CN102241401B - Separation method of quartz and silicon material in single crystal silicon crucible backing material - Google Patents
Separation method of quartz and silicon material in single crystal silicon crucible backing material Download PDFInfo
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- CN102241401B CN102241401B CN 201110178112 CN201110178112A CN102241401B CN 102241401 B CN102241401 B CN 102241401B CN 201110178112 CN201110178112 CN 201110178112 CN 201110178112 A CN201110178112 A CN 201110178112A CN 102241401 B CN102241401 B CN 102241401B
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Abstract
The invention relates to a separation method of quartz and a silicon material in a single crystal silicon crucible backing material and belongs to the technical field of semiconductor separation. The invention aims to provide a method with short time and low energy consumption for separating quartz and a silicon material in a single crystal silicon crucible backing material. The technical scheme adopted by the invention is as follows: 1) crushing the crucible backing material to be separated into particles of which the particle size is no more than 10mm; 2) using pure water at 50 DEG C to prepare 50L of 10wt% alkaline solution; 3) in a constant temperature water bath, pouring 10kg of the crushed crucible backing material into the 50L of alkaline solution prepared in the step 2, and stirring; 4) adding 10ml of foaming agent into the alkaline solution; 5) pumping air into the alkaline solution so as to ensure that the silicon material can float on the liquid level along with bubbles generated on the surface of the silicon material, collecting the floating silicon material; and 6) recycling the quartz at the bottom after collecting the floating silicon material. The separation methodis used for separating the quartz from the silicon material in the single crystal silicon crucible backing material.
Description
Technical field
The separation method of quartz and silicon material belongs to technical field of semiconductor separation in the monocrystalline silicon pot bottom material of the present invention, particularly relates to technique quartzy in a kind of separating single crystal silicon pot bottom material.
Background technology
Unavoidably can produce some residual silicon material in the produce single crystal silicon rod, the silicon material on these remain at the bottom of the crucible is called pot bottom material.On the silicon material can be melted at the bottom of the crucible of quartz crucible when monocrystal pulling silicon, quartz crucible resistates that therefore can adularescent was attached on the silicon material of grey, and these have adhered to quartzy silicon material, all are to belong to original useless silicon material.For the silicon material is fully used, the quartz in the pot bottom material must be separated with the silicon material, the silicon material of separating can be melted down pull on monocrystalline.
Method commonly used is that the silicon material is manually separated with quartz at present, and then a small amount of quartz with remained on surface at room temperature soaks with hydrofluoric acid, usually needs 2-5 days time quartz thoroughly could be reacted.This method is length consuming time not only, and expend a large amount of hydrofluoric acid, and environmental protection has high input.The with good grounds quartz of other method is different from the coefficient of expansion of silicon material and realize separating by heating, cooling, also there is the quartz of utilization different with the fusing point of silicon material, separate by the remelting realization, but these two kinds of methods not only need a large amount of high temperature heat, and the time of expending is also longer, in addition, pyroprocessing also causes impurity easily to silicon material internal divergence, reduces the quality that reclaims the silicon material.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, and technical problem to be solved has provided a kind of weak point consuming time, the separation method of quartz and silicon material in few monocrystalline silicon pot bottom material that consumes energy.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the separation method of quartz and silicon material in the monocrystalline silicon pot bottom material, carry out according to following step.
The first step, the pot bottom material that will separate are crushed to particle diameter and are no more than 10mm;
Second step, in alkaline-resisting container, be 10% basic solution 50L with 50 ℃ pure water preparation weight percents;
The 3rd step, under the water bath with thermostatic control, the pot bottom material 10kg that fragmentation is good pours in the 50L basic solution for preparing in the second step, stirs, and makes pot bottom material be distributed in uniformly container bottom and fully contacts with basic solution;
The 4th the step, in described basic solution, add pore forming material, add-on is 10ml;
The 5th step, in described basic solution, blast air, make the silicon material along with its surface and the bubble floating that the reaction of described basic solution produces go out liquid level, collect the silicon material of emersion;
The 6th step, collect the silicon material of emersion after, reclaim the quartz of bottom;
Described pore forming material or be secondary octanol, or be Virahol.
Described the 6th the step finish after, in remaining basic solution, pour again the broken good pot bottom material of 10kg into, add the alkaline matter in the described basic solution, guarantee that the concentration of basic solution is 10%, add described the 4th the step in the pore forming material add-on 10%, repeat above-mentioned the 5th the step and the 6th step.
Described basic solution or be sodium hydroxide solution, or be potassium hydroxide solution, or be tetramethyl ammonium hydroxide solution, or be sodium carbonate solution, or be solution of potassium carbonate.
The temperature of described water bath with thermostatic control is 40 ℃-60 ℃.
Pore forming material adding method for determination of amount is the pot bottom material of adding in described the 4th step: the pore forming material=1kg:1ml of adding.
The present invention compared with prior art has following beneficial effect.
Chemical reaction among the present invention only rests on silicon face, before deep reaction not, silicon emerges, so the alkali lye amount that consumes seldom, to separate the time spent very short, and employed medicament is not volatile, nonirritant γ-ray emission in the reaction process, and reacted raffinate easily recycles, economically feasible, high-efficiency environment friendly.
Embodiment
The separation method of quartz and silicon material carries out according to following step in the monocrystalline silicon pot bottom material of the present invention.
The first step, the pot bottom material that will separate are crushed to particle diameter and are no more than 10mm;
Second step, in alkaline-resisting container, be 10% basic solution 50L with 50 ℃ pure water preparation weight percents;
The 3rd step, under the water bath with thermostatic control, the pot bottom material 10kg that fragmentation is good pours in the 50L basic solution for preparing in the second step, stirs, and makes pot bottom material be distributed in uniformly container bottom and fully contacts with basic solution;
The 4th the step, in described basic solution, add pore forming material, add-on is 10ml;
The 5th step, in described basic solution, blast air, make the silicon material along with its surface and the bubble floating that the reaction of described basic solution produces go out liquid level, collect the silicon material of emersion;
The 6th step, collect the silicon material of emersion after, reclaim the quartz of bottom;
Described pore forming material or be secondary octanol, or be Virahol.
Described the 6th the step finish after, in remaining basic solution, pour again the broken good pot bottom material of 10kg into, add the alkaline matter in the described basic solution, guarantee that the concentration of basic solution is 10%, add described the 4th the step in the pore forming material add-on 10%, repeat above-mentioned the 5th the step and the 6th step.
Described basic solution or be sodium hydroxide solution, or be potassium hydroxide solution, or be tetramethyl ammonium hydroxide solution, or be sodium carbonate solution, or be solution of potassium carbonate.
The temperature of described water bath with thermostatic control is 40 ℃-60 ℃.
Pore forming material adding method for determination of amount is the pot bottom material of adding in described the 4th step: the pore forming material=1kg:1ml of adding.
Silicon can with the basic solution generation hydrogen that reacts, reaction formula is:
↑, though and quartzy can reacting with basic solution, without γ-ray emission.When the particle diameter of silicon when 5mm is following, the bubble hydrogen that the id reaction of its absorption produces is enough to make the silicon come-up, realizes and the separating of quartz; When the particle diameter of silicon during greater than 5mm and less than 10mm, the buoyancy that the bubble hydrogen that himself adsorbs produces is not enough so that its come-up, can be by adding pore forming material and adopting the air bubbling to increase the buoyancy that it makes progress, silicon will be carried by bubble and emerge like this, and realization separates with quartz; When the particle diameter of silicon during greater than 10mm, can can't make its come-up because silicon is too heavy.
Among the present invention, 10% the basic solution of a 50L of configuration can be processed pot bottom material 3-4 time, and each 10kg need separate such as pot bottom material in addition, then will reconfigure basic solution.This is because alkali and silicon material, quartz reaction can generate water glass, thereby has increased the viscosity of solution, and along with the solution prolongation of duration of service, viscosity increases, and the silicon material just is difficult to along with bubble floating has gone out liquid level.
Claims (3)
1. the separation method of quartz and silicon material in the monocrystalline silicon pot bottom material is characterized in that, carries out according to following step:
The first step, the pot bottom material that will separate are crushed to particle diameter and are no more than 10mm;
Second step, in alkaline-resisting container, be 10% basic solution 50L with 50 ℃ pure water preparation weight percents;
The 3rd step, under the water bath with thermostatic control, the pot bottom material 10kg that fragmentation is good pours in the 50L basic solution for preparing in the second step, stirs, and makes pot bottom material be distributed in uniformly container bottom and fully contacts with basic solution;
The 4th the step, in described basic solution, add pore forming material, add-on is 10mL;
The 5th step, in described basic solution, blast air, make the silicon material along with its surface and the bubble floating that the reaction of described basic solution produces go out liquid level, collect the silicon material of emersion;
The 6th step, collect the silicon material of emersion after, reclaim the quartz of bottom;
Described pore forming material or be secondary octanol, or be Virahol;
The temperature of described water bath with thermostatic control is 40 ℃-60 ℃;
Described basic solution or be sodium hydroxide solution, or be potassium hydroxide solution, or be tetramethyl ammonium hydroxide solution, or be sodium carbonate solution, or be solution of potassium carbonate.
2. the separation method of quartzy and silicon material in the monocrystalline silicon pot bottom material according to claim 1, it is characterized in that: described the 6th the step finish after, in remaining basic solution, pour again the broken good pot bottom material of 10kg into, add the alkaline matter in the described basic solution, the concentration that guarantees basic solution is 10%, add described the 4th the step in the pore forming material add-on 10%, repeat above-mentioned the 5th the step and the 6th step.
3. the separation method of quartzy and silicon material in the monocrystalline silicon pot bottom material according to claim 1 is characterized in that: pore forming material adds method for determination of amount and is the pot bottom material of adding in described the 4th step: the pore forming material=1kg:1mL of adding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110178112 CN102241401B (en) | 2011-06-29 | 2011-06-29 | Separation method of quartz and silicon material in single crystal silicon crucible backing material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110178112 CN102241401B (en) | 2011-06-29 | 2011-06-29 | Separation method of quartz and silicon material in single crystal silicon crucible backing material |
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| CN102241401A CN102241401A (en) | 2011-11-16 |
| CN102241401B true CN102241401B (en) | 2013-03-20 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106006646A (en) * | 2016-06-26 | 2016-10-12 | 河南盛达光伏科技有限公司 | Chemical quartz separation treatment method for broken-particle monocrystalline silicon pot bottom material |
| CN106276916B (en) * | 2016-08-01 | 2018-05-29 | 大工（青岛）新能源材料技术研究院有限公司 | The technique that a kind of achievable monocrystalline flavoring food effectively cleans |
| CN107098783A (en) * | 2017-05-27 | 2017-08-29 | 镇江环太硅科技有限公司 | The technique that fused silica crucible prepares siliceous fertilizer raw material after a kind of utilization polycrystalline silicon ingot casting |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3093456A (en) * | 1958-09-02 | 1963-06-11 | Texas Instruments Inc | Method for recovery and reuse of quartz containers |
| CN1459415A (en) * | 2002-05-20 | 2003-12-03 | 中国科技开发院浙江分院 | Technology of separating quartz in monocrystalline silicon pot bottom material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3093456A (en) * | 1958-09-02 | 1963-06-11 | Texas Instruments Inc | Method for recovery and reuse of quartz containers |
| CN1459415A (en) * | 2002-05-20 | 2003-12-03 | 中国科技开发院浙江分院 | Technology of separating quartz in monocrystalline silicon pot bottom material |
Non-Patent Citations (2)
| Title |
|---|
| Kyaw Zin OO et al..Study of Mutual Separation of Silicon and Quartz Using Liquid-Liquid Extraction.《International Journal of the Society of Materials Engineering for Resources》.2002,第10卷(第1期),第71-74页. |
| Study of Mutual Separation of Silicon and Quartz Using Liquid-Liquid Extraction;Kyaw Zin OO et al.;《International Journal of the Society of Materials Engineering for Resources》;20020331;第10卷(第1期);第71-74页 * |
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