CN104532012A - Method for recycling gallium and gold from gallium nitride chip production wastes - Google Patents

Method for recycling gallium and gold from gallium nitride chip production wastes Download PDF

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CN104532012A
CN104532012A CN201410785130.0A CN201410785130A CN104532012A CN 104532012 A CN104532012 A CN 104532012A CN 201410785130 A CN201410785130 A CN 201410785130A CN 104532012 A CN104532012 A CN 104532012A
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gallium
gold
nitride chip
gallium nitride
processing waste
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CN104532012B (en
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詹路
夏发发
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East China Normal University
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East China Normal University
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses a method for recycling gallium and gold from gallium nitride chip production wastes. The method disclosed by the invention comprises the following steps of crushing the gallium nitride chip production wastes, carrying out vacuum metallurgy separation of obtained particles containing gallium and gold, and recycling to obtain elementary gallium and gold. The method disclosed by the invention is capable of effectively recycling gallium and gold from gallium nitride chip production wastes, has the outstanding advantages of reducing environmental pollution and increasing the resource utilization rate, and has the characteristics of low cost, high efficiency, no pollution and the like.

Description

The method of gallium, gold is reclaimed from gallium nitride chip processing waste
Technical field
The present invention relates to a kind of method of Footwall drift gallium, gold from gallium nitride chip processing waste, belong to the recovery of metal, regeneration, resource technology field.
Background technology
Photodiode is the one in conventional electronic component diode, is a kind of a kind of device that electric energy can be become luminous energy, belongs to solid state light emitter.Current photodiode is widely used in research and production field, mainly comprises general illumination, landscape ornamental illumination, large screen display, backlight display, traffic signals display, auto lamp, road lighting etc.And the key of semiconductor lighting is its luminescence chip, mainly contain gallium arsenide and gan two kinds of chips at present, chip production mainly contains epitaxial wafer growth, makes the production links such as electrode, thinning, scribing, test, due to the restriction of state of the art, production process inevitably produces scrap stock and defect ware; Wherein the recovery of gallium arsenide chips processing waste is conducted extensive research and applied, such as vacuum method (Liu great Chun, Yang Bin etc., 2004), pickling process (Chen, W.T.; Tsai, L.C. etc., 2012), organic solvent extraction (Ahmed, I.; El-Nadi, Y. etc., 2013), ion-exchange (Filik, H.; Apak, R., 1998) and supercritical extraction (Chou, W.-L.; Wang, C.-T. etc., 2008) method such as.
And also rarely have people to set foot in for the recovery of gallium nitride chip processing waste, also be only to reclaiming containing gallium, ammonia-containing exhaust in production process in patent " blue light led epitaxy of gallium nitride process tail gas recycle (CN103130245A) ", and solids manufacture waste material is not adopted an effective measure.Owing to chip there being the electrode contacts of gold system, the mode that most of chip fabricators all takes chloroazotic acid to leach reclaims gold wherein, and effectively do not reclaimed as the gallium of chip main raw, and in leaching technology, producing acid waste water, environmental pollution is serious.In view of gallium nitride based light emitting diode is as most potential lighting system, its research and apply receives the extensive attention of national governments and supports energetically, progressively replaces conventional illumination sources at present, and the following gallium nitride chip market requirement has a extensive future.
Summary of the invention
The object of the invention is to solve the wasting of resources and problem of environmental pollution that gallium nitride chip processing waste causes, propose a kind of enriching and recovering method of gallium, gold in efficient, environmental protection, green gallium nitride chip processing waste, make gallium, gold is able to high efficiente callback, achieve the recovery of gallium nitride chip processing waste, regeneration and recycling treatment.
The present invention reclaims the method for gallium, gold from gallium nitride chip processing waste, to gallium nitride chip processing waste break process, the particulate matter containing gallium, golden composition obtained is carried out vacuum metallurgy recovery.
In recovery method of the present invention, under suitable operating parameters, the rate of recovery of gallium reaches more than 95%, and purity reaches more than 90%; The rate of recovery of gold reaches more than 95%, and purity is greater than 80%.In removal process of the present invention, the metal in gallium nitride chip processing waste all obtains efficient resourceization and reclaims.
The present invention reclaims in the method for gallium, gold from gallium nitride chip processing waste, adopts the process of vacuum metallurgy separation method to contain the particulate matter of gallium, golden composition, reclaims and obtain Metallic Gallium, gold; Described recovery method comprises the following steps:
(1) fragmentation of gallium nitride chip processing waste is obtained the particulate matter containing gallium, golden composition;
(2) particulate matter that step (1) obtains is placed in high-temperature crucible, then crucible is put into vacuum oven;
(3) start vacuum system after vacuum oven sealing to bleed, make the pressure of vacuum oven be 0.01 ~ 1.0Pa;
(4) start vacuum furnace power supply, the sample in crucible is heated to 1000 ~ 1300 DEG C, then keeps temperature-resistant, make fully decomposing containing gallium compound in raw material, gallium, gold fully evaporate, soaking time is 1.0 ~ 3.0h;
(5) gallium, golden steam are able to condensation respectively on condenser, reclaim and obtain Metallic Gallium, gold.
In described step (1), gallium nitride chip processing waste is carried out fragmentation, the particle diameter of the particulate matter that fragmentation obtains is 0.05-0.15mm.
In described step (5), the condensing temperature interval of gallium is 450 ~ 850 DEG C, and the rate of recovery of gallium reaches more than 95%, and purity is greater than 90%.The condensing temperature interval of gold is 750 ~ 1150 DEG C, and the rate of recovery of gold reaches more than 95%, and purity is greater than 80%.
In described step (5), remaining residue is mainly silicon-dioxide, and it can be used for preparing quartz ware.
In the present invention, described " gallium nitride chip processing waste " refers in epitaxial wafer growth, makes scrap stock and defect ware that the production links such as electrode, thinning, scribing and test produce.
Recovery method of the present invention, makes gallium, gold in gallium nitride chip processing waste obtain effective regeneration, namely facilitates the recycle of resource, decreases processing waste itself and conventional recovery method to the pollution of environment.In gallium nitride chip processing waste of the present invention, the recovery method of gallium, gold, has the features such as cost is low, efficient, pollution-free; Each component in gallium nitride chip processing waste is obtained for appropriate disposal of resources; Compare the method that tradition such as adopting acidleach reclaims valuable metal in electron wastes, recovery method of the present invention especially has advantage in minimizing environmental pollution and energy-saving and emission-reduction.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that the present invention reclaims gallium, golden method from gallium nitride chip processing waste.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Under the spirit and scope not deviating from inventive concept, the change that those skilled in the art can expect and advantage are all included in the present invention, and are protection domain with appending claims.Implement process of the present invention, condition, reagent, experimental technique etc., except the following content mentioned specially, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
Fig. 1 is the schematic diagram of gallium in gallium nitride chip processing waste of the present invention, golden recovery method.As shown in Figure 1, first gallium nitride chip processing waste is through broken, and the particle diameter of the mixture after fragmentation is 0.05-0.15mm; Described mixture is the particulate matter containing gallium, golden composition; Then, particulate matter containing gallium, golden composition is separated through vacuum metallurgy partition method, under suitable operating parameters, obtain gallium (purity >90%) and metallic gold (purity >80%).
Wherein, " gallium nitride chip processing waste " refers in epitaxial wafer growth, makes scrap stock and defect ware that the production links such as electrode, thinning, scribing and test produce.
Wherein, " suitable operating parameters " refers to system pressure 0.01 ~ 1.0Pa, Heating temperature 1000 ~ 1300 DEG C, soaking time 1.0 ~ 3.0h.
Embodiment 1
First gallium nitride chip processing waste is broken into the particulate matter that particle diameter is 0.05-0.08mm, then, the particulate matter obtained is put into crucible, then crucible is put into vacuum oven.Start vacuum system after vacuum oven sealing to bleed, the vacuum tightness of vacuum oven is between 0.05-0.08Pa.Start the heating member heating crucible in vacuum oven, particulate matter in crucible is heated to 1100 DEG C.Then keep temperature-resistant, make gallium in raw material, gold fully evaporates, evaporation time is 2.0 hours.Gallium steam is able to condensation on condenser, and in the present embodiment, the condensing temperature interval of gallium steam is 480 ~ 785 DEG C, and the rate of recovery of gallium is 95.7%, and purity is 92.3%; The condensation on condenser of gold steam, in the present embodiment, the condensing temperature interval of golden steam is 785 ~ 1050 DEG C, and the rate of recovery of gold is 95.3%, and purity is 81.4%.
In the inventive method, the condensing temperature interval of gallium is suitable for the temperature range of 450 ~ 850 DEG C, and the condensing temperature interval of gold is suitable for the temperature range of 750 ~ 1150 DEG C, all can realize the recovery of Metallic Gallium, elemental gold within the scope of said temperature.Gallium is chosen with golden condensing temperature interval, unrestricted mutually.
Embodiment 2
First gallium nitride chip processing waste is broken into the particulate matter that particle diameter is 0.06-0.10mm, then, the particulate matter obtained is put into crucible, then crucible is put into vacuum oven.Start vacuum system after vacuum oven sealing to bleed, the vacuum tightness of vacuum oven is between 0.07-0.1Pa.Start the heating member heating crucible in vacuum oven, particulate matter in crucible is heated to 1250 DEG C.Then keep temperature-resistant, make gallium in raw material, gold fully evaporates, evaporation time is 2.5 hours.Gallium steam is able to condensation on condenser, and in the present embodiment, the condensing temperature interval of gallium steam is 570 ~ 820 DEG C, and the rate of recovery of gallium is 96.1%, and purity is 93.1%; The condensation on condenser of gold steam, in the present embodiment, the condensing temperature interval of golden steam is 820 ~ 1113 DEG C, and the rate of recovery of gold is 96.2%, and purity is 82.4%.
Embodiment 3
First gallium nitride chip processing waste is broken into the particulate matter that particle diameter is 0.09-0.12mm, then, the particulate matter obtained is put into crucible, then crucible is put into vacuum oven.Start vacuum system after vacuum oven sealing to bleed, the vacuum tightness of vacuum oven is between 0.1-1.0Pa.Start the heating member heating crucible in vacuum oven, particulate matter in crucible is heated to 1300 DEG C.Then keep temperature-resistant, make gallium in raw material, gold fully evaporates, evaporation time is 3.0 hours.Gallium steam is able to condensation on condenser, and in the present embodiment, the condensing temperature interval of gallium steam is 610 ~ 850 DEG C, and the rate of recovery of gallium is 95.1%, and purity is 91.7%; The condensation on condenser of gold steam, in the present embodiment, the condensing temperature interval of golden steam is 850 ~ 1150 DEG C, and the rate of recovery of gold is 95.7%, and purity is 81.6%.
Embodiment 4
First gallium nitride chip processing waste is broken into the particulate matter that particle diameter is 0.11-0.15mm, then, the particulate matter obtained is put into crucible, then crucible is put into vacuum oven.Start vacuum system after vacuum oven sealing to bleed, the vacuum tightness of vacuum oven is between 0.01-0.05Pa.Start the heating member heating crucible in vacuum oven, particulate matter in crucible is heated to 1000 DEG C.Then keep temperature-resistant, make gallium in raw material, gold fully evaporates, evaporation time is 1.0 hours.Gallium steam is able to condensation on condenser, and in the present embodiment, the condensing temperature interval of gallium steam is 450 ~ 750 DEG C, and the rate of recovery of gallium is 98.7%, and purity is 96.2%; The condensation on condenser of gold steam, in the present embodiment, the condensing temperature interval of golden steam is 750 ~ 960 DEG C, and the rate of recovery of gold is 98.8%, and purity is 84.2%.

Claims (6)

1. from gallium nitride chip processing waste, reclaim a method for gallium, gold, it is characterized in that, by gallium nitride chip processing waste through broken, the particulate matter containing gallium, golden composition obtained is carried out vacuum metallurgy separation, reclaims and obtain Metallic Gallium and gold.
2. from gallium nitride chip processing waste, reclaim the method for gallium, gold as claimed in claim 1, it is characterized in that,
(1) fragmentation of gallium nitride chip processing waste is obtained particulate matter;
(2) particulate matter that step (1) obtains is placed in high-temperature crucible, crucible is put into vacuum oven;
(3) start vacuum system after vacuum oven sealing to bleed, make the pressure of vacuum oven be 0.01 ~ 1.0Pa;
(4) start vacuum furnace power supply, the sample in crucible is heated to 1000 ~ 1300 DEG C, then keeps temperature-resistant, make fully decomposing containing gallium compound in material, gallium, gold fully evaporate, soaking time is 1.0 ~ 3.0h;
(5) gallium, golden steam are able to condensation respectively on condenser, reclaim and obtain Metallic Gallium, gold.
3. from gallium nitride chip processing waste, reclaim the method for gallium, gold as claimed in claim 2, it is characterized in that, in described step (1), the particle diameter of described particulate matter is 0.05-0.15mm.
4. from gallium nitride chip processing waste, reclaim the method for gallium, gold as claimed in claim 2, it is characterized in that, in described step (5), the condensing temperature interval of gallium is 450 ~ 850 DEG C, the rate of recovery of described gallium reaches more than 95%, and purity is greater than 90%.
5. from gallium nitride chip processing waste, reclaim the method for gallium, gold as claimed in claim 2, it is characterized in that, in described step (5), the condensing temperature interval of gold is 750 ~ 1150 DEG C, the rate of recovery of described gold reaches more than 95%, and purity is greater than 80%.
6. recovery method as claimed in claim 2, is characterized in that, in described step (5), residue obtainedly comprises silicon-dioxide.
CN201410785130.0A 2014-12-17 2014-12-17 Produce from gallium nitride chip and waste material reclaims gallium, the method for gold Expired - Fee Related CN104532012B (en)

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Cited By (5)

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CN107267758A (en) * 2017-06-01 2017-10-20 华东师范大学 Recovery indium, the method for silver from the waste and old component of Hall containing indium
CN109055782A (en) * 2018-08-24 2018-12-21 华南理工大学 The leaching method of gallium in a kind of useless light emitting diode
TWI663001B (en) * 2017-07-24 2019-06-21 Dayeh University Method for recovering waste light-emitting diode grains
CN113652559A (en) * 2021-08-20 2021-11-16 安徽工业大学 Method for recovering rare and scattered metal gallium in gallium nitride waste material by pyrogenic process
CN115101636A (en) * 2022-08-24 2022-09-23 江苏第三代半导体研究院有限公司 Composite micro-nano semiconductor structure, preparation method and application thereof

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CN103276407A (en) * 2013-05-13 2013-09-04 攀枝花学院 Method for recovering gallium and iron from low-grade raw materials containing gallium and iron
CN203329414U (en) * 2013-05-08 2013-12-11 珠海经济特区方源有限公司 Absorbing tower for absorbing metal substances in electrolytic tail liquid
CN104017995A (en) * 2014-06-24 2014-09-03 株洲冶炼集团股份有限公司 Method for recycling copper, indium, gallium and selenium from indium gallium selenium wastes containing copper

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CN1598016A (en) * 2004-07-19 2005-03-23 昆明理工大学 Process for comprehensive recovering gallium and arsenic from industrial waste material of gallium arsenide
JP5133547B2 (en) * 2006-09-29 2013-01-30 古河機械金属株式会社 Purification method of gallium
CN101413066A (en) * 2008-10-29 2009-04-22 南京金美镓业有限公司 Vacuum decomposing method for separating gallium arsenide as metal gallium and metal arsenic
CN203329414U (en) * 2013-05-08 2013-12-11 珠海经济特区方源有限公司 Absorbing tower for absorbing metal substances in electrolytic tail liquid
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Publication number Priority date Publication date Assignee Title
CN107267758A (en) * 2017-06-01 2017-10-20 华东师范大学 Recovery indium, the method for silver from the waste and old component of Hall containing indium
CN107267758B (en) * 2017-06-01 2018-11-09 华东师范大学 The method of recovery indium, silver from the waste and old component of Hall containing indium
TWI663001B (en) * 2017-07-24 2019-06-21 Dayeh University Method for recovering waste light-emitting diode grains
CN109055782A (en) * 2018-08-24 2018-12-21 华南理工大学 The leaching method of gallium in a kind of useless light emitting diode
CN113652559A (en) * 2021-08-20 2021-11-16 安徽工业大学 Method for recovering rare and scattered metal gallium in gallium nitride waste material by pyrogenic process
CN113652559B (en) * 2021-08-20 2022-07-29 安徽工业大学 Method for recovering rare and scattered metal gallium in gallium nitride waste material by pyrogenic process
CN115101636A (en) * 2022-08-24 2022-09-23 江苏第三代半导体研究院有限公司 Composite micro-nano semiconductor structure, preparation method and application thereof
CN115101636B (en) * 2022-08-24 2022-12-02 江苏第三代半导体研究院有限公司 Composite micro-nano semiconductor powder structure, preparation method and application thereof

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