CN103286316B - A kind of method of stirring ball-milling processing CuInGa powders - Google Patents
A kind of method of stirring ball-milling processing CuInGa powders Download PDFInfo
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- CN103286316B CN103286316B CN201310212222.5A CN201310212222A CN103286316B CN 103286316 B CN103286316 B CN 103286316B CN 201310212222 A CN201310212222 A CN 201310212222A CN 103286316 B CN103286316 B CN 103286316B
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Abstract
The present invention proposes a kind of method of stirring ball-milling processing CuInGa powders, the other CuInGa metal dusts of grade and grinding aid are mixed into pulvis and load agate pot, the bead for adding a diameter of 2 5mm is some, the tank mouth of agate pot is sealed with baffle plate, agate pot is stretched into the stirring-head of translator, and the CuInGa powders of micron level are obtained with 1000rpm to 1500rpm rotating speed agitation grinding 5 to 10 hours, grinding.The present invention can effectively solve the infiltration sex chromosome mosaicism of the alloy powder that Cu, In, Ga are main body and abrading-ball, and grinding efficiency is higher, can effectively reduce the impurity elements such as Fe, Cr pollution CuInGa powders.
Description
Technical field
The present invention relates to metal alloy field, refers in particular to a kind of method of stirring ball-milling processing CuInGa powders.
Background technology
CIGS（CIGS）Thin film solar cell is because its absorptivity is high, band gap is adjustable, cost is cheap, conversion ratio is high, weak
The advantages that photosensitiveness is good, stable performance and capability of resistance to radiation are strong, and fall over each other the weight of exploitation as current industry circle and research institution
Point.In recent years under its premium properties and great demand background, including the U.S. regenerative resource laboratory NREL, Solar
The nearly numerous corporate facilitys in the whole world such as Frontier, Miasole, Global solar, Wurth Solar put into huge financial resources and
Manpower is researched and developed and produced, and 2011 annual capacities reach GW levels, show good growth momentum.
At present, in order to further reduce copper indium gallium selenide cell production cost, using the antivacuum of the low costs such as spraying, blade coating
Technology is just turning into the emphasis of current research.CIGS thin-film solar cell non-vacuum technique is generally by various physics or change
Method synthesizes nano-powder precursor powder, is then configured to ink, and preceding body is prepared into by the technique such as spraying or scratching
Body thin film, then it is particularly important by selenizing into CIGS thin-film, the handling process of its involved powder.In reality
In the production of border, the large batch of powder of batch processing is generally required, the crushing of primary, i.e., the milli provided by commercial materials provider are provided
The other powder of meter level is ground to micron level powder, then carries out follow-up grinding step processing again.If general ground using manual
Mill, workload will be very large, and repeatability also can be very poor, and wastes time and energy.And it can only be also directed to using planetary type ball-milling
CIGS powder containing selenium.In the attrition grinding processing procedure of CIGS powder, general quaternary CIGS powder, two
First selenides CuSe, Cu2Se、InSe、In2Se3、Ga2Se3And ternary selenides (In1-xGa)2Se3Compare Deng body containing selenium powder itself
It is more crisp, easily grinding, thus planetary type ball-milling etc. can be used to carry out primary breakup, but if alloyed powder using Cu, In, Ga
End is used as precursor, and due to the ductility of In, Ga metal, due to infiltrating sex chromosome mosaicism, powder will be attached to the abrading-balls such as zirconium oxide
On, it will be difficult to milled processed.
The content of the invention
In order to solve the problems, such as that existing grinding technique is difficult to be applied to the alloy powder that Cu, In, Ga are main body, the present invention carries
Gone out a kind of method of stirring ball-milling processing CuInGa alloy powders, can effectively solve alloy powder that Cu, In, Ga are main body and
The infiltration sex chromosome mosaicism of abrading-ball, grinding efficiency is higher, can effectively reduce the impurity elements such as Fe, Cr pollution CuInGa powders.
The technical solution adopted in the present invention is：A kind of method of stirring ball-milling processing CuInGa alloy powders, including such as
Lower step：The other CuInGa metal dusts of grade and grinding aid are mixed into pulvis and load agate pot, adds a diameter of 2-
5mm bead is some, and the tank mouth of agate pot is sealed with baffle plate, and agate pot is stretched into 1000rpm extremely with the stirring-head of translator
1500rpm rotating speed agitation grinding 5 to 10 hours, grinding obtain the CuInGa powders of micron level.
The present invention carries out primary breakup using novel stirring ball-milling, stirring ball-milling can according to feed intake number customize
Capacity and the abrading-ball proportioning of lapping apparatus, the large batch of primary grinding of CuInGa alloy powders can be achieved.Because stirring ball-milling is adopted
Mill ball is driven with stirring-head, rotating speed may be up to 1500 revs/min, thus grinding efficiency can improve than planetary type ball-milling.Meanwhile I
Use agate pot and bead abrading-ball, can effectively solve the infiltration sex chromosome mosaicism of powder and abrading-ball, it is very strong for ductility
CuInGa alloy powders, powder also without being adhered on abrading-ball.Furthermore stainless-steel grinding tank and abrading-ball are in stirring ball-milling process
In easily produce impurity, thus the present invention is ground using agate pot and bead, can effectively reduce the impurity elements such as Fe, Cr
Pollute CuInGa powders.
Preferably, described grinding aid is deionized water.Deionized water is eliminated in after ionic species impurity
Pure water, the doping other impurities for trying one's best few during grinding can make it that.
Preferably, described CuInGa metal dusts include Cu powder, In powder, Ga powder, CuIn alloy powders,
One or more in CuGa alloy powders or CuInGa alloy powders.It present invention can be suitably applied to Cu powder, In powder, Ga powder
At the grinding at end, the monomer powders of CuIn alloy powders, CuGa alloy powders or CuInGa alloy powders composition or mixed-powder
Reason.
Preferably, the stirring-head of the translator is the stainless steel impeller of translator.The stainless steel impeller of translator is borrowed
With the power of motor, powder is realized stable and effectively ground.
Preferably, polytetrafluoroethylene (PTFE) protective case is socketed with the stirring-head of the translator.On the stirring-head of translator
The appearance of impurity in process of lapping can further be reduced by being socketed with polytetrafluoroethylene (PTFE) protective case.
Preferably, described rotating speed is 1300rpm.By experiment, 1300rpm is optimum speed.
Preferably, described milling time is 6 hours.By experiment, 6 hours are optimal milling time.
Preferably, described alloy powder and the mass ratio of bead are 1:5 to 1:10.
Preferably, described alloy powder and the mass ratio of deionized water are 1:3 to 1:10.
The beneficial effects of the invention are as follows：Can effectively solve Cu, In, Ga to ask for the alloy powder of main body and the wellability of abrading-ball
Topic, grinding efficiency is higher, can effectively reduce the impurity elements such as Fe, Cr pollution CuInGa powders.
Brief description of the drawings
Fig. 1 is a kind of structural representation of device therefor of the present invention.
In figure, 1- agate pots, the stirring-head of 2- translators, 3- pulvis, 4- beades.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
Embodiment 1
As shown in figure 1, a kind of method of stirring ball-milling processing CuInGa powders, by the other CuInGa alloys of 30g grades
Powder and 150ml deionized waters as grinding aid 3 are mixed into pulvis 3 and load agate pot 1, add a diameter of 4.5mm of 300g
Bead 4, the tank mouth of agate pot 1 is sealed with baffle plate, agate pot 1 is stretched into 1300rpm rotating speed with the stirring-head 2 of translator
Agitation grinding 6 hours.Wherein the stirring-head 2 of translator is the stainless steel impeller of translator, is socketed with the stirring-head 2 of translator
Polytetrafluoroethylene (PTFE) protective case.By milled processed, the final CuInGa for obtaining diameter range at 0.331 micron to 1.001 microns
Alloy powder.
For CuInGa alloy powders toughness plasticity it is strong, be difficult to the characteristics of grinding, the present invention using novel stirring ball-milling come
Carry out primary breakup.Because stirring ball-milling is using stirring-head drive mill ball, rotating speed can reach 1300 revs/min, thus grind effect
Rate can increase substantially than planetary type ball-milling, under the collective effect of stirring head lobe slurry and abrading-ball, easily smash powder, grind
Carefully.Simultaneously as the ductility of In, Ga metal and the infiltration sex chromosome mosaicism between abrading-ball, it will cause CuInGa metal-powders
It is adhered in process of lapping on abrading-ball.For this difficulties, we are supporting using agate pot and bead abrading-ball
Experimental provision, can effectively solve the infiltration sex chromosome mosaicism of powder and abrading-ball, for the very strong CuInGa alloy powders of ductility, in height
During fast spin finishing, powder also without being adhered on abrading-ball.And the Mohs' hardness of glass marble is also greater than 6, thus will not
Because quality is soft and broken.Furthermore stainless-steel grinding tank and abrading-ball easily produce impurity, thus this hair during stirring ball-milling
It is bright to be ground using agate pot and bead, the impurity elements such as Fe, Cr pollution CuInGa powders can be effectively reduced, are further
Impurity is avoided, the protective case of polytetrafluoroethylene (PTFE) can be loaded onto on the impeller of stainless steel stirring-head, can effectively avoid Fe, Cr etc.
Pollution of the metal impurities to powder.
Embodiment 2
The other CuIn alloy powders of 30g grades and the 300ml deionized waters as grinding aid 3 are mixed into pulvis 3
Load agate pot 1, add a diameter of 2mm of 150g bead 4, the tank mouth of agate pot 1 is sealed with baffle plate, with the stirring of translator
First 2 stretch into agate pot 1 with 1000rpm rotating speed agitation grinding 10 hours, identical in other and embodiment 1, finally obtain diameter
CuIn alloy powder of the scope at 0.636 micron to 1.162 microns.
Embodiment 3
The other CuGa alloy powders of 30g grades and the 90ml deionized waters as grinding aid 3 are mixed into pulvis 3 and filled
Enter agate pot 1, add a diameter of 5mm of 300g bead, the tank mouth of agate pot 1 is sealed with baffle plate, with the stirring-head 2 of translator
Agate pot 1 is stretched into 1500rpm rotating speed agitation grinding 5 hours, it is identical in other and embodiment 1, finally obtain diameter range
In 0.742 micron to 1.348 microns of CuGa alloy powders.
The technological thought of above example only to illustrate the invention, it is impossible to protection scope of the present invention is limited with this, it is every
According to technological thought proposed by the present invention, any change done on the basis of technical scheme, protection model of the invention is each fallen within
Within enclosing.
Claims (8)
- A kind of 1. method of stirring ball-milling processing CuInGa powders, it is characterised in that：Comprise the following steps：Grade is other CuInGa metal dusts and grinding aid are mixed into pulvis and load agate pot, and it is some to add a diameter of 2-5mm bead, with gear Plate seals the tank mouth of agate pot, and agate pot is stretched into 1000rpm to 1500rpm rotating speed agitation grinding with the stirring-head of translator 5 to 10 hours, grinding obtained the CuInGa powders of micron level.
- A kind of 2. method of stirring ball-milling processing CuInGa powders according to claim 1, it is characterised in that：Described grinds Milling aid is deionized water.
- A kind of 3. method of stirring ball-milling processing CuInGa powders according to claim 1, it is characterised in that：It is described powered The stirring-head of machine is the stainless steel impeller of translator.
- A kind of 4. method of stirring ball-milling processing CuInGa powders according to claim 1 or 3, it is characterised in that：It is described Polytetrafluoroethylene (PTFE) protective case is socketed with the stirring-head of translator.
- A kind of 5. method of stirring ball-milling processing CuInGa powders according to claim 1, it is characterised in that：Described turns Speed is 1300rpm.
- A kind of 6. method of stirring ball-milling processing CuInGa powders according to claim 1, it is characterised in that：Described grinds Consume time as 6 hours.
- A kind of 7. method of stirring ball-milling processing CuInGa powders according to claim 1, it is characterised in that：Described conjunction The mass ratio of bronze end and bead is 1:5 to 1:10.
- A kind of 8. method of stirring ball-milling processing CuInGa powders according to claim 1, it is characterised in that：Described conjunction The mass ratio of bronze end and deionized water is 1:3 to 1:10.
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| CN103949649B (en) * | 2014-05-13 | 2016-03-02 | 中南大学 | The method of flake copper is prepared under a kind of water-based system |
| CN109877335B (en) * | 2019-03-12 | 2022-02-22 | 先导薄膜材料（广东）有限公司 | Preparation method of copper indium gallium selenide powder |
| CN110434346B (en) * | 2019-08-26 | 2021-10-26 | 华南理工大学 | Method for refining large-particle-size pure copper or copper alloy particles by high-energy ball milling method |
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| CN1736636A (en) * | 2005-09-12 | 2006-02-22 | 昆明理工恒达科技有限公司 | Low loose density sheet-like silver powder preparation method |
| CN101041183A (en) * | 2007-04-29 | 2007-09-26 | 东北轻合金有限责任公司 | Method of processing un-suspension powdered aluminium |
| WO2010024564A2 (en) * | 2008-08-25 | 2010-03-04 | 주식회사 잉크테크 | Method for manufacturing metal flakes |
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| US5985691A (en) * | 1997-05-16 | 1999-11-16 | International Solar Electric Technology, Inc. | Method of making compound semiconductor films and making related electronic devices |
| US7604843B1 (en) * | 2005-03-16 | 2009-10-20 | Nanosolar, Inc. | Metallic dispersion |
| CN102249549B (en) * | 2011-04-01 | 2013-05-22 | 中南大学 | Copper-indium-selenium photovoltaic film, powder and coating material for solar batteries and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736636A (en) * | 2005-09-12 | 2006-02-22 | 昆明理工恒达科技有限公司 | Low loose density sheet-like silver powder preparation method |
| CN101041183A (en) * | 2007-04-29 | 2007-09-26 | 东北轻合金有限责任公司 | Method of processing un-suspension powdered aluminium |
| WO2010024564A2 (en) * | 2008-08-25 | 2010-03-04 | 주식회사 잉크테크 | Method for manufacturing metal flakes |
| CN102202820A (en) * | 2008-08-25 | 2011-09-28 | 印可得株式会社 | Method for manufacturing metal flakes |
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