CN115894083B - Preparation method and application of negative photosensitive type black electronic device - Google Patents
Preparation method and application of negative photosensitive type black electronic device Download PDFInfo
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Abstract
The invention belongs to the technical field of negative photosensitive materials, and discloses a preparation method and application of a negative photosensitive black electronic device. The preparation method of the invention comprises the following steps: (1) The components are mixed according to the proportion, and then dispersed and ground to obtain negative photosensitive marking slurry; (2) Printing, exposing and developing the slurry, and then laminating with LTCC element to obtain a green body; cutting, discharging glue and sintering the obtained green embryo to obtain the black Mark marked LTCC, namely the negative photosensitive black electronic device. The Mark figure on the surface of the electronic device has uniform thickness, high resolution and strong firmness, and is not easy to be broken or fall off under the influence of external conditions.
Description
Technical Field
The invention belongs to the technical field of negative photosensitive materials, and particularly relates to a preparation method and application of a negative photosensitive black electronic device.
Background
With the development of communication technology, LTCCs are increasingly used in the communication field, and their excellent electronic, mechanical and thermal properties have become the preferred way to integrate and modularize electronic components in the future. Mark is typically printed or laser marked on top of LTCC in order to specify the direction of mounting to avoid mounting errors or manufacturing errors.
The conventional marking materials in the laminated electronic component generally use PVB system or acrylic resin of polyvinyl butyral or ethyl cellulose solvent, and the materials have uneven thickness and incomplete marking through printing, are unfixed together with porcelain body and are easy to fall off, so that the problems of low product percent of pass and high risk of mounting errors are caused.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a preparation method and application of a negative photosensitive black electronic device. The size used for the negative photosensitive black electronic device utilizes the characteristic of low-silicon acrylic photosensitive resin, generates active free radicals or cations after absorbing ultraviolet light under the irradiation of a UV light source, initiates monomer polymerization and crosslinking chemical reaction to cure the photosensitive resin, can effectively improve the linearity of the edge of a photoetching material, reduce burrs, can improve adhesive force, and has uniform thickness of a prepared Mark pattern layer, higher resolution and firm combination with a porcelain body. The qualification rate of marked products is obviously increased, and the risk of mounting errors is reduced.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for manufacturing a negative photosensitive black electronic device, comprising the steps of:
(1) Preparation of negative-type light-sensitive marking slurry: mixing a first solvent, a second solvent, a reactive diluent and photosensitive resin, dispersing at a low speed, adding a photoinitiator, a dispersing agent, a leveling agent, a defoaming agent and a coupling agent, dispersing at a high speed, and finally adding ceramic powder and black metal fuel for grinding to obtain negative photosensitive marking slurry with black characteristics;
(2) Preparation of negative photosensitive black electronic device: printing the negative photosensitive marking slurry obtained in the step (1) on a substrate with Mark patterns, and exposing by using a light source; developing with a developing solution to obtain a black Mark layer; laminating the black Mark layer with an LTCC element body to obtain an LTCC complete green embryo; cutting, discharging glue and sintering the obtained green embryo to obtain the black Mark marked LTCC, and obtaining the negative photosensitive type black electronic device.
Preferably, in the step (1), the adhesive is prepared from the following components in percentage by mass: 10-25% of photosensitive resin, 1-2% of photoinitiator, 2-3% of reactive diluent, 12-20% of first solvent, 15-30% of second solvent, 0.2-1.1% of dispersing agent, 0.2-1% of leveling agent, 0.5-1% of defoaming agent, 0.4-1% of coupling agent, 40-55% of ceramic powder and 1-2% of black metal dye; the photosensitive resin is low-silicon acrylic resin, and the molecular weight is 15000-25000; the photoinitiator is selected from 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl]-1-propanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ]]-one or more of 1-propanone, methyl benzoylformate; the reactive diluent is one or more selected from butyl acrylate, methacrylic acid, isobutyl acrylate and hexanediol diacrylate; the first solvent is one or more selected from terpineol, ethyl acetate and propyl acetate; the second solvent is one or more selected from butyl acetic acid, phthalyl butyraldehyde and ethyl cellulose; the dispersing agent is a polyurethane type high polymer dispersing agent; the leveling agent is one or more selected from polyacrylate, acrylated polysiloxane, polyether modified polysiloxane and polysiloxane polyether copolymer; the defoaming agent is a silyl ether copolymerization type defoaming agent; the ceramic powder is one or more selected from alumina-glass system ceramic powder and Ca-B-Si system ceramic powder, and the dielectric constant of the ceramic material is 4.5-6.0; the black metal dye is selected from CuO and Co 2 O 3 、MnO 2 One or more of NiO.
Preferably, in step (1), the coupling agent is a silane coupling agent.
More preferably, the silane coupling agent is one or more selected from a151 (vinyltriethoxysilane), a171 (vinyltrimethoxysilane), a172 (vinyltris (. Beta. -methoxyethoxy) silane).
Preferably, in the step (1), the low-speed dispersion speed is 200-600r/min and the time is 20-40min.
Preferably, in the step (1), the high-speed dispersion speed is 600-1100r/min and the time is 60-300min.
Preferably, in the step (1), the grinding mode is three-roller grinding, and the grinding time is 20-60min.
Preferably, in the step (2), the developing solution is one or more selected from sodium carbonate, sodium hydroxide and potassium hydroxide, and the concentration is 0.1-0.51%.
Preferably, in the step (2), the light source is a UV light source with a wavelength of 365nm and an exposure energy of 30-300mJ/cm 2 。
Preferably, in the step (2), the temperature of the adhesive discharge is 350-550 ℃ and the time is 40-60h.
Preferably, in the step (2), the sintering temperature is 820-920 ℃ and the sintering time is 4-6h.
Meanwhile, the invention claims a negative photosensitive black electronic device prepared by the method.
Meanwhile, the invention claims the application of the negative photosensitive black electronic device in the field of communication electronic devices.
Compared with the prior art, the invention has the following beneficial effects:
1. the black Mark pattern layer adhered to the surface of the LTCC prepared by printing, exposing, developing, laminating, green cutting, discharging glue and sintering the negative photosensitive marking paste can be firmly combined with the porcelain body, and can not fall off from the surface of the porcelain body or cause incomplete marking due to the influence of external conditions, so that the qualification rate of marked products is obviously increased, and the risk of mounting errors is reduced.
2. The invention utilizes the characteristic of photosensitive resin to mix porcelain powder of black alumina-glass system or Ca-B-Si system with photosensitive resin, and is matched with photoinitiator, solvent and other auxiliary agents, and then utilizes the semiconductor photo-etching process to realize ultra-high resolution Mark pattern layer with error of +/-1 um, which has ultra-uniformity and binding property with porcelain body, and can be laminated and matched with proper glue discharging sintering temperature curve to obtain clear, complete and well-bound Mark layer.
Drawings
FIG. 1 is a schematic diagram of an LTCC product with photosensitive black Mark;
FIG. 2 is a schematic diagram of printing a photosensitive black Mark paste onto an LTCC green tape;
FIG. 3 is an exposure sensitive black Mark layer;
FIG. 4 is a developed photosensitive black Mark layer;
FIG. 5 is a schematic illustration of LTCC green tape with a black Mark layer;
FIG. 6 is a schematic diagram of LTCC green tape with terminal electrodes printed to a black Mark layer;
FIG. 7 is a schematic diagram of an LTCC green tape with black Mark layer laminated with LTCC green bodies to obtain an LTCC green body;
FIG. 8 is a flow chart for preparing a negative-tone black Mark slurry;
FIG. 9 is a flow chart of LTCC for preparing a photosensitive Mark layer;
FIG. 10 is a diagram of a Mark normal LTCC device;
fig. 11 is a diagram of LTCC devices with Mark anomalies.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples. Of course, the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Although the steps of the present invention are arranged by reference numerals, the order of the steps is not limited, and the relative order of the steps may be adjusted unless the order of the steps is explicitly stated or the execution of a step requires other steps as a basis. It is to be understood that the term "and/or" as used herein relates to and encompasses any and all possible combinations of one or more of the associated listed items.
Unless otherwise specified, the chemical reagents and materials in the invention are all purchased through market routes.
Example 1
A method for manufacturing a negative photosensitive black electronic device, comprising the steps of:
(1) Preparation of negative-type light-sensitive marking slurry: mixing 150g of terpineol, 200g of butyl acetic acid, 20g of butyl acrylate and 100g of low-silicon acrylic resin with the molecular weight of 20000, dispersing at a low speed of 200r/min for 40min, adding 20g of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 10g of polyurethane type high molecular dispersing agent, 10g of polyacrylate, 10g of silicone copolymer defoamer and 10g of A151 (vinyl triethoxysilane), dispersing at a high speed of 600r/min for 300min, and finally adding 450g of alumina-glass system ceramic powder with the dielectric constant of 5.5 and 20g of CuO, and grinding for 20min by a three-roller machine to obtain negative-touch optical marking slurry with black characteristics;
(2) Preparation of negative photosensitive black electronic device: printing the negative photosensitive marking slurry obtained in the step (1) on a substrate with Mark patterns, and exposing the substrate with a UV light source with the wavelength of 365nm to light with the exposure intensity of 150mJ/cm 2 And developing with sodium carbonate with the concentration of 0.3% to obtain a black Mark pattern, laminating the black Mark pattern and an LTCC element body, cutting a green blank, discharging glue at 400 ℃ for 50h after cutting, and sintering at 870 ℃ for 5.5h to obtain the black Mark marked LTCC, thus obtaining the negative photosensitive black electronic device.
Repeating the experimental steps to prepare 10 negative photosensitive black electronic devices which are prepared from the same raw materials and obtained by the same preparation method for standby.
Example 2
A method for manufacturing a negative photosensitive black electronic device, comprising the steps of:
(1) Preparation of negative-type light-sensitive marking slurry: 150g of ethyl acetate, 150g of o-xylyl butyral, 25g of methacrylic acid and 150g of low-silicon acrylic resin with the molecular weight of 15000 are mixed and dispersed for 20min at a low speed of 600r/min, and then 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl is added]-1-propanone 20g. 10g of polyurethane type high molecular dispersing agent, 8g of acrylated polysiloxane, 7g of silyl ether copolymer defoamer and 10g of A171 (vinyl trimethoxy silane) and performing high-speed dispersion at 1100r/min for 60min, and finally adding 450g of alumina-glass system porcelain powder and Co 2 O 3 Grinding 20g for 60min by using a three-roller machine to obtain negative photosensitive marking slurry with black characteristics;
(2) Preparation of negative photosensitive black electronic device: printing the negative photosensitive marking slurry obtained in the step (1) on a substrate with Mark patterns, and exposing the substrate with a UV light source with the wavelength of 365nm to light with the exposure intensity of 200mJ/cm 2 And developing with sodium hydroxide with the concentration of 0.5% to obtain a black Mark pattern, laminating the black Mark pattern and an LTCC element body, cutting a green blank, discharging glue at 500 ℃ for 45h after cutting, and sintering at 900 ℃ for 5h to obtain the black Mark marked LTCC, thus obtaining the negative-type black electronic device.
Repeating the experimental steps to prepare 10 negative photosensitive black electronic devices which are prepared from the same raw materials and obtained by the same preparation method for standby.
Example 3
A method for manufacturing a negative photosensitive black electronic device, comprising the steps of:
(1) Preparation of negative-type light-sensitive marking slurry: 150g of propyl acetate, 150g of ethyl cellulose, 25g of isobutyl acrylate and 150g of low-silicon acrylic resin with the molecular weight of 25000 are mixed, dispersed for 30min at a low speed of 400r/min, and then 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl group is added]10g of-1-acetone, 10g of polyurethane type high molecular dispersing agent, 5g of polyether modified polysiloxane, 5g of silyl ether copolymerization type defoamer and 5g of A172 (vinyl tri (beta-methoxyethoxy) silane) and performing high-speed dispersion at 800r/min for 150min, and finally adding 400g of Ca-B-Si system ceramic powder and MnO 2 Grinding 20g for 40min by using a three-roller machine to obtain negative photosensitive marking slurry with black characteristics;
(2) Preparation of negative photosensitive black electronic device: printing the negative photosensitive marking slurry obtained in the step (1) on a substrate with Mark patterns, and then using U with the wavelength of 365nmV light source exposure with exposure intensity of 30mJ/cm 2 And developing with potassium hydroxide with the concentration of 0.1% to obtain a black Mark pattern, laminating the black Mark pattern and an LTCC element body, cutting a green blank, discharging glue at 350 ℃ for 60 hours after cutting, and sintering at 820 ℃ for 6 hours to obtain the black Mark marked LTCC, thus obtaining the negative-type black electronic device.
Repeating the experimental steps to prepare 10 negative photosensitive black electronic devices which are prepared from the same raw materials and obtained by the same preparation method for standby.
Comparative example 1
A method of manufacturing an electronic device, comprising the steps of:
(1) Preparation of marking slurry: mixing 150g of terpineol, 200g of butyl acetic acid, 20g of butyl acrylate and 100g of polyvinyl butyral, dispersing at a low speed of 200r/min for 40min, adding 20g of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 10g of polyurethane type high molecular dispersing agent, 10g of polyacrylate, 10g of silicone ether copolymer defoamer and 10g of A151 (vinyl triethoxysilane), dispersing at a high speed of 600r/min for 300min, and finally adding 450g of alumina-glass system porcelain powder with a dielectric constant of 5.5 and 20g of CuO, and grinding for 20min by a three-roll machine to obtain marking slurry;
(2) Preparation of an electronic device: printing the marking slurry obtained in the step (1) on a substrate with Mark patterns, and exposing the substrate with a UV light source with the wavelength of 365nm to light with the exposure intensity of 150mJ/cm 2 And developing with sodium carbonate with the concentration of 0.3% to obtain a Mark pattern, laminating the Mark pattern and an LTCC element body, cutting a green blank, discharging glue at 400 ℃ for 50h after cutting, and sintering at 870 ℃ for 5.5h to obtain the electronic device.
Repeating the experimental steps to prepare 10 electronic devices which are prepared from the same raw materials and obtained by the same preparation method for standby.
In order to investigate the uniformity difference of thickness and size between the products of examples 1 to 3 and comparative example 1, the present invention uses a metallographic polishing machine to perform physical cross section on the LTCC device DPA to obtain a Mark cross section, and then performs cross section measurement by a 3D high-definition imager, and the thicknesses of Mark layers and the sizes of Mark layers in the products of examples 1 to 3 and comparative example 1 (taking one side of a 200 x 200mm square pattern as an example) are measured, as shown in tables 1 and 2.
TABLE 1Mark layer thickness (Unit: um)
TABLE 2 size of Mark layer (Unit: mm)
As can be seen from Table 1, the Mark layer thickness difference value of the products obtained in examples 1-3 is between 0.6 and 0.8um, while the Mark layer thickness difference value of the product obtained in comparative example 1 is 3.3um, and the uniformity of the Mark layer thickness of the product obtained in the invention is obviously improved compared with that of the product obtained in comparative example; meanwhile, as shown in Table 2, the maximum difference of the Mark layer size of the product obtained by the invention is 0.004-0.005, while the maximum difference of the Mark layer size of the product obtained by comparative example 1 is 0.020, which indicates that the uniformity of the Mark layer size of the product obtained by the invention is also improved remarkably.
To further investigate the Mark layer release rate of the products obtained in examples 1 to 3 and comparative example 1, the present invention conducted the following tests:
the testing method comprises the following steps: the visual image detection principle of the six-face visual sorter was used for visual sorting of the elements, and the test results are shown in table 3.
TABLE 3 drop Rate of Mark layer
Results and analysis: as shown in Table 3, the Mark layer of the product obtained in the example was peeled off at a rate of 0.1 to 0.2% and the Mark layer of the product obtained in the comparative example 1 was peeled off at a rate of 0.8%. 4-8 times of the embodiment, the product obtained by the invention has better thickness uniformity and size uniformity of the Mark layer, and the falling rate of the product is obviously reduced compared with the prior art, so the product has wide development prospect in the aspect of preparing negative photosensitive black electronic devices.
It should be apparent to those skilled in the art that any modification of the present invention, equivalent substitution of raw materials for the product of the present invention, addition of auxiliary components, selection of specific modes, etc., falls within the scope of the present invention and the scope of disclosure.
Claims (7)
1. A method for manufacturing a negative photosensitive black electronic device, comprising the steps of:
(1) Preparation of negative-type light-sensitive marking slurry: mixing a first solvent, a second solvent, a reactive diluent and photosensitive resin, dispersing at a low speed, adding a photoinitiator, a dispersing agent, a leveling agent, a defoaming agent and a coupling agent, dispersing at a high speed, and finally adding ceramic powder and black metal fuel for grinding to obtain negative photosensitive marking slurry with black characteristics; the negative photosensitive marking slurry comprises photosensitive resin with the mass ratio of 10-25%, wherein the photosensitive resin is low-silicon acrylic resin, and the molecular weight is 15000-25000;
(2) Preparation of negative photosensitive black electronic device: printing the negative photosensitive marking slurry obtained in the step (1) on a substrate with a Mark pattern layer, and exposing by using a light source; developing with a developing solution to obtain a black Mark layer; laminating the black Mark layer with an LTCC element body to obtain an LTCC complete green embryo; cutting, discharging glue and sintering the obtained green embryo to obtain a black Mark marked LTCC, namely the negative photosensitive black electronic device; the developing solution is one or more selected from sodium carbonate, sodium hydroxide and potassium hydroxide, and the concentration is 0.1-0.51%; the sintering temperature is 820-920 ℃ and the sintering time is 4-6h;
in the step (1) described above, the step of (c) is performed,the composite material is prepared from the following components in percentage by mass: 10-25% of photosensitive resin, 1-2% of photoinitiator, 2-3% of reactive diluent, 12-20% of first solvent, 15-30% of second solvent, 0.2-1.1% of dispersing agent, 0.2-1% of leveling agent, 0.5-1% of defoaming agent, 0.4-1% of coupling agent, 40-55% of ceramic powder and 1-2% of black metal dye; the photoinitiator is selected from 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl]-1-propanone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ]]-one or more of 1-propanone, methyl benzoylformate; the reactive diluent is one or more selected from butyl acrylate, methacrylic acid, isobutyl acrylate and hexanediol diacrylate; the first solvent is one or more selected from terpineol, ethyl acetate and propyl acetate; the second solvent is one or more selected from butyl acetic acid, phthalyl butyraldehyde and ethyl cellulose; the dispersing agent is a polyurethane type high polymer dispersing agent; the leveling agent is one or more selected from polyacrylate, acrylated polysiloxane, polyether modified polysiloxane and polysiloxane polyether copolymer; the defoaming agent is a silyl ether copolymerization type defoaming agent; the coupling agent is one or more selected from A151 (vinyl triethoxysilane), A171 (vinyl trimethoxysilane) and A172 (vinyl tri (beta-methoxyethoxy) silane); the ceramic powder is one or more selected from alumina-glass system ceramic powder and Ca-B-Si system ceramic powder, and the dielectric constant of the ceramic material is 4.5-6.0; the black metal dye is selected from CuO and Co 2 O 3 、MnO 2 One or more of NiO.
2. The method for manufacturing a negative photosensitive black electronic device according to claim 1, wherein in the step (1), the low-speed dispersion rate is 200-600r/min and the time is 20-40min; the high-speed dispersion speed is 600-1100r/min, and the time is 60-300min.
3. The method for manufacturing a negative photosensitive black electronic device according to claim 1, wherein in the step (1), the grinding mode is three-roll grinding, and the grinding time is 20-60min.
4. The method for manufacturing a negative photosensitive black electronic device according to claim 1, wherein in the step (2), the light source is a UV light source with a wavelength of 365nm and an exposure energy of 30-300mJ/cm 2 。
5. The method of claim 1, wherein in the step (2), the temperature of the paste ejection is 350-550 ℃ and the time is 40-60h.
6. A negative-working black electronic device produced by the method of any one of claims 1 to 5.
7. Use of the negative-tone black electronic device of claim 6 in the field of communication electronics.
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