A method for preparing a color paste for black photoresist and its preparation method and application

Abstract

The invention provides a method for preparing a color paste for black photoresist, comprising the following steps: step 1: adding a resin and a solvent into a reaction kettle, dispersing and stirring them uniformly, and then sequentially adding a dispersant and a pretreated black pigment, dispersing and stirring them, to obtain a color paste precursor; step 2: performing nano-processing on the color paste precursor to obtain a photoresist color paste; wherein the black pigment is pretreated to improve its own dispersibility and insulation properties, and the prepared color paste has high stability and excellent performance, good insulation performance, is not prone to electrostatic interference, and has strong light shielding properties.

Description

Technical Field

[0001] The present invention relates to the field of polymer technology, and in particular to a method for preparing a color paste for black photoresist, and a preparation method and application thereof. Background Art

[0002] Photoresist is mainly composed of resin, monomer, photosensitive initiator, color paste and other raw materials. Color paste is the main raw material of color photoresist and determines the quality of display. Traditional photoresist color paste is usually prepared by adding dyes and pigments to reduce light scattering and improve contrast, but dyes are not environmentally friendly. Or black chromium oxide is added, but the etching cost is high, and the black matrix formed by chromium metal has a low aspect ratio and cannot meet higher process requirements. In addition, the high reflectivity of chromium affects the display quality, and chromium wastewater is not environmentally friendly. Carbon black and carbon materials or color pigments are mixed. Carbon black and carbon materials have strong covering power and coloring power and have a high cost-effectiveness, but poor insulation performance and are prone to electrostatic interference. Color pigments have poor light shielding properties. Therefore, a black photoresist color paste with high shielding effect, strong insulation performance and not easy to generate electrostatic interference has broad market prospects and application value. Summary of the Invention

[0003] Based on the above technical solution, the present invention has the following technical effects:

[0004] The present invention pre-treats the black pigment and couples it with a diazonium salt and a coupling agent, thereby improving its own dispersibility. The prepared black pigment has high insulation properties, overcomes the shortcomings of poor insulation performance and easy generation of electrostatic interference, and increases its own dispersibility.

[0005] The composite dispersant added in the present invention has a significant dispersing effect. Finally, the color paste is nano-processed, which increases the overall dispersibility of the color paste and reduces the amount of dispersant used.

[0006] The present invention provides the following technical solutions:

[0007] The present invention provides a method for preparing a color paste for black photoresist, comprising the following steps:

[0008] Step 1: Add resin and solvent into the reaction kettle and disperse and stir them evenly, then add dispersant and pretreated black pigment in sequence and disperse and stir them to obtain color paste;

[0009] Step 2: Nano-process the product obtained in step 1 to obtain a color paste for black photoresist.

[0010] According to further research, the color paste contains the following components by weight: 3-7 parts of acrylic resin, 3-5 parts of dispersant, 7-11 parts of solvent, and 10-15 parts of pretreated black pigment.

[0011] Further research shows that the color paste contains the following components by weight: 5 parts of acrylic resin, 4 parts of dispersant, 9 parts of solvent, and 12 parts of pretreated black pigment.

[0012] Further research shows that the pretreatment method of the black pigment described in step 2 is: add carbon black and titanium dioxide in a mass ratio of 1-3:1 to a reaction mixture with a volume multiple of 4-5 times, ultrasonically heat and disperse for 15-25 minutes, heat for 10-20 minutes, and the heating temperature is 60-80°C. Then, add a coupling agent with a final concentration of 10-14%, cool to 45-55°C, stir and react for 2-3 hours, and then dry to obtain a pretreated black pigment.

[0013] According to further research, the reaction mixture is a mixture of diazonium salt and water, and the mass ratio of diazonium salt to water is 1-3:9-11.

[0014] According to further research, the coupling agent includes but is not limited to one or more of KH550, KH560, KBM602, TMC-105, TMC101, and TMC-311w.

[0015] Further research shows that the dispersant is a compound system of sodium tridecyl sulfosuccinate and polyethylene glycol, and the mass ratio of sodium tridecyl sulfosuccinate to polyethylene glycol is 2:2-4.

[0016] According to further research, the solvent includes but is not limited to one or more of ethylene glycol ether, dimethylacetamide, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether.

[0017] According to further research, the dispersion stirring time is 60-80 min, the dispersion stirring temperature is 65-75° C., and the dispersion stirring frequency is 3000-4000 rpm.

[0018] Further research shows that the nano-processing is to grind the color paste, and the particle size of the color paste after grinding is 40-60nm.

[0019] Beneficial effects: The present invention provides a color paste for black photoresist, wherein the black pigment is pretreated to improve its own dispersibility and insulation. The prepared color paste has high stability and excellent performance, good insulation performance, is not prone to electrostatic interference, and has strong light shielding properties. DETAILED DESCRIPTION

[0020] The present invention is described below with reference to specific embodiments. It is hereby stated that the embodiments selected herein are only used to illustrate and explain the present invention and are not used to limit the present invention.

[0021] Example 1

[0022] This embodiment provides a method for preparing a black photoresist paste, comprising the following steps:

[0023] Step 1: Add resin and solvent into the reaction kettle and disperse and stir them evenly, then add dispersant and pretreated black pigment in sequence and disperse and stir them to obtain color paste;

[0024] Step 2: Nano-process the product obtained in step 1 to obtain a color paste for black photoresist.

[0025] The color paste comprises the following components in parts by weight: 5 parts of acrylic resin, 4 parts of dispersant, 8 parts of solvent, and 12 parts of pretreated black pigment.

[0026] The pretreatment method of the black pigment described in step 2 is: carbon black and titanium dioxide are added to a reaction mixture with a volume multiple of 4 times in a mass ratio of 2:1, ultrasonically heated and dispersed for 20 minutes, heated for 15 minutes at a heating temperature of 70°C, and then a coupling agent with a final concentration of 12% is added. The mixture is cooled to 50°C and stirred for reaction for 2 hours, and then dried to obtain a pretreated black pigment.

[0027] The reaction mixture is a mixture of diazonium salt and water, and the mass ratio of diazonium salt to water is 1-3:9-11.

[0028] The coupling agent is KH550.

[0029] The dispersant is a compound system of sodium tridecyl sulfosuccinate and polyethylene glycol, and the mass ratio of sodium tridecyl sulfosuccinate to polyethylene glycol is 2:3.

[0030] The solvent is ethylene glycol ether.

[0031] The dispersion stirring time is 70 minutes, the dispersion stirring temperature is 70° C., and the dispersion stirring frequency is 3500 rpm.

[0032] The nano-processing is as follows: grinding the color paste, and the particle size of the color paste after grinding is 50nm.

[0033] Example 2

[0034] This embodiment provides a method for preparing a black photoresist paste, comprising the following steps:

[0035] Step 1: Add resin and solvent into the reaction kettle and disperse and stir them evenly, then add dispersant and pretreated black pigment in sequence and disperse and stir them to obtain color paste;

[0036] Step 2: Nano-process the product obtained in step 1 to obtain a color paste for black photoresist.

[0037] The color paste comprises the following components in parts by weight: 3 parts of acrylic resin, 3 parts of dispersant, 7 parts of solvent, and 10 parts of pretreated black pigment.

[0038] The pretreatment method of the black pigment described in step 2 is: carbon black and titanium dioxide are added to a reaction mixture with a volume multiple of 4 times in a mass ratio of 1:1, ultrasonically heated and dispersed for 15 minutes, heated for 10 minutes at a heating temperature of 60°C, and then a coupling agent with a final concentration of 10% is added. The mixture is cooled to 45°C and stirred for reaction for 2 hours, and then dried to obtain a pretreated black pigment.

[0039] The reaction mixture is a mixture of diazonium salt and water, and the mass ratio of diazonium salt to water is 1:9.

[0040] The coupling agent is KBM602.

[0041] The dispersant is a compound system of sodium tridecyl sulfosuccinate and polyethylene glycol, and the mass ratio of sodium tridecyl sulfosuccinate to polyethylene glycol is 2:2.

[0042] The solvent is dimethylacetamide.

[0043] The dispersion stirring time is 60 min, the dispersion stirring temperature is 65° C., and the dispersion stirring frequency is 3000 rpm.

[0044] The nano-processing is as follows: grinding the color paste, and the particle size of the color paste after grinding is 40nm.

[0045] Example 3

[0046] This embodiment provides a method for preparing a black photoresist paste, comprising the following steps:

[0047] Step 1: Add resin and solvent into the reaction kettle and disperse and stir them evenly, then add dispersant and pretreated black pigment in sequence and disperse and stir them to obtain color paste;

[0048] Step 2: Nano-process the product obtained in step 1 to obtain a color paste for black photoresist.

[0049] The color paste comprises the following components in parts by weight: 7 parts of acrylic resin, 3-5 parts of dispersant, 11 parts of solvent, and 15 parts of pretreated black pigment.

[0050] The pretreatment method of the black pigment described in step 2 is: carbon black and titanium dioxide are added to a reaction mixture with a volume multiple of 5 times in a mass ratio of 3:1, ultrasonically heated and dispersed for 25 minutes, heated for 20 minutes at a heating temperature of 80°C, and then a coupling agent with a final concentration of 14% is added. The mixture is cooled to 55°C and stirred for reaction for 3 hours, and then dried to obtain a pretreated black pigment.

[0051] The reaction mixture is a mixture of diazonium salt and water, and the mass ratio of diazonium salt to water is 3:11.

[0052] The coupling agent is TMC-105.

[0053] The dispersant is a compound system of sodium tridecyl sulfosuccinate and polyethylene glycol, and the mass ratio of sodium tridecyl sulfosuccinate to polyethylene glycol is 2:4.

[0054] The solvent is ethylene glycol monobutyl ether.

[0055] The dispersion stirring time is 80 min, the dispersion stirring temperature is 75° C., and the dispersion stirring frequency is 4000 rpm.

[0056] The nano-processing is as follows: grinding the color paste, and the particle size of the color paste after grinding is 60nm.

[0057] Comparative Example 1

[0058] The difference between Comparative Example 1 and Example 1 is that the black pigment in Comparative Example 1 is a black pigment that has not been pretreated.

[0059] Comparative Example 2

[0060] The difference between Comparative Example 2 and Example 1 is that the black pigment of Comparative Example 2 is only added with carbon black.

[0061] Comparative Example 3

[0062] The difference between Comparative Example 3 and Example 1 is that the pretreatment method of the black pigment in Comparative Example 3 is different. The pretreatment method is: carbon black and titanium dioxide are added to water with a volume multiple of 4 times in a mass ratio of 2:1, ultrasonically heated and dispersed for 20 minutes, heated for 15 minutes at a heating temperature of 70°C, and then a coupling agent with a final concentration of 12% is added. The mixture is cooled to 50°C and stirred for reaction for 2 hours, and then dried to obtain a pretreated black pigment.

[0063] The coupling agent is KH550.

[0064] Comparative Example 4

[0065] The difference between Comparative Example 4 and Example 1 is that in Comparative Example 4, only polyethylene glycol in an amount equal to that of sodium tridecyl sulfosuccinate is added as the dispersant.

[0066] Comparative Example 5

[0067] The difference between Comparative Example 5 and Example 1 is that the color paste is not subjected to nano-processing in Comparative Example 5.

[0068] The ceramics prepared in the examples and comparative examples were subjected to performance tests, and the test results are shown in Table 1.

[0069] Effect test

[0070] The performance of the photoresist pigments prepared in the examples and comparative examples was analyzed.

[0071] The pretreated black pigment prepared in Example 1 and the black pigments of Comparative Examples 1 and 3 were pressed into compacts, and the volume resistivity of the compacts was tested according to the method specified in GB / T1410-2006. The test results showed that the volume resistivity of the pretreated black pigment prepared in Example 1 was 2.6×10 10 -3.1×10 10 The volume resistivity of the black pigments in Comparative Examples 1, 2 and 3 is 4.7×10 7 and 6.2×10 9 , 8.4×10 8 ; It can be seen from the test results that the pretreated black pigment of the present invention has high resistivity and good insulation properties; It can be seen from Comparative Examples 1-3 that the black pigment of the present invention uses carbon black and titanium dioxide and adopts a double coupling method to pretreat it, which significantly improves its insulation properties.

[0072] The color paste prepared in the present invention was subjected to a storage stability test and placed at a temperature of 25° C. for 1 year. The test results are shown in Table 1 below:

[0073] Table 1

[0074]

[0075] The results in Table 1 show that the color paste prepared by the present invention has high stability and maintains stable storage performance. Comparative Examples 1-3 show that the pretreatment of the black pigment by the present invention improves its dispersion stability compared to no treatment or other treatment methods. Comparative Example 4 shows that the dispersant added by the present invention is a compound of two dispersants, which has strong dispersibility. The stability of the color paste is improved. Comparative Example 5 shows that the nano-sizing treatment of the color paste by the present invention reduces the particle size of the color paste, further improving the dispersion stability of the color paste.

[0076] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a black photoresist paste, characterized in that: The preparation method comprises the following steps: Step 1: Add resin and solvent into the reaction kettle and disperse and stir them evenly, then add dispersant and pretreated black pigment in sequence and disperse and stir them to obtain color paste; Step 2: nano-processing the color paste obtained in step 1 to obtain a color paste for black photoresist; The pretreatment method of the black pigment described in step 1 is: adding carbon black and titanium oxide in a mass ratio of 1-3:1 to a reaction mixture with a volume multiple of 4-5 times, ultrasonically heating and dispersing for 15-25 minutes, heating for 10-20 minutes at a heating temperature of 60-80°C, then adding a coupling agent with a concentration of 10-14%, cooling to 45-55°C, stirring and reacting for 2-3 hours, and then drying to obtain a pretreated black pigment; the reaction mixture is a mixture of diazonium salt and water, and the mass ratio of diazonium salt to water is 1-3:9-11; The dispersant is a compound system of sodium tridecyl sulfosuccinate and polyethylene glycol, and the mass ratio of sodium tridecyl sulfosuccinate to polyethylene glycol is 2:2-4; The solvent includes but is not limited to one or more of ethylene glycol ether, dimethylacetamide, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether; The resin is acrylic resin.

2. The method for preparing a black photoresist paste according to claim 1, wherein: The color paste comprises the following components in parts by weight: 3-7 parts of acrylic resin, 3-5 parts of dispersant, 7-11 parts of solvent, and 10-15 parts of pretreated black pigment.

3. The method for preparing a black photoresist paste according to claim 1, wherein: The color paste comprises the following components in parts by weight: 5 parts of acrylic resin, 4 parts of dispersant, 9 parts of solvent, and 12 parts of pretreated black pigment.

4. The method for preparing a black photoresist paste according to claim 1, wherein: The coupling agent includes but is not limited to one or more of KH550, KH560, KBM602, TMC-105, TMC-101, and TMC-311w.

5. The method for preparing a black photoresist paste according to claim 1, wherein: The dispersion stirring time is 60-80 minutes, the dispersion stirring temperature is 65-75° C., and the dispersion stirring frequency is 3000-4000 rpm.

6. The method for preparing a black photoresist paste according to claim 1, wherein: The nano-processing comprises grinding the color paste, and the particle size of the color paste after grinding is 40-60nm.

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