ 53;
(5) silico briquette after step 4 process soaks 1 ~ 3min in the water of 70 ~ 80 DEG C; Then rinse 2 ~ 5 minutes with deionization, dry at 80 DEG C.
The invention has the beneficial effects as follows: first the inventive method utilizes alkali corrosion to react the removal carrying out silicon nitride, recycle mild acid wash technique afterwards and carry out secondary removing, the quick removal of the silicon nitride on silico briquette surface can be realized, whole technique is to the volume size no requirement (NR) of silicon material, the consume of silicon material is little, effectively can promote the rate of recovery of silicon material, simultaneously because technique has cyclicity, effectively can use manpower and material resources sparingly, reduce cost recovery.
specific examples
Embodiment 1: a kind of purging method of silico briquette surface nitrogen SiClx, it comprises the steps:
(1) caustic corrosion be separated: by have with silicon nitride silico briquette drop into massfraction be carry out in 30% sodium hydroxide solution corrosion separation, the temperature of sodium hydroxide solution is 70 DEG C; Silico briquette deionized water after corrosion being separated rinses 3 minutes repeatedly;
(2) hydrochloric acid soln that the silico briquette after step 1 being processed is 0.05mol/L in concentration soaks 60 seconds; Deionized water rinsing 90 seconds are used after soaking;
(3) silico briquette after step 2 being processed soaks 60 seconds in the mixed solution of hydrofluoric acid and hydrogen peroxide, and wherein the mass ratio of hydrofluoric acid and hydrogen peroxide is 1:0.5;
(4) silico briquette after step 3 being processed soaks 60 seconds in the mixing acid of hydrofluoric acid and nitric acid, and the mass ratio of described hydrofluoric acid and nitric acid is 1:53;
(5) silico briquette after step 4 process soaks 3min in the water of 80 DEG C; Then rinse 5 minutes with deionization, dry at 80 DEG C.
Embodiment 2
A purging method for silico briquette surface nitrogen SiClx, it comprises the steps:
(1) caustic corrosion be separated: by have with silicon nitride silico briquette drop into massfraction be carry out in 60% sodium hydroxide solution corrosion separation, the temperature of sodium hydroxide solution is 50 DEG C; Silico briquette deionized water after corrosion being separated rinses 4 minutes repeatedly;
(2) hydrochloric acid soln that the silico briquette after step 1 being processed is 0.5mol/L in concentration soaks 30 seconds; Deionized water rinsing 90 seconds are used after soaking;
(3) silico briquette after step 2 being processed soaks 30 seconds in the mixed solution of hydrofluoric acid and hydrogen peroxide, and wherein the mass ratio of hydrofluoric acid and hydrogen peroxide is 1:3;
(4) silico briquette after step 3 being processed soaks 30 seconds in the mixing acid of hydrofluoric acid and nitric acid, and the mass ratio of described hydrofluoric acid and nitric acid is 1:11;
(5) silico briquette after step 4 process soaks 3min in the water of 70 DEG C; Then rinse 2 minutes with deionization, dry at 80 DEG C.
To sum up, the inventive method combines alkali corrosion reaction with mild acid wash technique, the quick removal of the silicon nitride on silico briquette surface can be realized, whole technique is to the build size no requirement (NR) of silicon material, the consume of silicon material is little, effectively can promote the rate of recovery of silicon material, simultaneously because technique has cyclicity, effectively can use manpower and material resources sparingly, reduce cost recovery.
Claims (1)
1. a purging method for silico briquette surface nitrogen SiClx, is characterized in that, comprises the steps:
(1) caustic corrosion be separated: by have with silicon nitride silico briquette drop into massfraction be carry out in 30% ~ 60% sodium hydroxide solution corrosion separation, the temperature of sodium hydroxide solution is 50 DEG C ~ 70 DEG C; Silico briquette deionized water after corrosion being separated rinses 2 ~ 5 minutes repeatedly;
(2) hydrochloric acid soln that the silico briquette after step 1 being processed is 0.05 ~ 0.5mol/L in concentration soaks 30 ~ 60 seconds; Deionized water rinsing 30 ~ 90 seconds are used after soaking;
(3) silico briquette after step 2 being processed soaks 30 ~ 60 seconds in the mixed solution of hydrofluoric acid and hydrogen peroxide, and wherein the mass ratio of hydrofluoric acid and hydrogen peroxide is 1:0.5 ~ 3;
(4) silico briquette after step 3 being processed soaks 30 ~ 60 seconds in the mixing acid of hydrofluoric acid and nitric acid, and the mass ratio of described hydrofluoric acid and nitric acid is 1:11 ~ 53;
(5) silico briquette after step 4 being processed soaks 1 ~ 3min in the water of 70 ~ 80 DEG C; Then rinse 2 ~ 5 minutes with deionization, dry at 80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410527036.5A CN104445206A (en) | 2014-10-09 | 2014-10-09 | Method for cleaning silicon nitride on surface of silicon block |
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| CN201410527036.5A CN104445206A (en) | 2014-10-09 | 2014-10-09 | Method for cleaning silicon nitride on surface of silicon block |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106952805A (en) * | 2017-04-11 | 2017-07-14 | 东方日升新能源股份有限公司 | A kind of graphite boat cleaning |
| CN109848122A (en) * | 2018-12-29 | 2019-06-07 | 晶能光电（江西）有限公司 | The cleaning method of SiC panel surface AlN film layer |
| CN115376915A (en) * | 2022-10-27 | 2022-11-22 | 合肥新晶集成电路有限公司 | Selective etching method and apparatus |
| CN115989192A (en) * | 2020-08-27 | 2023-04-18 | 株式会社德山 | Broken polycrystalline silicon blocks and manufacturing method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001058811A (en) * | 1999-08-20 | 2001-03-06 | Showa Alum Corp | Purification of silicon |
| CN101218176A (en) * | 2005-07-04 | 2008-07-09 | 夏普株式会社 | Recycling method for silicon, silicon and silicon ingot prepared by the method |
| JP2009535289A (en) * | 2006-04-25 | 2009-10-01 | ジ・アリゾナ・ボード・オブ・リージェンツ・オン・ビハーフ・オブ・ザ・ユニバーシティ・オブ・アリゾナ | Silicon purification process |
| CN101973552A (en) * | 2010-09-21 | 2011-02-16 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silicon from impurities |
| CN102757051A (en) * | 2012-04-19 | 2012-10-31 | 镇江环太硅科技有限公司 | Method for performing recovery treatment on waste layer silicon material |
-
2014
- 2014-10-09 CN CN201410527036.5A patent/CN104445206A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001058811A (en) * | 1999-08-20 | 2001-03-06 | Showa Alum Corp | Purification of silicon |
| CN101218176A (en) * | 2005-07-04 | 2008-07-09 | 夏普株式会社 | Recycling method for silicon, silicon and silicon ingot prepared by the method |
| JP2009535289A (en) * | 2006-04-25 | 2009-10-01 | ジ・アリゾナ・ボード・オブ・リージェンツ・オン・ビハーフ・オブ・ザ・ユニバーシティ・オブ・アリゾナ | Silicon purification process |
| CN101973552A (en) * | 2010-09-21 | 2011-02-16 | 江西赛维Ldk太阳能高科技有限公司 | Method for separating silicon from impurities |
| CN102757051A (en) * | 2012-04-19 | 2012-10-31 | 镇江环太硅科技有限公司 | Method for performing recovery treatment on waste layer silicon material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106952805A (en) * | 2017-04-11 | 2017-07-14 | 东方日升新能源股份有限公司 | A kind of graphite boat cleaning |
| CN106952805B (en) * | 2017-04-11 | 2019-12-13 | 东方日升新能源股份有限公司 | graphite boat cleaning process |
| CN109848122A (en) * | 2018-12-29 | 2019-06-07 | 晶能光电（江西）有限公司 | The cleaning method of SiC panel surface AlN film layer |
| CN115989192A (en) * | 2020-08-27 | 2023-04-18 | 株式会社德山 | Broken polycrystalline silicon blocks and manufacturing method thereof |
| CN115989192B (en) * | 2020-08-27 | 2024-02-02 | 株式会社德山 | Broken polysilicon block and its manufacturing method |
| CN115376915A (en) * | 2022-10-27 | 2022-11-22 | 合肥新晶集成电路有限公司 | Selective etching method and apparatus |
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Application publication date: 20150325 |