CN111363401B - Slurry for semiconductor device glass passivation layer and preparation method thereof - Google Patents
Slurry for semiconductor device glass passivation layer and preparation method thereof Download PDFInfo
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- CN111363401B CN111363401B CN201811587571.4A CN201811587571A CN111363401B CN 111363401 B CN111363401 B CN 111363401B CN 201811587571 A CN201811587571 A CN 201811587571A CN 111363401 B CN111363401 B CN 111363401B
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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
- C09D11/02—Printing inks
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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
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention provides a slurry for a glass passivation layer of a semiconductor device, which comprises the following components in percentage by weightThe following components: 30-35% of butyl carbitol; ethyl cellulose: 1.2-4%; lubricant: 0.05 to 0.5 percent; thixotropic agent: 0.6-1.4%; glass powder: 60-65%; the glass powder is SiO 2 Particles having a size of 2-30 μm. The slurry is prepared by dissolving ethyl cellulose and a lubricant into alcohol solution containing butyl carbitol, heating, mixing and stirring, then sequentially adding a thixotropic agent and glass powder, and stirring and mixing at constant temperature. The glass passivation protective layer printed by the paste has good integrity and thickness uniformity, and can ensure that the voltage on the electrode surface is qualified.
Description
Technical Field
The invention belongs to the field of semiconductor device printing, and particularly relates to slurry for a glass passivation layer of a semiconductor device and a preparation method thereof.
Background
At present, a layer of slurry is printed on a silicon wafer with a groove on one surface by adopting a screen printing technology, and then a glass passivation protective layer is formed after low-temperature drying and high-temperature sintering, wherein the printing integrity, the protective layer quality and the printing efficiency are determined to a great extent by the quality of the slurry. The thixotropic agent is an important component in the slurry, is mainly used for suspending and thickening organic colloid, enables glass powder in the slurry to be uniformly dispersed without agglomeration and sedimentation, has an adjusting effect on the viscosity and the adhesiveness of the slurry, and can improve the printing quality and the process performance of the slurry. The existing slurry has the problems of poor surface integrity and uneven thickness of glass layers in a groove after the slurry is printed due to the viscosity matching problem, and meanwhile, the non-groove part, namely the electrical property of an electrode surface, is unqualified due to the viscosity problem of the slurry.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the slurry for the glass passivation layer of the semiconductor device and the preparation method thereof, the protective layer printed by using the slurry has good uniformity and qualified thickness, and meanwhile, the electrical property of the electrode surface also meets the requirement, so that a transparent, smooth and complete glass passivation layer is formed on the front surface of the silicon chip. The invention also provides a preparation method of the slurry.
The technical purpose of the invention is realized by the following technical scheme:
the slurry for the passivation layer of the glass of the semiconductor device comprises the following components in parts by weight: 30-35% of butyl carbitol; ethyl cellulose: 1.2-4%; lubricant: 0.05 to 0.5 percent; thixotropic agent: 0.6-1.4%; glass powder: 60-65%; the glass powder is SiO 2 Particles having a size of 2-30 μm.
Preferably, the thixotropic agent is present in an amount of 0.8 to 1.2%.
Preferably, the glass frit has a particle size of 2 to 16 μm.
Further, the thixotropic agent is selected from castor oil, fumed silica or polyamide wax.
Preferably, the thixotropic agent is castor oil.
A preparation method of slurry for a semiconductor device glass passivation layer comprises the following steps:
a: dissolving ethyl cellulose and a lubricant in butyl carbitol according to weight percentage, and stirring for 4 hours in an automatic stirrer at constant temperature: 70-120 ℃;
b: adding castor oil into the solution in the step A according to the weight percentage, and stirring for 2 hours at the temperature of 30-60 ℃;
c: adding glass powder into the mixture obtained in the step B according to the weight percentage;
d: stirring for 24h at constant temperature of 30-60 ℃;
f: and D, printing the slurry prepared in the step D on a silicon chip with a groove on one surface by a screen printing mode, and drying and vacuum sintering to form a glass passivation layer.
Further, in the step F, the drying temperature is: 130-200 ℃; the sintering temperature is 550-820 ℃, and the vacuum pressure in the sintering furnace is as follows: -1X 10 5 -0.5×10 5 MPa。
Compared with the prior art, the technical scheme has the following advantages and beneficial effects:
according to the slurry for the semiconductor device glass passivation layer, the combination range of the slurry is determined through a large number of tests, the glass passivation layer obtained by printing the slurry provided by the technical scheme has good integrity and thickness uniformity, and the voltage of the electrode surface can be guaranteed to be qualified.
Drawings
FIG. 1 is a plan view of a passivation layer of trench glass in accordance with a first embodiment of the present invention;
FIG. 2 is a plan view of a passivation layer of trench glass in a second embodiment of the present invention;
FIG. 3 is a plan view of the passivation layer of trench glass in a third embodiment of the present invention;
FIG. 4 is a plan view of the passivation layer of trench glass in the fourth embodiment of the present invention;
FIG. 5 is a plan view of the passivation layer of the trench glass in the comparative example of the present invention;
fig. 6 is a plan view of the passivation layer of the trench glass in the comparative example of the present invention.
Detailed Description
The invention is further illustrated by the following examples and comparative examples:
in the following examples and comparative examples, the integrity of the glass passivation layer is shown by visually observing the surface appearance of the fired channel, whether the width of the glass passivation layer in the channel is uniform or not and whether the glass passivation layer has a coagulation accumulation phenomenon or not can be visually observed, and if the width of the glass passivation layer in the channel is uniform and no coagulation accumulation hard object exists, the integrity of the glass passivation layer on the surface of the channel is good; the thickness (mum) is used for representing the uniformity of the glass passivation layer, the standard range value of the value is 40 +/-5μm, and the value is more than or less than the standard value, which indicates that the glass passivation layer is not uniform; the electrical property of the electrode surface is represented by a reverse voltage (V), and the larger the value is, the better the electrical property of the electrode surface is, the better the viscosity of the slurry is, and the slurry does not flow to the electrode surface to influence the voltage.
The first embodiment is as follows:
as shown in table 1, 4% by weight of ethyl cellulose and 0.05% by weight of lubricant are poured into 35% by weight of butyl carbitol, dissolved in a stirring kettle at 70-120 ℃, and stirred for 4 hours at constant temperature; then cooling to 30-60 ℃, adding 0.8 wt% of castor oil, and stirring for 2h at constant temperature; then adding 60 percent by weight of glass powder, wherein the temperature is still 30-60 ℃, and stirring the obtained solution at constant temperature for 24 hours to prepare a slurry solution. Printing the glass slurry on a silicon wafer with a groove on one surface by adopting a screen printing technology, drying and curing at 130-200 ℃, and then performing vacuum pressure: -1X 10 5 -0.5×10 5 Sintering in a high-temperature sintering furnace under MPa, wherein the sintering temperature is 550-820 ℃, and the constant temperature of high-temperature sintering is 820 +/-20 ℃, so as to obtain a layer of glass passivation layer.
In this embodiment, the thixotropic agent is castor oil, the weight ratio is 0.8%, the mixture ratio of other components is within the range, the surface of the obtained glass passivation layer under a microscope of 100 times is shown in fig. 1, the surface width of the glass passivation layer in the groove is uniform, no aggregation occurs, and the completeness of the glass passivation layer on the surface of the groove is good; the thickness is 38-44 μm, wherein the thickness at the bottom of the groove is larger than the thickness at the two sides of the groove, because the slurry at the two sides of the groove flows downwards along the slope of the side surface during the printing process, but the whole thickness is also within the standard range value of 40 +/-5 μm; and testing the electrode surface of the non-groove part, wherein the voltage value is 1200-1300V, and the performance requirement of the silicon wafer is met.
Example two:
as shown in table 1, 3% by weight of ethyl cellulose and 0.5% by weight of lubricant are poured into 32% by weight of butyl carbitol, dissolved in a stirring kettle at 70-120 ℃, and stirred for 4 hours at constant temperature; then cooling to 30-60 ℃, adding 1.2 wt% of castor oil, and stirring for 2h at constant temperature; adding 63% glass powder by weight, stirring the obtained solution at constant temperature for 24h to prepare a slurry solution, wherein the temperature is still 30-60 ℃. Adopting a screen printing technology, printing glass slurry on a silicon chip with a groove on one surface, drying and curing at 130-200 ℃, and then performing vacuum pressure: -1X 10 5 -0.5×10 5 Sintering in a high-temperature sintering furnace under MPa, wherein the sintering temperature is 550-820 ℃, and the constant temperature of high-temperature sintering is 820 +/-20 ℃, so as to obtain a layer of glass passivation layer.
In this embodiment, the thixotropic agent is castor oil, the weight ratio is 1.2%, the mixture ratio of other components is within the range, the surface of the obtained glass passivation layer under a microscope of 100 times is shown in fig. 2, and the surface width of the glass passivation layer in the groove is uniform and free of aggregation; the thickness is 38-44 μm, and is 40 + -5 μm within the standard range; and the voltage of the electrode surface is 1200-1300V, so that the performance requirement of the silicon wafer is met.
Example three:
as shown in table 1, 1% by weight of ethyl cellulose and 0.05% by weight of lubricant are poured into 30% by weight of butyl carbitol, dissolved in a stirring kettle at 70-120 ℃, and stirred for 4 hours at constant temperature; then cooling to 30-60 ℃, and adding a mixture of 0.6 wt% of castor oil and fumed silica, wherein the ratio of the castor oil to the fumed silica is as follows: 6-8, stirring for 2-4 hours at constant temperature; then adding 65 percent by weight of glass powder, wherein the temperature is still 30-60 ℃, and stirring the obtained solution at constant temperature for 24 hours to prepare a slurry solution. The glass slurry is printed on a silicon wafer with a groove on one surface by adopting a screen printing technology and is processed by 130-200 DEG CAfter drying and curing, the vacuum pressure is as follows: -1X 10 5 -0.5×10 5 Sintering in a high-temperature sintering furnace under MPa, wherein the sintering temperature is 550-820 ℃, and the constant temperature of high-temperature sintering is 820 +/-20 ℃, so as to obtain a layer of glass passivation layer.
In this example, the thixotropic agent is a mixture of castor oil and fumed silica in the following proportions: 6-8, the weight ratio of the mixture is 0.6%, the mixture ratio of other components is within the range, the surface of the obtained glass passivation layer under a microscope of 100 times is shown in figure 3, and the surface width of the glass passivation layer in the groove is uniform and free of aggregation; the thickness is 38-44 μm, and is 40 + -5 μm within the standard range; and the voltage of the electrode surface is 1200-1300V, so that the performance requirement of the silicon wafer is met.
Example four:
as shown in table 1, 3% by weight of ethyl cellulose and 0.5% by weight of lubricant are poured into 30% by weight of butyl carbitol, dissolved in a stirring kettle at 70-120 ℃, and stirred for 4 hours at constant temperature; then cooling to 30-60 ℃, adding a mixture of castor oil and polyamide wax with the weight ratio of 1.4%, wherein the ratio of the castor oil to the fumed silica is as follows: 6-8, stirring for 2-4 hours at constant temperature; then adding 65 percent by weight of glass powder, wherein the temperature is still 30-60 ℃, and stirring the obtained solution at constant temperature for 24 hours to prepare a slurry solution. Adopting a screen printing technology, printing glass slurry on a silicon chip with a groove on one surface, drying and curing at 130-200 ℃, and then performing vacuum pressure: -1X 10 5 -0.5×10 5 Sintering in a high-temperature sintering furnace under the pressure of MPa, wherein the sintering temperature is 550-820 ℃, and the constant temperature of high-temperature sintering is 820 +/-20 ℃, so that a glass passivation layer is obtained.
In this example, the thixotropic agent is a mixture of castor oil and a polyamide wax, the ratio of castor oil to fumed silica being: 6-8, the weight ratio of the mixture is 1.4%, the mixture ratio of other components is within the range, the surface of the obtained glass passivation layer under a microscope of 100 times is shown in figure 4, and the surface width of the glass passivation layer in the groove is uniform and free of aggregation; the thickness is 38-44 μm, and is 40 + -5 μm within the standard range; and the voltage of the electrode surface is 1200-1300V, so that the performance requirement of the silicon wafer is met.
Comparative example one:
as shown in table 1, 3% by weight of ethyl cellulose and 0.5% by weight of lubricant are poured into 35% by weight of butyl carbitol, dissolved in a stirring kettle at 70-120 ℃, and stirred for 4 hours at constant temperature; then cooling to 30-60 ℃, and adding a mixture of fumed silica and polyamide wax with the weight ratio of 1.4%, wherein the proportion of fumed silica to polyamide wax is as follows: 5-7, stirring for 2 hours at constant temperature; then adding 60 percent by weight of glass powder, wherein the temperature is still 30-60 ℃, and stirring the obtained solution at constant temperature for 24 hours to prepare a slurry solution. Printing the glass slurry on a silicon wafer with a groove on one surface by adopting a screen printing technology, drying and curing at 130-200 ℃, and then performing vacuum pressure: -1X 10 5 -0.5×10 5 Sintering in a high-temperature sintering furnace under MPa, wherein the sintering temperature is 550-820 ℃, and the constant temperature of high-temperature sintering is 820 +/-20 ℃, so as to obtain a layer of glass passivation layer.
In this example, the thixotropic agent is a mixture of fumed silica and polyamide wax, the proportions of fumed silica and polyamide wax being: 5-7, the weight ratio after mixing is 1.4%, the mixture ratio of other components is within the range, the surface of the obtained glass passivation layer under a microscope of 100 times is shown in figure 5, and the surface of the glass in the groove is uneven and has a local top phenomenon; the thickness is 32-48 mu m, which is not in the standard range value, thus indicating that the thickness of the passivation layer of the printed glass is not uniform; and the voltage of the electrode surface is 800-1000V, and the voltage is lower, which indicates that a large amount of glass slurry is remained on the electrode surface, the viscosity of the glass slurry is not good, and the electrical property requirement of the electrode surface cannot be met.
Comparative example two:
in this example, no thixotropic agent was added, and the ratios of other ingredients were within the ranges, and the specific parameters are shown in table 1. The surface of the obtained glass passivation layer under a microscope of 100 times is shown in FIG. 6, and the glass surface in the groove is not uniform, and the groove width is not uniform; the thickness is 32-48 mu m, which is not in the standard range value, thus indicating that the thickness of the passivation layer of the printed glass is not uniform; the voltage of the electrode surface is 800-1000V, and the voltage is lower, which indicates that a large amount of glass slurry is left on the electrode surface, the viscosity of the glass slurry is not good, and the electrical property requirement of the electrode surface cannot be met.
Experimental data show that the appearance and thickness of the glass passivation layer and the voltage of the electrode surface in each example and each comparative example are obviously superior to the slurry of the comparative example in both single performance and comprehensive performance.
TABLE 1
This technical scheme has following advantage and beneficial effect:
the thixotropic agent plays an important role in the viscosity of the slurry, preferably, the thixotropic agent at least comprises castor oil, so that a glass passivation layer with good integrity and uniform thickness can be obtained and meets the standard requirement; meanwhile, the voltage of the electrode surface meets the electrical requirement.
The slurry for the semiconductor device glass passivation layer provided by the invention determines the combination range of the slurry through a large number of tests, and the glass passivation layer obtained by printing the slurry provided by the technical scheme has good integrity and thickness uniformity, and meanwhile, the qualified voltage on the electrode surface can be ensured.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (3)
1. The slurry for the passivation layer of the glass of the semiconductor device is characterized by comprising the following components in parts by weight: butyl carbid30-35% of alcohol; ethyl cellulose: 1.2-4%; lubricant: 0.05 to 0.5 percent; thixotropic agent: 0.8 to 1.2 percent; glass powder: 60 to 65 percent; the glass powder is SiO 2 Particles having a size of 2-16 μm; the thixotropic agent is castor oil;
the preparation method of the slurry for the semiconductor device glass passivation layer comprises the following steps:
a: dissolving ethyl cellulose and a lubricant in butyl carbitol, and stirring for 4 hours at a constant temperature, wherein the stirring temperature is as follows:
70-120℃；
b: adding castor oil into the solution obtained in the step A, and stirring for 2 hours in a container at the temperature of 30-60 ℃;
c: adding glass powder into the step B;
d: stirring for 24h at constant temperature of 30-60 ℃;
f: and D, printing the slurry prepared in the step D on a silicon chip with a groove on one surface by a screen printing mode, and drying and vacuum sintering to form a glass passivation layer.
2. A method for preparing the slurry for the glass passivation layer of the semiconductor device according to claim 1, comprising the following steps:
a: dissolving ethyl cellulose and a lubricant in butyl carbitol, and stirring for 4 hours at a constant temperature, wherein the stirring temperature is as follows:
70-120℃；
b: adding castor oil into the solution obtained in the step A, and stirring for 2 hours in a container at the temperature of 30-60 ℃;
c: adding glass powder into the step B;
d: stirring for 24h at constant temperature of 30-60 ℃;
f: and D, printing the slurry prepared in the step D on a silicon chip with a groove on one surface by a screen printing mode, and drying and vacuum sintering to form a glass passivation layer.
3. The method according to claim 2, wherein the drying temperature in step F is: 130-200 ℃; the sintering temperature is 550-820 ℃, and the pressure of vacuum sintering is as follows: -1X 10 5 -0.5×10 5 MPa。
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| CN101459059A (en) * | 2007-12-11 | 2009-06-17 | 林楠 | Glass passivating technique process for semi-conductor device with silicon large diameter round wafer |
| CN101615637B (en) * | 2009-07-08 | 2010-09-15 | 西安交通大学苏州研究院 | Sizing agent for forming electrode of solar cell and preparation method thereof |
| CN101794639B (en) * | 2010-03-16 | 2011-10-05 | 彩虹集团公司 | Environment-friendly glass frit and preparation method thereof |
| CN103130413B (en) * | 2011-11-24 | 2015-05-27 | 比亚迪股份有限公司 | Glass raw material composition, inorganic glass powder, crystalline silicon solar battery aluminum conductive paste and preparation method of the crystalline silicon solar battery aluminum conductive paste |
| CN105470150B (en) * | 2015-12-21 | 2018-07-10 | 中国电子科技集团公司第五十五研究所 | A kind of glass passivating method of silicon mesa diode |
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