CN107445176B - Tin Sb doped light color electrical isolation laser activation can metallize the preparation method of powder - Google Patents
Tin Sb doped light color electrical isolation laser activation can metallize the preparation method of powder Download PDFInfo
- Publication number
- CN107445176B CN107445176B CN201710764519.0A CN201710764519A CN107445176B CN 107445176 B CN107445176 B CN 107445176B CN 201710764519 A CN201710764519 A CN 201710764519A CN 107445176 B CN107445176 B CN 107445176B
- Authority
- CN
- China
- Prior art keywords
- solution
- attapulgite
- powder
- hcl
- tin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000843 powder Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000004913 activation Effects 0.000 title abstract description 7
- 238000002955 isolation Methods 0.000 title abstract 2
- 229960000892 attapulgite Drugs 0.000 claims abstract description 44
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 44
- 239000000243 solution Substances 0.000 claims abstract description 42
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 25
- GVFOJDIFWSDNOY-UHFFFAOYSA-N antimony tin Chemical compound [Sn].[Sb] GVFOJDIFWSDNOY-UHFFFAOYSA-N 0.000 claims description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- RAOSIAYCXKBGFE-UHFFFAOYSA-K [Cu+3].[O-]P([O-])([O-])=O Chemical compound [Cu+3].[O-]P([O-])([O-])=O RAOSIAYCXKBGFE-UHFFFAOYSA-K 0.000 claims description 14
- 229910052802 copper Inorganic materials 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 229910019142 PO4 Inorganic materials 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 10
- 239000010452 phosphate Substances 0.000 claims description 10
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 3
- 239000000908 ammonium hydroxide Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 20
- 239000000463 material Substances 0.000 description 11
- 229920005989 resin Polymers 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 150000001879 copper Chemical class 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 238000007772 electroless plating Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229940116318 copper carbonate Drugs 0.000 description 4
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 230000020477 pH reduction Effects 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 235000010215 titanium dioxide Nutrition 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 239000004927 clay Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000007306 functionalization reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001465 metallisation Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- PEVJCYPAFCUXEZ-UHFFFAOYSA-J dicopper;phosphonato phosphate Chemical compound [Cu+2].[Cu+2].[O-]P([O-])(=O)OP([O-])([O-])=O PEVJCYPAFCUXEZ-UHFFFAOYSA-J 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B17/00—Insulators or insulating bodies characterised by their form
- H01B17/56—Insulating bodies
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
It can metallize the preparation method of powder the invention discloses tin Sb doped light color electrical isolation laser activation, including, attapulgite is mixed with HCl solution, mantoquita, formation mixed solution are added after standing；Ammonium hydroxide is slowly dropped in mixed solution, filtration washing after standing obtains solid；It will be calcined after solid drying.The light attapulgite powder of the electric insulation layer of tin Sb doped concave convex rod micro-porous adsorption mantoquita obtained by the present invention, pass through tin Sb doped compound, further decrease the influence to color, so that the light attapulgite powder of preparation can be applied to the occasion of particular color, the application range of product is expanded.
Description
Technical Field
The invention belongs to the technical field of electronics and electricity, and particularly relates to a preparation method of tin-antimony doped light-color electrically-insulated laser-activated metallizable powder.
Background
As some parts in the related field of electronics and electronics are developed toward miniaturization, functionalization and integration, it is necessary to integrate a conductive circuit on an electronic device to meet various requirements of the electronic device, especially to meet three-dimensional design requirements of a circuit diagram. In the process of manufacturing an ultra-fine circuit pattern (MID), Laser Direct Structuring (LDS) is the most effective, most advanced and most potential technical means, which is to directly transfer a design pattern to the surface of a workpiece by performing laser lithography on a resin material containing a laser sensitive additive, and simultaneously make an illumination area platable. The computer controls the movement of the laser beam over the part to activate the plastic surface where the conductive path is to be placed, creating an electronic circuit after electroless plating. By means of the laser direct structuring method, the width of the conducting paths can be 150 microns or less, the space available for the carrier is increased, in addition, the interval between the conducting paths can also be 150 microns or less, parts such as circuit boards and the like are omitted, and the space and the weight of electronic parts are saved by the formed circuit diagram. Another advantage of laser direct structuring is design flexibility, which allows direct modification of circuit patterns using drawing software such as CAD; antenna routing may also be implemented in areas (rounded corners, small gaps, etc.) that some conventional antennas cannot involve.
In order to overcome the defects and shortcomings of the prior art and avoid potential environmental risks, the invention needs to provide nano functional powder which does not contain heavy metal chromium and has selective deposited metal, can be subjected to composite functionalization with various resin-based materials, is finally molded by processes such as injection molding, molding and the like to obtain a required assembly, and realizes metallization of an electronic circuit structure after certain processes such as laser activation, chemical plating and the like.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above and/or the technical gap in the existing methods for preparing tin-antimony doped, light-colored, electrically insulated, laser-activated metallizable powders.
Therefore, the invention aims to solve the defects in the prior art and provide a preparation method of tin-antimony doped light-color electrically-insulated laser-activated metallizable powder.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of tin-antimony doped light-color electrically-insulated laser-activated metallizable powder comprises mixing attapulgite with a first HCl solution, standing, and adding copper salt to form a mixed solution; SnCl4And SbCl3Adding the mixture into a second HCl solution to form a mixed pre-solution; slowly dropwise adding ammonia water and the mixed pre-solution into the mixed solution, keeping the pH constant in the process, standing, filtering and washing to obtain a solid; the solid is dried and then calcined.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the above-mentionedSnCl4With SbCl3The mass ratio of (A) to (B) is 4-10: 1, and the SnCl4The mass ratio of the second HCl solution to the second HCl solution is 0.5-1: 1.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the concentration of the second HCl is 1-4 mol/L.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the copper salt comprises one or more of copper phosphate, copper pyrophosphate, copper chloride, copper carbonate or basic copper phosphate.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the concentration of the first HCl solution is 0.1-1 mol/L.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the addition amount of the attapulgite is 15-30 g per liter of the HCl solution.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the concentration of the ammonia water is 13.3-14.8 mol/L, and the molar ratio of the ammonia water to the copper salt is 4-4.5: 1.
as a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: slowly dripping ammonia water and the mixed solution into the mixed solution, wherein the mixed solution needs to be stirred in the dripping process, and the stirring speed is 50-70 rpm; the dropping speed of the slow dropping is 0.01-0.1 ml/s.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the attapulgite is 500-700 nm in length and 15-30 nm in width.
As a preferred embodiment of the method for preparing tin-antimony doped light-colored electrically-insulated laser-activated metallizable powder according to the present invention, wherein: the concentration of the copper salt in the mixed solution is 0.01-1 mol/L.
The invention has the following beneficial effects:
(1) the light-colored attapulgite powder of the electrical insulating layer for copper salt adsorption of the stannum-stibium-doped attapulgite micropores, prepared by the invention, overcomes the defects of high heavy metal content, high cost and the like of the existing LDS laser sensitive additive.
(2) The technology aims at the preparation of laser-activated metallized nano powder, the obtained attapulgite powder is used for a resin material with direct laser structuring, and the manufacturing of an electronic device superfine circuit pattern (MID) is realized through processes such as molding, laser activation, chemical plating and the like.
(3) The invention provides a novel preparation method for functionalizing tin-antimony doped light-colored attapulgite powder aiming at light-colored electrically-insulated nano powder capable of being subjected to laser activation metallization.
(4) The influence on the color is further reduced by the tin-antimony doped compound, so that the prepared light-color attapulgite powder can be applied to occasions with specific colors, such as apple white and the like.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
weighing 10g of attapulgite (the length is 500-700 nm, the width is 15-30 nm), adding the attapulgite into 0.5mol/L HCl solution (0.5L) for acidification, soaking for 1.5h, and adding 0.035mol of copper phosphate to obtain a copper phosphate mixed solution with the concentration of 0.07 mol/L.
6.1g of SnCl4And 1g of SbCl3The mixture was added to 2mol/L HCl to prepare a pre-mixture.
Slowly dropwise adding ammonia water (the concentration of the ammonia water is 14.8mol/L) into an HCl-copper phosphate solution containing attapulgite at a molar ratio of the ammonia water to copper phosphate of 4.2:1, wherein the dropping speed is 0.1ml/s, and simultaneously dropwise adding the prepared mixed pre-solution, keeping the pH of the system unchanged in the dropwise adding process, stirring the HCl-copper phosphate solution while dropwise adding, and the stirring speed is 60 rpm; after the dripping is finished, standing for 3 hours to prepare a seed crystal solution for later use; filtering, washing the obtained solid with deionized water, drying the obtained solid in a vacuum drying oven at 70 ℃ for 24 hours, and then calcining in a muffle furnace (250 ℃ for 6 hours); grinding to obtain light-color electrically insulating powder, uniformly mixing the electrically insulating powder with a resin material and other auxiliaries, and pressing the mixture by using a hot press and a forming die to obtain a sample, wherein the components are shown in the table below.
| Raw material | Example 1 |
| Epoxy resin | 37％ |
| Curing agent | 37％ |
| The obtained light-colored electrically insulating powder | 10％ |
| Accelerator | 1％ |
| Titanium white powder | 10％ |
| Fumed silica | 2％ |
| Talcum powder | 3％ |
| Plating time | 20min |
| Completion time | 40min |
| Baige test | Qualified |
After irradiation with 1064nm laser (16W/100 kHz laser parameters), electroless plating was carried out in an electroless copper plating bath at a plating index of 0.70.
Example 2:
weighing 15g of attapulgite (the length is 500-700 nm, the width is 15-30 nm), adding the attapulgite into 0.5mol/L HCl solution (0.5L) for acidification, soaking for 1.5h, and adding 0.064mol of copper phosphate to obtain a copper phosphate mixed solution with the concentration of 0.128 mol/L.
6.1g of SnCl4And 1g of SbCl3The mixture was added to 2mol/L HCl to prepare a pre-mixture.
Slowly dropwise adding ammonia water (the concentration of the ammonia water is 13.3mol/L) into an HCl-copper phosphate solution containing attapulgite at the molar ratio of the ammonia water to copper phosphate of 4.5:1, wherein the dropping speed is 0.05ml/s, and simultaneously dropwise adding the prepared mixed pre-solution, keeping the pH of the system unchanged in the dropwise adding process, stirring the HCl-copper phosphate solution while dropwise adding, and the stirring speed is 70 rpm; after the dripping is finished, standing for 3 hours to prepare a seed crystal solution for later use; filtering, washing the obtained solid with deionized water, drying the obtained solid in a vacuum drying oven at 65 ℃ for 28h, and calcining in a muffle furnace (320 ℃ for 4 h); grinding to obtain light-color electrically insulating powder, uniformly mixing the electrically insulating powder with a resin material and other auxiliaries, and pressing the mixture by using a hot press and a forming die to obtain a sample, wherein the components are shown in the table below.
| Raw material | Example 1 |
| Epoxy resin | 37％ |
| Curing agent | 37％ |
| The obtained light-colored electrically insulating powder | 10％ |
| Accelerator | 1％ |
| Titanium white powder | 10％ |
| Fumed silica | 2％ |
| Talcum powder | 3％ |
| Plating time | 25min |
| Completion time | 45min |
| Baige test | Qualified |
After irradiation with 1064nm laser (16W/100 kHz laser parameters), electroless plating was carried out in an electroless copper plating bath at a plating index of 0.88.
Example 3:
weighing 7.5g of attapulgite (the length is 500-700 nm, the width is 15-30 nm), adding the attapulgite into 0.5mol/L HCl solution (0.5L) for acidification, soaking for 1.5h, and adding 0.02mol of copper phosphate to obtain a copper phosphate mixed solution with the concentration of 0.04 mol/L.
4.6g SnCl4And 1g of SbCl3The mixture was added to 2mol/L HCl to prepare a pre-mixture.
Slowly dropwise adding ammonia water (the concentration of the ammonia water is 14.8mol/L) into an HCl-copper phosphate solution containing attapulgite at a molar ratio of the ammonia water to copper phosphate of 4.5:1, wherein the dropping speed is 0.1ml/s, and simultaneously dropwise adding the prepared mixed pre-solution, keeping the pH of the system unchanged in the dropwise adding process, stirring the HCl-copper phosphate solution while dropwise adding, and the stirring speed is 50 rpm; after the dripping is finished, standing for 3 hours to prepare a seed crystal solution for later use; filtering, washing the obtained solid with deionized water, drying the obtained solid in a vacuum drying oven at 75 ℃ for 28h, and calcining in a muffle furnace (400 ℃ for 4 h); grinding to obtain light-color electrically insulating powder, uniformly mixing the electrically insulating powder with a resin material and other auxiliaries, and pressing the mixture by using a hot press and a forming die to obtain a sample, wherein the components are shown in the table below.
| Raw material | Example 1 |
| Epoxy resin | 37％ |
| Curing agent | 37％ |
| The obtained light-colored electrically insulating powder | 10％ |
| Accelerator | 1％ |
| Titanium white powder | 10％ |
| Fumed silica | 2％ |
| Talcum powder | 3％ |
| Plating time | 30min |
| Completion time | 50min |
| Baige test | Qualified |
After irradiation with 1064nm laser (16W/100 kHz laser parameters), electroless plating was carried out in an electroless copper plating bath at a plating index of 0.68.
Example 4:
weighing 7.5g of attapulgite (the length is 500-700 nm, the width is 15-30 nm), adding the attapulgite into 0.2mol/L HCl solution (0.5L) for acidification, soaking for 1.5h, and adding 0.04mol of copper carbonate to obtain a copper carbonate mixed solution with the concentration of 0.08 mol/L.
4.6g SnCl4And 1g of SbCl3The mixture was added to 2mol/L HCl to prepare a pre-mixture.
Slowly dropwise adding ammonia water (the concentration of the ammonia water is 14.8mol/L) into an HCl-copper phosphate solution containing attapulgite at the mol ratio of the ammonia water to copper carbonate of 4.2:1, wherein the dropping speed is 0.1ml/s, and simultaneously dropwise adding the prepared mixed solution, keeping the pH of the system unchanged in the dropwise adding process, stirring the HCl-copper phosphate solution while dropwise adding, and the stirring speed is 60 rpm; after the dripping is finished, standing for 3 hours to prepare a seed crystal solution for later use; filtering, washing the obtained solid with deionized water, drying the obtained solid in a vacuum drying oven at 70 ℃ for 24 hours, and then calcining in a muffle furnace (300 ℃, 10 hours); grinding to obtain light-color electrically insulating powder, uniformly mixing the electrically insulating powder with a resin material and other auxiliaries, and pressing the mixture by using a hot press and a forming die to obtain a sample, wherein the components are shown in the table below.
| Raw material | Example 1 |
| Epoxy resin | 37％ |
| Curing agent | 37％ |
| The obtained light-colored electrically insulating powder | 10％ |
| Accelerator | 1％ |
| Titanium white powder | 10％ |
| Fumed silica | 2％ |
| Talcum powder | 3％ |
| Plating time | 32min |
| Completion time | 54min |
| Baige test | Qualified |
After irradiation with 1064nm laser (16W/100 kHz laser parameters), electroless plating was carried out in an electroless copper plating bath at a plating index of 0.76.
The optimized attapulgite overcomes the defects of high heavy metal content, high cost and the like of the existing LDS laser sensitive additive. More rarely, the length and width of the attapulgite clay preferred by our invention are the specific size, so that the attapulgite clay can absorb more than 97% of copper ions, and after pretreatment, the attapulgite clay can form excellent interface combination with resin materials, and plays a role of physical entanglement, thereby enhancing the mechanical properties of the materials. If not, brittle characteristics will appear. Further, the preferable amount of attapulgite in the invention of our invention can disperse the attapulgite uniformly in the HCl solution, when ammonia is dripped, the dropping speed of the ammonia and the stirring speed of the mixed solution are optimized, the two conditions and the addition amount of the attapulgite can form a synergistic effect, the specific stirring speed can ensure that the attapulgite with the specific addition amount of the attapulgite is continuously subjected to pressure brought by the wall of a container in the mixed solution, at the moment, the ammonia is specifically selected instead of sodium hydroxide to be added at the specific dropping speed, the energy generated by the neutralization reaction in the mixed solution can properly impact the pores of the attapulgite, more porous structures are formed mildly, the action area during electroplating is increased, thereby improving the binding force between the light-color electric insulation powder prepared during electroplating and the plating layer and leading the plating index to reach a high level in the chemical plating process. The influence on the color is further reduced by the tin-antimony doped compound, so that the prepared light-color attapulgite powder can be applied to occasions with specific colors, and the application range of the product is greatly expanded.
Therefore, the light-colored attapulgite powder of the electric insulating layer for adsorbing the copper salt by the attapulgite micropores overcomes the defects of high heavy metal content, high cost and the like of the traditional LDS laser sensitive additive. The technology aims at the preparation of laser-activated metallized nano powder, the obtained attapulgite powder is used for a resin material with direct laser structuring, and the manufacturing of an electronic device superfine circuit pattern (MID) is realized through processes such as molding, laser activation, chemical plating and the like. The invention provides a novel preparation method for light-colored attapulgite powder functionalization aiming at light-colored electrical insulation and laser activation metallization nanometer powder preparation, the method reduces the consumption of LDS powder, and the size and the special structure of the attapulgite improve the binding force of a chemical plating layer, the plating index and the precision of a circuit for materials. The influence on the color is further reduced by the tin-antimony doped compound, so that the prepared light-color attapulgite powder can be applied to occasions with specific colors, such as apple white and the like.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (1)
1. A preparation method of tin-antimony doped light-color electrically-insulated laser-activated metallizable powder is characterized by comprising the following steps of: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
mixing attapulgite with 0.5mol/L HCl solution, standing, and adding copper phosphate to form a mixed solution with the concentration of the copper phosphate being 0.128 mol/L;
SnCl4And SbCl3Adding the mixture into 2mol/L HCl solution to form mixed pre-solution;
slowly dripping 13.3mol/L ammonia water into an HCl-copper phosphate solution containing attapulgite according to a molar ratio of the ammonia water to copper phosphate of 4.5:1, wherein the dripping speed is 0.05ml/s, simultaneously dripping the prepared mixed pre-solution, keeping the pH of the system unchanged in the dripping process, stirring the HCl-copper phosphate solution while dripping, keeping the stirring speed at 70rpm, standing for 3 hours after finishing dripping to obtain a seed crystal solution, filtering, washing the obtained solid with deionized water, drying in a vacuum drying oven at 65 ℃ for 28 hours, then calcining in a 320 ℃ muffle furnace for 4 hours, and grinding to obtain light-color electric insulation powder; wherein,
the addition amount of the attapulgite is 30g per liter of the HCl solution;
the SnCl4With SbCl3In a mass ratio of 6.1:1, the SnCl4The mass ratio of the HCl solution to 2mol/L HCl solution is 0.5-1: 1;
the attapulgite is 500-700 nm in length and 15-30 nm in width.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710764519.0A CN107445176B (en) | 2017-08-30 | 2017-08-30 | Tin Sb doped light color electrical isolation laser activation can metallize the preparation method of powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710764519.0A CN107445176B (en) | 2017-08-30 | 2017-08-30 | Tin Sb doped light color electrical isolation laser activation can metallize the preparation method of powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107445176A CN107445176A (en) | 2017-12-08 |
| CN107445176B true CN107445176B (en) | 2019-11-19 |
Family
ID=60494596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710764519.0A Active CN107445176B (en) | 2017-08-30 | 2017-08-30 | Tin Sb doped light color electrical isolation laser activation can metallize the preparation method of powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107445176B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1894043A (en) * | 2003-10-15 | 2007-01-10 | 托尔萨公司 | Method of preparing metallic nanoparticles and materials thus obtained |
| CN101264445A (en) * | 2008-05-08 | 2008-09-17 | 南开大学 | A kind of supported nano-catalyst and preparation method thereof for low-temperature carbon monoxide oxidation |
| CN101288847A (en) * | 2008-06-18 | 2008-10-22 | 山东齐鲁华信高科有限公司 | Attapulgite clay loaded copper oxide catalyst and its application in carbon monoxide oxidation |
| CN102500372A (en) * | 2011-09-30 | 2012-06-20 | 合肥工业大学 | Copper oxide loaded attapulgite catalyst and preparation method and applications thereof |
| CN104192856A (en) * | 2014-08-21 | 2014-12-10 | 江苏启弘新材料科技有限公司 | Preparation method of light-coloured conductive nano-montmorillonite powder |
| CN105396605A (en) * | 2015-11-09 | 2016-03-16 | 常州大学 | Preparation method of silicate clay/copper/carbon nitride composite material |
| CN106237982A (en) * | 2016-10-25 | 2016-12-21 | 安庆师范大学 | CuO/ attapulgite catalyst-sorbent and for removing the method for Elemental Mercury in flue gas |
| CN106423061A (en) * | 2016-10-29 | 2017-02-22 | 吴迪 | Preparation method of composite high-activity demercuration adsorbent |
-
2017
- 2017-08-30 CN CN201710764519.0A patent/CN107445176B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1894043A (en) * | 2003-10-15 | 2007-01-10 | 托尔萨公司 | Method of preparing metallic nanoparticles and materials thus obtained |
| CN101264445A (en) * | 2008-05-08 | 2008-09-17 | 南开大学 | A kind of supported nano-catalyst and preparation method thereof for low-temperature carbon monoxide oxidation |
| CN101288847A (en) * | 2008-06-18 | 2008-10-22 | 山东齐鲁华信高科有限公司 | Attapulgite clay loaded copper oxide catalyst and its application in carbon monoxide oxidation |
| CN102500372A (en) * | 2011-09-30 | 2012-06-20 | 合肥工业大学 | Copper oxide loaded attapulgite catalyst and preparation method and applications thereof |
| CN104192856A (en) * | 2014-08-21 | 2014-12-10 | 江苏启弘新材料科技有限公司 | Preparation method of light-coloured conductive nano-montmorillonite powder |
| CN105396605A (en) * | 2015-11-09 | 2016-03-16 | 常州大学 | Preparation method of silicate clay/copper/carbon nitride composite material |
| CN106237982A (en) * | 2016-10-25 | 2016-12-21 | 安庆师范大学 | CuO/ attapulgite catalyst-sorbent and for removing the method for Elemental Mercury in flue gas |
| CN106423061A (en) * | 2016-10-29 | 2017-02-22 | 吴迪 | Preparation method of composite high-activity demercuration adsorbent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107445176A (en) | 2017-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101280125B (en) | Production method of superfine silicon powder for electronic grade low-heat expansion coefficient copper clad laminate | |
| JP2911429B2 (en) | Production method of copper fine powder | |
| KR20120082820A (en) | Method for the selective metallization of a substrate and a circuit carrier produced according to this method | |
| WO2008029376A3 (en) | Deposition of conductive polymer and metallization of non-conductive substrates | |
| CN108326293B (en) | Method for producing silver-coated nickel powder | |
| CN107445176B (en) | Tin Sb doped light color electrical isolation laser activation can metallize the preparation method of powder | |
| CN107172819A (en) | The method that high frequency flexible print circuit board is made using ion implanting and plating mode | |
| CN104974468A (en) | Thermosetting laser-induced metallization thermal-conduction composite material with stable high dielectric constant | |
| KR20150095834A (en) | Method for producing an electrically conductive structure on a non-conductive substrate material, and additive and substrate material intended therefor | |
| CN107500304B (en) | Preparation method of light-color electrically-insulated laser-activated metallizable powder | |
| KR100931248B1 (en) | Method of manufacturing antenna function using copper plating, nickel plating and gold plating on circuit pattern by double injection method of transceiver housing | |
| CN104005027B (en) | A kind of metallized method of siliceous epoxy resin surface | |
| KR20090049692A (en) | Manufacturing method of fabric with plated conductive metal | |
| CN102508583B (en) | Preparation method for metal lead of capacitance type touch screen | |
| WO2014038839A1 (en) | Method for manufacturing highly functional thin film material made of two kinds of materials | |
| TWI669413B (en) | Metallization method of dielectric substrate surface and dielectric substrate with metal film | |
| CN111768893B (en) | Yellowing-resistant low-temperature sintered silver paste and preparation method thereof | |
| CN104582278B (en) | A kind of circuit board and preparation method thereof | |
| CN103915684A (en) | Conductive circuit manufacturing method, mobile phone antenna manufacturing method and mobile phone antenna | |
| CN104674542A (en) | Laser direct structured flexible fabric | |
| CN102543261A (en) | Electrode silver paste for ferrite magnetic core, preparation method and application thereof | |
| CN103022664B (en) | Three-dimensional antenna manufacture method | |
| CN111524697A (en) | Preparation method of 35 carbonyl iron powder core with magnetic conductivity | |
| CN113025230A (en) | Heat-conducting and electric-conducting copper paste, preparation method and application thereof | |
| TWI544847B (en) | Chemical plating product and method forming thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |