CN112680110A - Novel environment-friendly microemulsion type diamond polishing solution - Google Patents
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Abstract
A novel environment-friendly microemulsion type diamond polishing solution belongs to the technical field of fine chemical engineering. The micro-emulsion regulator in the polishing solution simultaneously introduces groups with hydrophilic and oleophilic groups, so that a stable system is easier to form, the polishing rate of the micro-emulsion type diamond polishing solution is equivalent to that of an oil-based diamond polishing solution, and the polishing solution has the characteristics of environmental protection and easiness in discharge, and the harm to the environment is not required to be worried. Meanwhile, by compounding the surfactant and the cosurfactant, the micro-emulsion regulator with the short carbon chain and the small structure can be rapidly inserted between the surfactant molecules, the hydrophilicity of the surfactant is improved by the short carbon chain and the hydroxyl structure, a stable oil-water system is more easily formed, and the uniform and transparent property and no layering are maintained for a long time. The polishing solution has the advantages of simple preparation method, simple required equipment and mild operation conditions, and can realize high-efficiency industrial production.
Description
Technical Field
The invention relates to a novel environment-friendly microemulsion type diamond polishing solution, belonging to the technical field of fine chemical engineering.
Background
With the development of the LED industry, chip substrates are gradually developed to large size and high quality. Among them, sapphire wafer is the preferred substrate sheet in the current LED industry, sapphire is a general term for alumina single crystal material, has excellent chemical stability, optical transparency and ideal mechanical properties, and is often used as a material for optoelectronic components, such as optical transmission windows, light emitting diodes, substrates for microelectronic integrated circuit applications, and substrates for gallium nitride growth.
The chemical mechanical polishing technology is one of the key technologies for semiconductor surface processing at present, and is also widely applied in the polishing stage of the sapphire crystal wafer. In the chemical mechanical polishing process, the diamond polishing solution polishes the surface of the crystal by using the mechanical force of a polishing machine, and the polishing solution is used for achieving the removal amount required by processing a workpiece according to the requirements of downstream products.
Currently, the commonly used diamond polishing solutions typically need to include both aqueous and oil. The aqueous polishing solution has the advantages of environmental protection and easy discharge, but the aqueous polishing solution has the defects of low grinding rate and easy scratch in the actual production, and diamond abrasive particles are easy to gather in the grinding process, so that the service life of the abrasive is short, and the roughness value of the surface of a workpiece is large. Compared with aqueous polishing solutions, the oily polishing solution has good lubricating property, high polishing speed, stable speed and cooling effect, but the oily polishing solution is not easy to clean and discharge and can cause damage to the environment.
Therefore, it is necessary to develop a diamond polishing solution having the advantages of environmental protection, easy discharge, good lubricating property of oily polishing solution and high grinding speed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a novel environment-friendly microemulsion type diamond polishing solution, and aims to maintain the high polishing rate of an oily diamond polishing solution and simultaneously have the advantages of easy cleaning and environment friendliness of a water-based polishing solution. The composition of the detergent contains solvent oil capable of dissolving oily dirt and water capable of dissolving water-soluble dirt; secondly, the wetting, emulsifying and solubilizing actions of a large amount of added surfactants also have an auxiliary effect on decontamination, and simultaneously, the pollution of a large amount of oily solvents to the environment can be overcome.
The preparation method of the microemulsion-type diamond polishing solution provided by the invention has the advantages that the front step and the back step are closely connected, the method is simple and rapid, the operation is easy, the operation condition is mild, the industrial production can be realized, and the economic benefit is very good.
The technical scheme of the application is as follows: the novel environment-friendly microemulsion-type diamond polishing solution comprises 1-20% of a microemulsion regulator with the following structure:
other components and contents thereof are as follows:
diamond powder: 0.5 to 5 percent;
surfactant (b): 1% -10%;
cosurfactant: 1% -10%;
dispersing agent: 0.1-5%;
wetting agent: 0.1 to 5 percent
Suspending agent: 0.1-5%;
sodium chloride brine (mass concentration is 2%): 1% -20%;
the balance being white oil.
Specifically, the diamond micropowder comprises one or more of single crystal diamond micropowder, polycrystalline diamond-like micropowder and polycrystalline diamond micropowder, and is preferably polycrystalline diamond micropowder, and the D50 range is 1-10 μm.
The surfactant can be one or more of sorbitan trioleate, polyoxyethylene sorbitol beeswax derivatives, sorbitan tristearate, polyoxyethylene sorbitol hexastearate, ethylene glycol fatty acid ester, glyceryl monostearate, sorbitan monostearate and propylene glycol monolaurate, and is preferably sorbitan monostearate.
The cosurfactant is polyoxyethylene lauryl ether, polyoxyethylene sorbitan trioleate, polyoxyethylene monooleate, polyoxyethylene sorbitan monolaurate and polyoxyethylene sorbitan monooleate, and preferably polyoxyethylene sorbitan monooleate.
The dispersing agent is generally polyoxyethylene ether substances, and can be any one or more of octyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, benzyl phenol polyoxyethylene ether, fatty amine polyoxyethylene ether, phenethyl phenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether, and preferably is fatty alcohol polyoxyethylene ether.
The wetting agent may be polyoxyethylene stearate, polyoxyethylene abietate, fatty acid esters, glycerol and diglycerol, preferably polyoxyethylene stearate.
The suspending agent can be one or more of castor oil derivatives, modified hydrogenated castor oil, organic bentonite and polyvinyl alcohol, and is preferably polyoxyethylene alcohol.
The white oil may be one or more of a naphthenic hydrocarbon or an aromatic hydrocarbon solvent, preferably a naphthenic hydrocarbon.
The preparation method of the diamond polishing solution comprises the following steps:
(1) weighing a certain amount of white oil at room temperature, adding sorbitan monostearate, stirring for 5min, adding polyoxyethylene sorbitan monooleate, and stirring for 30 min;
(2) heating the solution obtained in the step (1) to 40 ℃, adding butyl cellosolve under the continuous stirring of 300rpm, and stirring for 30 min;
(3) slowly dropwise adding sodium chloride brine (the mass concentration is 2%) into the solution obtained in the step (2) under the condition of continuous stirring, controlling the speed at 10ml/min until the solution is transparent, and stopping dropwise adding;
(4) weighing fatty alcohol-polyoxyethylene ether and stearic acid-polyoxyethylene ether, sequentially adding the fatty alcohol-polyoxyethylene ether and the stearic acid-polyoxyethylene ether into the solution obtained in the step (3), and stirring for 10min to form a uniform solution;
(5) and (3) weighing organic bentonite, adding the organic bentonite into the solution obtained in the step (4), stirring for 60min to form a stable solution, finally adding diamond micropowder with the D50 being 5 mu m, and stirring for 60min to obtain the novel environment-friendly micro-emulsion type diamond polishing solution.
According to another technical scheme of the application, the application of the material is provided, and the material can be used for polishing substrates such as sapphire and silicon carbide.
The beneficial effects that this application can produce include: the group with hydrophilic and oleophilic groups is simultaneously introduced into the microemulsion regulator with a specific structure, so that a stable system is easier to form, the polishing rate of the microemulsion diamond polishing solution is equivalent to that of an oil diamond polishing solution, and the microemulsion diamond polishing solution has the characteristics of environmental protection and easiness in discharge, and does not need to worry about the harm to the environment. Meanwhile, by compounding the surfactant and the cosurfactant, the micro-emulsion regulator with the short carbon chain and the small structure can be rapidly inserted between the surfactant molecules, the hydrophilicity of the surfactant is improved by the short carbon chain and the hydroxyl structure, a stable oil-water system is more easily formed, and the uniform and transparent property and no layering are maintained for a long time. The polishing solution has the advantages of simple preparation method, simple required equipment, mild operation condition and capability of realizing efficient industrial production.
Drawings
FIG. 1: comparative example 2 is a schematic diagram of the cleaning effect.
FIG. 2: the cleaning effect of embodiment 1 of the invention is schematically shown.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Example 1:
according to one embodiment of the present application, a novel environment-friendly micro-emulsion type diamond polishing solution comprises, by weight:
diamond powder: 0.5 percent;
surfactant (b): 1% of sorbitan monostearate;
cosurfactant: 1% of polyoxyethylene sorbitan monooleate;
a microemulsion regulator: 1 percent;
dispersing agent: 1% of fatty alcohol-polyoxyethylene ether;
wetting agent: stearic acid polyoxyethylene ester 0.1%
Suspending agent: 1% of organic bentonite;
sodium chloride brine (mass concentration is 2%): 1 percent;
the balance being white oil.
The preparation method of the microemulsion-type diamond polishing solution comprises the following steps:
(1) weighing 93.4% by mass of white oil at room temperature, adding 1% by mass of sorbitan monostearate, stirring for 5min, adding 1% by mass of polyoxyethylene sorbitan monooleate, and stirring for 30 min;
(2) heating the solution obtained in the step (1) to 40 ℃, adding 1% of microemulsion regulator by mass under the continuous stirring of 300rpm, and stirring for 30 min;
(3) slowly dropwise adding 1% by mass of sodium chloride saline (the mass concentration is 2%) into the solution obtained in the step (2) under the condition of continuous stirring, controlling the speed at 10ml/min until the solution is transparent, and stopping dropwise adding;
(4) weighing 1 mass percent of fatty alcohol-polyoxyethylene ether and 0.1 mass percent of stearic acid-polyoxyethylene ether, sequentially adding the fatty alcohol-polyoxyethylene ether and the stearic acid-polyoxyethylene ether into the solution obtained in the step (3), and stirring for 10min to form a uniform solution;
(5) and (3) weighing 1% of organic bentonite in parts by mass, adding the organic bentonite into the solution obtained in the step (4), stirring for 60min to form a stable solution, finally adding diamond micropowder with the D50 being 5 microns, and stirring for 60min to obtain the novel environment-friendly micro-emulsion type diamond polishing solution.
By adopting the preparation method, the polishing solution is prepared according to the components and the contents of the novel environment-friendly microemulsion type sapphire polishing solution in the following table examples 2-16.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
The above-mentioned examples were prepared according to the specific preparation procedure of the above-mentioned polishing solutions.
Polishing experiment with polishing solution:
polishing the instrument: a precision single-side grinder (EL-380).
Conditions are as follows: pressure (Down force): 10 Kpa.
The polishing pad rotation speed (pad speed) was 60 rpm.
Polishing head speed (Carrier speed) 60 rpm.
Temperature: 25-30 ℃.
The flow Rate of the polishing solution (Feed Rate) was 100 ml/min.
Polishing time: and (3) 30 min.
Polishing solution: the polishing solutions obtained in the above examples were tested.
Example 17 evaluation of Material removal Rate
There are generally two methods of detecting material removal rate: direct and indirect processes. The inventor adopts a method of measuring the quality of the substrate before and after polishing and indirectly calculating the thickness of the removed sapphire layer according to the density and the area of the substrate. The method has the greatest characteristic of simple and convenient measurement, and the removal rate can be rapidly obtained. The evaluation of the material removal rate in the examples of the present application is as follows:
and polishing the sapphire substrate by adopting a precise single-side grinding and polishing machine, wherein the rotating speed is 60rpm, the flow of polishing solution is 600mL/min, the pressure is 10kg, the temperature is 25 ℃, and the time is 15 min.
MRR＝△m/(ρSt)
Wherein: and Δ m is the mass change before and after sapphire polishing, ρ is the sapphire density, S is the circular area of the sapphire wafer, and t is the polishing time.
Example 18 suspension stability evaluation
And (3) putting a certain amount of polishing solution in a test tube, standing for a certain time, observing the change of the liquid level height, recording the good suspension property when the change of the liquid level height is less than 1cm, and recording the poor suspension property when the change of the liquid level height is more than 1 cm.
Example 19 evaluation of cleaning ability
When the disc surface is cleaned after polishing, the cleaning is easier and the cleaning ability is stronger, whereas the mark is worse.
To illustrate the effectiveness of this patent, a commercially available MetaDi Supreme polycrystalline diamond oil and aqueous polishing slurry from BUEHLER was used for comparison.
Description of comparative examples
Comparative example 1 is a commercially available aqueous polishing solution of MetaDi Superme polycrystalline diamond from BUEHLER, the polycrystalline diamond powder D50 being selected to be 5 μm;
the formulation of the commercially available MetaDi Supreme polycrystalline diamond aqueous polishing solution of BUEHLER is as follows:
water: 30 to 70 percent
Propylene glycol: 20 to 60 percent
Diamond powder: 0 to 1 percent.
Comparative example 2 is a commercially available MetaDi Superme polycrystalline diamond oil polishing solution from BUEHLER, with a polycrystalline diamond powder D50 selected to be 5 μm.
The formulation of a commercially available MetaDi Supreme polycrystalline diamond oil polishing solution of BUEHLER is as follows: petroleum fractions, hydrogenated light oil: 65 to 95 percent
Organic bentonite: 2 to 6 percent
Diamond powder: 0 to 1 percent.
The following table shows the removal rate of the sapphire substrate after polishing and the suspension stability and chip removal capability of the polishing solution of each example:
from the comparison of the material removal rates described above, it was demonstrated that the removal rates of the examples of the invention were all superior to the comparative example commercially available BUEHLER MetaDi Supreme polycrystalline diamond aqueous polishing solution, and that the cleaning capabilities of the examples of the invention (see fig. 2) were significantly superior to the commercially available BUEHLER MetaDi Supreme polycrystalline diamond oily polishing solution (see fig. 1).
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (9)
1. A novel environment-friendly microemulsion type diamond polishing solution is characterized in that: the polishing solution comprises the following components in parts by weight:
diamond micro powder: 0.5 to 5 percent;
surfactant (b): 1% -10%;
cosurfactant: 1% -10%;
dispersing agent: 0.1-5%;
wetting agent: 0.1 to 5 percent
Suspending agent: 0.1-5%;
sodium chloride brine: 1% -20%;
a microemulsion regulator: 1% -20%;
the balance of white oil;
the diamond micro powder is one or more of single crystal diamond micro powder, polycrystal-like diamond micro powder and polycrystal diamond micro powder;
the surfactant is one or more of sorbitan trioleate, polyoxyethylene sorbitol beeswax derivatives, sorbitan tristearate, polyoxyethylene sorbitol hexastearate, ethylene glycol fatty acid ester, glyceryl monostearate, sorbitan monostearate and propylene glycol monolaurate;
the cosurfactant is polyoxyethylene stearate, polyoxyethylene oleate, polyoxyethylene lauryl ether, polyoxyethylene sorbitan trioleate, polyoxyethylene monooleate, polyoxyethylene sorbitan monolaurate and polyoxyethylene sorbitan monooleate;
the dispersing agent is a polyoxyethylene ether substance, and the polyoxyethylene ether substance is one or more of octyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, benzyl phenol polyoxyethylene ether, fatty amine polyoxyethylene ether, phenethyl phenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether;
the wetting agent is polyoxyethylene stearate, polyoxyethylene abietate, fatty acid ester, glycerol or diglycerol;
the suspending agent is one or more of castor oil derivatives, modified hydrogenated castor oil, organic bentonite and polyvinyl alcohol;
the mass concentration of the sodium chloride brine is 2%;
the structure of the microemulsion regulator is as follows:
the white oil adopts naphthenic hydrocarbon or aromatic hydrocarbon solvent.
2. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the diamond micro powder is polycrystalline diamond micro powder, and the D50 range is 1-10 mu m.
3. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the surfactant is sorbitan monostearate or sorbitan tristearate.
4. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the cosurfactant is polyoxyethylene sorbitan monooleate or polyoxyethylene monooleate.
5. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the polyoxyethylene ether substance is fatty alcohol-polyoxyethylene ether, phenethyl phenol-polyoxyethylene ether or fatty alcohol-polyoxyethylene ether.
6. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the wetting agent is polyoxyethylene stearate or polyoxyethylene abietate.
7. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the suspending agent is polyoxyethylene alcohol or organic bentonite.
8. The novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, is characterized in that: the cycloalkane is a C5-C12 cycloalkane.
9. The use of the novel environment-friendly microemulsion-type diamond polishing solution according to claim 1, wherein the novel environment-friendly microemulsion-type diamond polishing solution comprises the following components in percentage by weight: the polishing solution is applied to polishing of sapphire or silicon carbide substrates.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113462294A (en) * | 2021-06-29 | 2021-10-01 | 南京青锐风新材料科技有限公司 | Oily polycrystalline diamond grinding and polishing solution and production and preparation process thereof |
| CN114949939A (en) * | 2022-04-29 | 2022-08-30 | 广州安达净水材料有限公司 | Defoaming agent for landfill leachate evaporation and preparation method thereof |
| CN115044299A (en) * | 2022-07-04 | 2022-09-13 | 浙江奥首材料科技有限公司 | Water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent, preparation method and application thereof, and grinding fluid containing water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent |
| CN115521714A (en) * | 2022-10-24 | 2022-12-27 | 浙江奥首材料科技有限公司 | Oily diamond polishing solution, preparation method and application thereof |
| CN115746789A (en) * | 2022-12-12 | 2023-03-07 | 郑州磨料磨具磨削研究所有限公司 | Stable full-suspension diamond grinding fluid for grinding and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462294A (en) * | 2021-06-29 | 2021-10-01 | 南京青锐风新材料科技有限公司 | Oily polycrystalline diamond grinding and polishing solution and production and preparation process thereof |
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| CN114949939A (en) * | 2022-04-29 | 2022-08-30 | 广州安达净水材料有限公司 | Defoaming agent for landfill leachate evaporation and preparation method thereof |
| CN114949939B (en) * | 2022-04-29 | 2023-10-03 | 广州安达净水材料有限公司 | Defoaming agent for landfill leachate evaporation and preparation method thereof |
| CN115044299A (en) * | 2022-07-04 | 2022-09-13 | 浙江奥首材料科技有限公司 | Water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent, preparation method and application thereof, and grinding fluid containing water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent |
| CN115044299B (en) * | 2022-07-04 | 2023-11-17 | 浙江奥首材料科技有限公司 | Water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent, preparation method and application thereof, and grinding fluid containing water-soluble high-specific-gravity large-size abrasive suspension auxiliary agent |
| CN115521714A (en) * | 2022-10-24 | 2022-12-27 | 浙江奥首材料科技有限公司 | Oily diamond polishing solution, preparation method and application thereof |
| CN115521714B (en) * | 2022-10-24 | 2023-10-24 | 浙江奥首材料科技有限公司 | Oily diamond polishing solution, and preparation method and application thereof |
| CN115746789A (en) * | 2022-12-12 | 2023-03-07 | 郑州磨料磨具磨削研究所有限公司 | Stable full-suspension diamond grinding fluid for grinding and preparation method thereof |
| CN115746789B (en) * | 2022-12-12 | 2024-03-22 | 郑州磨料磨具磨削研究所有限公司 | Diamond grinding fluid for stable full-suspension grinding and preparation method thereof |
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