CN100406110C - Purification of powder particle in cold plasma - Google Patents
Purification of powder particle in cold plasma Download PDFInfo
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- CN100406110C CN100406110C CNB2004101555511A CN200410155551A CN100406110C CN 100406110 C CN100406110 C CN 100406110C CN B2004101555511 A CNB2004101555511 A CN B2004101555511A CN 200410155551 A CN200410155551 A CN 200410155551A CN 100406110 C CN100406110 C CN 100406110C
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- reaction chamber
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- reative cell
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention relates to the purification of powder particles in cold plasma; powder material is purified by a mode that cold plasma is adopted. The present invention comprises a semiconductor and ceramic powder material. The technology is mainly used for increasing the purity of silicon with the crystal particles and the power particles whose size is within a range of 50 mu m to 150 mu m to 99.99% from 99%; the present invention is the specific application for ' the metallurgical effect ' of the discovered cold plasma. The present invention adopts a vertical reaction chamber structure for increasing powder particle stroke; the regulation of gas blowback and effective gas pumping rate (KS) is adopted, which causes the descending speed of the powder particles to be reduced, and the collecting purpose is also achieved. The vibration sprinkling is used for preventing the conglobation of the powder particles. A reaction gas distributor makes gas uniformly blown upwards. Because of the measures, the purification speed rate is improved, the sedimentation time is lengthened, and the impurity quality removed by one-time sedimentation is increased; when a discharging power is 1000W, 400 grams of silicon powder whose purity is 99% can be purified to 99.99% per hour.
Description
Technical field
The invention belongs to plasma application, relate to purification devices and the technology of a kind of cold plasma, especially be suitable for the purification of semiconductor powders such as silicon, to make solar cell to powder.
Background technology
For the semiconductor grade silicon of extreme high purity, method of purification mainly is the thermal decomposition and the hydrogen reduction of tetrachloro silicane or trichlorosilane, then through vertical pulling or the further physical purification of zone-melting process and make large diameter silicon single crystal.This method at first also needs to hang down pure industrial silicon and makes chlorosilane, so cost is high and bring very big environmental pollution.For making purity is the so-called solar-grade silicon of 99.99% to 99.99999% this class, develops tens of kinds of different technology, as the method for hydrometallurgy, air-blowing, scum silica frost, metallic reducing, electro-deposition etc. and the above-mentioned semiconductor grade silicon preparation of simplification.All these methods be not exist the expense costliness be exactly purify undesirable.Under an atmospheric pressure, the low temperature plasma that gas discharge forms is used for the also extensive use of purifying, and is 99% silicon as can make purity with coke reduction silica.This method is about 3000 ℃ owing to ambient temperature, and the equipment complexity must be used crucible, thereby to refining material very big staining is arranged, and can't make more highly purified silicon.We have found the metallurgical effect of cold plasma (ambient temperature is a room temperature) to deposition materials at the mid-80.Research through more than ten years progressively has breakthrough this effect technically, just has using value so far.
Summary of the invention
The invention provides the device and the technology of gas discharge plasma under a kind of low pressure (cold plasma) purification silica flour, through purification process, the purity of silica flour can improve two magnitudes, is 99% as material purity promptly, and the purity of product can reach 99.99%.
Realize that the powder purification devices of the object of the invention includes vertical exoelectrical reaction chamber, charge can and the reaction gas distribution device of reative cell top cover and reative cell shell, described vertical exoelectrical reaction chamber is to use the cold plasma of gas discharge generation under the low pressure to finish the reative cell that powder is purified, and the surface that is contained in the indoor interior electrode of described vertical exoelectrical reaction is provided with triangular groove; The described reaction gas distribution device of reaction gas and cushion gas introducing vertical response chamber is contained in the indoor bottom of vertical response, the bleeding point of reaction gas and cushion gas being extracted out the vertical response chamber then is located on the reative cell top cover, makes that air-flow is opposite with the silt deposition direction to form blowback; Below the indoor charge can outlet of vertical response, be provided with vibratory sieve; There is a powder loop back device to include the loopback pipe, one end of this loopback pipe links to each other with the powder valve that is contained in the outlet of lower end, vertical exoelectrical reaction chamber by pipeline, the other end is transmitted back to the described charge can that is positioned at vertical response outdoor top, the left-handed passage of then closing loopback pipe and the outlet of lower end, vertical exoelectrical reaction chamber of powder valve allows the outlet of lower end, vertical exoelectrical reaction chamber be communicated with the powder gatherer; The dextrorotation of powder valve then is communicated with the passage of loopback pipe and the outlet of lower end, vertical exoelectrical reaction chamber, closes the interface channel of outlet of lower end, vertical exoelectrical reaction chamber and powder gatherer.
Above-mentioned vibratory sieve can be connected with a vibration rod, and this vibration rod stretches out outside the described reative cell top cover.Above-mentioned vibratory sieve can be provided with multi-layer silk screen.
The vertical response chamber can be cylindrical shape or rectangle, and as being that the then interior electrode of cylindrical shape is a negative electrode, shell is anode (ground connection), and it is even to guarantee discharge that cathode surface is carved triangular groove.
The present invention is more effective owing to having taked following measure that the purifying of powder is able to: 1, select the supplier of raw material (industrial silicon), cooling (curing) technology of molten silicon after regulation is come out of the stove is to satisfy polysilicon grain degree requirement (50 μ m to 150 μ m).Pulverize back powder granularity and should be equal to or less than the polysilicon grain granularity, all be presented on the powder surface to guarantee the impurity in most powders.2, the vertical installation of electrode surface (for plate electrode) or axis (to cylinder electrode) makes the silt deposition direction parallel with electrode, and chamber volume is only with the fall first power increase of journey of powder.Being easy to increase powder falls journey (sedimentation time increase) and increases Impurity removal amount in infall process.3, powder is thrown to loose through vibration and can guarantee that powder evenly distributes also in reative cell
Prevent agglomerating sedimentation.4, reaction gas and cushion gas are introduced from the reative cell bottom through distributor, and bleeding point makes air-flow opposite with the silt deposition direction in reactor top, form blowback.Therefore the maximal rate of powder decline is:
Wherein, d
gBe respectively gas molecule (on average) and powder diameter with d; Ps is the mass density of powder; The g afterburning speed of attaching most importance to; M
gMean molecule quantity for gas; T is a reaction chamber temperature; A is long-pending for being reflected at chamber cross-section; S is the pumping speed rate of straight empty unit; K is a proportionality coefficient, and is relevant with the opening degree of the structure of vacuum system (comprising connecting pipe) and choke valve.After deliberation, the average speed of silt deposition and V
zAlmost equal, at the suspension time and the V of reaction zone
zBe inversely proportional to.The measure that increases suspension time is to increase KS, but must guarantee V
z＞0.Otherwise powder will be taken away by vacuum machine level.4, reacting gas adopts HCl or HBr etc., and buffer gas adopts Ar.H appears at reaction zone
+, Cl
+Or Br
+, Ar
+Plasma and their atom.These reaction particles can with the collision that reacts of silicon grain surface.The etching phenomenon takes place in the sheath district to improve purification speed.5, increase cathode self bias, moderate reative cell gross pressure (about 3Pa), suitably increase the sheath layer thickness and further improve purifying speed with concentration and the speed (kinetic energy) that improves reaction particle.6, increase the powder loop back device, realize repeatedly purifying repeatedly, not only increase the Impurity removal amount but also realize that the powder surface impurity removes uniformly.This is particularly important to low pure raw material.
Description of drawings
Fig. 1 is the structural representation of powder purification devices.
Fig. 2 is the principle schematic of powder purifying.
In the accompanying drawing 1,1, charge can; 2, vibration rod; 3, reative cell top cover; 4, multilayer vibratory sieve; 5, interior electrode insulation cover; 6, interior electrode; 7, reative cell shell; 8 reaction gas distribution devices; 9, powder valve; 10, powder gatherer; 11, powder loop back device.In the accompanying drawing 2,6, interior electrode; 7, external electrode.
The specific embodiment
Embodiment 1 is a small amount of preparation of product, is used to the silica flour of purifying, and raw material is 99% industrial silicon.Selecting polysilicon grain is 100 μ m left and right sides silico briquettes, through broken, pulverize to such an extent that particle is a silica flour about 100 μ m, the sorting of sieving.In the purifier apparatus, interior electrode 6 external diameters are 4cm, and external electrode 7 internal diameters are 8cm, the about 18cm of region of discharge effective length.The powder batch can of packing into.Be evacuated to earlier about 1Pa, Ar gas carries HCl gas through the hydrochloric acid tank bubbling and sends into reative cell, adjusts discharge parameter and chamber pressure, again the silicon material is spread into vibratory sieve through control valve.Powder valve 9 is swung to the right, allow the powder of having purified be recycled to charge can continuation purification, after several hours, valve is turned on the left side, the results product.Be to implement this programme, discharge power needs about 1 kilowatt, and the about 3Pa of reative cell air pressure per hour on average can obtain purity and is 99.99% silicon material 400 and restrain the powder rate of recovery about 85%.Embodiment 2 is the silico briquette that has cured earlier for material purity has 99.9%.The same mode of equipment and method of operating, purifying can meet the demands but powder only needs successively.Therefore valve always is threaded to the right.It is 15 kilograms of 99.995% silica flours that this mode per hour can get purity.Embodiment 3 increases to 10 times with reative cell cross section A.Electrode length is increased to 3 times, keeps discharge energy density constant.Its ability of handling powder of this purification system enlarges 20 times and 10 times respectively than mode 1 and 2.
Except that semiconductor silicon etc. is carried out the purifying, purifier apparatus can also be to TiO
2, SiO
2, Al
2O
3Carry out purifying Deng ceramic powder
Claims (3)
1. powder purification devices, the vertical exoelectrical reaction chamber, charge can (1), the reaction gas distribution device (8) that include reative cell top cover (3) and reative cell shell (7), it is characterized in that: described vertical exoelectrical reaction chamber is to use the cold plasma of gas discharge generation under the low pressure to finish the reative cell that powder is purified, and the surface that is contained in the indoor interior electrode (6) of described vertical exoelectrical reaction is provided with triangular groove; Described reaction gas distribution device (8) is contained in the indoor bottom of vertical response, and bleeding point then is located on the reative cell top cover (3); Below in the indoor charge can of vertical response (1) outlet is provided with vibratory sieve (4); Have a powder loop back device (11) to include the loopback pipe, an end of this loopback pipe links to each other with the powder valve (9) that is contained in the outlet of lower end, vertical exoelectrical reaction chamber by pipeline, and the other end is transmitted back to the described charge can (1) that is positioned at vertical response outdoor top; The left-handed passage of then closing loopback pipe and the outlet of lower end, vertical exoelectrical reaction chamber of powder valve (9) allows the outlet of lower end, vertical exoelectrical reaction chamber be communicated with powder gatherer (10); Powder valve (9) dextrorotation then is communicated with the passage of loopback pipe and the outlet of lower end, vertical exoelectrical reaction chamber, closes the interface channel of outlet of lower end, vertical exoelectrical reaction chamber and powder gatherer (10).
2. powder purification devices according to claim 1 is characterized in that: described vibratory sieve (4) is connected with a vibration rod (2), and this vibration rod (2) stretches out outside the described reative cell top cover (3).
3. powder purification devices according to claim 1 is characterized in that: described vibratory sieve (4) is provided with multi-layer silk screen.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004101555511A CN100406110C (en) | 2004-12-21 | 2004-12-21 | Purification of powder particle in cold plasma |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2004101555511A CN100406110C (en) | 2004-12-21 | 2004-12-21 | Purification of powder particle in cold plasma |
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| CN1669630A CN1669630A (en) | 2005-09-21 |
| CN100406110C true CN100406110C (en) | 2008-07-30 |
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| CNB2004101555511A Expired - Fee Related CN100406110C (en) | 2004-12-21 | 2004-12-21 | Purification of powder particle in cold plasma |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100423828C (en) * | 2006-12-22 | 2008-10-08 | 华中科技大学 | Silicon powder surface etching device |
| CN101723377A (en) * | 2008-10-28 | 2010-06-09 | 刘铁林 | Method and device for purification of silicon |
| CN115724433B (en) * | 2022-11-23 | 2023-06-23 | 湖北冶金地质研究所(中南冶金地质研究所) | Quartz sand plasma gas-solid reaction purification device and purification method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3330864A1 (en) * | 1983-08-26 | 1985-03-14 | Siemens AG, 1000 Berlin und 8000 München | Apparatus for depositing silicon oxide layers on semiconductor substrates using a CVD coating technique |
| US4689075A (en) * | 1984-10-16 | 1987-08-25 | National Research Institute For Metals | Process for producing mixed ultrafine powder of metals or ceramics |
| CN2510154Y (en) * | 2001-10-26 | 2002-09-11 | 吴征威 | Plasma mixed gas-phase-method nanometer-particle preparation appatatus |
| CN1382547A (en) * | 2002-02-08 | 2002-12-04 | 宁波广博纳米材料有限公司 | Equipment for preparing nano metal powder |
-
2004
- 2004-12-21 CN CNB2004101555511A patent/CN100406110C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3330864A1 (en) * | 1983-08-26 | 1985-03-14 | Siemens AG, 1000 Berlin und 8000 München | Apparatus for depositing silicon oxide layers on semiconductor substrates using a CVD coating technique |
| US4689075A (en) * | 1984-10-16 | 1987-08-25 | National Research Institute For Metals | Process for producing mixed ultrafine powder of metals or ceramics |
| CN2510154Y (en) * | 2001-10-26 | 2002-09-11 | 吴征威 | Plasma mixed gas-phase-method nanometer-particle preparation appatatus |
| CN1382547A (en) * | 2002-02-08 | 2002-12-04 | 宁波广博纳米材料有限公司 | Equipment for preparing nano metal powder |
Non-Patent Citations (2)
| Title |
|---|
| 粉粒沉降过程中冷等离子体纯化效果研究. 陶甫廷等.广西工学院学报，第12卷第2期. 2001 |
| 粉粒沉降过程中冷等离子体纯化效果研究. 陶甫廷等.广西工学院学报，第12卷第2期. 2001 * |
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