CN104356764B - Black pigment liquid, black matrix preparation method and black matrix - Google Patents
Black pigment liquid, black matrix preparation method and black matrix Download PDFInfo
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- CN104356764B CN104356764B CN201410643481.8A CN201410643481A CN104356764B CN 104356764 B CN104356764 B CN 104356764B CN 201410643481 A CN201410643481 A CN 201410643481A CN 104356764 B CN104356764 B CN 104356764B
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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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/005—Carbon black
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
Abstract
The invention discloses a kind of black pigment liquid and preparation method thereof and black pigment liquid, black matrix preparation method and black matrix, relate to technical field of liquid crystal display, the black matrix of high resistance can be prepared, thus effectively overcome liquid-crystal display and to start shooting bad defect.Black pigment liquid and preparation method thereof disclosed by the invention comprises: mix, the acrylic resin of first dispersion agent of second carbon black of first carbon black of 11 ~ 15wt%, 0.5 ~ 2.5wt%, 9 ~ 13wt%, the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and 1wt% to be mixed with mixed solution; After mixing for first scheduled time, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%; After continuing mixing second scheduled time, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%; Mixed for the 3rd scheduled time continuously again.The present invention is applicable in black pigment liquid and black matrix preparation process.
Description
Technical field
The present invention relates to technical field of liquid crystal display, particularly relate to a kind of black pigment liquid, black matrix preparation method and black matrix.
Background technology
Liquid-crystal display, with its superior performance, proven technique and huge cause group, becomes and shows the leading of field now.
Liquid-crystal display produces electric field mainly through electrode and makes liquid crystal deflection to complete display task; but usually can produce induction field at booting moment; this unwanted induction field can make liquid crystal molecule rotate, and generation start is bad, such as can produce speckle.
Summary of the invention
Main purpose of the present invention is, provides a kind of black pigment liquid and preparation method thereof, black matrix preparation method and black matrix, can prepare the black matrix of high resistance, thus effectively overcomes liquid-crystal display and to start shooting bad defect.
For achieving the above object, the present invention adopts following technical scheme:
On the one hand, the invention provides a kind of black pigment liquid and preparation method thereof, wherein, comprising:
The acrylic resin of first dispersion agent of second carbon black of first carbon black of 11 ~ 15wt%, 0.5 ~ 2.5wt%, 9 ~ 13wt%, the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and 1wt% is mixed, to be mixed with mixed solution;
After mixing for first scheduled time, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing mixing second scheduled time, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Mixed for the 3rd scheduled time continuously again.
Particularly, described method specifically comprises:
The acrylic resin of first dispersion agent of second carbon black of first carbon black of 13wt%, 1 ~ 2wt%, 11wt%, the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and 1wt% is mixed, to be mixed with mixed solution;
After mixing for first scheduled time, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing mixing second scheduled time, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Mixed for the 3rd scheduled time continuously again.
Alternatively, described first scheduled time is 0.5h ~ 2h; Described second scheduled time is 10min ~ 1h; Described 3rd scheduled time is 1.5h ~ 3.5h.
Alternatively, the mode of mixing is included in concussion mixing and/or sand milling mixing in sand mill in oscillator.
Further particularly, described method specifically comprises:
Being added on by the 1-Methoxy-2-propyl acetate of second carbon black of first carbon black of 13wt%, 2wt%, first dispersion agent of 11wt% and 52 ~ 53wt% is equipped with in the cultivation shaking flask of zirconium pearl, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution;
In earthquake machine after concussion mixing 2h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing concussion mixing 1h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Concussion mixes 3h continuously again.
Or described method specifically comprises:
Being added on by the 1-Methoxy-2-propyl acetate of first dispersion agent of second carbon black of first carbon black of 13wt%, 1wt%, 11wt%, second dispersion agent of 1wt% and 52 ~ 53wt% is equipped with in the cultivation shaking flask of zirconium pearl, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution;
In earthquake machine after concussion mixing 2h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing concussion mixing 1h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Concussion mixes 3h continuously again.
Or described method specifically comprises:
The 1-Methoxy-2-propyl acetate of second carbon black of first carbon black of 13wt%, 2wt%, first dispersion agent of 11wt% and 52 ~ 53wt% is added in the reactor, under stirring and evenly mixing condition, then adds the acrylic resin of 1wt%, to be mixed with mixed solution;
In sand mill after sand milling mixing 0.5h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing sand milling mixing 10min, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Continuous sand milling 2h again.
Correspondingly, the embodiment of the present invention additionally provides a kind of black pigment liquid, and wherein, the black pigment liquid and preparation method thereof that described black pigment liquid is provided by above-mentioned arbitrary technical scheme is prepared from.
On the other hand, the embodiment of the present invention additionally provides a kind of black matrix preparation method, and wherein, described method comprises:
Black pigment liquid prepared by above-mentioned arbitrary technical scheme is mixed with alkali soluble resin, initiator, flow agent and monomer;
By obtained mixture successively through smear, exposure, developing process.
Correspondingly, present invention also offers a kind of black matrix, wherein, the black matrix preparation method that described black matrix uses above-mentioned arbitrary technical scheme to provide is prepared from.
The black pigment liquid and preparation method thereof that the embodiment of the present invention provides and black pigment liquid, black matrix preparation method and black matrix, in preparation process, first by the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and the acrylic resin of 1wt% and the first carbon black, the second carbon black and the first dispersant, the 1-Methoxy-2-propyl acetate of 14 ~ 15wt% is added again after mixing for first scheduled time, the 1-Methoxy-2-propyl acetate of 5wt% and the acrylic resin of 1wt% is added again after continuing mixing second scheduled time, after mixing for the 3rd scheduled time continuously again, just obtain black pigment liquid, it should be noted that, the dispersion effect of black pigment liquid depends primarily on dispersing technology, the embodiment of the present invention is according to the material properties of each component, adopt different orders of addition and different additions, thus make the black pigment liquid dispersing property for preparing better, particle diameter is less, narrow distribution, and in finely dispersed black pigment liquid, first and second carbon blacks are evenly distributed in colloid, insulating property are even, fine and close, there will not be the region not having the first or second carbon black distribution, so the insulating property of whole black pigment liquogel are better, and the higher black matrix of impedance can be prepared, thus efficiently avoid liquid-crystal display booting moment generation induction field, avoid liquid crystal molecule is rotated, thus overcome liquid-crystal display and to start shooting bad defect.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
A kind of black pigment liquid and preparation method thereof schema that Fig. 1 provides for the embodiment of the present invention;
The grain size distribution of the black pigment liquid that Fig. 2 provides for comparative example 1;
The grain size distribution of the black pigment liquid that Fig. 3 provides for comparative example 2;
The grain size distribution of the black pigment liquid that Fig. 4 provides for embodiment 1;
The grain size distribution of the black pigment liquid that Fig. 5 provides for comparative example 3;
The grain size distribution of the black pigment liquid that Fig. 6 provides for embodiment 2;
The grain size distribution of the black pigment liquid that Fig. 7 provides for comparative example 4;
The grain size distribution of the black pigment liquid that Fig. 8 provides for embodiment 3.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
As shown in Figure 1, embodiments provide a kind of black pigment liquid and preparation method thereof, wherein, comprising:
S1, by the mixing of the acrylic resin of the 1-Methoxy-2-propyl acetate (PMA) of first dispersion agent of second carbon black of first carbon black of 11 ~ 15wt%, 0.5 ~ 2.5wt%, 9 ~ 13wt%, 52 ~ 53wt% and 1wt%, to be mixed with mixed solution;
S2, mixed for first scheduled time after, then add the 1-Methoxy-2-propyl acetate of 14 ~ 15wt% in mixed solution;
S3, to continue after mixing second scheduled time, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 5wt% and the acrylic resin of 1wt%;
S4, more continuously mix the 3rd scheduled time.
The black pigment liquid and preparation method thereof that the embodiment of the present invention provides, in preparation process, first by the acrylic resin of PMA and 1wt% of 52 ~ 53wt% and the first carbon black, the second carbon black and the first dispersant, the PMA of 14 ~ 15wt% is added again after mixing for first scheduled time, the acrylic resin of PMA and 1wt% of 5wt% is added again after continuing mixing second scheduled time, after mixing for the 3rd scheduled time continuously again, just obtain black pigment liquid, it should be noted that, the dispersion effect of black pigment liquid depends primarily on dispersing technology, the embodiment of the present invention is according to the material properties of each component, adopt different orders of addition and different additions, thus make the black pigment liquid dispersing property for preparing better, particle diameter is less, narrow distribution, and in finely dispersed black pigment liquid, first and second carbon blacks are evenly distributed in colloid, insulating property are even, fine and close, there will not be the region not having the first or second carbon black distribution, so the insulating property of whole black pigment liquogel are better, and the higher black matrix of impedance can be prepared, thus efficiently avoid liquid-crystal display booting moment generation induction field, avoid liquid crystal molecule is rotated, thus overcome liquid-crystal display and to start shooting bad defect.
It should be noted that, in the embodiment of the present invention, various component all can be obtained by commercially available mode.Wherein, the first carbon black can be the carbon black of C54 for the trade mark, and the second carbon black can be the carbon black of C3 for the trade mark; First dispersion agent can be commercially available BYK Series Dispersant, such as BYK-2000 dispersion agent; Acrylic resin can be 611 commercially available resins.
In the embodiment of the present invention, first carbon black of 11 described ~ 15wt% refers to that the first carbon black accounts for the weight percent of whole black pigment liquid, namely with finally obtained black pigment liquid for benchmark carries out calculating; In like manner, the acrylic resin of second carbon black of 0.5 ~ 2.5wt%, first dispersion agent of 9 ~ 13wt%, the 1-Methoxy-2-propyl acetate (PMA) of 52 ~ 53wt% and 1wt% all with finally obtained black pigment liquid for benchmark carries out calculating.
The black pigment liquid and preparation method thereof that above-described embodiment provides is specifically as follows:
S11, by the acrylic resin of first dispersion agent of second carbon black of first carbon black of 13wt%, 1 ~ 2wt%, 11wt%, the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and 1wt% mix, to be mixed with mixed solution;
S21, mixed for first scheduled time after, then add the 1-Methoxy-2-propyl acetate of 14 ~ 15wt% in mixed solution;
S31, to continue after mixing second scheduled time, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 5wt% and the acrylic resin of 1wt%;
S41, more continuously mix the 3rd scheduled time.
Particularly, in the embodiment of the present invention, first scheduled time can be 0.5h ~ 2h, can be such as 0.5h, 1h, 1.5h or 2h; Second scheduled time can be 10min ~ 1h, can be such as 10min, 30min or 1h; 3rd scheduled time can be 1.5h ~ 3.5h, can be such as 1.5h, 2h, 2.5h, 3h or 3.5h.
In the embodiment of the present invention, the mode of mixing can be included in concussion mixing and/or sand milling mixing in sand mill in oscillator.
Further particularly, the black pigment liquid and preparation method thereof that the embodiment of the present invention provides specifically can comprise:
S12, the 1-Methoxy-2-propyl acetate of second carbon black of first carbon black of 13wt%, 2wt%, first dispersion agent of 11wt% and 52 ~ 53wt% is added on zirconium pearl is housed cultivation shaking flask (shake bottle) in, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution;
In S22, earthquake machine after concussion mixing 2h, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After S32, continuation concussion mixing 1h, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 5wt% and the acrylic resin of 1wt%;
S42, more continuous concussion mixing 3h.
Or, specifically can comprise:
S13, the 1-Methoxy-2-propyl acetate of first dispersion agent of second carbon black of first carbon black of 13wt%, 1wt%, 11wt%, second dispersion agent of 1wt% and 52 ~ 53wt% is added on and is equipped with in the cultivation shaking flask of zirconium pearl, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution; Wherein, the second dispersion agent can be acrylic dispersants, and it can be obtained by commercially available mode, and such as commercially available model is the dispersion agent of D21.
In S23, earthquake machine after concussion mixing 2h, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After S33, continuation concussion mixing 1h, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 5wt% and the acrylic resin of 1wt%;
S43, more continuous concussion mixing 3h.
Or, specifically can comprise:
S14, by the 1-Methoxy-2-propyl acetate of second carbon black of first carbon black of 13wt%, 2wt%, first dispersion agent of 11wt% and 52 ~ 53wt% add in the reactor, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution;
S24, in sand mill after sand milling mixing 0.5h, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After S34, continuation sand milling mixing 10min, then in mixed solution, add the 1-Methoxy-2-propyl acetate of 5wt% and the acrylic resin of 1wt%;
S44, more continuous sand milling 2h.
Correspondingly, the embodiment of the present invention additionally provides a kind of black pigment liquid, wherein, this black pigment liquid provided by the embodiment of the present invention any one described in black pigment liquid and preparation method thereof be prepared from, therefore this black pigment liquid has identical or corresponding technical characteristic with above-mentioned black pigment liquid and preparation method thereof, and can reach identical beneficial effect, at this, it is no longer repeated in the present invention.
Particularly, the median size of the black pigment liquid that the embodiment of the present invention provides is 72 ~ 74nm, such as, can be 72nm, 73nm or 74nm.
On the other hand, the embodiment of the present invention additionally provides a kind of black matrix preparation method, and wherein, the method comprises:
Any one the black pigment liquid embodiment of the present invention provided mixes with alkali soluble resin, initiator, flow agent and monomer;
By obtained mixture successively through smear, exposure, developing process.
That is, in the black matrix preparation method that the embodiment of the present invention provides, mainly make use of any one black pigment liquid that the embodiment of the present invention provides, after it is mixed with alkali soluble resin, initiator, flow agent and monomer, by the mixture of preparation successively through techniques such as smear, exposure, developing process, thus obtain black matrix.
The black pigment liquid dispersing property provided due to the embodiment of the present invention is better, particle diameter is less, narrow distribution, thus, the black matrix impedance prepared by this black pigment liquid is higher, thus efficiently avoid liquid-crystal display booting moment generation induction field, avoid liquid crystal molecule is rotated, thus overcome liquid-crystal display and to start shooting bad defect.
Correspondingly, the embodiment of the present invention additionally provides a kind of black matrix, wherein, this black matrix is that the black matrix preparation method of any one provided by the embodiment of the present invention is prepared from, therefore this black matrix has identical or corresponding technical characteristic with above-mentioned black matrix preparation method, and can reach identical beneficial effect, at this, it is no longer repeated in the present invention.
To be described in detail to black pigment liquid and preparation method thereof provided by the invention and black pigment liquid, black matrix preparation method and black matrix by specific embodiment below.
First group of embodiment and comparative example:
Comparative example 1
Comparative example 1 is method conventional when preparing black pigment liquid and black matrix in prior art, and detailed process is as follows:
The preparation of black pigment liquid:
In the BYK-2000 dispersion agent that the C54 carbon black of 13g and the C3 carbon black of 2g are added on the 11g in the shake bottle that 50g zirconium pearl is housed and 72gPMA mixed solution, under stirring and evenly mixing condition, then add 611 resins of 2g;
Take out after continuous oscillation 5 ~ 6h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 5.32cp, and median size is about 92nm, and its grain size distribution as shown in Figure 2.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin coating at 600 rpm (spin) smear;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 4.3, resistance 1.1 × 10*16 Ω/; Wherein, OD value refers to optical density(OD), and be used for characterizing the shading performance of black matrix, its numerical value is through the negative derivative of light and light source ratio.
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.4um, OD value is 4.5, resistance 1.16 × 10*16 Ω/.
Comparative example 2
Comparative example 2 adopts the black pigment liquid that provides with the embodiment of the present invention and the similar method of black matrix preparation method, its key distinction is, in black pigment liquid preparation process, outside the addition numerical range that the addition of PMA and 611 resins limits in the embodiment of the present invention, formed with the method provided with the following example 1 and contrast, PMA and the order of addition of 611 resins and the importance of addition in the outstanding embodiment of the present invention; The detailed process of comparative example 2 is as follows:
The preparation of black pigment liquid:
In the BYK-2000 dispersion agent that the C54 carbon black of 13g and the C3 carbon black of 2g are added on the 11g in the shake bottle that 50g zirconium pearl is housed and 52gPMA mixed solution, under stirring and evenly mixing condition, then add 611 resins of 0.5g;
By vibration mixing 2h in this shake bottle earthquake machine, take out, then in shake bottle, add the PMA (12wt%) of 12g;
Again after vibration mixing 1h, take out, then in shake bottle, add the PMA (8wt%) of 8g and 611 (1.5wt%) resin of 1.5g;
Take out after continuous oscillation mixing 3h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 4.12cp, and median size is about 85nm, and its grain size distribution as shown in Figure 3.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin smear at 600 rpm;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 5.4, resistance 1.2 × 10*16 Ω/;
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.4um, OD value is 5.6, resistance 1.22 × 10*16 Ω/.
Embodiment 1
The preparation of black pigment liquid:
In the BYK-2000 dispersion agent that the C54 carbon black of 13g and the C3 carbon black of 2g are added on the 11g in the shake bottle that 50g zirconium pearl is housed and 52gPMA mixed solution, under stirring and evenly mixing condition, then add 611 resins of 1g;
By vibration mixing 2h in this shake bottle earthquake machine, take out, then in shake bottle, add the PMA (15wt%) of 15g;
Again after vibration mixing 1h, take out, then in shake bottle, add the PMA (5wt%) of 5g and 611 (1wt%) resin of 1g;
Take out after continuous oscillation mixing 3h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 4.12cp, and median size is about 74nm, and its grain size distribution as shown in Figure 4.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin smear at 600 rpm;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 5.4, resistance 2.2 × 10*16 Ω/;
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.4um, OD value is 5.6, resistance 2.27 × 10*16 Ω/.
Results contrast:
From the test result of above-mentioned comparative example 1 with embodiment 1, relative to prior art comparative example 1, the median size of the black pigment liquid that embodiment 1 is obtained reduces to about 74nm by about 92nm, decreases 20% nearly; And from Fig. 2 and Fig. 4, the particle diameter distribution width PDI value of black pigment liquid reduces to 0.127 by 0.211, and the particle diameter distribution width at peak 1 reduces to about 34nm by about 50nm, decreases 32%; The obtained black resistance matrix of embodiment 1 brings up to 2.27 × 10*16 Ω/ by 1.16 × 10*16 Ω/, improves 96% nearly.
This explanation, embodiment 1 is when preparing black pigment liquid, substep interpolation PMA and 611 resins can reduce median size and the distribution range of black pigment liquid effectively, effectively improve the dispersing property of black pigment liquid, thus effectively improve the impedance of black matrix.
From the test result of above-mentioned comparative example 2 with embodiment 1, the median size of the black pigment liquid that embodiment 1 is obtained reduces to about 74nm by about 85nm, decreases 13% nearly; And from Fig. 3 and Fig. 4, the particle diameter distribution width PDI value of black pigment liquid reduces to 0.127 by 0.193, and the particle diameter distribution width at peak 1 reduces to about 34nm by about 51nm, decreases 33%; The obtained black resistance matrix of embodiment 1 brings up to 2.27 × 10*16 Ω/ by 1.22 × 10*16 Ω/, improves 86% nearly.
This explanation, when preparing black pigment liquid, the method adopting the embodiment of the present invention to provide first adds a part of PMA and 611 resins, PMA and 1wt% of 5wt% is added in the PMA of 14 ~ 15wt%, again continuation again 611 resins after mixing for some time are added after mixing for some time, effectively can improve the dispersing property of black pigment liquid, thus effectively improve the impedance of black matrix.That is, in the embodiment of the present invention, the dispersing property of black pigment liquid mainly relies on substep to add the method for PMA and 611 resins, and the content decision of the PMA added in often walking and 611 resins, if and only use substep adds the method for PMA and 611 resins, but outside the numerical value that the PMA often added in step and the content range of 611 resins provide in the embodiment of the present invention, the outstanding beneficial effect that the embodiment of the present invention can reach can not be obtained, when the substep that this just effectively demonstrates experiment aspect provides in the embodiment of the present invention adds PMA and 611 resin, the PMA often added in step and the content importance of 611 resins.
Second group of embodiment and comparative example:
Comparative example 3
The preparation of black pigment liquid:
In the BYK-2000 dispersion agent that the D21 dispersion agent of the C54 carbon black of 13g, the C3 carbon black of 1g and 1g is added on the 11g in the shake bottle that 50g zirconium pearl is housed and 72gPMA mixed solution, under stirring and evenly mixing condition, then add 611 resins of 2g;
Take out after continuous oscillation 5 ~ 6h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 5.62cp, and median size is about 85nm, and its grain size distribution as shown in Figure 5.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin smear at 600 rpm;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 4.2, resistance 1.7 × 10*16 Ω/;
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.3um, OD value is 4.3, resistance 1.76 × 10*16 Ω/.
Embodiment 2
The preparation of black pigment liquid:
In the BYK-2000 dispersion agent that the D21 dispersion agent of the C54 carbon black of 13g, the C3 carbon black of 1g and 1g is added on the 11g in the shake bottle that 50g zirconium pearl is housed and 52gPMA mixed solution, under stirring and evenly mixing condition, then add 611 resins of 1g;
By the 2h that vibrates in this shake bottle earthquake machine, take out, then in shake bottle, add the PMA (15%wt) of 15g;
Again vibrate after 1h, take out, then in shake bottle, add the PMA (5%wt) of 5g and 611 (1%wt) resin of 1g;
Take out after continuous oscillation 3h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 4.67cp, and median size is about 74nm, and its grain size distribution as shown in Figure 6.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin smear at 600 rpm;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 5.1, resistance 2.1 × 10*16 Ω/;
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.3um, OD value is 5.4, resistance 2.16 × 10*16 Ω/.
Results contrast:
From the test result of above-mentioned comparative example 3 with embodiment 2, relative to prior art comparative example 3, the median size of the black pigment liquid that embodiment 2 is obtained reduces to about 74nm by about 85nm, decreases 13% nearly; And from Fig. 5 and Fig. 6, the particle diameter distribution width PDI value of black pigment liquid reduces to 0.141 by 0.182, and the particle diameter distribution width at peak 1 reduces to about 34nm by about 40nm, decreases 15%; The black resistance matrix that embodiment 2 obtains brings up to 2.16 × 10*16 Ω/ by 1.76 × 10*16 Ω/, improves about 23%.
This explanation, embodiment 2 is when preparing black pigment liquid, substep interpolation PMA and 611 resins can reduce median size and the distribution range of black pigment liquid effectively, effectively improve the dispersing property of black pigment liquid, thus effectively improve the impedance of black matrix.
Second group of embodiment and comparative example:
Comparative example 4
The preparation of black pigment liquid:
The C54 carbon black of 130g and the C3 carbon black of 20g being added on is equipped with in the BYK-2000 dispersion agent of 110g and the reactor of 720gPMA mixed solution, under stirring and evenly mixing condition, then adds 611 resins of 20g;
Above-mentioned reactor is taken out after continuous sand milling 2.5 ~ 3h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 4.56cp, and median size is about 83nm, and its grain size distribution as shown in Figure 7.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin smear at 600 rpm;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 5.1, resistance 1.6 × 10*16 Ω/;
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.5um, OD value is 5.12, resistance 1.63 × 10*16 Ω/.
Embodiment 3
The preparation of black pigment liquid:
The C54 carbon black of 130g and the C3 carbon black of 20g are added in the reactor that the BYK-2000 dispersion agent of 110g and the mixed solution of 520gPMA are housed, under stirring and evenly mixing condition, then add 611 resins of 10g;
By above-mentioned reactor 1200rpm sand milling 0.5h in sand mill, then add the PMA (15%wt) of 150g in the reactor;
Again after sand milling 10min, then add the PMA (5%wt) of 50g and 611 (1%wt) resin of 10g in the reactor;
Take out after continuous sand milling 2h, obtained black pigment liquid.
Testing this obtained black pigment fluid viscosity is 3.77cp, and median size is about 73nm, and its grain size distribution as shown in Figure 8.
The preparation of black matrix:
Above-mentioned obtained black pigment liquid is mixed with alkali soluble resin, initiator, flow agent, monomer etc.;
Spin smear at 600 rpm;
Front baking 2min at 90 DEG C;
Exposure 12s; Development 94s, obtained black matrix; The thickness testing this black matrix is 1.6um, OD value is 5.6, resistance 2.1 × 10*16 Ω/;
Then dry 30min after at 230 DEG C, after drying after test, the thickness of black matrix is 1.5um, OD value is 5.74, resistance 2.13 × 10*16 Ω/.
Results contrast:
From the test result of above-mentioned comparative example 4 with embodiment 3, relative to comparative example 4, the median size of the black pigment liquid that embodiment 3 is obtained reduces to about 73nm by about 83nm, decreases about 12%; And from Fig. 7 and Fig. 8, the particle diameter distribution width PDI value of black pigment liquid reduces to 0.108 by 0.148, and the particle diameter distribution width at peak 1 reduces to about 29nm by about 41nm, decreases 29%; The black resistance matrix that embodiment 3 obtains brings up to 2.13 × 10*16 Ω/ by 1.63 × 10*16 Ω/, improves about 31%.
This explanation, embodiment 3 is when preparing black pigment liquid, substep interpolation PMA and 611 resins can reduce median size and the distribution range of black pigment liquid effectively, effectively improve the dispersing property of black pigment liquid, thus effectively improve the impedance of black matrix.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (9)
1. a black pigment liquid and preparation method thereof, is characterized in that, comprising:
The acrylic resin of first dispersion agent of second carbon black of first carbon black of 11 ~ 15wt%, 0.5 ~ 2.5wt%, 9 ~ 13wt%, the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and 1wt% is mixed, to be mixed with mixed solution;
After mixing 0.5h ~ 2h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing mixing 10min ~ 1h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Mix 1.5h ~ 3.5h continuously again.
2. black pigment liquid and preparation method thereof according to claim 1, is characterized in that, described method specifically comprises:
The acrylic resin of first dispersion agent of second carbon black of first carbon black of 13wt%, 1 ~ 2wt%, 11wt%, the 1-Methoxy-2-propyl acetate of 52 ~ 53wt% and 1wt% is mixed, to be mixed with mixed solution;
After mixing 0.5h ~ 2h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing mixing 10min ~ 1h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Mix 1.5h ~ 3.5h continuously again.
3. black pigment liquid and preparation method thereof according to claim 2, is characterized in that, the mode of mixing is included in concussion mixing and/or sand milling mixing in sand mill in oscillator.
4. black pigment liquid and preparation method thereof according to claim 2, is characterized in that, described method specifically comprises:
Being added on by the 1-Methoxy-2-propyl acetate of second carbon black of first carbon black of 13wt%, 2wt%, first dispersion agent of 11wt% and 52 ~ 53wt% is equipped with in the cultivation shaking flask of zirconium pearl, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution;
In earthquake machine after concussion mixing 2h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing concussion mixing 1h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Concussion mixes 3h continuously again.
5. black pigment liquid and preparation method thereof according to claim 2, is characterized in that, described method specifically comprises:
Being added on by the 1-Methoxy-2-propyl acetate of first dispersion agent of second carbon black of first carbon black of 13wt%, 1wt%, 11wt%, second dispersion agent of 1wt% and 52 ~ 53wt% is equipped with in the cultivation shaking flask of zirconium pearl, under stirring and evenly mixing condition, add the acrylic resin of 1wt% again, to be mixed with mixed solution;
In earthquake machine after concussion mixing 2h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing concussion mixing 1h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Concussion mixes 3h continuously again.
6. black pigment liquid and preparation method thereof according to claim 2, is characterized in that, described method specifically comprises:
The 1-Methoxy-2-propyl acetate of second carbon black of first carbon black of 13wt%, 2wt%, first dispersion agent of 11wt% and 52 ~ 53wt% is added in the reactor, under stirring and evenly mixing condition, then adds the acrylic resin of 1wt%, to be mixed with mixed solution;
In sand mill after sand milling mixing 0.5h, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 14 ~ 15wt%;
After continuing sand milling mixing 10min, then in described mixed solution, add the described 1-Methoxy-2-propyl acetate of 5wt% and the described acrylic resin of 1wt%;
Continuous sand milling 2h again.
7. a black pigment liquid, is characterized in that, the black pigment liquid and preparation method thereof according to any one of claim 1 ~ 6 is prepared from.
8. a black matrix preparation method, is characterized in that, is mixed by black pigment liquid according to claim 7 with alkali soluble resin, initiator, flow agent and monomer;
By obtained mixture successively through smear, exposure, developing process.
9. a black matrix, is characterized in that, uses the black matrix preparation method described in claim 8 to be prepared from.
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| CN108329758B (en) * | 2018-03-07 | 2021-03-12 | 京东方科技集团股份有限公司 | Pigment liquid for black matrix, black matrix and preparation method thereof, and display panel |
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| JP2001164172A (en) * | 1999-12-10 | 2001-06-19 | Tokai Carbon Co Ltd | Aqueous dispersion of carbon black pigment |
| JP2004251946A (en) * | 2003-02-18 | 2004-09-09 | Mikuni Color Ltd | Carbon black dispersed solution for color filter, carbon black-containing resin composition and black matrix |
| CN101324754A (en) * | 2007-06-14 | 2008-12-17 | 东洋油墨制造株式会社 | Photosensitive black composition and color filter |
| CN101541897A (en) * | 2006-11-30 | 2009-09-23 | 阪田油墨株式会社 | Pigment dispersion composition for black matrix and pigment dispersed resist composition for black matrix containing the same |
| CN102816477A (en) * | 2012-07-19 | 2012-12-12 | 京东方科技集团股份有限公司 | Pigment dispersing liquid and preparation method thereof |
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| JP2001164172A (en) * | 1999-12-10 | 2001-06-19 | Tokai Carbon Co Ltd | Aqueous dispersion of carbon black pigment |
| JP2004251946A (en) * | 2003-02-18 | 2004-09-09 | Mikuni Color Ltd | Carbon black dispersed solution for color filter, carbon black-containing resin composition and black matrix |
| CN101541897A (en) * | 2006-11-30 | 2009-09-23 | 阪田油墨株式会社 | Pigment dispersion composition for black matrix and pigment dispersed resist composition for black matrix containing the same |
| CN101324754A (en) * | 2007-06-14 | 2008-12-17 | 东洋油墨制造株式会社 | Photosensitive black composition and color filter |
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