CN108219537A - A kind of novel macreous pigment and preparation method thereof - Google Patents
A kind of novel macreous pigment and preparation method thereof Download PDFInfo
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- CN108219537A CN108219537A CN201711382816.5A CN201711382816A CN108219537A CN 108219537 A CN108219537 A CN 108219537A CN 201711382816 A CN201711382816 A CN 201711382816A CN 108219537 A CN108219537 A CN 108219537A
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- Prior art keywords
- aluminium
- sputtering
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- natural
- pigment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
- C01P2006/37—Stability against thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/10—Interference pigments characterized by the core material
- C09C2200/102—Interference pigments characterized by the core material the core consisting of glass or silicate material like mica or clays, e.g. kaolin
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/40—Interference pigments comprising an outermost surface coating
- C09C2200/401—Inorganic protective coating
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/20—PVD, CVD methods or coating in a gas-phase using a fluidized bed
Abstract
The present invention relates to the novel macreous pigments that a kind of clad is aluminium nitride.The clad is plated to substrate layer surface by reactive sputtering process.Using metallic aluminium of the purity higher than 98% as sputtering target material, 7 10A of sputtering current, 20 60min of sputtering time, using nitrogen of the purity higher than 99% as reaction gas, nitrogen is 0.25~1 with argon gas volume flow ratio.Beneficial effects of the present invention：(1) it is environmentally protective；(2) cost is reduced；(3) wearability is good；(4) stability is good.
Description
Technical field：
The present invention relates to a kind of pearly-lustre face of a kind of pearlescent pigment and preparation method thereof more particularly to clad for aluminium nitride
Material and preparation method thereof.
Technical background：
Pearly-lustre class pigment is widely used in the fields such as plastics, colored paint, cosmetics.Existing artificial synthesized pearly-lustre class pigment
Cladded type structure is used mostly：Laminated structure of the internal layer for low-refraction, such as mica sheet, glass flake；It is coated on outer layer
It is one or more layers high refractive index layer, such as titanium dioxide, di-iron trioxide.
Aluminium nitride film has many advantages, such as high refractive index, high-transmission rate, low extinction coefficient, can be applied to pearly-lustre class pigment
External sheath.In the optical property research of aluminium nitride, Yim et al. obtains the aluminium nitride of high quality, polycrystalline aluminum nitride film
Refractive index is about 1.9；Single-crystal aluminum nitride refractive index is about 2.2；Epitaxial nitride aluminium film refractive index is about 2.1；Non- crystalline aluminum nitride
Film refractive index is about 1.8.
Aluminium nitride is in nature and is not present, until 1862 Christian eras ability is by two scholars of Geuther and Briegleb
It is obtained with liquid aluminium and nitrogen reaction synthesis.Aluminium nitride product is mostly powder particle form on the market, using aluminium powder in elevated pressure nitrogen
Conbustion synthesis in gas, the synthesis technology are dfficult to apply to pearlescent pigment external sheath, so while aluminium nitride film has high roll over
The advantages that penetrating rate, high-transmission rate, low extinction coefficient, but the pearlescent pigment for rarely having external sheath to be aluminium nitride film layer on the market.
From generation 30 or 40 years in last century, research workers produce film, and in 60 or seven ten years using sputtering experiment for the first time
Generation realize commercial Application since, in short many decades by its it is unique deposition raw material and in a manner of rapidly develop, new technique skill
Art constantly improve, and the new function material prepared with such method also emerges in an endless stream.Sputtering is the incoming particle with high energy
The process of target is bombarded, needing to be passed through a small amount of inert gas (such as argon gas) in vacuum system makes its electric discharge generate ion, inertia
Gas ion bombards target after electric field acceleration, and part momentum is passed to target atom, sputters out target atom, reaches
Film is formed on substrate.Meanwhile in sputtering process, lead to simultaneously into a small amount of active gases (reaction gas) in vacuum cavity, make
Sputtering particle is chemically reacted with active gases, by the way that deposition characteristics are modified or controlled, obtains the novel substance different from target
Film, the technical process, that is, reactive sputtering.
Invention content：
The invention mainly relates to a kind of novel macreous pigments and preparation method thereof.A kind of novel macreous pigment includes hypothallus
And clad.
The hypothallus includes natural mica, artificial mica synthesis, native graphite, Delanium, natural kyanite, natural
Garnet, natural pyrophyllite, natural talcum, wollastonite, Er Liuization Molybdenum, glass flake, hollow glass micropearl, flaky crystal oxidation
Aluminium, metal aluminium flake, high molecular polymer thin slice, artificial synthesized silicon wafer, quartz sand, enamel, alundum (Al2O3), cube nitridation
Boron, silicon carbide, calcite etc.；0.1~500 μm of particle size range.
The clad is nitridation aluminium coat, and thickness is 0.01~1 μm.
The clad is plated to substrate layer surface by reactive sputtering process.It is higher than 98% metallic aluminium conduct using purity
Sputtering target material, sputtering current 7-10A, sputtering time 20-60min, using nitrogen of the purity higher than 99% as reaction gas, nitrogen
Gas is 0.25~1 with argon gas volume flow ratio.
Beneficial effects of the present invention：(1) it is environmentally protective：Nitridation aluminium pill delustering pigment, reaction are synthesized with reactive sputtering process
Simply, no waste generates；(2) cost is reduced：Traditional pearlescent pigment multiselect selects nitridation by the use of titanium dioxide as clad
Clad of the aluminium as pearlescent pigment, it is only necessary to which product can be greatly lowered as main consumptive material in cheap aluminium and nitrogen
Cost；(3) wearability is good：Aluminium nitride rigidity is very high, close to the hardness of quartz, can effectively improve such pearlescent pigment and exist
Wear-resisting property during processing and use；(4) stability is good：Aluminium nitride material is not higher than 700 DEG C of air environment in temperature
In it is highly stable, can improve such pearlescent pigment thermal stability by clad of aluminium nitride.
Specific embodiment：
Embodiment 1：
By 10~30 microns of mica sheet powder merging magnetron sputtered vacuum inside cavities of 50g, vacuumize, be passed through 50sccm
Argon gas and 25sccm nitrogen.Using the metallic aluminium that purity is 99.5% as sputtering target material, sputtering current is set as 8A, control is reacted
Sputtering time 20min, in about 1 micron of nitridation aluminium coat of mica sheet surface cladding thickness.After, powder is taken out, obtain 10~
30 microns of natural mica matrix aluminium nitride pearlescent pigments.The aluminium nitride pearlescent pigment appearance color is milky, shows pearly-lustre effect
Fruit is similar with market equal grain size pearlescent pigment effect on sale.
Embodiment 2：
90~230 urn glass scale powders of 60g are placed in magnetron sputtered vacuum inside cavity.It vacuumizes, is passed through
70sccm argon gas and 42sccm nitrogen.It is 99.9% metallic aluminium as sputtering target material using purity, sets sputtering current as 10A.
Reactive sputtering time 30min is controlled, in about 0.1 micron of nitridation aluminium coat of glass flake surface cladding thickness.After, take out powder
Body obtains 90~230 urn glass scale matrix aluminium nitride pearlescent pigments.The aluminium nitride pearlescent pigment, flickering acutance is high, appearance
Color is transparent slightly milky, and the appearance glass baseplate class pearlescent pigment on sale with market approaches.
Embodiment 3：
90~230 urn glass scale powders of 20g are placed in magnetron sputtered vacuum inside cavity.It vacuumizes, is passed through
40sccm argon gas and 16sccm nitrogen.It is 99.8% metallic aluminium as sputtering target material using purity, sets sputtering current as 7A.Control
Reactive sputtering time 60min processed, in about 0.5 micron of nitridation aluminium coat of glass flake surface cladding thickness.After, take out powder
Body obtains 1~10 micron of artificial mica synthesis matrix aluminium nitride pearlescent pigment.The aluminium nitride pearlescent pigment effect is fine and smooth, appearance face
Color is milky, and spraying effect is consistent with similary base material and grain size class pearlescent pigment that market is on sale.
Claims (6)
1. a kind of novel macreous pigment, it is characterised in that：Including hypothallus and clad, the clad is nitridation aluminium coat.
2. a kind of novel macreous pigment according to claim 1, it is characterised in that：The hypothallus include natural mica,
Artificial mica synthesis, native graphite, Delanium, natural kyanite, natural garnet, natural pyrophyllite, natural talcum, silicon ash
Stone, two sulphur Molybdenum, glass flake, hollow glass micropearl, flaky crystal aluminium oxide, metal aluminium flake, high molecular polymer thin slice, people
Work synthesis silicon wafer, quartz sand, enamel, alundum (Al2O3), cubic boron nitride, silicon carbide, calcite.
3. a kind of novel macreous pigment according to claim 1, it is characterised in that：The hypothallus grain size is 0.1~500
μm。
4. a kind of novel macreous pigment according to claim 1, it is characterised in that：The coating thickness is 0.1~1 μ
m。
5. a kind of method for preparing novel macreous pigment, includes the following steps：
(1) hypothallus powder is placed in magnetron sputtered vacuum inside cavity；
(2) it vacuumizes, is passed through nitrogen and argon gas, using metallic aluminium as sputtering target material, open sputtering current, control sputtering time,
In about 1 micron of nitridation aluminium coat of substrate layer surface cladding thickness.
(3) after sputtering, powder is taken out, obtains the pearlescent pigment that clad is aluminium nitride.
6. a kind of method for preparing novel macreous pigment according to claim 5, it is characterised in that：In the step (2)
Nitrogen is 0.25~1 with argon gas volume flow ratio, and sputtering target material aluminium purity is higher than 98%, sputtering current 7-10A, sputtering time
20-60min。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711382816.5A CN108219537A (en) | 2017-12-20 | 2017-12-20 | A kind of novel macreous pigment and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711382816.5A CN108219537A (en) | 2017-12-20 | 2017-12-20 | A kind of novel macreous pigment and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN108219537A true CN108219537A (en) | 2018-06-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201711382816.5A Pending CN108219537A (en) | 2017-12-20 | 2017-12-20 | A kind of novel macreous pigment and preparation method thereof |
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| CN (1) | CN108219537A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020215139A1 (en) | 2019-04-25 | 2020-10-29 | União Brasileira De Educação E Assistência | Equipment and method for depositing sprayed materials on particulate materials |
-
2017
- 2017-12-20 CN CN201711382816.5A patent/CN108219537A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020215139A1 (en) | 2019-04-25 | 2020-10-29 | União Brasileira De Educação E Assistência | Equipment and method for depositing sprayed materials on particulate materials |
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Application publication date: 20180629 |
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| WD01 | Invention patent application deemed withdrawn after publication |