Oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing and preparation method of oil-soluble diamond micro-powder paste

Abstract

The invention relates to oil-soluble diamond micro-powder paste for final polishing of ultralow subsurface damage sapphire and a preparation method of the oil-soluble diamond micro-powder paste, the oil-soluble diamond micro-powder paste comprises a mixture of nano cerium oxide-diamond core-shell hybrid particles and polycarboxylate system oily diamond gypsum, the nano cerium oxide-diamond core-shell hybrid particles account for 0.05-0.8%, and the polycarboxylate system oily diamond gypsum accounts for 0.05-0.8%. And the cerium oxide in the nano cerium oxide-diamond core-shell hybrid particles is 8-15 nm. The method has the advantages that after sapphire is subjected to final polishing, the subsurface damage depth is greatly reduced to be smaller than or equal to 8 nm from 25-35 nm of a traditional polycarboxylate paste, meanwhile, the removal rate is kept to be larger than or equal to 0.18 micron / min, and the surface roughness Ra is smaller than or equal to 0.2 nm.

Description

TECHNICAL FIELD

[0001] The present application relates to an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing and a preparation method thereof. BACKGROUND

[0002] Currently, when polishing sapphire, the existing polycarboxylate system oil-based diamond paste (including BYK-9076, Priolube3970 and other formulations) has achieved Ra 0.2-0.3 nm and high removal rate, but due to pure mechanical action, the subsurface damage layer of sapphire after final polishing is still generally 25-40 nm under TEM actual measurement, which seriously restricts downstream processing projects such as the strength of ultra-thin windows (<100 μm), the laser-induced damage threshold (LIDT) of high-power laser windows and the sidewall steepness of LED patterned substrates (PSS), and currently there is no patent or document disclosing the addition of a second phase nanoparticle with chemical polishing function to the oil-based diamond paste to solve this pain point. SUMMARY

[0003] The purpose of the present application is to overcome the shortcomings of the prior art and provide an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing and a preparation method thereof, so that the subsurface damage depth of sapphire after final polishing is greatly reduced from 25-35 nm of the traditional polycarboxylate paste to ≤8 nm, while maintaining a removal rate ≥0.18 μm / min and a surface roughness Ra ≤0.2 nm.

[0004] In order to achieve the above-mentioned purpose, the first technical solution of the present application is realized, which is an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing, characterized in that it comprises: A mixture of nano cerium oxide-diamond core-shell hybrid particles and a polycarboxylate system oil-based diamond paste, wherein the proportion of nano cerium oxide-diamond core-shell hybrid particles is 0.05-0.8%.

[0005] In the present technical solution, the cerium oxide in the nano cerium oxide-diamond core-shell hybrid particles is 8-15 nm, the diamond is 1-2 μm, and the cerium oxide coating rate is 30-50%.

[0006] In the present technical solution, the polycarboxylate system oil-based diamond paste comprises a mixture of 8-12% of single crystal diamond micro-powder of W1.5, 6-9% of polycarboxylate dispersant, 40-50% of synthetic ester base oil, 20-28% of PAO6 or PAO8, 5-8% of PMA thickening agent, 5-8% of oil-soluble polyether and lanolin, 0.3-0.7% of antioxidant and defoaming agent mixture.

[0007] The ratio of the oil-soluble polyether and lanolin is 2:1-3:1, and the ratio of the antioxidant and the defoaming agent is 1:1-3:1.

[0008] To achieve the above object, the second technical solution of the present application is implemented as follows: a preparation method of an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing, characterized by comprising the following steps: The polycarboxylate system oil-based diamond paste is added with 0.05-0.8% of surface-modified nano cerium oxide-diamond core-shell hybrid particles in mass ratio, and is fully mixed.

[0009] In the technical solution, the polycarboxylate system oil-based diamond paste comprises 8-12% of W1.5 single crystal diamond micro-powder, 6-9% of polycarboxylate dispersant, 40-50% of synthetic ester-based oil, 20-28% of PAO6 or PAO8, 5-8% of PMA thickening agent, 5-8% of a mixture of oil-soluble polyether and lanolin, and 0.3-0.7% of a mixture of antioxidant and defoaming agent.

[0010] In the technical solution, the nano cerium oxide-diamond core-shell hybrid particle has 8-15 nm of cerium oxide and 1-2 μm of diamond, and a cerium oxide coating rate of 30-50%.

[0011] The ratio of the oil-soluble polyether and lanolin is 2:1-3:1, and the ratio of the antioxidant and the defoaming agent is 1:1-3:1.

[0012] Compared with the prior art, the present application has the following advantages: after sapphire final polishing, the depth of subsurface damage is greatly reduced from 25-35 nm of the traditional polycarboxylate paste to ≤8 nm, while the removal rate is kept ≥0.18 μm / min, and the surface roughness Ra is ≤0.2 nm. DETAILED DESCRIPTION

[0013] The specific embodiments of the present application are further described below. It should be noted that the description of the embodiments is used to help understand the present application, but does not constitute a limitation on the present application. In addition, the technical features involved in the various embodiments of the present application described below can be combined with each other as long as they do not conflict with each other. EMBODIMENT

[0014] It is an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing, comprising: A mixture of nano cerium oxide-diamond core-shell hybrid particles and polycarboxylate system oil-based diamond paste, wherein the nano cerium oxide-diamond core-shell hybrid particles account for 0.8%.

[0015] In processing, the nano ceria-diamond core-shell hybrid particles are added into the oil-based polycarboxylate system at a super low proportion of 0.8%; in polishing, mechanical and chemical instantaneous synergistic polishing is realized, under the polishing tin disc speed of 200-300 rpm, the ceria shell layer has an instantaneous soft chemical reaction with the sapphire surface, the amorphous layer induced by mechanical scratches is removed immediately, and the SSD is less than or equal to 8 nm under the verification of TEM; due to the extremely small amount of nano ceria-diamond core-shell hybrid particles, the paste fluidity, disc cleanliness and original removal rate are not affected, and even slightly improved.

[0016] In the embodiment, the nano ceria-diamond core-shell hybrid particles have a ceria of 15 nm and a diamond of 2 μm, and the ceria coating rate is 50%.

[0017] In the embodiment, the oil-based diamond paste of the polycarboxylate system includes 8% of single crystal diamond powder of W1.5, 6% of polycarboxylate dispersant, 50% of synthetic ester-based oil, 20% of PAO6 or PAO8, 8% of PMA thickening agent, 7.7% of a mixture of oil-soluble polyether and lanolin, 0.3% of antioxidant and defoaming agent mixture.

[0018] In the embodiment, the ratio of the oil-soluble polyether and lanolin is 2:1, and the ratio of the antioxidant and defoaming agent is 1:11. Embodiment

[0019] It is a preparation method of an oil-soluble diamond paste for ultra-low subsurface damage sapphire final polishing, characterized in that 0.8% of surface modified nano ceria-diamond core-shell hybrid particles are added into the oil-based diamond paste of the polycarboxylate system in terms of mass ratio, and fully mixed.

[0020] In processing, the nano ceria-diamond core-shell hybrid particles are added into the oil-based polycarboxylate system at a super low proportion of 0.8%; in polishing, mechanical and chemical instantaneous synergistic polishing is realized, under the polishing tin disc speed of 200-300 rpm, the ceria shell layer has an instantaneous soft chemical reaction with the sapphire surface, the amorphous layer induced by mechanical scratches is removed immediately, and the SSD is less than or equal to 8 nm under the verification of TEM; due to the extremely small amount of nano ceria-diamond core-shell hybrid particles, the paste fluidity, disc cleanliness and original removal rate are not affected, and even slightly improved.

[0021] In the embodiment, the oil-based diamond paste of the polycarboxylate system includes: the oil-based diamond paste of the polycarboxylate system includes 8% of single crystal diamond powder of W1.5, 6% of polycarboxylate dispersant, 50% of synthetic ester-based oil, 20% of PAO6 or PAO8, 8% of PMA thickening agent, 7.7% of a mixture of oil-soluble polyether and lanolin, 0.3% of antioxidant and defoaming agent mixture.

[0022] In the embodiment, the nano ceria-diamond core-shell hybrid particles have 15 nm of ceria, 2 μm of diamond, and 50% of ceria coating rate.

[0023] In the embodiment, the ratio of the oil-soluble polyether and lanolin is 2:1, and the ratio of the antioxidant and the defoaming agent is 1:1. Embodiment

[0024] It is an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing and a preparation method thereof, comprising: The mixture of the nano ceria-diamond core-shell hybrid particles and the polycarboxylate system oil-based diamond paste, wherein the nano ceria-diamond core-shell hybrid particles account for 0.05%.

[0025] During processing, the nano ceria-diamond core-shell hybrid particles are added into the polycarboxylate system at an ultra-low proportion of 0.8%; during polishing, instantaneous synergistic polishing of mechanical and chemical is realized, under the polishing tin disc speed of 200-300 rpm, instantaneous soft chemical reaction occurs between the ceria shell layer and the sapphire surface, the amorphous layer induced by mechanical scratches is immediately removed, and the SSD is less than or equal to 8 nm under TEM verification; due to the extremely small amount of nano ceria-diamond core-shell hybrid particles, the paste fluidity, disc cleanliness and original removal rate are not affected, and even slightly improved.

[0026] In the embodiment, the nano ceria-diamond core-shell hybrid particles have 8 nm of ceria, 1 μm of diamond, and 30% of ceria coating rate.

[0027] In the embodiment, the polycarboxylate system oil-based diamond paste comprises: 12% of single crystal diamond micro-powder of W1.5, 8.3% of polycarboxylate dispersant, 40% of synthetic ester base oil, 28% of PAO6 or PAO8, 5% of PMA thickening agent, 6% of a mixture of oil-soluble polyether and lanolin, and 0.7% of a mixture of antioxidant and defoaming agent.

[0028] In the embodiment, the ratio of the oil-soluble polyether and lanolin is 2.5:1, and the ratio of the antioxidant and the defoaming agent is 2:1. Embodiment

[0029] It is an oil-soluble diamond micro-powder paste for ultra-low subsurface damage sapphire final polishing, characterized in that The surface modified nano ceria-diamond core-shell hybrid particles are added into the polycarboxylate system oil-based diamond paste at a mass ratio of 0.05%, and mixed sufficiently.

[0030] In processing, the nano ceria-diamond core-shell hybrid particles are added into the oil-based polycarboxylate system at a super low proportion of 0.05%; in polishing, mechanical and chemical instantaneous synergistic polishing is realized, at a polishing tin disc speed of 200-300 rpm, the ceria shell layer has an instantaneous soft chemical reaction with the sapphire surface, the amorphous layer induced by mechanical scratches is immediately removed, and the SSD is less than or equal to 8 nm verified by TEM; due to the extremely small amount of nano ceria-diamond core-shell hybrid particles, the paste fluidity, disc cleanliness and original removal rate are not affected, and even slightly improved.

[0031] In this embodiment, the oil-based diamond paste of the polycarboxylate system includes 12% of single crystal diamond micro powder of W1.5, 8.3% of polycarboxylate dispersant, 40% of synthetic ester base oil, 28% of PAO6 or PAO8, 5% of PMA thickening agent, 6% of a mixture of oil-soluble polyether and lanolin, 0.7% of a mixture of antioxidants and defoaming agents.

[0032] In this embodiment, the nano ceria-diamond core-shell hybrid particles have a ceria of 8 nm, a diamond of 1 μm, and a ceria coating rate of 30%.

[0033] In this embodiment, the ratio of the oil-soluble polyether and lanolin is 2.5:1, and the ratio of the antioxidants and the defoaming agents is 2:1. Embodiment

[0034] It is an oil-soluble diamond micro powder paste for ultra-low sub-surface damage sapphire final polishing, including mass ratios of: A mixture of nano ceria-diamond core-shell hybrid particles and oil-based diamond paste of the polycarboxylate system, wherein the nano ceria-diamond core-shell hybrid particles account for 0.425% In processing, the nano ceria-diamond core-shell hybrid particles are added into the oil-based polycarboxylate system at a super low proportion of 0.425%; in polishing, mechanical and chemical instantaneous synergistic polishing is realized, at a polishing tin disc speed of 200-300 rpm, the ceria shell layer has an instantaneous soft chemical reaction with the sapphire surface, the amorphous layer induced by mechanical scratches is immediately removed, and the SSD is less than or equal to 8 nm verified by TEM; due to the extremely small amount of nano ceria-diamond core-shell hybrid particles, the paste fluidity, disc cleanliness and original removal rate are not affected, and even slightly improved.

[0035] In this embodiment, the nano ceria-diamond core-shell hybrid particles have a ceria of 8 nm, a diamond of 1 μm, and a ceria coating rate of 30%.

[0036] In the present embodiment, the polycarboxylate system oily diamond paste comprises 12% of single crystal diamond powder of W1.5, 8.3% of polycarboxylate dispersant, 40% of synthetic ester base oil, 28% of PAO6 or PAO8, 5% of PMA thickening agent, 6% of mixture of oil-soluble polyether and lanolin, 0.7% of antioxidant and defoaming agent mixture.

[0037] In the present embodiment, the ratio of the oil-soluble polyether and lanolin is 3:1, and the ratio of the antioxidant and defoaming agent is 3:1. Embodiment

[0038] It is a preparation method of an oil-soluble diamond paste for ultra-low subsurface damage sapphire final polishing, characterized in that 0.425% of surface modified nano cerium oxide-diamond core-shell hybrid particles are added to a polycarboxylate system oily diamond paste and fully mixed.

[0039] During processing, the nano cerium oxide-diamond core-shell hybrid particles are added to the oil polycarboxylate system at an ultra-low proportion of 0.425%; during polishing, instantaneous synergistic polishing of mechanical and chemical is achieved; at a polishing tin disc speed of 200-300 rpm, a soft chemical reaction occurs between the cerium oxide shell layer and the sapphire surface, and the amorphous layer induced by mechanical scratches is immediately removed, with SSD≤8 nm verified by TEM; due to the extremely small amount of added nano cerium oxide-diamond core-shell hybrid particles, the paste fluidity, disc cleanliness and original removal rate are not affected, and even slightly improved.

[0040] In the present embodiment, the polycarboxylate system oily diamond paste comprises 10% of single crystal diamond powder of W1.5, 7.5% of polycarboxylate dispersant, 45% of synthetic ester base oil, 24% of PAO6 or PAO8, 6.75% of PMA thickening agent, 6.2% of mixture of oil-soluble polyether and lanolin, 0.55% of antioxidant and defoaming agent mixture.

[0041] In the present embodiment, the nano cerium oxide-diamond core-shell hybrid particles have a cerium oxide of 6.75 nm and a diamond of 1.5 μm, and a cerium oxide coating rate of 40%.

[0042] In the present embodiment, the ratio of the oil-soluble polyether and lanolin is 3:1, and the ratio of the antioxidant and defoaming agent is 3:1.

[0043] The embodiments of the present application are described in detail above, but the present application is not limited to the described embodiments. For those skilled in the art, various changes, modifications, replacements and deformations of the embodiments without departing from the principles and purposes of the present application still fall within the protection scope of the present application.

Claims

1. An oil-soluble diamond micron powder paste for final polishing of sapphire with ultra-low subsurface damage, characterized in that... include: A mixture of nano-cerium oxide-diamond core-shell hybrid particles and polycarboxylate system oily diamond paste, wherein the proportion of nano-cerium oxide-diamond core-shell hybrid particles is 0.05-0.8%, and the cerium oxide in the nano-cerium oxide-diamond core-shell hybrid particles is 8-15 nm.

2. The oil-soluble diamond micron powder paste for final polishing of sapphire with ultra-low subsurface damage according to claim 1, characterized in that... The diamond in the nano-cerium oxide-diamond core-shell hybrid particles is 1-3 μm, and the cerium oxide coating rate is 30-50%.

3. The oil-soluble diamond micron powder paste for ultra-low subsurface damage sapphire final polishing according to claim 1, characterized in that... The polycarboxylate system oily diamond paste comprises 8-12% W1.5 single-crystal diamond micron powder, 6-9% polycarboxylate dispersant, 40-50% synthetic ester-based oil, 20-28% PAO6 or PAO8, 5-8% PMA thickener, 5-8% a mixture of oil-soluble polyether and lanolin, and 0.3-0.7% a mixture of antioxidant and defoamer.

4. The oil-soluble diamond micron powder paste for final polishing of ultra-low subsurface damage sapphire according to claim 3, characterized in that... The ratio of oil-soluble polyether to lanolin is 2:1 to 3:1, and the ratio of antioxidant to defoamer is 1:1 to 3:

1.

5. The preparation method of the oil-soluble diamond micron powder paste for ultra-low subsurface damage sapphire final polishing according to claim 1, characterized in that... Includes the following steps: Surface-modified nano-cerium oxide-diamond core-shell hybrid particles with a mass ratio of 0.05–0.8% were added to the polycarboxylate-based oily diamond paste and thoroughly mixed.

6. The preparation method of the oil-soluble diamond micron powder paste for ultra-low subsurface damage sapphire final polishing according to claim 5, characterized in that... The polycarboxylate-based oily diamond paste comprises 8-12% W1.5 single-crystal diamond micron powder, 6-9% polycarboxylate dispersant, 40-50% synthetic ester-based oil, 20-28% PAO6 or PAO8, 5-8% PMA thickener, 5-8% a mixture of oil-soluble polyether and lanolin, and 0.3-0.7% a mixture of antioxidant and defoamer. The proportion of nano-cerium oxide-diamond core-shell hybrid particles is 0.05-0.8%, and the cerium oxide in the nano-cerium oxide-diamond core-shell hybrid particles is 8-15 nm.

7. The preparation method of the oil-soluble diamond micron powder paste for ultra-low subsurface damage sapphire final polishing according to claim 5, characterized in that... The diamond in the nano-cerium oxide-diamond core-shell hybrid particles is 1-3 μm, and the cerium oxide coating rate is 30-50%.

8. The preparation method of the oil-soluble diamond micron powder paste for ultra-low subsurface damage sapphire final polishing according to claim 6, characterized in that... The ratio of oil-soluble polyether to lanolin is 2:1 to 3:1, and the ratio of antioxidant to defoamer is 1:1 to 3:1.