CN110732802A - Corrosion inhibition soldering flux for bonding of fine-pitch bonding pads and preparation method thereof - Google Patents
Corrosion inhibition soldering flux for bonding of fine-pitch bonding pads and preparation method thereof Download PDFInfo
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- CN110732802A CN110732802A CN201811232640.XA CN201811232640A CN110732802A CN 110732802 A CN110732802 A CN 110732802A CN 201811232640 A CN201811232640 A CN 201811232640A CN 110732802 A CN110732802 A CN 110732802A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
- B23K35/3613—Polymers, e.g. resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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Abstract
The invention provides corrosion inhibition soldering flux for bonding fine-pitch pads and a preparation method thereof, and the corrosion inhibition soldering flux is prepared from the following components, by weight, 12-18 parts of pentaerythritol ester, 24-30 parts of an active agent, 16-22 parts of a corrosion inhibitor, 8-16 parts of an inorganic salt, 3-9 parts of monocetylate, 5-10 parts of dodecylamine, 7-14 parts of lauric acid, 14-20 parts of diethylene glycol hexyl ether, 12-16 parts of isopropanol, 16-26 parts of ethylene glycol butyl ether and 34-42 parts of deionized water.
Description
Technical Field
The invention relates to the field of electronic additives, in particular to a corrosion inhibition soldering flux for bonding a fine-pitch bonding pad and a preparation method thereof.
Background
The invention discloses a fine-pitch bonding pad, which is characterized in that a fine-pitch bonding pad is a small-size bonding pad with the length and width of less than 90 mu m and the pitch of less than 150 mu m, and a conventional bonding mode is not suitable for bonding the small-size fine-pitch bonding pad due to small size, so that mutual interference among welding spots can be caused, even short circuit can be caused and the welding spots can be damaged due to the conventional bonding mode.
Disclosure of Invention
The technical problem to be solved is as follows:
the invention aims to provide corrosion inhibition soldering flux for bonding of fine-pitch bonding pads and a preparation method thereof, and the prepared soldering flux has good soldering assistance performance and good corrosion inhibition performance, can inhibit the corrosion degree of a test piece to a certain extent at , and can meet the use requirement.
The technical scheme is as follows:
the invention provides a corrosion inhibition soldering flux for bonding of fine-pitch bonding pads, which is prepared from the following components in parts by weight:
12-18 parts of pentaerythritol ester,
24-30 parts of active agent,
16-22 parts of corrosion inhibitor,
8-16 parts of inorganic salt,
3-9 parts of mono-hexadecanoate,
5-10 parts of laurylamine,
7-14 parts of lauric acid,
14-20 parts of diethylene glycol hexyl ether,
12-16 parts of isopropanol,
16-26 parts of ethylene glycol butyl ether,
34-42 parts of deionized water.
Preferably, the corrosion inhibition soldering flux for bonding the fine-pitch bonding pad is prepared by the following preparation method:
(1) washing sweet clover seeds with deionized water, culturing until the seeds germinate, culturing with vermiculite, washing roots with deionized water when the seeds grow to about 8cm in height of sweet clover seedlings, transferring to phosphorus-deficient culture solution, culturing in an artificial incubator, changing nutrient solution for times every 3 days, and culturing for 30 days;
(2) collecting cultured root 10g of sweet clover, adding 40mL80 wt% ethanol solution, mechanically crushing into slurry, transferring into a sealed container, extracting with water bath, and extracting with 20000 r.min-1Centrifuging for 20min, and filtering the supernatant with 0.45 μm filter membrane to obtain the active agent.
the preferable preparation method of the active agent comprises the step (2) of extracting with water bath at 65-70 deg.C for 20-40 min.
Preferably, the corrosion inhibition scaling powder for bonding the fine-pitch bonding pad is prepared by mixing sodium sulfite, potassium chloride and sodium chloride according to a weight ratio of 11.24:7.9: 1.8.
Preferably, the corrosion inhibition soldering flux for bonding the fine-pitch bonding pad is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1.
The invention also provides a preparation method of the corrosion inhibition soldering flux for bonding the fine-pitch bonding pads, which comprises the following preparation steps: (1) heating 34-42 parts of deionized water to 60 ℃ in a stirrer, adding 14-20 parts of diethylene glycol hexyl ether, 12-16 parts of isopropanol and 16-26 parts of butyl cellosolve, mixing for 20min, adding 12-18 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 24-30 parts of an active agent, 16-22 parts of a corrosion inhibitor, 8-16 parts of an inorganic salt and 3-9 parts of a mono-hexadecanoate, stirring for 30min, adding 5-10 parts of dodecylamine and 7-14 parts of lauric acid, mixing for 40min, filtering with 5 layers of gauze, and cooling to room temperature to obtain the corrosion inhibition scaling powder for bonding the fine-pitch bonding pads.
Has the advantages that:
(1) the inorganic active agent has strong acidity and strong corrosivity, and is rarely used in electronic industries, the sweet clover is subjected to phosphorus-deficient culture, so that the root of the sweet clover generates various organic acid active substances, and the extracted substances are applied to the soldering flux disclosed by the invention, so that the soldering flux has a good soldering effect.
(2) The soldering flux prepared by the invention has stable appearance and physical properties, storage resistance, good usability, good spreading performance, low corrosivity and higher application value.
Detailed Description
The following examples are presented to enable one of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The active agents of examples 1-5 and comparative examples 1, 3 were prepared by the following preparation method:
(1) washing sweet clover seeds with deionized water, culturing until the seeds germinate, culturing with vermiculite, washing roots with deionized water when the seeds grow to about 8cm in height of sweet clover seedlings, transferring to phosphorus-deficient culture solution, culturing in an artificial incubator, changing nutrient solution for times every 3 days, and culturing for 30 days;
(2) collecting cultured root 10g of sweet clover, adding 40mL80 wt% ethanol solution, mechanically crushing into slurry, transferring into a sealed container, extracting with water bath at 60 deg.C for 30min, and extracting with 20000 r.min-1Centrifuging for 20min, and filtering the supernatant with 0.45 μm filter membrane to obtain the active agent.
The phosphorus-deficient culture solution comprises the following components: 0.75mol/L magnesium sulfate, 0.95mol/L potassium sulfate, 1.2mol/L potassium chloride, 1.1X 10-3mol/L manganese sulfate, 1.3X 10-4Copper sulfate in mol/L, calcium nitrate in 2.4mol/L, 1X 10-3mol/L zinc sulfate.
Example 1
(1) Heating 42 parts of deionized water to 60 ℃ in a stirrer, adding 14 parts of diethylene glycol hexyl ether, 16 parts of isopropanol and 16 parts of butyl cellosolve, mixing for 20min, adding 18 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 24 parts of an active agent, 22 parts of a corrosion inhibitor, 8 parts of an inorganic salt and 9 parts of a mono-hexadecanoate, stirring for 30min, adding 5 parts of dodecylamine and 14 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pads.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1.
Example 2
(1) Heating 34 parts of deionized water to 60 ℃ in a stirrer, adding 20 parts of diethylene glycol hexyl ether, 12 parts of isopropanol and 26 parts of butyl cellosolve, mixing for 20min, adding 12 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 30 parts of an active agent, 16 parts of a corrosion inhibitor, 16 parts of an inorganic salt and 3 parts of a mono-hexadecanoate, stirring for 30min, adding 10 parts of dodecylamine and 7 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pads.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1.
Example 3
(1) Heating 40 parts of deionized water in a stirrer to 60 ℃, adding 16 parts of diethylene glycol hexyl ether, 15 parts of isopropanol and 18 parts of butyl cellosolve, mixing for 20min, adding 16 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 26 parts of an active agent, 20 parts of a corrosion inhibitor, 10 parts of an inorganic salt and 8 parts of a mono-hexadecanoate, stirring for 30min, adding 6 parts of dodecylamine and 12 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pads.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1.
Example 4
(1) Heating 36 parts of deionized water to 60 ℃ in a stirrer, adding 18 parts of diethylene glycol hexyl ether, 13 parts of isopropanol and 24 parts of butyl cellosolve, mixing for 20min, adding 14 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 28 parts of an active agent, 18 parts of a corrosion inhibitor, 14 parts of an inorganic salt and 4 parts of a mono-hexadecanoate, stirring for 30min, adding 9 parts of dodecylamine and 9 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pads.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1.
Example 5
(1) Heating 38 parts of deionized water to 60 ℃ in a stirrer, adding 17 parts of diethylene glycol hexyl ether, 14 parts of isopropanol and 21 parts of butyl cellosolve, mixing for 20min, adding 15 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 27 parts of an active agent, 19 parts of a corrosion inhibitor, 12 parts of an inorganic salt and 6 parts of a mono-hexadecanoate, stirring for 30min, adding 7.5 parts of dodecylamine and 11 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pad.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1. Comparative example 1
This comparative example differs from example 1 in that no inorganic salt is contained. Specifically, the method comprises the following steps:
(1) heating 42 parts of deionized water to 60 ℃ in a stirrer, adding 14 parts of diethylene glycol hexyl ether, 16 parts of isopropanol and 16 parts of butyl cellosolve, mixing for 20min, adding 18 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 24 parts of an active agent, 22 parts of a corrosion inhibitor and 9 parts of monocetylate, stirring for 30min, adding 5 parts of dodecylamine and 14 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion inhibition soldering flux for bonding the fine-pitch bonding pad.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1. Comparative example 2
This comparative example differs from example 1 in that it does not contain an active agent. Specifically, the method comprises the following steps:
(1) heating 42 parts of deionized water to 60 ℃ in a stirrer, adding 14 parts of diethylene glycol hexyl ether, 16 parts of isopropanol and 16 parts of butyl cellosolve, mixing for 20min, adding 18 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 22 parts of corrosion inhibitor, 8 parts of inorganic salt and 9 parts of mono-hexadecanoate, stirring for 30min, adding 5 parts of dodecylamine and 14 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pad.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 2:1: 1. Comparative example 3
This comparative example differs from example 1 in the formulation of the corrosion inhibitor. Specifically, the method comprises the following steps:
(1) heating 42 parts of deionized water to 60 ℃ in a stirrer, adding 14 parts of diethylene glycol hexyl ether, 16 parts of isopropanol and 16 parts of butyl cellosolve, mixing for 20min, adding 18 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 24 parts of an active agent, 22 parts of a corrosion inhibitor, 8 parts of an inorganic salt and 9 parts of a mono-hexadecanoate, stirring for 30min, adding 5 parts of dodecylamine and 14 parts of lauric acid, mixing for 40min, filtering by using 5 layers of gauze, and cooling to room temperature to obtain the corrosion-inhibiting soldering flux for bonding the fine-pitch bonding pads.
The inorganic salt is formed by mixing sodium sulfite, potassium chloride and sodium chloride according to the weight ratio of 11.24:7.9: 1.8.
The corrosion inhibitor is prepared by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to the weight ratio of 1:1: 2. The performance of the corrosion-inhibiting flux for bonding of fine-pitch pads prepared in examples 1 to 5 and comparative examples 1 to 3 was tested:
and the corrosion inhibition performance is measured by adopting a static weight loss method, the test piece is cleaned, dried and soaked in the soldering flux for 72 hours, the surface corrosion layer is erased, cleaned and dried to constant weight, and the corrosion inhibition rate is calculated.
Appearance, physical stability test: stirring the soldering flux for a few minutes, then sealing and freezing to 6 ℃, keeping for 1 hour, observing whether layered crystals are separated out or not, judging that the surface is qualified if the phenomena do not occur, then exposing the soldering flux in a 45 ℃ oven, keeping for 1 hour, observing whether the layer is separated out or not, and judging that the surface is qualified if the layer is not separated out.
Spreading performance test comprises placing solder balls on a test piece of 50mm × 50mm × 0.3mm, dripping 0.1mL soldering flux between the solder balls, heating at 10 deg.C for 5min, heating at 260 deg.C for 30s, taking out the test piece, horizontally standing to room temperature, and measuring the spreading area.
The test results are given in the following table:
TABLE 1
Corrosion rate/%) | Spreading area/mm2 | |
Example 1 | 87.42 | 70.55 |
Example 2 | 90.98 | 74.81 |
Example 3 | 93.68 | 76.54 |
Example 4 | 94.17 | 78.31 |
Example 5 | 96.33 | 79.86 |
Comparative example 1 | 86.37 | 64.39 |
Comparative example 2 | 87.11 | 63.19 |
Comparative example 3 | 80.12 | 70.23 |
TABLE 2
According to test results, the prepared corrosion inhibition soldering flux for bonding the fine-pitch bonding pad has high appearance and physical stability, good spreadability, and better corrosion inhibition performance, can improve the solderability of the solder and the bonding pad, can inhibit the corrosion degree of a test piece to a certain extent of , and can meet the use requirements, the formula in the embodiment 5 is the best formula in the invention, the soldering flux prepared according to the formula in the embodiment 5 of the invention has the corrosion inhibition rate of 96.33%, and the spreading area of 79.86mm2。
The inorganic salt sodium sulfite, potassium chloride and sodium chloride are added, the viscosity of the system can be adjusted by adding the inorganic salt, the interfacial tension is properly reduced, the soldering flux can be better diffused, and the spreading performance of the soldering flux is improved.
According to the invention, the sweet clover is subjected to phosphorus-deficient culture, so that a plurality of organic acid active substances are generated at the root of the sweet clover, and are extracted and applied to the soldering flux of the invention.
N-arylpyrroles are non-toxic compounds, which contain N-arylpyrroles in many natural products, which have excellent corrosion inhibiting properties. The methyl triphenyl phosphonium bromide can be adsorbed on the surface of the metal under the action of electrostatic attraction and van der Waals force, and then the chemical adsorption is carried out on the metal, so that the corrosion inhibition efficiency is improved. The weight ratio of the methyl triphenyl phosphonium bromide to the N-aryl pyrrole to the fatty acid ester is 2:1:1, which is the optimal ratio.
Claims (6)
1. The corrosion inhibition scaling powder for bonding the fine-pitch bonding pads is characterized by comprising the following components in parts by weight:
12-18 parts of pentaerythritol ester,
24-30 parts of active agent,
16-22 parts of corrosion inhibitor,
8-16 parts of inorganic salt,
3-9 parts of mono-hexadecanoate,
5-10 parts of laurylamine,
7-14 parts of lauric acid,
14-20 parts of diethylene glycol hexyl ether,
12-16 parts of isopropanol,
16-26 parts of ethylene glycol butyl ether,
34-42 parts of deionized water.
2. The corrosion inhibiting flux for bonding a fine pitch pad according to claim 1, wherein said activator is prepared by the following preparation method:
(1) washing sweet clover seeds with deionized water, culturing until the seeds germinate, culturing with vermiculite, washing roots with deionized water when the seeds grow to about 8cm in height of sweet clover seedlings, transferring to phosphorus-deficient culture solution, culturing in an artificial incubator, changing nutrient solution for times every 3 days, and culturing for 30 days;
(2) collecting cultured root 10g of sweet clover, adding 40mL80 wt% ethanol solution, mechanically crushing into slurry, transferring into a sealed container, extracting with water bath, and collecting the solution at 20000 r.min-1Centrifuging for 20min, collecting supernatant, and filtering with 0.45 μm filter membraneObtaining the active agent.
3. The method for preparing an active agent according to claim 2, wherein the temperature of the water bath extraction in the step (2) is 65-70 ℃ and the reaction time is 20-40 min.
4. The corrosion inhibiting flux for bonding of fine pitch pads according to claim 1, wherein said inorganic salt is a mixture of sodium sulfite, potassium chloride and sodium chloride in a weight ratio of 11.24:7.9: 1.8.
5. The corrosion inhibition scaling powder for bonding the fine-pitch bonding pad according to claim 1, wherein the corrosion inhibitor is formed by mixing methyl triphenyl phosphonium bromide, N-aryl pyrrole and grease acid ester according to a weight ratio of 2:1: 1.
6. The preparation method of the corrosion inhibition soldering flux for bonding the fine-pitch bonding pads is characterized by comprising the following preparation steps of:
(1) heating 34-42 parts of deionized water to 60 ℃ in a stirrer, adding 14-20 parts of diethylene glycol hexyl ether, 12-16 parts of isopropanol and 16-26 parts of butyl cellosolve, mixing for 20min, adding 12-18 parts of pentaerythritol ester, and stirring for 15 min;
(2) and continuously adding 24-30 parts of an active agent, 16-22 parts of a corrosion inhibitor, 8-16 parts of an inorganic salt and 3-9 parts of a mono-hexadecanoate, stirring for 30min, adding 5-10 parts of dodecylamine and 7-14 parts of lauric acid, mixing for 40min, filtering with 5 layers of gauze, and cooling to room temperature to obtain the corrosion inhibition scaling powder for bonding the fine-pitch bonding pads.
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Citations (5)
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CN101264123A (en) * | 2007-03-15 | 2008-09-17 | 天津丹溪国药研究所 | Natural medicine dropping pills for treating hemorrhoidal disease |
CN102178725A (en) * | 2011-05-10 | 2011-09-14 | 长春中医药大学 | Melilotus officinalis total saponin, preparation method thereof and medicinal application |
CN103785975A (en) * | 2014-02-20 | 2014-05-14 | 苏州龙腾万里化工科技有限公司 | Soldering flux for improving corrosion inhibition |
CN107252427A (en) * | 2012-07-09 | 2017-10-17 | 比托普股份公司 | For the composition for including active material for the bodily tissue regeneration for promoting damage |
CN107982135A (en) * | 2017-12-25 | 2018-05-04 | 深圳市芭格美生物科技有限公司 | A kind of shampoo and preparation method thereof |
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2018
- 2018-10-22 CN CN201811232640.XA patent/CN110732802A/en not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101264123A (en) * | 2007-03-15 | 2008-09-17 | 天津丹溪国药研究所 | Natural medicine dropping pills for treating hemorrhoidal disease |
CN102178725A (en) * | 2011-05-10 | 2011-09-14 | 长春中医药大学 | Melilotus officinalis total saponin, preparation method thereof and medicinal application |
CN107252427A (en) * | 2012-07-09 | 2017-10-17 | 比托普股份公司 | For the composition for including active material for the bodily tissue regeneration for promoting damage |
CN103785975A (en) * | 2014-02-20 | 2014-05-14 | 苏州龙腾万里化工科技有限公司 | Soldering flux for improving corrosion inhibition |
CN107982135A (en) * | 2017-12-25 | 2018-05-04 | 深圳市芭格美生物科技有限公司 | A kind of shampoo and preparation method thereof |
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Application publication date: 20200131 |