High-temperature-resistant low-volatility guide rail lubricating grease for semiconductor manufacturing process and preparation method thereof

Abstract

The invention provides a preparation method of lubricating grease, which comprises the following steps: adding 70% of ester oil into a reaction kettle, adding isocyanate, and stirring at the temperature of 45 DEG C and the rotating speed of 45 rpm; and after the isocyanate in the reaction kettle is melted and the temperature in the kettle is 40-45 DEG C, taking organic amine, mixing, adding the mixed organic amine into the kettle, and carrying out an exothermic reaction with the isocyanate for 1.5-2 hours. The high-temperature-resistant and low-volatility guide rail lubricating grease for the semiconductor manufacturing process can meet the lubricating requirement in an automatic equipment guide rail, can also meet the thermal stability of grease under the high-temperature condition, has the low volatility characteristic under the high-temperature condition, and avoids poor thermal stability under the high-temperature condition.

Description

Technical Field

[0001] The invention relates to the technical field of lubricating grease, and in particular to a high-temperature resistant and low-volatile guide rail lubricating grease used in semiconductor manufacturing processes and a preparation method thereof. Background Art

[0002] The main functions of grease are lubrication, friction reduction, sealing and protection of mechanical equipment. It is extremely important to select suitable lubricating grease under different working conditions. Lubricating grease is made of different types of thickeners thickened by base oils of different types and viscosities, and additives suitable for the corresponding working conditions are added to assist in improving the performance of grease. With the development of the times and the development of industrial technology, in recent years, the global semiconductor industry has experienced cyclical fluctuations while showing an overall growth trend. Benefiting from the global economic recovery and the promotion of new technologies such as 5, artificial intelligence, and the Internet of Things, the semiconductor market has achieved significant growth. In semiconductor manufacturing, semiconductor manufacturing automation is a key development trend in the semiconductor industry. Automation can reduce the uncertainty and errors caused by manual intervention and reduce production costs. In semiconductor manufacturing, there are strict requirements for the application of lubricating grease, requiring excellent chemical stability, thermal stability, and low volatility. In the lubrication process, improper selection of grease and poor thermal stability under high temperature conditions will cause the loss of grease, which is easy to cause grease to throw away contaminated products when the equipment is running. Excessive volatility can easily cause oil pollution to float in the air and contaminate products. Based on the above problems, the present invention provides a high-temperature resistant and low-volatile guide rail grease for semiconductor manufacturing processes and a preparation method thereof. Summary of the invention

[0003] In view of the defects of the prior art, the purpose of the present invention is to provide a high-temperature resistant and low-volatile guide rail grease for use in semiconductor manufacturing processes and a preparation method thereof, so as to solve the problems raised in the above-mentioned background technology.

[0004] The present invention solves the technical problem by adopting the following technical solution:

[0005] The present invention provides a high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process, comprising the following raw materials in parts by weight:

[0006]

[0007] Preferably, the viscosity range of the ester oil (kinematic viscosity at 40°C) is 100-120 mm2 / s, and pentaerythritol ester, trimethylolpropane ester, neopentyl glycol ester, dioctyl adipate, trimellitic acid ester, polyester, diester, and saturated polyol ester can be selected.

[0008] Preferably, the organic amine is one of dodecylamine, octadecylamine, aniline and cyclohexylamine.

[0009] Preferably, the isocyanate is one of MDI and TDI.

[0010] Preferably, the guide rail grease further contains 2-5% of a modified sodium silicate agent based on the total amount of the guide rail grease;

[0011] The preparation method of modified sodium silicate agent is:

[0012] 2-5 parts of sodium alginate powder, 4-7 parts of phosphate buffer solution with a pH of 5.0 and 3-5 parts of silicon carbide powder are mixed and stirred thoroughly to obtain modified sodium alginate;

[0013] Add 2-5 parts of 6% sodium silicate solution to 4-7 parts of 2-5% yttrium nitrate solution, then add 1-3 parts of modified sodium alginate and 2-4 parts of stearic acid, mix and stir thoroughly, and finally filter and dry to obtain modified sodium silicate agent.

[0014] Preferably, the rust inhibitor is one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and oxidized wax ester.

[0015] Preferably, the antioxidant is diphenylamine, di-tert-butyl-p-cresol, or a hindered phenol compound.

[0016] Preferably, the anti-wear extreme pressure agent is one of phosphate ester, phosphite, and melamine polyphosphate.

[0017] Preferably, the preparation method of the grease is:

[0018] Add 70% of ester oil to the reactor, add isocyanate, set the temperature to 45°C, and stir at 45 rpm;

[0019] After the isocyanate in the reaction kettle is melted and the temperature in the kettle is 40-45°C, an organic amine is mixed and then added into the kettle to react with the isocyanate for an exothermic reaction of 1.5-2h;

[0020] After the exothermic reaction is completed, the temperature is set to 100°C and kept constant for 1 to 1.5 hours; during the constant temperature process, the fat is taken out for infrared spectrum detection to detect whether there are any residual isocyanate peaks, until no isocyanate remains;

[0021] After the constant temperature is completed, add 3% of the total amount of water for dehydration reaction and set the temperature to 185°C;

[0022] When the temperature of the material in the kettle rises to 180-185°C, stop heating, add the remaining 20% ​​of ester oil to cool down to 70-80°C, add antioxidant, rust inhibitor, anti-wear extreme pressure agent and modified sodium silicate agent and stir for 10-15 minutes, pour it into the grease receiving tray and cool to room temperature after mixing evenly;

[0023] When the material temperature drops to low, grind it on a three-roll mill for 2 to 3 times;

[0024] After grinding, high vacuum dispersion is performed, and degassing is performed at a rotation speed of 315 rpm and 0.9 MPa to obtain the finished product.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] The present invention discloses a high-temperature resistant and low-volatile guide rail grease for use in semiconductor manufacturing processes. The grease can not only meet the lubrication requirements in the guide rails of automated equipment, but also meet the thermal stability of grease under high temperature conditions and the low volatility characteristics under high temperature conditions, thereby avoiding the adverse effects on equipment, materials and products in the semiconductor production process caused by poor thermal stability under high temperature conditions and high volatility, and reducing the defective rate caused by the lubricating grease performance not meeting the requirements. DETAILED DESCRIPTION

[0027] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] The high temperature resistant and low volatility guide rail lubricating grease used in a semiconductor manufacturing process of this embodiment comprises the following raw materials in parts by weight:

[0029]

[0030] The viscosity range of the ester oil in this embodiment (40°C kinematic viscosity) is 100-120 mm2 / s, and pentaerythritol ester, trimethylolpropane ester, neopentyl glycol ester, dioctyl adipate, trimellitic acid ester, polyester, diester, and saturated polyol ester can be selected.

[0031] The organic amine in this embodiment is one of dodecylamine, octadecylamine, aniline and cyclohexylamine.

[0032] The isocyanate in this embodiment is one of MDI and TDI.

[0033] The guide rail lubricating grease of this embodiment also contains 2-5% of the total amount of the guide rail lubricating grease as modified sodium silicate agent;

[0034] The preparation method of modified sodium silicate agent is:

[0035] 2-5 parts of sodium alginate powder, 4-7 parts of phosphate buffer solution with a pH of 5.0 and 3-5 parts of silicon carbide powder are mixed and stirred thoroughly to obtain modified sodium alginate;

[0036] Add 2-5 parts of 6% sodium silicate solution to 4-7 parts of 2-5% yttrium nitrate solution, then add 1-3 parts of modified sodium alginate and 2-4 parts of stearic acid, mix and stir thoroughly, and finally filter and dry to obtain modified sodium silicate agent.

[0037] The rust inhibitor of this embodiment is one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate, and oxidized wax ester.

[0038] The antioxidants in this embodiment are diphenylamine, di-tert-butyl-p-cresol, and hindered phenol compounds.

[0039] The anti-wear extreme pressure agent of this embodiment is one of phosphate ester, phosphite ester and melamine polyphosphate.

[0040] The preparation method of the grease of this embodiment is:

[0041] Add 70% of ester oil to the reactor, add isocyanate, set the temperature to 45°C, and stir at 45 rpm;

[0042] After the isocyanate in the reaction kettle is melted and the temperature in the kettle is 40-45°C, an organic amine is mixed and then added into the kettle to react with the isocyanate for an exothermic reaction of 1.5-2h;

[0043] After the exothermic reaction is completed, the temperature is set to 100°C and kept constant for 1 to 1.5 hours; during the constant temperature process, the fat is taken out for infrared spectrum detection to detect whether there are any residual isocyanate peaks, until no isocyanate remains;

[0044] After the constant temperature is completed, add 3% of the total amount of water for dehydration reaction and set the temperature to 185°C;

[0045] When the temperature of the material in the kettle rises to 180-185°C, stop heating, add the remaining 20% ​​of ester oil to cool down to 70-80°C, add antioxidant, rust inhibitor, anti-wear extreme pressure agent and modified sodium silicate agent and stir for 10-15 minutes, pour it into the grease receiving tray and cool to room temperature after mixing evenly;

[0046] When the material temperature drops to low, grind it on a three-roll mill for 2 to 3 times;

[0047] After grinding, high vacuum dispersion is performed, and degassing is performed at a rotation speed of 315 rpm and 0.9 MPa to obtain the finished product.

[0048] Example 1:

[0049]

[0050] In this example, the ester oil is a mixture of saturated polyol esters 3970 and 3987 (kinematic viscosity at 40°C): 100mm2 / s) as base oil A, the ratio is 16.65:83.35, the organic amine is octadecylamine and aniline, the ratio is 3:1, the isocyanate is MDI, the rust inhibitor is barium petroleum sulfonate, the antioxidant is diphenylamine, the anti-wear extreme pressure agent is melamine polyphosphate, and the particle size is 6 microns.

[0051] Example 2:

[0052]

[0053] In this example, the ester oil is a mixture of saturated polyol esters 3970 and 3987 (kinematic viscosity at 40°C): 100mm2 / s) as base oil A, the ratio is 16.65:83.35, the organic amine is octadecylamine and aniline, the ratio is 3:1, the isocyanate is MDI, the rust inhibitor is barium petroleum sulfonate, the antioxidant is diphenylamine, the anti-wear extreme pressure agent is melamine polyphosphate, and the particle size is 6 microns.

[0054] Example 3:

[0055]

[0056] In this example, the ester oil is a mixture of saturated polyol esters 3970 and 3987 (40°C kinematic viscosity: 100mm2 / s) as base oil A, with a ratio of 16.65:83.35, the organic amines are octadecylamine and aniline, with a ratio of 3:1, the isocyanate is MDI, the rust inhibitor is barium petroleum sulfonate, the antioxidant is diphenylamine, the anti-wear extreme pressure agent is melamine polyphosphate, and the particle size is 6 microns.

[0057] The guide rail grease also contains a modified sodium silicate agent at 3.5% of the total amount of the guide rail grease;

[0058] The preparation method of modified sodium silicate agent is:

[0059] 3.5 parts of sodium alginate powder, 5 parts of phosphate buffer solution with a pH of 5.0 and 4 parts of silicon carbide powder are mixed and stirred thoroughly to obtain modified sodium alginate;

[0060] 3.5 parts of 6% sodium silicate solution were added to 5.5 parts of 3.5% yttrium nitrate solution, and then 2 parts of modified sodium alginate and 3 parts of stearic acid were added, the mixture was fully mixed and stirred, and finally filtered and dried to obtain a modified sodium silicate agent.

[0061] Comparative Example 1

[0062]

[0063] In this comparative example, PAO is a mixture of PAO10 and PAO20 (40°C kinematic viscosity): 100mm2 / s) as base oil B, the ratio is 59.48:40.52, the organic amine is octadecylamine and aniline, the ratio is 3:1, the isocyanate is MDI, the rust inhibitor is barium petroleum sulfonate, the antioxidant is diphenylamine, the anti-wear extreme pressure agent is melamine polyphosphate, and the particle size is 6 microns.

[0064] Comparative Example 2

[0065]

[0066] In this comparative example, the PAO+ester oil is a mixture of PAO10 (kinematic viscosity at 40°C): 100 mm2 / s) and saturated polyol ester 3987 as base oil C, the ratio is 49.6:50.4, the organic amine is octadecylamine and aniline, the ratio is 3:1, the isocyanate is MDI, the rust inhibitor is barium petroleum sulfonate, the antioxidant is diphenylamine, the anti-wear extreme pressure agent is melamine polyphosphate, and the particle size is 6 microns.

[0067] In the comparative example, the refining process is the same as that in the example except for the difference in the types of base oil A, base oil B, and base oil C.

[0068] Add 70% of base oil B (base oil C) to the reactor, add isocyanate, set the temperature to 45°C, and stir at 45 rpm;

[0069] After the isocyanate in the reaction kettle is melted and the temperature in the kettle is 40-45°C, an organic amine is mixed and then added into the kettle to react with the isocyanate for an exothermic reaction of 1.5-2h;

[0070] After the exothermic reaction is completed, the temperature is set to 100°C and kept constant for 1 to 1.5 hours; during the constant temperature process, the fat is taken out for infrared spectrum detection to detect whether there are any residual isocyanate peaks, until no isocyanate remains;

[0071] After the constant temperature is completed, add 3% of the total amount of water for dehydration reaction and set the temperature to 185°C;

[0072] When the temperature of the material in the kettle rises to 180-185℃, stop heating, add the remaining 20% ​​of ester oil and cool it down to 70-80℃, add antioxidant, rust inhibitor, anti-wear extreme pressure agent and stir for 10-15 minutes, pour it into the grease receiving tray and cool it to room temperature.

[0073] When the material temperature drops to a low level, grind it 2 to 3 times on a three-roll mill.

[0074] After grinding, high vacuum dispersion is performed, and degassing is performed at a rotation speed of 315 rpm and 0.9 MPa to obtain the finished product.

[0075] Through the refining of examples and comparative examples, data detection was carried out, and the detection and comparison data are as follows:

[0076]

[0077]

[0078] Through the test comparison of the examples and comparative examples, in terms of cone penetration data, due to the same ratio of organic amine and isocyanate, the data after the reaction into fat are all within the range of No. 2 fat, and the data are slightly different. In the detection of PB value and PD value data, in the examples, due to the different addition amounts, the values ​​are different. As the addition amount increases, the values ​​also increase, and the anti-wear and extreme pressure bearing capacity are also improved. In the evaporation data of the high-temperature test items, the proportions of the examples are the same except for the addition amount of the anti-wear extreme pressure agent. After testing its evaporation, the data basically remains consistent below 0.1, and the increase in the anti-wear extreme pressure agent does not cause its evaporation data to increase. The comparative example adopts the same addition amount as Example 3, and other materials remain unchanged. However, under the condition of different base oil types and proportions, the evaporation data are tested. The data are all larger than the data of Examples 1, 2, and 3. The volatilization data of Comparative Example 1 is nearly 16 times larger;

[0079] The volatility data of comparative example 2 is nearly 8.6 times greater, from which it can be concluded that the selection of base oil is the key, and the examples can all achieve the effect of low volatility. At the same time, the high temperature stability test was carried out under 100°C. By testing the roller stability values ​​of the examples and the comparative examples and comparing the 0-time cone penetration, the change values ​​in the examples are all smaller than the change values ​​in the comparative examples;

[0080] It can be seen from this that its high-temperature stability is also affected by the base oil. Through comparative testing, the high-temperature stability and volatility in the example are better than those in the control example, and are effectively improved in practical applications. It effectively improves the poor thermal stability of grease under high temperature conditions and the adverse effects on equipment, materials and products in the semiconductor production process caused by high volatility, and reduces the defective rate caused by grease performance not meeting the requirements.

[0081] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0082] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process, characterized in that: It includes the following raw materials in parts by weight: Ester oil: 61~76.5% Organic amine: 10-15% Isocyanate: 10-15% Rust inhibitor: 1-3% Antioxidant: 0.5-1% Anti-wear extreme pressure agent: 3-5%.

2. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 1, characterized in that: The viscosity range of the ester oil (kinematic viscosity at 40° C.) is 100 to 120 mm2 / s, and pentaerythritol ester, trimethylolpropane ester, neopentyl glycol ester, dioctyl adipate, trimellitic acid ester, polyester, diester, and saturated polyol ester can be selected.

3. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 2, characterized in that: The organic amine is one of dodecylamine, octadecylamine, aniline and cyclohexylamine.

4. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 2, characterized in that: The isocyanate is one of MDI and TDI.

5. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 1, characterized in that: The guide rail lubricating grease is further added with a modified sodium silicate agent in an amount of 2-5% of the total amount of the guide rail lubricating grease; The preparation method of modified sodium silicate agent is: 2-5 parts of sodium alginate powder, 4-7 parts of phosphate buffer solution with a pH of 5.0 and 3-5 parts of silicon carbide powder are mixed and stirred thoroughly to obtain modified sodium alginate; Add 2-5 parts of 6% sodium silicate solution to 4-7 parts of 2-5% yttrium nitrate solution, then add 1-3 parts of modified sodium alginate and 2-4 parts of stearic acid, mix and stir thoroughly, and finally filter and dry to obtain modified sodium silicate agent.

6. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 2, characterized in that: The rust inhibitor is one of barium petroleum sulfonate, barium dinonylnaphthalene sulfonate and oxidized wax ester.

7. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 2, characterized in that: The antioxidants are diphenylamine, di-tert-butyl-p-cresol and hindered phenol compounds.

8. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 1, characterized in that: The anti-wear extreme pressure agent is one of phosphate, phosphite and melamine polyphosphate.

9. The high temperature resistant and low volatility guide rail lubricating grease for semiconductor manufacturing process according to claim 1, characterized in that: The preparation method of the lubricating grease is: Add 70% of ester oil to the reactor, add isocyanate, set the temperature to 45°C, and stir at 45 rpm; After the isocyanate in the reaction kettle is melted and the temperature in the kettle is 40-45°C, an organic amine is mixed and then added into the kettle to react with the isocyanate for an exothermic reaction of 1.5-2h; After the exothermic reaction is completed, the temperature is set to 100°C and kept constant for 1 to 1.5 hours; during the constant temperature process, the fat is taken out for infrared spectrum detection to detect whether there are any residual isocyanate peaks, until no isocyanate remains; After the constant temperature is completed, add 3% of the total amount of water for dehydration reaction and set the temperature to 185°C; When the temperature of the material in the kettle rises to 180-185°C, stop heating, add the remaining 20% ​​of ester oil to cool down to 70-80°C, add antioxidant, rust inhibitor, anti-wear extreme pressure agent and modified sodium silicate agent and stir for 10-15 minutes, pour it into the grease receiving tray and cool to room temperature after mixing evenly; When the material temperature drops to low, grind it on a three-roll mill for 2 to 3 times; After grinding, high vacuum dispersion is performed, and degassing is performed at a rotation speed of 315 rpm and 0.9 MPa to obtain the finished product.

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