CN113174487A - Recovery method of aluminum residual target for liquid crystal panel - Google Patents
Recovery method of aluminum residual target for liquid crystal panel Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 107
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- 238000000034 method Methods 0.000 title claims abstract description 65
- 239000004973 liquid crystal related substance Substances 0.000 title claims abstract description 15
- 238000011084 recovery Methods 0.000 title claims description 11
- 230000004907 flux Effects 0.000 claims abstract description 64
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- 238000005406 washing Methods 0.000 claims abstract description 36
- 239000003513 alkali Substances 0.000 claims abstract description 33
- 238000003466 welding Methods 0.000 claims abstract description 30
- 230000008569 process Effects 0.000 claims abstract description 28
- 238000004140 cleaning Methods 0.000 claims abstract description 26
- 238000005498 polishing Methods 0.000 claims abstract description 24
- 238000004064 recycling Methods 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims description 33
- 238000000227 grinding Methods 0.000 claims description 24
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- 238000005273 aeration Methods 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 abstract description 31
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 abstract description 26
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000007517 polishing process Methods 0.000 abstract 1
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- 239000013077 target material Substances 0.000 description 15
- 229910000679 solder Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 238000000746 purification Methods 0.000 description 8
- 238000005070 sampling Methods 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910052718 tin Inorganic materials 0.000 description 6
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 5
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- 239000007787 solid Substances 0.000 description 5
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- 239000002253 acid Substances 0.000 description 4
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- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
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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
- C22B7/005—Separation by a physical processing technique only, e.g. by mechanical breaking
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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
- C22B21/00—Obtaining aluminium
- C22B21/0038—Obtaining aluminium by other processes
- C22B21/0069—Obtaining aluminium by other processes from scrap, skimmings or any secondary source aluminium, e.g. recovery of alloy constituents
-
- 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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention relates to a method for recovering aluminum residual targets for a liquid crystal panel. A method for recycling aluminum residual targets for liquid crystal panels comprises the following steps: (1) taking a small sample from the residual aluminum target, and removing a flux adhesion layer on the surface of the small sample; (2) measuring the flux adhesion depth of the sample treated in the step (1); (3) according to the flux adhesion depth obtained by the small sample measurement, four-side polishing is carried out on the residual aluminum target; (4) carrying out alkali washing on the residual aluminum target treated in the step (3); (5) cleaning the residual aluminum target treated in the step (4); (6) and (5) drying. According to the method, the thickness of the indium content on the surface is measured by adopting a glow discharge texture analyzer excitation mode, so that a polishing process can be correspondingly formulated, and the residual welding flux is completely removed; the polishing and alkali washing combined treatment process has high efficiency and better cleaning effect, and can effectively ensure the purity of the recycled raw materials.
Description
Technical Field
The invention belongs to the technical field of target material recovery, and particularly relates to a recovery method of an aluminum residual target for a liquid crystal panel.
Background
Sputtering is one of the main techniques for preparing thin film materials, and utilizes ions generated by an ion source to form an ion beam flow with high-speed flow through accelerated aggregation in vacuum, so as to bombard the surface of a solid, and kinetic energy exchange is carried out between the ions and atoms on the surface of the solid, so that the atoms on the surface of the solid are separated from the solid and are deposited on the surface of a substrate. The bombarded solid is the starting material for depositing thin films by sputtering, known as the sputtering target.
When the aluminum target for the liquid crystal panel is used, the aluminum target is generally bound with a copper back plate. The binding process is welding. Solder is often used to solder the aluminum target to the copper backing plate, and the solder is usually indium, tin, or the like. The sputtering yield of the planar target for liquid crystal panels was only 30%, and the remaining 70% became a residual target.
At present, the residual 70 percent of aluminum targets are not purified, and are changed to industrial waste aluminum for treatment. The purity of the aluminum residual target substrate is usually more than 99.999%, and the residual target is affected by the purity of the flux which is mainly adhered to the surface of the residual target: indium, tin, and the like. The development of the purification treatment process of the residual aluminum target can greatly improve the recovery value of the pure residual aluminum target and reduce the energy waste.
In the prior art, a cleaning method for recovering a sputtering target material discloses a method for recovering and cleaning an aluminum target material, which comprises the steps of soaking in an acid solution with the mass solubility of 10-75%, then soaking in a sodium hydroxide solution with the mass solubility of 10-20% for neutralization, and drying. However, the 10-75% acid solution used in the technology belongs to high-concentration strong acid, and is high in danger and serious in environmental pollution in the industrial use process, so that the technology is not suitable for industrial use.
In the prior art, an analysis method for detecting the indium element content and distribution of a high-purity aluminum target material after acid washing by using EPMA (electrophoretic deposition) adopts a method for detecting a high-purity aluminum sample. And after the high-purity aluminum sample is pickled, detecting the distribution of the indium element by adopting EPMA (Epstein-Barr MA) for guiding the pickling process. However, the pickling process of the aluminum residual target is not clear in the invention, and the guiding significance of indium distribution detection on pickling is limited, and the pickling process is mainly the thickness of the indium solder due to influence.
A recovery device and a recovery method of a target material in the prior art are disclosed. The device comprises a temperature control system and a filtering system. The method is used for quickly dropping the residual metal on the surface of the target material, and improves the utilization efficiency of the target material. However, this method is a single cleaning process and apparatus for the aluminum residual target. Practical application processes show that flux residue on the surface of the residual target cannot be quickly and effectively realized only by a cleaning process.
In view of the above, the present invention provides a novel method for recycling aluminum residue targets for liquid crystal panels
Disclosure of Invention
The invention aims to provide a method for recovering aluminum residual targets for liquid crystal panels, which adopts a glow discharge mass spectrometer to detect the thickness of a welding flux layer on the surface of the residual target, and carries out polishing and alkali washing process passes, so that the complete removal of residual metals on the surface can be pertinently realized, a high-purity aluminum raw material with the purity being 99.999 percent of that of an original target material is prepared, and the most efficient recycling of the aluminum residual targets is realized.
In order to realize the purpose, the adopted technical scheme is as follows:
a method for recycling aluminum residual targets for liquid crystal panels comprises the following steps:
(1) taking a small sample from the residual aluminum target, and removing a flux adhesion layer on the surface of the small sample;
(2) measuring the flux adhesion depth of the sample treated in the step (1);
(3) according to the flux adhesion depth obtained by the small sample measurement, four-side polishing is carried out on the residual aluminum target;
(4) carrying out alkali washing on the residual aluminum target treated in the step (3);
(5) cleaning the residual aluminum target treated in the step (4);
(6) and (5) drying.
Further, in the step (1), a glow discharge mass spectrometer is adopted to excite the flux adhesion layer on the surface of the aluminum residual target.
Still further, in the step (1), the excitation process continuously monitors the detection values of the main flux component, and the excitation is stopped when 10 continuous detection values are displayed as the blank components;
in the step (2), after the central part of the excitation hole is sawed, the depth of the excitation hole is detected by using a scanning electron microscope, namely the adhesion depth of the welding flux.
Still further, in the step (1), the glow discharge mass spectrometer sets 5-10 elements to be detected; the number of times of excitation is 30-80.
Furthermore, at least 2 samples are taken from the aluminum residual target, and grinding is carried out by taking the deepest adhering depth of the welding flux as a reference.
Furthermore, in the step (3), four surfaces of the aluminum residual target are a sputtering surface, a welding surface and two side edges of the aluminum residual target;
the single polishing depth of the contact surface of the aluminum residual target and the polisher is 100-200 μm.
Still further, the recovery method further comprises: and (5) when the flux adhesion depth is larger than the single grinding depth, repeating the steps (3) to (5) until the surface flux is removed.
Further, in the step (4), the concentration of the alkali liquor is 3-5 wt% during alkali washing, the temperature is 30-50 ℃, and the soaking time is 5-10 min.
Still further, in the step (4), aeration is continuously carried out during the alkali washing.
Further, in the step (5), high-purity water is adopted for cleaning, and the cleaning time is 2-3 min;
in the step (6), the drying temperature is 70-80 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the method mainly adopts a glow discharge mass spectrometer to excite the surface of the aluminum residual target to adhere the flux, and then uses a scanning electron microscope to observe and measure the thickness of the flux adhesion layer. And determining the cleaning treatment pass according to the thickness so as to ensure the effective removal of the flux on the surface of the residual target. The purification treatment process comprises grinding → alkali washing → drying, so that the surface treatment loss of the residual aluminum target is less, the recovery rate of the recovered residual aluminum target is 90-95 wt%, and the recovery rate is high.
2. The components of welding flux such as indium, tin and the like after the aluminum residual target is remelted are less than 0.2ppm, and the component standard of the nonferrous technology industry for Al99.999 percent is met. Namely, the remelted components can be used as raw materials for preparing the target material for recycling. Compared with the three-layer electrolytic method and the segregation method which are commonly used for purifying high-purity aluminum, the method has the advantage that the components of the recovered aluminum residual target are far lower than the purification cost.
Drawings
FIG. 1 is a diagram showing the fluctuation pattern/ppm of the contents of Si and In detected by the excitation of a glow discharge profiler In example 2.
Detailed Description
In order to further illustrate the recycling method of the aluminum residue target for liquid crystal display panel of the present invention and achieve the desired objects, the following embodiments are combined with the preferred embodiments to provide a recycling method of the aluminum residue target for liquid crystal display panel, the detailed description of the embodiments, the structure, the features and the effects thereof. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The following will describe in further detail a method for recycling aluminum residue targets for liquid crystal panels according to the present invention with reference to specific embodiments:
according to the invention, the panel and the back plate are heated at high temperature, and the back plate is separated from the residual target after the flux is melted. And (4) after separation, sampling the residual target, and exciting by adopting a glow discharge texture analyzer until the flux components in the sample are completely removed to reach the base component standard. And taking out the sample, and detecting and confirming the excitation depth by adopting an SEM (scanning Electron microscope), namely the depth required by polishing and cleaning the surface of the residual target.
Cutting the residual target to a fixed size, polishing the surface of the residual target once by using a grinding machine, and soaking the residual target once by using alkali liquor, washing the residual target by using a high-pressure water gun and drying the residual target after polishing; and after drying, carrying out secondary polishing, flushing by using a high-pressure water gun and drying until the polishing depth exceeds the depth required by cleaning the surface of the residual target. And judging that the residual target is completely placed in the raw material area for standby.
Specifically, the technical scheme of the invention is as follows:
a method for recycling aluminum residual targets for liquid crystal panels comprises the following steps:
(1) a sample is taken out from the aluminum residual target, and the flux adhesion layer on the surface of the sample is removed.
(2) And (3) measuring the flux adhesion depth of the small sample treated in the step (1).
(3) The resulting flux adhesion depth was measured from the small sample, and the aluminum stub target was ground on four sides.
(4) And (4) carrying out alkali washing on the residual aluminum target treated in the step (3).
The polished aluminum residual target has uneven surface, and the polished flux and dust can adhere to the aluminum residual target. The invention can make the polished surface as uniform as possible by alkali cleaning, and remove the welding flux and dust which are polished off and attached to the aluminum residual target.
(5) And (4) cleaning the residual aluminum target treated in the step (4).
(6) And (5) drying.
Preferably, in the step (1), a glow discharge mass spectrometer is used for exciting the flux adhesion layer on the surface of the aluminum residual target.
Further preferably, in the step (1), the excitation process continuously monitors the detection value of the main flux component, and the excitation is stopped when 10 detection values are continuously displayed as the green components;
in the step (2), after the sample which is subjected to excitation is sawed from the center of the excitation hole, the depth of the excitation hole is detected by using a scanning electron microscope, and the depth is the adhesion depth of the welding flux.
The welding flux depth on the surface of the target welded and separated by different processes may be different, and the subsequent purification treatment depth is confirmed according to different depths.
Further preferably, in the step (1), the glow discharge mass spectrometer sets 5-10 elements to be detected; the number of times of excitation is 30-80.
Preferably, the sample is ground by taking at least 2 samples from the aluminum residual target and taking the deepest adhering depth of the welding flux as a reference.
Preferably, in the step (3), four faces of the aluminum residual target are a sputtering face, a welding face and two side edges of the aluminum residual target;
the single polishing depth of the contact surface of the aluminum residual target and the polisher is 100-200 μm. The material of the residual target polishing grinding head is a steel wire wheel.
Further preferably, the recycling method further comprises: and (5) when the flux adhesion depth is larger than the single grinding depth, repeating the steps (3) to (5) until the surface flux is removed.
Preferably, in the step (4), the concentration of the alkali liquor is 3-5 wt% during the alkali washing, the temperature is 30-50 ℃, and the soaking time is 5-10 min.
Further preferably, in the step (4), aeration is continuously carried out during the alkali washing.
Further, in the step (5), high-purity water is adopted for cleaning, and the cleaning time is 2-3 min;
in the step (6), the drying temperature is 70-80 ℃.
Example 1.
The specific operation steps are as follows:
(1) exciting a flux layer on the surface of the aluminum stub: and (4) separating the residual aluminum target and the copper back plate after the heating flux melts. Sawing a sample of 25-25mm from the residual aluminum target after separation. And (3) polishing a visible welding layer on the surface of the sample by using waterproof abrasive paper and washing the visible welding layer. And (3) exciting the flux adhesion layer on the surface of the aluminum residual target by adopting a glow discharge mass spectrometer. Random sampling, 3 samples are recommended.
Setting 5-10 elements to be detected by a glow discharge mass spectrometer; the excitation current is set. The number of times of excitation is 30-80. The activation process continuously monitors the primary flux component test values and stops activation when 10 consecutive test values are displayed as green components.
(2) And (3) detecting the depth of the welding flux: and (4) after the glow discharge mass spectrometer is excited, the sample is sawed at the center of the excitation hole, and then the depth of the excitation hole is detected by using a scanning electron microscope. The depth value of 3 samples is the maximum depth, and the depth is the adhesion depth of the aluminum residual target welding flux and the depth of the treatment required by the grinding process. The detection analysis of the adhesion depth of the flux on the surface of the aluminum target material is 300-400 μm.
(3) Polishing: the aluminum residual target grinding machine is used for grinding four surfaces, namely a sputtering surface, a welding surface and two side edges of the aluminum residual target. The most adherent flux is the soldering surface. A small amount of welding flux adheres to the sputtering surface and the two side edges, and the welding flux is molten when the target material is separated from the back plate and easily drops to other parts during separation, so that the four surfaces are required to be polished.
The single grinding depth of the contact surface of the aluminum residual target and the grinding machine is 100-200 mu m. And (5) polishing the residual aluminum target and then waiting for alkaline cleaning.
(4) Alkali washing: the concentration of alkali liquor is 3-5 wt% when the aluminum residue target is subjected to alkaline washing; the residual target 4 surfaces are completely immersed in the alkali liquor, the immersion temperature of the alkali liquor is 30-50 ℃, and the immersion time is 5-10 min.
The bottom of the alkaline washing tank is added with a vent pipe, and the vent hole diameter of the vent pipe is 1 mm. The alkaline washing process was continuously aerated. The bubbles introduced from the bottom can accelerate the dropping of reactants of the aluminum residual target surface and the alkali liquor and accelerate the alkali washing process.
(5) Cleaning with pure water: and taking out the residual aluminum target after the reaction with the alkali liquor, and placing the residual aluminum target in a cleaning pool. The water gun is used for spraying water in four directions for washing. And (4) washing until the surface of the residual aluminum target is washed clean. The time of single washing is 2-3 min.
The resistivity of the rinsing pure water was > 14 M.OMEGA.. multidot.cm.
(6) Drying: the residual target washed by pure water is placed in a drying pool, and a hot air device is adopted. The temperature of the hot air outlet is 70-80 ℃. Drying with hot air for 5-10min, and placing in a material preparation area for smelting.
(7) Polishing, alkali washing and washing are repeated: the thickness of the solder adhesion layer on the surface of the aluminum target material is detected and analyzed to be 300-400 mm. The single polishing depth is 100-200 μm, and 4 passes of repeated processing are needed to ensure complete removal of the solder in order to realize complete processing of the solder on the surface of the aluminum stub target.
(8) The safety protection process during polishing and alkali washing of the residual target comprises the following steps:
aluminum dust generated during the polishing of the residual target has accident risks such as explosion and the like. Therefore, the polishing device is provided with an aluminum dust absorption and treatment device.
The reaction equation during alkaline washing of the residual aluminum target is as follows:
2Al+2NaOH+2H2O＝2NaAlO2+3H2↑
the hydrogen and alkali liquor volatile gas generated in the alkali washing process are both provided with a gas absorption and discharge device.
(9) Smelting: and placing the treated residual aluminum target in a smelting material preparation area for waiting for feeding. The content of the indium welding flux after the residual target is treated by the method and smelted is less than 0.2 ppm.
Example 2.
The specific operation steps are as follows:
(1) two 25 by 20mm assay coupons were sawed head to tail from a 200 by 20 by 2800mm size aluminum stub target. The target and the surface of the back plate are made of high-purity indium by using a welding flux. And putting the sample into a set glow discharge mass spectrometer for detection. The number of detection elements was set to 10 (B, Mg, Si, P, Mn, Fe, Ni, Cu, In, Sn), and the excitation current was set. And starting detection, and continuously monitoring the detection value in the detection process. The In content was 0.0497ppm when the measurement value reached 42 th. Excitation was continued up to 52 detection values. The results of analyzing the Si and In elements are shown In fig. 1.
(2) And taking out the sample after excitation. After a sample is sawed from the center of the excitation hole by using a water jet cutter, the depth of the excitation hole is observed to be mum by adopting an EVO 50 scanning electron microscope.
(3) And taking the minimum value of the single grinding thickness of the grinding machine as 100 mu m, and calculating the grinding times of 320/100-3.2-4 times.
(4) And (4) cutting the residual aluminum target, wherein the size of the cut plate is 200 x 1000 x 20 mm. In order to meet the requirements of crucible smelting with the diameter of 700 x 900mm, 60 plates are polished in a single time.
(5) After polishing, the plates are placed in a vertical material rack in batches, the temperature of the alkali liquor is raised to 35 ℃, and the bottom is ventilated. And completely soaking the material rack in alkali liquor for 10 min. And taking the material frame out and putting the material frame into a flushing area after soaking. And sequentially finishing the alkali washing treatment of 60 plates.
(6) After the alkaline washing, the target is placed in a material rack, and a high-pressure water gun is started from four directions simultaneously to wash the plate by adopting the high-pressure water gun. The water pressure is concentrated at the bonding surface, i.e. the indium adhesion surface. When the aluminum plate is washed, partial residual indium sheets can be observed on the surface, and the surface has metallic luster which is higher than the bottom color of the aluminum plate and smooth finish. The rinsing time was 3 min.
(7) The washing aluminum plate is placed in a drying pool, and hot air is started. Controlling the temperature of hot air at 75 deg.C, and oven drying for 10 min.
(8) And (5) repeating the same process for 3 times before stacking the dried plates to a grinding machine. And (3) when the plate is washed after alkali washing in the 3 rd pass, no indium solder is adhered to the surface, and the solder can be judged to be completely cleaned macroscopically. And 4, grinding and cleaning in the 4 th pass, namely completely removing the welding flux on the surface of the plate to ensure the microscopic degree.
(9) The completely processed plate is placed In a high-purity graphite crucible with the diameter of 700 mm x 900mm, the temperature is increased to be smelted to the aluminum liquid temperature of 750 ℃, a sampling spoon is adopted to sample and cast a detection sample with the diameter of 30mm x 30mm, a GDMS glow discharge quality analyzer is adopted to detect that the In content is 0.05ppm, and the component standard of a 5N high-purity aluminum target material is met.
Example 3.
The specific operation steps are as follows:
(1) two 25 by 20mm assay coupons were sawed head to tail from a 200 by 20 by 2800mm size aluminum stub target. The target and the surface of the back plate are made of high-purity indium by using a welding flux. And putting the sample into a set glow discharge mass spectrometer for detection. The number of detection elements was set to 10 (B, Mg, Si, P, Mn, Fe, Ni, Cu, In, Sn), and the excitation current was set. And starting detection, and continuously monitoring the detection value in the detection process. The In content was 0.0501ppm when the value reached 45 th measurement. Excitation was continued to 57 detection values.
(2) And taking out the sample after excitation. After the sample is sawed from the center of the excitation hole by using a water jet cutter, the depth of the excitation hole is observed to be 350 μm by adopting an EVO 50 scanning electron microscope.
(3) Taking the minimum value of the single grinding thickness of the grinding machine as 100 mu m, and calculating the grinding times as 350/100 as 3.5 passes.
(4) And (4) cutting the residual aluminum target, wherein the size of the cut plate is 200 x 1000 x 20 mm. In order to meet the requirements of crucible smelting with the diameter of 700 x 900mm, 60 plates are polished in a single time.
(5) The same purification treatment process as in example 2 was performed. To verify the necessity of the 4 th pass, only 3 passes of the cleaning treatment process were performed.
(6) The completely processed plate is placed In a high-purity graphite crucible with the diameter of 700 mm x 900mm, the temperature is increased to be smelted to the aluminum liquid temperature of 750 ℃, a sampling spoon is adopted to sample and cast a detection sample with the diameter of 30mm x 30mm, and a GDMS glow discharge quality analyzer is adopted to detect that the In content is 0.32 ppm. The detection value meets the standard that the single element of the 5N high-purity aluminum target material is less than 0.5ppm, but deviates from the stable control range of the components and does not meet the use requirement.
Example 4.
The specific operation steps are as follows:
(1) and (4) carrying out flux depth detection on the uncut sample, and carrying out purification treatment on the residual target only through visual observation.
(2) The residual aluminum target was cut, and 60 plates were cut to a size of 200 × 1000 × 20 mm.
(3) The same purification treatment process as in example 2 was performed. And observing the flux residue on the surface of the residual target after one time. There is no residual indium on the concave surface of sputtering, there are no residual indium sheets on both sides, but there are few visible indium sheets on the bonding surface.
(4) The second pass purification treatment process was performed according to example 2. And after the second pass, all surfaces of the residual target have no visible residual indium sheet.
(5) Placing the treated plate In a high-purity graphite crucible with the diameter of 700 mm x 900mm, heating and smelting the plate to the temperature of the molten aluminum of 750 ℃, sampling by using a sampling spoon, casting a detection sample with the diameter of 30mm x 30mm, and detecting the In content of 1.2ppm by using a GDMS glow discharge texture analyzer. This test value does not satisfy the 5N high purity aluminum target single element < 0.5ppm standard, i.e., whether the indium solder is removed or not cannot be confirmed completely by visual observation.
Example 5.
The specific operation steps are as follows:
(1) two 25 by 20mm assay coupons were sawed head to tail from a 200 by 20 by 2800mm size aluminum stub target. The target and the surface of the back plate are made of high-purity indium by using a welding flux. And putting the sample into a set glow discharge mass spectrometer for detection. The number of detection elements was set to 10 (B, Mg, Si, P, Mn, Fe, Ni, Cu, In, Sn), and the excitation current was set. And starting detection, and continuously monitoring the detection value in the detection process. The In content was 0.0405ppm by the 42 th measurement value. Excitation was continued up to 54 detection values.
(2) And taking out the sample after excitation. After the sample was sawed from the center of the excitation hole using a water jet, the depth of the excitation hole was observed to be 330 μm using an EVO 50 scanning electron microscope.
(3) And taking the minimum value of the single grinding thickness of the grinding machine as 100 mu m, and calculating the grinding times of 330/100-3.3 and 4.
(4) And (4) cutting the residual aluminum target, wherein the size of the cut plate is 200 x 1000 x 20 mm. 60 plates were polished in a single pass.
(5) And hoisting the polished plates to a cleaning pool, and simultaneously opening high-pressure water guns in four directions to clean the plates by using the high-pressure water guns. The water pressure is concentrated at the bonding surface, i.e. the indium adhesion surface. The rinsing time was 3 min.
(6) The washing aluminum plate is placed in a drying pool, and hot air is started. Controlling the temperature of hot air at 75 deg.C, and oven drying for 10 min.
(7) And observing the adhesion of more indium solder on the surface of the plate in the washing and drying processes. The adhesive flux is sheet-shaped, and only one end of most indium sheets is adhered to the surface of the plate but does not fall off during washing.
(8) This treatment process was repeated for 3 additional passes. And observing that small residual indium sheets still exist in the partial area of the welding surface of the residual target, wherein the area of the adhered indium sheets is smaller and is 3-5mm, and only one end of the adhered indium sheets is adhered to the surface of the aluminum plate. Can be peeled off by hand.
(9) In order to ensure that the flux is completely removed by visual observation, the visible flux on the surface of the residual target is completely removed after the process is repeated for 2 times.
(10) Placing the treated plate In a high-purity graphite crucible with the diameter of 700 mm x 900mm, heating and smelting to the temperature of aluminum liquid of 750 ℃, sampling by using a sampling spoon, casting a detection sample with the diameter of 30mm x 30mm, and detecting the In content of 0.45ppm by using a GDMS glow discharge quality analyzer. The detection value meets the standard that a single element of a 5N high-purity aluminum target material is less than 0.5ppm, but deviates from the stable control range of components and does not meet the use requirement.
Therefore, the alkaline cleaning treatment after each polishing is necessary, so that the polished surface can be as uniform as possible, the welding flux and dust which are adhered to the aluminum residual target and are polished off can be removed, and the finally treated aluminum residual target can meet the use requirement.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (10)
1. A method for recycling residual aluminum targets for liquid crystal panels is characterized by comprising the following steps:
(1) taking a small sample from the residual aluminum target, and removing a flux adhesion layer on the surface of the small sample;
(2) measuring the flux adhesion depth of the sample treated in the step (1);
(3) according to the flux adhesion depth obtained by the small sample measurement, four-side polishing is carried out on the residual aluminum target;
(4) carrying out alkali washing on the residual aluminum target treated in the step (3);
(5) cleaning the residual aluminum target treated in the step (4);
(6) and (5) drying.
2. The recycling method according to claim 1,
in the step (1), a glow discharge mass spectrometer is adopted to excite the flux adhesion layer on the surface of the aluminum residual target.
3. The recycling method according to claim 2,
in the step (1), the excitation process continuously monitors the detection values of the main welding flux components, and the excitation is stopped when 10 continuous detection values are displayed as blank components;
in the step (2), after the central part of the excitation hole is sawed, the depth of the excitation hole is detected by using a scanning electron microscope, namely the adhesion depth of the welding flux.
4. The recycling method according to claim 3,
in the step (1), a glow discharge mass spectrometer sets 5-10 elements to be detected; the number of times of excitation is 30-80.
5. The recycling method according to claim 1,
at least 2 samples are taken from the aluminum residual target, and grinding is carried out by taking the deepest welding flux adhesion depth as a reference.
6. The recycling method according to claim 1,
in the step (3), the four surfaces of the residual aluminum target are a sputtering surface, a welding surface and two side edges of the residual aluminum target;
the single polishing depth of the contact surface of the aluminum residual target and the polisher is 100-200 μm.
7. The recycling method according to claim 6,
the recovery method further comprises the following steps: and (5) when the flux adhesion depth is larger than the single grinding depth, repeating the steps (3) to (5) until the surface flux is removed.
8. The recycling method according to claim 1,
in the step (4), the concentration of the alkali liquor is 3-5 wt% during the alkali washing, the temperature is 30-50 ℃, and the soaking time is 5-10 min.
9. The recycling method according to claim 8,
in the step (4), aeration is continuously carried out in the process of alkali washing.
10. The recycling method according to claim 1,
in the step (5), high-purity water is adopted for cleaning, and the cleaning time is 2-3 min;
in the step (6), the drying temperature is 70-80 ℃.
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| CN115505752A (en) * | 2022-10-25 | 2022-12-23 | 同创普润(上海)机电高科技有限公司 | Recovery method of high-purity aluminum residual target for liquid crystal panel |
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