CN107778991A - One kind is without zirconium ultrawhite inkjet printing aqueous ceramic ink and preparation method thereof - Google Patents
One kind is without zirconium ultrawhite inkjet printing aqueous ceramic ink and preparation method thereof Download PDFInfo
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- CN107778991A CN107778991A CN201711064663.XA CN201711064663A CN107778991A CN 107778991 A CN107778991 A CN 107778991A CN 201711064663 A CN201711064663 A CN 201711064663A CN 107778991 A CN107778991 A CN 107778991A
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- powder
- ceramic ink
- zirconium
- ultrawhite
- inkjet printing
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/324—Inkjet printing inks characterised by colouring agents containing carbon black
- C09D11/326—Inkjet printing inks characterised by colouring agents containing carbon black characterised by the pigment dispersant
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to one kind without zirconium ultrawhite inkjet printing aqueous ceramic ink and preparation method thereof, by adding solvent and dispersant after nano-zinc oxide powder and nanometer hydroxyapatite powder mixing and ball milling, simultaneously ultrasonic disperse obtains ball milling the aqueous ceramic ink again.The present invention is mixed using two kinds of Inorganic white colorant zinc oxide and hydroxyapatite nano-powder, because two kinds of powder granule characteristics are different, intergranular interaction weakens, so as to avoid particle aggregation, therefore in the presence of dispersant, the uniform particle sizes of ceramic ink, average grain diameter are less than 290nm, after standing 8 days, ink is not without being layered and settle, stability is good, and the Hunter whiteness average value decorated after glaze paint is more than 92, meets the requirement of ceramic ink jet printing ink.
Description
Technical field
The present invention relates to one kind without zirconium super white ceramic ink and preparation method thereof, it is mainly used in ceramic ink jet printing, belongs to
Ceramic ink field.
Background technology
Ceramic ink jet printing technology is a kind of contactless, without printing plate printing technology, and electronic image directly can made pottery
Porcelain is imaged on surface, is matched colors by intellectuality, is made pattern well arranged, in a short time can complete small lot, multi-color
Experiment or production.Than screen printing and roller printing, inkjet technology has efficient convenient, energy-conserving and environment-protective advantages, is
A kind of ceramic decoration technology of great application value.Ceramic ink is the core of ceramic ink jet printing technology, is researched and developed at present
The ceramic ink of work(has as many as 14 kinds, including blueness, brown, yellow, pink colour etc..Such as Chinese invention patent《A kind of ink-jet is beaten
Print Red ceramic ink and its application method》(CN103045003 A) discloses one kind by soluble metal complex and had
The inkjet printing Red ceramic ink of solvent composition.Chinese invention patent《Inkjet printing Yellow ceramic ink》(CN
103342917 B) disclose a kind of inkjet printing use being made up of inorganic color powder, surfactant, solvent and dispersant
Yellow ceramic ink.Chinese invention patent《A kind of preparation method of blue ceramic ink》(A of CN 106009897) discloses one
The preparation method of kind inkjet printing blue ceramic ink.
At present, the research about whiteware ink is mostly to contain zirconium, titaniferous oily ink using organic matter as additive, in vain
Degree and stability are difficult to be guaranteed.Such as Chinese invention patent《Oil-based white ink for inkjet recording》(CN 101027370
B one kind) is disclosed using titanium oxide as ceramic pigment, and addition resin, organic solvent and nonionic surfactant are made into oiliness
White ink.Chinese invention patent《A kind of ceramic ink jet printing white enamel ink and preparation method thereof》(CN
103224725 B) disclose a kind of oil-based white ink compound with many oxides such as silica, aluminum oxide.Oily ink
The problems such as organic solvent is poisonous be present, water-miscible organic solvent is the developing direction of ceramic ink from now on.Chinese invention patent《One
Kind extra white aqueous ceramic jetted ink and preparation method thereof》(B of CN 103804993) discloses one kind and uses collosol and gel legal system
The aqueous white ink of standby zirconium oxide and silica mixing colorant.Zirconium oxide as inkjet printing with white material have whiteness it is high,
The advantages that stability is good, but zirconium, easily with hafnium symbiosis, hafnium has certain radioactivity, and zirconium oxide prepares cost height, therefore develops few
Zirconium or white water-borne ceramic ink without zirconium have the meaning of energy-conserving and environment-protective.
The content of the invention
The technical problems to be solved by the invention are for above shortcomings in the prior art, there is provided a kind of whiteness
It is high, ink rheological characteristic is good, suitable for ceramic ink jet printing ultrawhite without zirconium water-based ink-jet printing ceramic ink and its preparation side
Method.
In order to solve the above technical problems, technical scheme provided by the invention is：
One kind is provided without zirconium ultrawhite inkjet printing aqueous ceramic ink, the aqueous ceramic ink is by nano zinc oxide powder
Solvent and dispersant are added behind end and nanometer hydroxyapatite powder mixing and ball milling, and simultaneously ultrasonic disperse obtains ball milling again.
By such scheme, the nano-zinc oxide powder average grain size is 21.9~61.8nm, by following methods system
It is standby to obtain：Triammonium citrate powder is added into the acetic acid zinc solution that concentration is 0.1~0.3mol/L, is uniformly mixing to obtain transparent
Solution, zinc hydroxide suspension is obtained after adding absolute ethyl alcohol, with ammonia spirit adjust zinc hydroxide suspension pH value to 8~
10, zinc hydroxide suspension is then heated into 2~4h in 60~80 DEG C and obtains colloidal sol, is calcined after colloidal sol is dried and obtains nano oxygen
Change zinc powder.
By such scheme, zinc acetate and Triammonium citrate mass ratio are 50~60 in the clear solution：40~50.
By such scheme, the drying temperature is 80~100 DEG C, and drying time is 5~10h, and the calcining heat is 500
~700 DEG C, calcination time is 8~12h.
By such scheme, the nanometer hydroxyapatite powder average grain size is 21.9~61.8nm, by with lower section
Method is prepared：By Ca (NO3)2Solution and (NH4)2HPO4Solution is mixed to get mixed liquor, and pH of mixed is adjusted with ammonia spirit
Then mixed liquor is heated 2~4h in 60~80 DEG C and obtains gel, calcining after gel drying is obtained into a nanometer hydroxyl by value to 8~10
Base apatite powder.
By such scheme, the Ca (NO3)2Solution and (NH4)2HPO4Liquor capacity concentration is 40~60%.
By such scheme, the drying temperature is 80~100 DEG C, and drying time is 5~10h, and the calcining heat is 600
~700 DEG C, calcination time is 8~12h.
The present invention also provides the preparation method of above-mentioned no zirconium ultrawhite inkjet printing aqueous ceramic ink, and its step is as follows：
By nano-zinc oxide powder and nanometer hydroxyapatite powder in mass ratio 10~90：3~6h of ball milling is obtained after 10~90 mixing
Composite powder, solvent and dispersant are added into gained composite powder, continue 2~4h of ball milling mixing and obtain suspension, then will
Suspension ultrasonic disperse uniformly obtains whiteware ink.
Preferably, the solvent is ethanol, and the dispersant is polyethylene glycol, neopelex, PVP
One kind in K30, glycerine or the mixture more than any two in any proportion.
Preferably, the mass percent of composite powder and solvent, dispersant is in the suspension：Composite powder 30~
40%, solvent 50~60%, dispersant 5~10%.
Preferably, the ultrasonic disperse time is 30~60min.
The present invention prepares the high nano zine oxide of size uniform, purity and nanometer hydroxyapatite powder using sol-gal process
Body, then add solvent, suspension, dispersant etc. be made without zirconium, without heavy metal ultrawhite inkjet printing aqueous ceramic ink
Water.Hydroxyapatite can effectively suppress zinc oxide and be grown up in calcination process, and the mixing of two kinds of nano-powders can be to greatest extent
Ground plays the reflection and scattering process to light, therefore its whiteness is suitable with colorant containing zirconium white.Meanwhile the selection addition of additive can be very
Play a part of antisolvent precipitation well, promote to suspend, protect whiteness, as STTP can eliminate the electrostatic attraction between powder granule, increase row
Repulsion, break micelle cohesion, the Free water of parcel discharge, glaze slurry viscosity decline, rheological characteristic increase, finally give whiteness height,
Ink rheological characteristic is good, suitable for ceramic ink jet printing ultrawhite without zirconium water-based ink-jet printing ceramic ink.
The beneficial effects of the present invention are：
1st, the present invention is mixed using two kinds of inorganic nano zinc oxide and hydroxy apatite powder, due to two kinds of powders
Grain characteristic is different, hydroxyl be present in hydroxyapatite, easily acts on forming surface parcel with organic additive, makes intergranular mutual
Declines, ethanol then further reduces the attraction between hydroapatite particles as solvent, so as to avoid particle
Aggregation, therefore in the presence of dispersant, the uniform particle sizes of ceramic ink, average grain diameter is less than 290nm, after standing 8 days, ink
Without not being layered and settling, stability is good, and the Hunter whiteness average value decorated after glaze paint is more than 92, meets ceramic ink jet printing use
The requirement of ink.
2nd, ultrawhite of the invention is simple without zircon ceramic ink preparation technology, wherein the calcining heat only 600 of compound white material
~700 DEG C, and zirconium oxide pigment need to be made in calcination under 1500 DEG C of high temperature in the prior art.Therefore, whiteware of the invention
The cost of ink is only 1/3~1/2 of the ink containing zirconium.
Brief description of the drawings
Fig. 1 is the XRD spectra of the zinc oxide and the compound white material of hydroxyapatite prepared by the embodiment of the present invention 1；
Fig. 2 is the grading curve of the ceramic ink prepared by embodiment 1.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made below in conjunction with the accompanying drawings into
One step is described in detail.
Embodiment 1
Prepare without zirconium ultrawhite inkjet printing aqueous ceramic ink, comprise the following steps that：
1) preparation of compound white material
1. the preparation of nanometer Zinc oxide powder
Triammonium citrate powder is added in the acetic acid zinc solution that concentration is 0.1mol/L, magnetic agitation mixing 30min is obtained
To clear solution, zinc hydroxide suspension is obtained after adding absolute ethyl alcohol, add the ammoniacal liquor that percentage by volume is 5% adjust pH to
Colloidal sol is obtained after 8,80 DEG C of water-bath 2h, through 80 DEG C of dry 8h in Constant Temp. Oven, through 500 DEG C of calcinings in resistance furnace
12h obtains nano-zinc oxide powder.
The mass fraction of zinc acetate is 60% in above-mentioned clear solution, and the mass fraction of Triammonium citrate is 40%.
2. the preparation of nano hydroxyapatite powder
By Ca (NO3)2(NH4)2HPO4Solution mixing 30min obtains mixed liquor, is adjusted with the ammoniacal liquor that percentage by volume is 5%
PH to 8 is saved, gel is obtained after 60 DEG C of water-bath 2h, through 80 DEG C of dry 5h in Constant Temp. Oven, through 600 DEG C in resistance furnace
Calcining 9h obtains nanometer hydroxyapatite powder.
Ca (NO in above-mentioned mixed liquor3)2Solution and (NH4)2HPO4The percentage by volume of solution is 50%.
3. prepared by nano zine oxide and hydroxyapatite complex powder
1. the nano zine oxide obtained in and 2. and nano hydroxyapatite powder are mixed by weight percent：Zinc oxide
70%th, hydroxyapatite 30%, mix, compound white material is obtained after ball milling 3h.
2) preparation of whiteware ink
Solvent is added in 3. composite powder that above-mentioned steps obtain and dispersant obtains mixture, is obtained after ball milling mixing 2h
To suspension, ultrasonic 30min obtains whiteware ink in ultrasonic cleaner.
Above-mentioned solvent is ethanol, and dispersant is 1 in polyethylene glycol and glycerine:1 mixture.The wherein amount of composite powder
The 40% of mixture gross mass is accounted for, the addition of solvent accounts for the 55% of mixture gross mass, and the addition of dispersant accounts for mixture
The 5% of gross mass.
It is as shown in Figure 1 the XRD spectra of the zinc oxide prepared by the present embodiment and the compound white material of hydroxyapatite, can be with
Find out, the crystallization of zinc oxide and hydroxyapatite is more complete.Fig. 2 is the grain size distribution of ceramic ink manufactured in the present embodiment,
As can be seen that diameter of particle is uniform in ceramic ink, in normal distribution.
After tested, the average grain size of nano zine oxide of the invention and hydroxyapatite complex powder is 33nm, institute
The average grain diameter of obtained whiteware ink is 290nm, and the Hunter whiteness decorated after glaze paint is 93, meets ceramic ink jet and beats
The requirement of print ink.
Embodiment 2
Prepare without zirconium ultrawhite inkjet printing aqueous ceramic ink, comprise the following steps that：
1) preparation of compound white material
1. the preparation of nanometer Zinc oxide powder
Triammonium citrate powder is added in the acetic acid zinc solution that concentration is 0.3mol/L, magnetic agitation mixing 50min is obtained
To clear solution, zinc hydroxide suspension is obtained after adding absolute ethyl alcohol, add the ammoniacal liquor that percentage by volume is 6% adjust pH to
Colloidal sol is obtained after 10,60 DEG C of water-bath 4h, through 100 DEG C of dry 5h in Constant Temp. Oven, through 700 DEG C of calcinings in resistance furnace
8h obtains nano-zinc oxide powder.
The mass fraction of zinc acetate is 40% in above-mentioned clear solution, and the mass fraction of Triammonium citrate is 60%.
2. the preparation of nano hydroxyapatite powder
By Ca (NO3)2(NH4)2HPO4Solution mixing 30min obtains mixed liquor, is adjusted with the ammoniacal liquor that percentage by volume is 5%
PH to 9 is saved, gel is obtained after 70 DEG C of water-bath 3h, through 100 DEG C of dry 5h in Constant Temp. Oven, through 500 in resistance furnace
DEG C calcining 12h obtain nanometer hydroxyapatite powder.
Ca (NO in above-mentioned mixed liquor3)2The percentage by volume of solution is 60%, (NH4)2HPO4The percentage by volume of solution is
40%.
3. prepared by nano zine oxide and hydroxyapatite complex powder
1. the nano zine oxide obtained in and 2. and nano hydroxyapatite powder are mixed by weight percent：Zinc oxide
50%th, hydroxyapatite 50%, mix, compound white material is obtained after ball milling 4h.
2) preparation of whiteware ink
Solvent is added in 3. composite powder that above-mentioned steps obtain and dispersant obtains mixture, is obtained after ball milling mixing 3h
To suspension, ultrasonic 50min obtains whiteware ink in ultrasonic cleaner.
Above-mentioned solvent is ethanol, and dispersant is the mixing of polyethylene glycol, neopelex and PVP K30 composition
Thing, 30%, 30% and 40% is accounted for respectively.The amount of wherein composite powder accounts for the 30% of mixture gross mass, and the addition of solvent accounts for
The 60% of mixture gross mass, the addition of dispersant account for the 10% of mixture gross mass.
After tested, the average grain size of nano zine oxide of the invention and hydroxyapatite complex powder is 42nm, institute
The average grain diameter of obtained whiteware ink is 275nm, and the Hunter whiteness decorated after glaze paint is 92, meets ceramic ink jet and beats
The requirement of print ink.
Claims (10)
1. one kind is without zirconium ultrawhite inkjet printing aqueous ceramic ink, it is characterised in that：The aqueous ceramic ink is by nano oxygen
Solvent and dispersant are added after change zinc powder and nanometer hydroxyapatite powder mixing and ball milling, and simultaneously ultrasonic disperse obtains ball milling again.
2. no zirconium ultrawhite inkjet printing aqueous ceramic ink according to claim 1, it is characterised in that：The nano oxygen
It is 21.9~61.8nm to change zinc powder average grain size, is prepared by following methods：It is 0.1~0.3mol/L's to concentration
Triammonium citrate powder is added in acetic acid zinc solution, is uniformly mixing to obtain clear solution, hydroxide is obtained after adding absolute ethyl alcohol
Zinc suspension liquid, zinc hydroxide suspension pH value is adjusted to 8~10 with ammonia spirit, then by zinc hydroxide suspension in 60~80
DEG C heating 2~4h obtain colloidal sol, after colloidal sol is dried calcining obtain nano-zinc oxide powder.
3. no zirconium ultrawhite inkjet printing aqueous ceramic ink according to claim 2, it is characterised in that：It is described transparent molten
Zinc acetate and Triammonium citrate mass ratio are 50~60 in liquid：40~50.
4. no zirconium ultrawhite inkjet printing aqueous ceramic ink according to claim 2, it is characterised in that：The dry temperature
Spend for 80~100 DEG C, drying time is 5~10h, and the calcining heat is 500~700 DEG C, and calcination time is 8~12h.
5. no zirconium ultrawhite inkjet printing aqueous ceramic ink according to claim 1, it is characterised in that：The nanometer hydroxyl
Base apatite powder average grain size is 21.9~61.8nm, is prepared by following methods：By Ca (NO3)2Solution and
(NH4)2HPO4Solution is mixed to get mixed liquor, mixed liquor pH value is adjusted to 8~10 with ammonia spirit, then by mixed liquor in 60
~80 DEG C of 2~4h of heating obtain gel, and calcining after gel drying is obtained into nanometer hydroxyapatite powder.
6. no zirconium ultrawhite inkjet printing aqueous ceramic ink according to claim 5, it is characterised in that：The Ca
(NO3)2Solution and (NH4)2HPO4Liquor capacity concentration is 40~60%.
7. no zirconium ultrawhite inkjet printing aqueous ceramic ink according to claim 5, it is characterised in that：The dry temperature
Spend for 80~100 DEG C, drying time is 5~10h, and the calcining heat is 600~700 DEG C, and calcination time is 8~12h.
8. a kind of any described preparation methods without zirconium ultrawhite inkjet printing with aqueous ceramic ink of claim 1-7, it is special
Sign is that step is as follows：By nano-zinc oxide powder and nanometer hydroxyapatite powder in mass ratio 10~90：10~90 mixing
3~6h of ball milling obtains composite powder afterwards, and solvent and dispersant are added into gained composite powder, continues 2~4h of ball milling mixing and obtains
To suspension, suspension ultrasonic disperse is uniformly then obtained into whiteware ink.
9. preparation method according to claim 8, it is characterised in that the solvent is ethanol, and the dispersant is poly- second two
One kind in alcohol, neopelex, PVP K30, glycerine or the mixture more than any two in any proportion.
10. preparation method according to claim 8, it is characterised in that composite powder and solvent in the suspension, scattered
The mass percent of agent is：Composite powder 30~40%, solvent 50~60%, dispersant 5~10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711064663.XA CN107778991B (en) | 2017-11-02 | 2017-11-02 | Zirconium-free ultra-white water-based ceramic ink for ink-jet printing and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711064663.XA CN107778991B (en) | 2017-11-02 | 2017-11-02 | Zirconium-free ultra-white water-based ceramic ink for ink-jet printing and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107778991A true CN107778991A (en) | 2018-03-09 |
| CN107778991B CN107778991B (en) | 2021-05-04 |
Family
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| CN201711064663.XA Active CN107778991B (en) | 2017-11-02 | 2017-11-02 | Zirconium-free ultra-white water-based ceramic ink for ink-jet printing and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641479A (en) * | 2018-04-13 | 2018-10-12 | 山东国瓷康立泰新材料科技有限公司 | A kind of inkjet printing super white ceramic ink and preparation method thereof |
| CN109535846A (en) * | 2018-12-21 | 2019-03-29 | 湖北工业大学 | A kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink |
| CN109749516A (en) * | 2018-12-29 | 2019-05-14 | 武汉理工大学 | A kind of inkjet printing photochromic ceramic ink and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641479A (en) * | 2018-04-13 | 2018-10-12 | 山东国瓷康立泰新材料科技有限公司 | A kind of inkjet printing super white ceramic ink and preparation method thereof |
| CN108641479B (en) * | 2018-04-13 | 2021-09-07 | 山东国瓷康立泰新材料科技有限公司 | Ultra-white ceramic ink for ink-jet printing and preparation method thereof |
| CN109535846A (en) * | 2018-12-21 | 2019-03-29 | 湖北工业大学 | A kind of preparation method based on hydroxide radical phosphorite nanocrystalline fluorescence invisible ink |
| CN109749516A (en) * | 2018-12-29 | 2019-05-14 | 武汉理工大学 | A kind of inkjet printing photochromic ceramic ink and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN107778991B (en) | 2021-05-04 |
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