CN107285643A - A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely - Google Patents

A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely Download PDF

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Publication number
CN107285643A
CN107285643A CN201710586962.3A CN201710586962A CN107285643A CN 107285643 A CN107285643 A CN 107285643A CN 201710586962 A CN201710586962 A CN 201710586962A CN 107285643 A CN107285643 A CN 107285643A
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CN
China
Prior art keywords
magnetic
glass microballoon
glass
aluminized
entirely
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Pending
Application number
CN201710586962.3A
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Chinese (zh)
Inventor
范春平
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HEFEI DINGLIANG OPTICAL TECHNOLOGY Co Ltd
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HEFEI DINGLIANG OPTICAL TECHNOLOGY Co Ltd
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Priority to CN201710586962.3A priority Critical patent/CN107285643A/en
Publication of CN107285643A publication Critical patent/CN107285643A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3649Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer made of metals other than silver
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3607Coatings of the type glass/inorganic compound/metal
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/25Metals
    • C03C2217/251Al, Cu, Mg or noble metals
    • C03C2217/252Al
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/20Materials for coating a single layer on glass
    • C03C2217/25Metals
    • C03C2217/261Iron-group metals, i.e. Fe, Co or Ni
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/73Anti-reflective coatings with specific characteristics
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/11Deposition methods from solutions or suspensions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/11Deposition methods from solutions or suspensions
    • C03C2218/112Deposition methods from solutions or suspensions by spraying

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemically Coating (AREA)

Abstract

A kind of preparation method for the reflective glass beads aluminized entirely the invention discloses magnetic, Technology of Chemical Composite Plating is used in the present invention first, magnetic Ni P alloy-layers are provided with the surface of glass microballoon core, after through high temperature plating twice handle, aluminium coated is precipitated in alloyed layer, comprehensive aluminize is realized on glass microsphere surface, it can ensure after planting pearl processing, being not embedded into the glass microballoon surface attachment of beads formed film has aluminium coated, increase substantially its retro-reflecting coefficient, with excellent reflecting effect, there is magnetic using the product prepared by glass microballoon of the present invention, strengthen its performance, apply in terms of warning reflection labeling, it is easy to use, beneficial to replacing, cleaning is not resulted in difficult.

Description

A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely
Technical field
The present invention relates to the manufacturing technology field of reflective glass beads, and in particular to the rear reflector that a kind of magnetic is aluminized entirely The preparation method of microballon.
Background technology
Glass microballoon is the primary raw material for manufacturing reflectorized material, can be widely applied to highway, railway, airport, harbour, ocean fortune In the reflectorized material of the field such as defeated, mine, tunnel, fire-fighting, urban construction.Increasing with China to infrastructure construction dynamics of investment, The demand of glass microballoon is increasing, while to the performance requirement of glass microballoon also more and more higher.Current China only has minority Producer grasps the production technology of high refractive index glass micro pearl, and its properties of product is very unstable, and reflective function does not reach reality still Demand, it is impossible to meet market demands.
Therefore, in actual applications, all processing of aluminizing directly or indirectly can be carried out to glass microballoon surface, it is inverse to increase Reflecting effect.It is many at present to be aluminized or half aluminum plating glass microballon using part, in fields such as reflective ink, warning labeling, ornaments, rise To the effect of reflective warning, but in use, due to half aluminum plating glass microballoon, when planting pearl, pearl is inverse in random distribution Reflectance factor is greatly lowered.
More than reflecting mark plaster commonly used at present vehicle body, road mark post are fixed on by the way of adhesive tape or glue are pasted Deng surface, stick and be not easy to tear it down, cause cleaning difficult, and can not reuse, use cost is high.
The content of the invention
The preparation method for the reflective glass beads aluminized entirely the invention provides a kind of magnetic, in the table of glass microballoon core Face is provided with Ni-P alloy interlayers, and outer layer is provided with aluminium coated, with excellent retroreflective energy.
The present invention is achieved by the following technical solutions:
A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely, including step in detail below:
(1)Prepare plating solution:
By 2-8 parts of NiCl2·6H2O, 1-5 parts of sodium citrates, 0.1-1 parts of sodium potassium tartrate tetrahydrates are dissolved in 50-100 parts of distilled water, then Take the NaH that 50-150 parts of concentration are 3-5wt%2PO2·H2The O aqueous solution is added thereto, and is finally added 6-9 parts of concentration thereto again and is 25-28wt% ammoniacal liquor, obtains plating solution after stirring;
(2)Plating:
Glass microballoon is put into the plating solution of above-mentioned preparation after pretreatment, with 2-5 DEG C/min heating speed under stirring Rate is heated to being incubated 20-40 minutes after 67-75 DEG C, filters, with distillation water washing, the magnetic glass of cladding Ni-P alloy-layers is made Microballon;
(3)Plant pearl:
The acrylic resins of painting adhesive on PET film A, after being dried through 105-120 DEG C of drying tunnel, by step(2)Magnetic glass Microballon sticks to adhesive layer side;
(4)Once aluminize:
By step(3)Splash is carried out after basement membrane winding after planting pearl, in feeding vacuum coating equipment to glass microballoon side to aluminize, Make the glass microballoon part adhesion aluminium coated for exposing gluing oxidant layer;
(5)It is compound:
In PET basement membrane B surface adhesive coatings, after drying, will there are the one side and step of adhesive(4)Aluminium coated compound suppressing exists Together, glass microballoon is made to be completely embedded into gluing oxidant layer;
(6)Peel off and aluminize:
PET film A is divested, exposes the glass microballoon one side for not plating magnetic alloy, is then fed into devices of coiled vacuum coating machine In, under high vacuum state, aluminium coated is formed in glass microballoon side;
(7)PET basement membranes B is divested, adhesive is removed after being rinsed with water, dries, obtains the reflective glass beads that magnetic is aluminized entirely.
Wherein, the step(2)Glass microballoon is to use solid microbeads of the particle size range at 20-100 μm, and refractive index exists 1.90-2.21。
Wherein, the step(2)The pretreatment of glass microballoon refers to after conventional wash, acid-wash activation.
Wherein, the pretreatment concrete technology of the glass microballoon is as follows:The Na for being first 10-20wt% with concentration2CO3The aqueous solution Glass microballoon is cleaned, then is cleaned by ultrasonic 10-20 minutes with 2-10wt% aqueous hydrochloric acid solution, then after washing drying, Be put into the 0.5-2wt% HF aqueous solution, after processing 0.5-3 hour, then wash through EtOH Sonicate, drying.
Compared with prior art, Technology of Chemical Composite Plating is used in the present invention first, is set on the surface of glass microballoon core Be magnetic Ni-P alloy-layers, after through high temperature plating twice handle, alloyed layer precipitate aluminium coated, on glass microsphere surface Realize comprehensive aluminize, it is ensured that after planting pearl processing, being not embedded into the glass microballoon surface attachment of beads formed film has aluminium coated, Its retro-reflecting coefficient is increased substantially, with excellent reflecting effect, excellent eye-catching warning function is played;It is simultaneously micro- in glass Bead surface adheres to magnetic Ni-P alloy-layers, the certain magnetic of glass microballoon is imparted, using prepared by glass microballoon of the present invention Product has certain magnetic, strengthens its performance, applies in terms of warning reflection labeling, easy to use, will not beneficial to replacing Cause cleaning difficult.
Embodiment
A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely, including step in detail below:
(1)Prepare plating solution:
By 6 parts of NiCl2·6H2O, 3 parts of sodium citrates, 0.5 part of sodium potassium tartrate tetrahydrate are dissolved in 80 parts of distilled water, then take 80 parts of concentration For 5wt% NaH2PO2·H2The O aqueous solution is added thereto, and it is 25wt% ammoniacal liquor finally to add 6 parts of concentration thereto again, is stirred Obtain plating solution afterwards;
(2)Plating:
Glass microballoon is put into the plating solution of above-mentioned preparation after pretreatment, with 4 DEG C/min heating rate under stirring It is heated to being incubated 40 minutes after 70 DEG C, filters, with distillation water washing, the magnetic glass microballon of cladding Ni-P alloy-layers is made;
(3)Plant pearl:
The acrylic resins of painting adhesive on PET film A, after being dried through 110 DEG C of drying tunnels, by step(2)Magnetic glass microballon Stick to adhesive layer side;
(4)Once aluminize:
By step(3)Splash is carried out after basement membrane winding after planting pearl, in feeding vacuum coating equipment to glass microballoon side to aluminize, Make the glass microballoon part adhesion aluminium coated for exposing gluing oxidant layer;
(5)It is compound:
In PET basement membrane B surface adhesive coatings, after drying, will there are the one side and step of adhesive(4)Aluminium coated compound suppressing exists Together, glass microballoon is made to be completely embedded into gluing oxidant layer;
(6)Peel off and aluminize:
PET film A is divested, exposes the glass microballoon one side for not plating magnetic alloy, is then fed into devices of coiled vacuum coating machine In, under high vacuum state, aluminium coated is formed in glass microballoon side;
(7)PET basement membranes B is divested, adhesive is removed after being rinsed with water, dries, obtains the reflective glass beads that magnetic is aluminized entirely.
Wherein, the step(2)Glass microballoon is to use solid microbeads of the particle size range at 20-100 μm, and refractive index exists 1.90-2.21。
Wherein, the pretreatment concrete technology of the glass microballoon is as follows:The Na for being first 20wt% with concentration2CO3The aqueous solution pair Glass microballoon is cleaned, then is cleaned by ultrasonic 15 minutes with 8wt% aqueous hydrochloric acid solution, then after washing drying, is put into In the 0.8wt% HF aqueous solution, after processing 3 hours, then wash through EtOH Sonicate, dry.

Claims (4)

1. the preparation method for the reflective glass beads that a kind of magnetic is aluminized entirely, it is characterised in that including step in detail below:
(1)Prepare plating solution:
By 2-8 parts of NiCl2·6H2O, 1-5 parts of sodium citrates, 0.1-1 parts of sodium potassium tartrate tetrahydrates are dissolved in 50-100 parts of distilled water, then Take the NaH that 50-150 parts of concentration are 3-5wt%2PO2·H2The O aqueous solution is added thereto, and is finally added 6-9 parts of concentration thereto again and is 25-28wt% ammoniacal liquor, obtains plating solution after stirring;
(2)Plating:
Glass microballoon is put into the plating solution of above-mentioned preparation after pretreatment, with 2-5 DEG C/min heating speed under stirring Rate is heated to being incubated 20-40 minutes after 67-75 DEG C, filters, with distillation water washing, the magnetic glass of cladding Ni-P alloy-layers is made Microballon;
(3)Plant pearl:
The acrylic resins of painting adhesive on PET film A, after being dried through 105-120 DEG C of drying tunnel, by step(2)Magnetic glass Microballon sticks to adhesive layer side;
(4)Once aluminize:
By step(3)Splash is carried out after basement membrane winding after planting pearl, in feeding vacuum coating equipment to glass microballoon side to aluminize, Make the glass microballoon part adhesion aluminium coated for exposing gluing oxidant layer;
(5)It is compound:
In PET basement membrane B surface adhesive coatings, after drying, will there are the one side and step of adhesive(4)Aluminium coated compound suppressing exists Together, glass microballoon is made to be completely embedded into gluing oxidant layer;
(6)Peel off and aluminize:
PET film A is divested, exposes the glass microballoon one side for not plating magnetic alloy, is then fed into devices of coiled vacuum coating machine In, under high vacuum state, aluminium coated is formed in glass microballoon side;
(7)PET basement membranes B is divested, adhesive is removed after being rinsed with water, dries, obtains the reflective glass beads that magnetic is aluminized entirely.
2. the preparation method for the reflective glass beads that a kind of magnetic according to claims 1 is aluminized entirely, it is characterised in that The step(2)Glass microballoon is that refractive index is in 1.90-2.21 in 20-100 μm of solid microbeads using particle size range.
3. the preparation method for the reflective glass beads that a kind of magnetic according to claims 1 is aluminized entirely, it is characterised in that The step(2)The pretreatment of glass microballoon refers to after conventional wash, acid-wash activation.
4. the preparation method for the reflective glass beads that a kind of magnetic according to claims 1,3 is aluminized entirely, its feature exists In the pretreatment concrete technology of the glass microballoon is as follows:The Na for being first 10-20wt% with concentration2CO3The aqueous solution is to glass microballoon Cleaned, then be cleaned by ultrasonic 10-20 minutes with 2-10wt% aqueous hydrochloric acid solution, then after washing drying, be put into 0.5- In the 2wt% HF aqueous solution, after processing 0.5-3 hour, then wash through EtOH Sonicate, drying.
CN201710586962.3A 2017-07-18 2017-07-18 A kind of preparation method for the reflective glass beads that magnetic is aluminized entirely Pending CN107285643A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112608639A (en) * 2020-12-04 2021-04-06 浙江龙游道明光学有限公司 Preparation method of high-brightness colored microspheres

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101265032A (en) * 2008-04-18 2008-09-17 上海华威环保技术有限公司 Technique for plating nickel on glass particles surface
KR20120014467A (en) * 2010-08-09 2012-02-17 박원일 Glass bead and method for manufacturing glass bead
CN103823265A (en) * 2014-03-04 2014-05-28 四川中科倍特尔技术有限公司 Full-aluminizing high-refractive-index glass microbead as well as production process thereof
CN105776892A (en) * 2016-01-29 2016-07-20 中北大学 Magnetic Ag-plated glass bead and preparing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101265032A (en) * 2008-04-18 2008-09-17 上海华威环保技术有限公司 Technique for plating nickel on glass particles surface
KR20120014467A (en) * 2010-08-09 2012-02-17 박원일 Glass bead and method for manufacturing glass bead
CN103823265A (en) * 2014-03-04 2014-05-28 四川中科倍特尔技术有限公司 Full-aluminizing high-refractive-index glass microbead as well as production process thereof
CN105776892A (en) * 2016-01-29 2016-07-20 中北大学 Magnetic Ag-plated glass bead and preparing method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112608639A (en) * 2020-12-04 2021-04-06 浙江龙游道明光学有限公司 Preparation method of high-brightness colored microspheres
CN112608639B (en) * 2020-12-04 2021-10-22 浙江龙游道明光学有限公司 Preparation method of high-brightness colored microspheres

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