CN100571911C - The manufacture method of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip - Google Patents

The manufacture method of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip Download PDF

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CN100571911C
CN100571911C CNB200510062114XA CN200510062114A CN100571911C CN 100571911 C CN100571911 C CN 100571911C CN B200510062114X A CNB200510062114X A CN B200510062114XA CN 200510062114 A CN200510062114 A CN 200510062114A CN 100571911 C CN100571911 C CN 100571911C
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silicon chip
integrated circuit
silicon
solar energy
manufacture method
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CN1810394A (en
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刘培东
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Zhejiang Dongyuan Electronics Co., Ltd.
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刘培东
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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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/20—Waste processing or separation
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]

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Abstract

The invention discloses a kind of manufacture method of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip.It is with integrated circuit waste silicon chip HCl, H 2SO 4Remove magnesium, aluminium, manganese, zinc, chromium, iron, nickel, tin, metal that lead ratio hydrogen is active, use HNO 3Remove copper, mercury, silver-colored transition metal, with HF, HNO 3Nitration mixture is removed metal silicide, Si oxide, silicon nitride, the method of using thinning single surface, twin grinding attenuate again is with the active area in the removal devices technology, obtain the silicon chip of original resistivity, and, produce the silicon chip of used for solar batteries through cleaning, classification, detection, stepping.The present invention has effectively utilized the discarded silicon chip in the integrated circuit production, through a series of processing, removed the silicon Physical layer in the silicon chip certain thickness, simultaneously that this is a part of impurity and structure variation are together removed, resulting silicon chip has still less impurity and perfect crystal structure more than general solar silicon wafers, and the solar device of producing has higher photoelectric transformation efficiency.

Description

The manufacture method of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip
Technical field
The present invention relates to a kind of manufacture method of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip.
Background technology
The silicon chip that is applied to solar cell generally has two kinds of manufacture methods, a kind of is the method for casting polycrystalline silicon, this method technology is simple, production cost is low, can directly cut into the square crystal ingot, thereby cut into the used square silicon chip of solar cell easily, but the silicon chip that this method is produced, structural form is the polycrystalline attitude, defective is many, the impurity content height, and the solar cell photoelectric conversion efficiency of producing is also low.Another kind method is the method that vertical pulling method (Czochralski method) is produced silicon single crystal, the silicon chip crystal structure that this method is produced is more complete than casting polycrystalline silicon sheet, impurity content is lower than casting polycrystalline silicon sheet, solar cell photoelectric conversion efficiency height with this silicon chip production, but the desired policrystalline silicon quality requirement of this method height, the production cost height also needs in the silicon chip working process disk is cut into accurate side's sheet.
Produce solar cell with silicon chip, through years of development, technology is increasingly mature, production cost is well controlled, utilize the solar cell power generation technology to enter the extensive civil nature stage, the contradiction of the mankind's of the world today the unprecedented exploitation and the limited energy becomes increasingly conspicuous, countries such as the particularly Japanese U.S. of national governments Europe, use financial subsidies, vigorously support the utilization of solar energy, the silicon solar cell development is very rapid, and causes the international market polycrystalline silicon raw material very in short supply, price is doubled, and price increases to 120 dollars from more than 20 dollar of past especially on the black market.
A large amount of monocrystalline silicon pieces that use high-quality in semiconductor integrated circuit is produced, these silicon chip crystal structures are complete, and impurity content is very low.In the semiconductor integrated circuit production process, electronic devices and components all are integrated in several microns to tens microns zones of silicon chip surface, and obvious variation does not take place for the silicon structure of silicon chip inside and composition.Integrated circuit is produced each operation, there is this waste silicon chip that causes component failure to produce because of a variety of causes in the capital, in addition, semiconductor integrated circuit is produced each operation also to be needed to use test pieces and accompanies sheet, and 10%～20% of the sheet amount of throwing is generally arranged, and this part can not be used for the waste silicon chip of integrated circuit through handling, be applied to again in the production of solar cell, help the resource circulation utilization, can reduce the production cost of solar cell greatly, market is used very wide.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip.
It is with integrated circuit waste silicon chip HCl, H 2SO 4Remove magnesium, aluminium, manganese, zinc, chromium, iron, nickel, tin, metal that lead ratio hydrogen is active, use HNO 3Remove copper, mercury, silver-colored transition metal, with HF, HNO 3Nitration mixture is removed metal silicide, Si oxide, silicon nitride, the method of using thinning single surface, twin grinding attenuate again is with the active area in the removal devices technology, obtain the silicon chip of original resistivity, and, produce the silicon chip of used for solar batteries through cleaning, classification, detection, stepping.
Described HF, HNO 3Add CH in the nitration mixture 3COOH, H 3PO 4Or CH 3COOH and H 3PO 4Buffer.The concentration of HCl is 10～30%, H 2SO 4Concentration be 10～60%.HNO 3Concentration be 10～70%.HF in the nitration mixture: HNO 3Proportioning be 1: 1～1: 10.Thinning single surface adopts single face mechanical reduction machine or single face sand-blasting machine.Wafer lapping machine is adopted in twin grinding.
The present invention has effectively utilized the discarded silicon chip in the integrated circuit production, through a series of processing, removed the silicon Physical layer in the silicon chip certain thickness, simultaneously that this is a part of impurity and structure variation are together removed, resulting silicon chip has still less impurity and perfect crystal structure more than general solar silicon wafers, and the solar device of producing has higher photoelectric transformation efficiency.
The specific embodiment
Technological process of the present invention and technical essential
1. the metal of silicon chip surface, silicide are peeled off
In integrated circuit technology, because the needs of electrode pin lead-in wire, the silicon chip surface sputter layer of metal of being everlasting film, common metal has aluminium, copper etc., in addition, metal contacts with silicon and forms metal silicide, and silicon and oxygen, nitrogen form Si oxide and silicon nitride, this part metal and compound must at first be removed with chemical method as objectionable impurities.Concrete grammar is as follows:
1) watery hydrochloric acid or dilute sulfuric acid are peeled off light metal
Waste silicon chip is loaded with the special-purpose indigo plant (horse) of spending, and places in watery hydrochloric acid or the dilution heat of sulfuric acid, and metal more active than hydrogen in the metal active sequence list can both react with diluted acid.
As 2Al+3H 2SO 4=Al 2(SO 4) 3+ 3H 2↑
Common metal activity command is as follows
K?Ca?Na?Mg?Al?Zn?Fe?Sn?Pb(H)Cu?Hg?Ag?Pt?Au
Reaction is cleaned with deionized water after do not have gas and produce.
Watery hydrochloric acid or dilute sulfuric acid concentration are selected to consider enough fast reaction speed, to consider the convenience and the safety of use simultaneously, because the strong volatility of concentrated hydrochloric acid and the concentrated sulfuric acid is high dehydrated and oxidisability, the watery hydrochloric acid concentration that suggestion is used is 10～30%, and the concentration of dilution heat of sulfuric acid is 10～60%.
2) nitric acid is peeled off transition metal
In the metallized metal activity command, be positioned at hydrogen metal afterwards, can not peel off, at this moment need peel off HNO with nitric acid with watery hydrochloric acid or dilute sulfuric acid 3Concentration be 10～70%.As follows as copper and rare nitric acid and red fuming nitric acid (RFNA) reaction:
3Cu+8HNO 3(rare)=3Cu (NO 3) 2+ 2NO ↑+4H 2O
Cu+4HNO 3(dense)=Cu (NO 3) 2+ 2NO 2↑+2H 2O
Silicon chip is put equally in the Hua Lan (horse) and is reacted with salpeter solution, because metal and nitric acid reaction produce pernicious gas NO, NO 2So,, reaction must be carried out in fume hood, and tail gas discharges after will absorbing pernicious gas with the absorption tower.
Precious metal gold and platinum not with nitric acid reaction, at this moment to use chloroazotic acid, and recyclable Precious Metals-Gold of reacted solution and platinum, the processing of can classifying of this part waste silicon chip is not as content of the present invention.
3) hydrofluoric acid and nitric acid mixed acid stripping metal silicide, Si oxide, nitride.
Removed the silicon chip surface of light metal and heavy metal, metal silicide, Si oxide, nitride etc. may also residually be arranged, these compounds are except with nitration mixture reaction and the dissolving, both do not made and reacted with nitration mixture, because hydrofluoric acid and nitric acid mixed acid and surperficial pasc reaction, along with the dissolving of the silicon substrate that supports these compounds, these compounds also can be peeled off with reaction.
Si+6HF+4HNO 3＝H 2SiF 6+4NO 2↑+4H 2O
Above-mentioned reaction is an exothermic reaction, along with the temperature of carrying out solution of reaction is more and more higher, reaction speed is also more and more faster, too fast reaction speed can cause the inhomogeneities of reacting, it is thick more to make that silicon chip goes at the edge, it is big that thereby the gross thickness that makes silicon chip poor (TTV) becomes, for the control reaction speed can add CH in nitration mixture 3COOH, H 3PO 4Or CH 3COOH and H 3PO 4Buffer.HF in the nitration mixture: HNO 3Proportioning be 1: 1～1: 10.Reaction goes thick amount to be as the criterion with control, is generally 10um.
The nitrogen oxide that forms in the reaction (NO, NO 2) be toxic and harmful, be reflected in the equipment of ventilation and carry out, tail gas discharges after will absorbing pernicious gas with the absorption tower.
2. single face subtracts the book technology, removes the silicon layer of silicon chip front surface device active region
In integrated circuit technology, the device area of silicon chip front surface, through diffusion, ion injection, oxidation etc., this layer silicon of silicon chip front surface, very big variation has all taken place in its chemical composition and structure, subtracts the book machine with single face, uses cutting or grinding knife tool, remove the certain thickness silicon layer of front surface, with the removal devices active area.
Thinning single surface machine and single face sand-blasting machine can be realized the thinning single surface of silicon chip, but this method need be used special-purpose machine, and cost is higher, so, when active area not too thick, generally be no more than 20um can directly remove silicon simultaneously with the method for two-sided attenuate tow sides, can save thinning single surface thus.
3. the two-sided book technology that subtracts
The front surface of integrated circuit silicon chip is the active area of device, this part silicon layer must be removed, impurity-absorbing technique outside silicon chip back adopts in integrated circuit processing, make objectionable impurities enrichment overleaf, surface contamination in the process also makes silicon chip back that more impurity is arranged simultaneously, therefore, the silicon layer of the several microns in the silicon chip back side (um) also must be removed.
Double cutting separating disk machine with routine carries out twin grinding to silicon chip, can remove the silicon layer of the positive and negative of silicon chip simultaneously.General abrasive disc removes thick 60～80um, and positive and negative can be removed 30～40um simultaneously.The most of machining damage that produces in the operation before abrasive disc can be removed can reduce the roughness of silicon chip surface and make surfacing simultaneously.
The selection of abrasive disc thickness is according to the decision of silicon chip of solar cell desired thickness, and general silicon chip of solar cell thickness is at 300～350um, and integrated circuit silicon chip is all more than 500um, so the integrated circuit silicon waste-slice has enough thickness to remove.Bao slice, thin piece can adopt thinning single surface to add a spot of twin grinding and control the final thickness of silicon chip especially.
4. silicon chip cleans
Silicon chip is residual through the twin grinding rear surface grit and a chemical reagent, and the metal impurities that grind on the mill, these impurity have a strong impact on generation to road, back device operation, usually with special-purpose cleaning agent and add the ultrasonic wave cleaning, clean with deionized water again, dry silicon chip surface with drier at last.
5. the check of silicon chip, test, classification, stepping
The integrated circuit silicon waste-slice is handled through multistep as above, the silicon structure and the component variation layer of silicon chip surface have been removed, the silicon body that stays is the seldom silicon single crystal flake of structural integrity of impurity, and the silicon chip of handling need reach requirement to confirm recycling through verification test.
To confirm that at first the active area or the graph layer of silicon chip front surface removed totally, method is that two surfaces with the microscopic examination silicon chip have not had integrated circuit pattern, measure the resistivity of each point in the silicon chip with the four point probe resistivity tester, the resistivity measurement of each point except have the distinctive radially resistivity of silicon single crystal flake inhomogeneous, can not have because of changing the resistivity contrasts that test point causes.
The minority carrier lifetime of its less important measurement silicon chip or diffusion length reach requirement with the content of confirming the beavy metal impurity in the silicon.
By the silicon chip of above-mentioned measurement, the discarded sheet that proves integrated circuit has better characteristic through handling the qualitative characteristics that has recovered former monocrystalline silicon piece than general solar energy battery adopted silicon chip.
General silicon for solar cell monocrystalline uses poor policrystalline silicon raw material, the silicon single crystal growing furnace simplicity of design, and the graphite piece purity requirement in the thermal field system is low, the not strict control of defective during crystal growth, the monocrystalline that grows allows dislocation.So the monocrystalline silicon piece of used for solar batteries is not high aspect the requiring of impurity and defective, the monocrystalline silicon piece that the application integrated circuit waste silicon chip is produced can satisfy the requirement of used for solar batteries monocrystalline silicon piece fully.
Because different producers adopts different production method and technology to make solar cell, there is different requirements in the manufacturing firm of solar cell to silicon single crystal flake, so, need mainly contain following several to the further testing classification of the silicon single crystal flake of handling well.
1) conduction type, crystal orientation test.
The integrated circuit waste silicon chip seldom can also be by the assortment of silicon chip and since be not each producer all by standard-required, can not discern the kind of silicon chip by the major-minor plane of reference, so the conduction type of silicon chip and crystal orientation need testing classification again.
The silicon chip of gently mixing is measured conduction type with three probes, and this is a kind of method of testing commonly used, and it still is the P type that instrument is directly read the N type.
The available X ray orientation of the measurement in crystal orientation is measured, this method can accurately measure the crystal orientation and the crystal orientation of crystal and depart from, another kind of simple method can judge simply silicon crystal be＜111 or＜100, it is to shine silicon chip surface with infrared light, infrared light spot according to reflection is judged, if " Y " font then is＜111 〉, if " ten " font then is＜100 〉.
2) measurement of resistivity and stepping
With four point probe resistivity tester or ADE non-contact type resistivity tester, silicon chip is carried out resistivity measurement and stepping, to satisfy different customer requirements, resistivity can be divided into many grades from 0.5～50 Ω .cm.
3) measurement of thickness and stepping
With amesdial or ADE non-contact type Thickness measuring instrument, silicon chip is carried out thickness measure and stepping, to satisfy different customer requirements.
6. silicon wafer is divided into accurate side's sheet of used for solar batteries
Solar cell components is that a plurality of silicon chip of solar cell are combined, and long-pending for obtaining photoirradiated surface as much as possible, the amalgamation of silicon chip is the best with no gap, and square silicon chip can not have the gap combination, so the policrystalline silicon sheet is cut into square sheet.Silicon single crystal flake is a disk, if be cut into positive side silicon wafer waste too much, therefore, silicon wafer is cut into accurate square usually, and specific requirement also has client oneself processing according to client's needs.

Claims (6)

1. the manufacture method of an application integrated circuit waste silicon chip production solar energy battery adopted silicon chip is characterized in that, with integrated circuit waste silicon chip HCl, H 2SO 4Remove magnesium, aluminium, manganese, zinc, chromium, iron, nickel, tin, metal that lead ratio hydrogen is active, use HNO 3Remove copper, mercury, silver-colored transition metal, with HF, HNO 3Nitration mixture is removed metal silicide, Si oxide, silicon nitride, the method of using thinning single surface, twin grinding attenuate again is with the active area in the removal devices technology, obtain the silicon chip of original resistivity, and through cleaning, classification, detection, stepping, produce the silicon chip of used for solar batteries, HF in the described nitration mixture: HNO 3Proportioning be 1: 1～1: 10, HF, HNO 3Add CH in the nitration mixture 3COOH, H 3PO 4Or CH 3COOH and H 3PO 4Buffer.
2. the manufacture method of a kind of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip according to claim 1, the concentration that it is characterized in that described HCl is 10～30%,
3. the manufacture method of a kind of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip according to claim 1 is characterized in that described H 28O 4Concentration be 10～60%.
4. the manufacture method of a kind of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip according to claim 1 is characterized in that described HNO 3Concentration be 10～70%.
5. the manufacture method of a kind of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip according to claim 1 is characterized in that described thinning single surface adopts single face mechanical reduction machine or single face sand-blasting machine.
6. the manufacture method of a kind of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip according to claim 1 is characterized in that described twin grinding employing wafer lapping machine.
CNB200510062114XA 2005-12-19 2005-12-19 The manufacture method of application integrated circuit waste silicon chip production solar energy battery adopted silicon chip Expired - Fee Related CN100571911C (en)

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CN102306687B (en) * 2011-09-28 2012-12-05 湖南红太阳新能源科技有限公司 Crystalline silica solar energy cell PECVD rainbow film reworking method
CN102496657A (en) * 2011-12-27 2012-06-13 湖南红太阳新能源科技有限公司 Method for improving abnormal crystalline silicon solar cell
WO2017100443A1 (en) * 2015-12-10 2017-06-15 Arizona Board Of Regents On Behalf Of Arizona State University Recovery of valuable or toxic metals from silicon solar cells
CN105845774A (en) * 2016-04-06 2016-08-10 东莞市祖科能源科技有限公司 Method utilizing waste silicon chips, waste cells or cells to manufacture photovoltaic solar cell panel
CN107457250B (en) * 2017-07-19 2020-05-05 中国环境科学研究院 Method for classifying and recycling resources of crystalline silicon solar cells
CN108339831B (en) * 2018-02-09 2020-11-24 中南大学 Method for disposing silicon solar cell
CN109830577B (en) * 2019-01-18 2021-06-15 深圳市广盛浩科技有限公司 Manufacturing method of high-quality light-emitting diode

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