CN108754435A - A kind of recovery method of copper indium gallium selenide waste material - Google Patents
A kind of recovery method of copper indium gallium selenide waste material Download PDFInfo
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- CN108754435A CN108754435A CN201810622869.8A CN201810622869A CN108754435A CN 108754435 A CN108754435 A CN 108754435A CN 201810622869 A CN201810622869 A CN 201810622869A CN 108754435 A CN108754435 A CN 108754435A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
An embodiment of the present invention provides a kind of recovery method of copper indium gallium selenide waste material, the method includes：Copper indium gallium selenide waste material is evaporated in vacuo, separation obtains selenium and distillation waste material；The distillation waste material is restored, copper and indium gallium target raw material is obtained；Using the technique of vacuum distillation separation selenium, the boiling point of selenium only has 685 DEG C, boiling point than three kinds of elements of copper and indium gallium is much lower, vacuum distillation separation selenium can be used, remaining distillation waste material is mainly that copper and indium gallium also has a small amount of oxide, and the higher copper and indium gallium target raw material of purity can be obtained with the mode that hydrogen reduction is handled.Copper and indium gallium ternary component need not chemically separating-purifying again, it is directly used as target raw material after hydrogen reduction processing, it is reduced or avoided and leaches material using chemical reagent, keep production technology more environmentally friendly, shorten technological process, production efficiency and the rate of recovery are improved, acid extracting is solved and the existing wastewater flow rate that generates of sulfating roasting method is big, the problem that technological process is long, organic efficiency is low and cost recovery is high.
Description
Technical field
The present invention relates to metal and Nonmetal waste recovery technology fields, more particularly to a kind of returning for copper indium gallium selenide waste material
Receiving method.
Background technology
Copper-indium-galliun-selenium film solar cell be it is a kind of efficiently, easily solar cell, it and currently marketed crystalline substance
Silicon solar cell is compared with the advantages such as flexible, high conversion rate, applied widely, is the master of the following theCourse of PV Industry
Stream.Copper indium gallium selenium solar cell will produce a large amount of defective material in the production process, in these defective materials other than copper indium gallium selenide
Impurities are less, have prodigious recovery value.Have for the current recovery method of this material：Sulfating roasting method, acid
Molten method etc..
Sulfating roasting is to use sulfuric acid baking copper indium gallium selenide waste material, absorbs recycling selenium with lye, then go out copper and indium gallium with water logging.
Acid extracting mainly adds hydrogen peroxide to leach copper indium gallium selenide waste material with sulfuric acid, then is separated and recovered with the methods of reduction, chemical precipitation, extraction
Copper indium gallium selenide.
Acid extracting and sulfating roasting method are the problem is that the waste water generated is more, pollutes the environment, extraction and separation
Method operating environment is poor, technological process is long, the recovery process operating process that above-mentioned method combines is long, organic efficiency is low,
It is of high cost.
Invention content
The embodiment of the present invention provides a kind of recovery method of copper indium gallium selenide waste material, to solve acid extracting and sulfating roasting method
In conjunction with recovery process operating process is long, organic efficiency is low, the of high cost above problem.
To solve the above-mentioned problems, the embodiment of the invention discloses a kind of recovery method of copper indium gallium selenide waste material, the sides
Method includes：
Copper indium gallium selenide waste material is evaporated in vacuo, separation obtains selenium and distillation waste material；
The distillation waste material is restored, copper and indium gallium target raw material is obtained.
Preferably, described that copper indium gallium selenide waste material is evaporated in vacuo, separation obtains selenium and distillation waste material, including：
Copper indium gallium selenide waste material is evaporated in vacuo, selenium steam and distillation waste material are obtained；
The selenium steam is condensed by condensing unit, obtains selenium.
Preferably, described that the distillation waste material is restored, copper and indium gallium target raw material is obtained, including：
Distillation waste material is passed through hydrogen and carries out reduction reaction, obtains copper and indium gallium target raw material.
Preferably, the method further includes：
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure, obtains copper and indium gallium target.
Preferably, described that copper indium gallium selenide waste material is evaporated in vacuo, separation obtains selenium and distillation waste material, including：
Copper indium gallium selenide waste material is evaporated in vacuo according to default distillation condition, separation obtains selenium and distillation waste material.
Preferably, it is 10Pa to 20Pa that the default distillation condition, which includes vacuum degree,；Vapo(u)rizing temperature is 400 DEG C to 600 DEG C；
Distillation time is 2 hours to 3 hours.
Preferably, described to be condensed the selenium steam by condensing unit, selenium is obtained, including：
The selenium steam is condensed by condensing unit according to default condensing condition, obtains selenium.
Preferably, it is 50 DEG C to 150 DEG C that the default condensing condition, which includes condensation temperature,.
Preferably, described that distillation waste material is passed through hydrogen progress reduction reaction, copper and indium gallium target raw material is obtained, including：
Waste material will be distilled according to default reducing condition and is passed through hydrogen progress reduction reaction, obtain copper and indium gallium target raw material.
Preferably, it is 500 DEG C to 600 DEG C that the default reducing condition, which includes reduction temperature,；Recovery time is 2 hours to 3
Hour.
The embodiment of the present invention includes following advantages：
In the embodiment of the present invention, using the technique of vacuum distillation separation selenium, the boiling point of selenium only has 685 DEG C, than copper and indium gallium three
The boiling point of kind of element is much lower, can be used vacuum distillation separation selenium, remaining distillation waste material be mainly copper and indium gallium also have it is a small amount of
The higher copper and indium gallium target raw material of purity can be obtained with the mode that hydrogen reduction is handled in oxide.Copper and indium gallium ternary component does not need
Chemically separating-purifying, hydrogen reduction are directly used as target raw material after handling, are reduced or avoided and are leached using chemical reagent again
Material keeps production technology more environmentally friendly, shortens technological process, improves production efficiency and the rate of recovery, solve acid extracting and sulfuric acid
The existing generation wastewater flow rate of change roasting method is big, and the operating environment of extraction separating method is poor, technological process is long, organic efficiency is low and returns
Receive problem of high cost.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, other are can also be obtained according to these attached drawings
Attached drawing
Fig. 1 is a kind of flow chart of the recovery method of copper indium gallium selenide waste material of the embodiment of the present invention.
Specific implementation mode
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, below in conjunction with the accompanying drawings and specific real
Applying mode, the present invention is described in further detail.
Referring to Fig.1, it illustrates a kind of flow chart of the recovery method of copper indium gallium selenide waste material described in the embodiment of the present invention,
The method includes：
Step 101, copper indium gallium selenide waste material is evaporated in vacuo, separation obtains selenium and distillation waste material；
In the embodiment of the present invention, the boiling point of selenium only has 685 DEG C, and the boiling point than three kinds of elements of copper and indium gallium is much lower, according to selenium
Low boiling dot characteristics, the mode that vacuum distillation can be used detaches selenium, i.e., copper indium gallium selenide waste material is put into vacuum drying oven and distilled,
Selenium steam is obtained first, and remaining distillation waste material is mainly copper and indium gallium ternary component and a small amount of oxide.
Specifically, copper indium gallium selenide waste material is evaporated in vacuo according to default distillation condition, separation obtains selenium and distillation
Waste material；Wherein, it is 10Pa to 20Pa that the default distillation condition, which includes vacuum degree,；Vapo(u)rizing temperature is 400 DEG C to 600 DEG C；Distillation
Time is 2 hours to 3 hours, and certainly, one of the citing of the only embodiment of the present invention of above-mentioned default distillation condition, this is default
Distillation condition can be any condition that those skilled in the art set according to actual conditions, and the embodiment of the present invention does not make this
Limitation.
It is further applicable in the embodiment of the present invention, the selenium steam is condensed, obtain selenium；Specifically, by cold
Solidifying device, such as condenser condense the selenium steam, obtain selenium；It should be noted that can be according to default condensing condition
The selenium steam is condensed by condensing unit, wherein the default condensing condition includes that condensation temperature is 50 DEG C to 150
℃；Certainly, one of the citing of the only embodiment of the present invention of above-mentioned default condensing condition, which can be this
Any condition that field technology personnel set according to actual conditions, the embodiment of the present invention are not restricted this.
It should be noted that handling the technique of copper indium gallium selenide waste material with vacuum distillation method, selenium recovery is high, distills
Selenium purity is high.
Step 102, the distillation waste material is restored, obtains copper and indium gallium target raw material.
It is specifically applied in the embodiment of the present invention, the distillation waste material can be restored, it is former to obtain copper and indium gallium target
Material, it is available with the mode of hydrogen reduction because the selenium in copper indium gallium selenide waste material is separated by way of vacuum distillation
The higher copper and indium gallium target raw material of purity, need not chemically separating-purifying again, be directly used as target after hydrogen reduction processing
Raw material is reduced or avoided and leaches material using chemical reagent, keeps production technology more environmentally friendly, shortens technological process.
In a step 102, distillation waste material can be passed through hydrogen and carries out reduction reaction, obtain copper and indium gallium target raw material；Tool
Body, it is put into hydrogen reduction furnace according to default reducing condition by waste material is distilled, is passed through hydrogen and carries out reduction reaction, it is described to preset also
Old terms includes that reduction temperature is 500 DEG C to 600 DEG C；Recovery time is 2 hours to 3 hours.
It should be noted that the method further includes：The copper and indium gallium target raw material is crushed, copper and indium gallium gold is obtained
Belong to powder；The copper and indium gallium metal powder is suppressed under the conditions of preset pressure, obtains copper and indium gallium target.
It can be directed to the processing that copper and indium gallium target raw material makees a step, obtaining copper and indium gallium target specifically can be by copper and indium
Gallium target raw material is crushed, it is preferable that can be ground copper and indium gallium target raw material, be obtained the copper and indium gallium gold of certain mesh number
Belong to powder, such as the copper and indium gallium metal powder of 350 mesh to 450 mesh, the embodiment of the present invention are not restricted this；Further, by this
Copper and indium gallium metal powder is added in target model well prepared in advance and is suppressed with preset pressure, and copper and indium gallium target is obtained；It needs
It is noted that the copper and indium gallium target can be used for making the light absorbing layer of thin-film solar cells；May be used hydraulic press into
The compacting of row target, preset pressure can be any numerical value that those skilled in the art set according to actual conditions, for example, in advance
If pressure can be 140 tons to 160 tons.
In the embodiment of the present invention, using the technique of vacuum distillation separation selenium, the boiling point of selenium only has 685 DEG C, than copper and indium gallium three
The boiling point of kind of element is much lower, can be used vacuum distillation separation selenium, remaining distillation waste material be mainly copper and indium gallium also have it is a small amount of
The higher copper and indium gallium target raw material of purity can be obtained with the mode that hydrogen reduction is handled in oxide.Copper and indium gallium ternary component does not need
Chemically separating-purifying, hydrogen reduction are directly used as target raw material after handling, are reduced or avoided and are leached using chemical reagent again
Material keeps production technology more environmentally friendly, shortens technological process, improves production efficiency and the rate of recovery, solve acid extracting and sulfuric acid
The existing generation wastewater flow rate of change roasting method is big, and the operating environment of extraction separating method is poor, technological process is long, organic efficiency is low and returns
Receive problem of high cost.
To make those skilled in the art more fully understand the present invention, illustrate this hair below by way of multiple specific embodiments
The recovery method of the copper indium gallium selenide waste material of bright embodiment.
Embodiment 1
Copper indium gallium selenide waste material is evaporated in vacuo, the vacuum degree of vacuum drying oven is 10Pa, and vapo(u)rizing temperature is 400 DEG C, distillation
Time is 2 hours, obtains selenium steam and distillation waste material；
Selenium steam is condensed to obtain selenium by condenser, condensation temperature is 50 DEG C；Gained selenium purity is more than 99.99%, returns
Yield > 99%；
Above-mentioned distillation waste material is put into hydrogen reduction furnace, hydrogen is passed through and carries out reduction reaction, reduction temperature is 500 DEG C, also
The former time is 2 hours, obtains copper and indium gallium target raw material；Impurity content < 0.001% in copper and indium gallium target raw material；
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；The copper and indium gallium metal powder
Mesh number is 350 mesh；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure is 140 tons, obtains copper and indium gallium target.
Embodiment 2
Copper indium gallium selenide waste material is evaporated in vacuo, the vacuum degree of vacuum drying oven is 20Pa, and vapo(u)rizing temperature is 600 DEG C, distillation
Time is 3 hours, obtains selenium steam and distillation waste material；
Selenium steam is condensed to obtain selenium by condenser, condensation temperature is 150 DEG C；Gained selenium purity is more than 98%, recycling
Rate > 99%；
Above-mentioned distillation waste material is put into hydrogen reduction furnace, hydrogen is passed through and carries out reduction reaction, reduction temperature is 600 DEG C, also
The former time is 3 hours, obtains copper and indium gallium target raw material；Impurity content < 0.001% in copper and indium gallium target raw material；
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；The copper and indium gallium metal powder
Mesh number is 450 mesh；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure is 160 tons, obtains copper and indium gallium target.
Embodiment 3
Copper indium gallium selenide waste material is evaporated in vacuo, the vacuum degree of vacuum drying oven is 12Pa, and vapo(u)rizing temperature is 450 DEG C, distillation
Time is 2.3 hours, obtains selenium steam and distillation waste material；
Selenium steam is condensed to obtain selenium by condenser, condensation temperature is 70 DEG C；Distillation gained selenium purity is more than
99.99%, rate of recovery > 96%；
Above-mentioned distillation waste material is put into hydrogen reduction furnace, hydrogen is passed through and carries out reduction reaction, reduction temperature is 530 DEG C, also
The former time is 2.3 hours, obtains copper and indium gallium target raw material；Impurity content < 0.001% in copper and indium gallium target raw material；
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；The copper and indium gallium metal powder
Mesh number is 380 mesh；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure is 143 tons, obtains copper and indium gallium target.
Embodiment 4
Copper indium gallium selenide waste material is evaporated in vacuo, the vacuum degree of vacuum drying oven is 15Pa, and vapo(u)rizing temperature is 500 DEG C, distillation
Time is 2.5 hours, obtains selenium steam and distillation waste material；
Selenium steam is condensed to obtain selenium by condenser, condensation temperature is 100 DEG C；Distillation gained selenium purity is more than
99.99%, rate of recovery > 98%；
Above-mentioned distillation waste material is put into hydrogen reduction furnace, hydrogen is passed through and carries out reduction reaction, reduction temperature is 550 DEG C, also
The former time is 2.5 hours, obtains copper and indium gallium target raw material；Impurity content < 0.001% in copper and indium gallium target raw material；
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；The copper and indium gallium metal powder
Mesh number is 400 mesh；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure is 150 tons, obtains copper and indium gallium target.
Embodiment 5
Copper indium gallium selenide waste material is evaporated in vacuo, the vacuum degree of vacuum drying oven is 18Pa, and vapo(u)rizing temperature is 550 DEG C, distillation
Time is 2.8 hours, obtains selenium steam and distillation waste material；
Selenium steam is condensed to obtain selenium by condenser, condensation temperature is 120 DEG C；Distillation gained selenium purity is more than
99.99%, rate of recovery > 97%；
Above-mentioned distillation waste material is put into hydrogen reduction furnace, hydrogen is passed through and carries out reduction reaction, reduction temperature is 580 DEG C, also
The former time is 2.8 hours, obtains copper and indium gallium target raw material；Impurity content < 0.001% in copper and indium gallium target raw material；
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；The copper and indium gallium metal powder
Mesh number is 430 mesh；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure is 155 tons, obtains copper and indium gallium target.
Although the preferred embodiment of the embodiment of the present invention has been described, once a person skilled in the art knows bases
This creative concept, then additional changes and modifications can be made to these embodiments.So the following claims are intended to be interpreted as
Including preferred embodiment and fall into all change and modification of range of embodiment of the invention.
Finally, it is to be noted that, herein, relational terms such as first and second and the like be used merely to by
One entity or operation are distinguished with another entity or operation, without necessarily requiring or implying these entities or operation
Between there are any actual relationship or orders.Moreover, the terms "include", "comprise" or its any other variant meaning
Covering non-exclusive inclusion, so that the process, method, article or equipment including a series of elements includes not only that
A little elements, but also include other elements that are not explicitly listed, or further include for this process, method, article or
The intrinsic element of equipment.In the absence of more restrictions, the element limited by sentence "including a ...", is not arranged
Except there is also other identical elements in the process, method, article or apparatus that includes the element.
Above to a kind of recovery method of copper indium gallium selenide waste material provided by the present invention, it is described in detail, herein
Applying specific case, principle and implementation of the present invention are described, and the explanation of above example is only intended to help
Understand the method and its core concept of the present invention；Meanwhile for those of ordinary skill in the art, according to the thought of the present invention,
There will be changes in the specific implementation manner and application range, in conclusion the content of the present specification should not be construed as to this
The limitation of invention.
Claims (10)
1. a kind of recovery method of copper indium gallium selenide waste material, which is characterized in that the method includes：
Copper indium gallium selenide waste material is evaporated in vacuo, separation obtains selenium and distillation waste material；
The distillation waste material is restored, copper and indium gallium target raw material is obtained.
2. the recovery method of copper indium gallium selenide waste material according to claim 1, which is characterized in that described by copper indium gallium selenide waste material
It being evaporated in vacuo, separation obtains selenium and distillation waste material, including：
Copper indium gallium selenide waste material is evaporated in vacuo, selenium steam and distillation waste material are obtained；
The selenium steam is condensed by condensing unit, obtains selenium.
3. the recovery method of copper indium gallium selenide waste material according to claim 1 or 2, which is characterized in that described to the distillation
Waste material is restored, and copper and indium gallium target raw material is obtained, including：
Distillation waste material is passed through hydrogen and carries out reduction reaction, obtains copper and indium gallium target raw material.
4. the recovery method of copper indium gallium selenide waste material according to claim 1 or 2, which is characterized in that the method further includes：
The copper and indium gallium target raw material is crushed, copper and indium gallium metal powder is obtained；
The copper and indium gallium metal powder is suppressed under the conditions of preset pressure, obtains copper and indium gallium target.
5. the recovery method of copper indium gallium selenide waste material according to claim 1, which is characterized in that described by copper indium gallium selenide waste material
It being evaporated in vacuo, separation obtains selenium and distillation waste material, including：
Copper indium gallium selenide waste material is evaporated in vacuo according to default distillation condition, separation obtains selenium and distillation waste material.
6. the recovery method of copper indium gallium selenide waste material according to claim 5, which is characterized in that the default distillation condition packet
It is 10Pa to 20Pa to include vacuum degree；Vapo(u)rizing temperature is 400 DEG C to 600 DEG C；Distillation time is 2 hours to 3 hours.
7. the recovery method of copper indium gallium selenide waste material according to claim 2, which is characterized in that described to be incited somebody to action by condensing unit
The selenium steam is condensed, and selenium is obtained, including：
The selenium steam is condensed by condensing unit according to default condensing condition, obtains selenium.
8. the recovery method of copper indium gallium selenide waste material according to claim 7, which is characterized in that the default condensing condition packet
It is 50 DEG C to 150 DEG C to include condensation temperature.
9. the recovery method of copper indium gallium selenide waste material according to claim 3, which is characterized in that described to be passed through distillation waste material
Hydrogen carries out reduction reaction, obtains copper and indium gallium target raw material, including：
Waste material will be distilled according to default reducing condition and is passed through hydrogen progress reduction reaction, obtain copper and indium gallium target raw material.
10. the recovery method of copper indium gallium selenide waste material according to claim 9, which is characterized in that the default reducing condition
It it is 500 DEG C to 600 DEG C including reduction temperature；Recovery time is 2 hours to 3 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109777966A (en) * | 2019-03-04 | 2019-05-21 | 昆明理工大学 | A method of vacuum distillation separating indium copper alloy |
-
2018
- 2018-06-15 CN CN201810622869.8A patent/CN108754435A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109777966A (en) * | 2019-03-04 | 2019-05-21 | 昆明理工大学 | A method of vacuum distillation separating indium copper alloy |
| CN109777966B (en) * | 2019-03-04 | 2020-11-17 | 昆明理工大学 | Method for separating indium-copper alloy by vacuum distillation |
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Application publication date: 20181106 |