CN114774003A - NiP modified layer chemical mechanical polishing solution and preparation method and application thereof - Google Patents

NiP modified layer chemical mechanical polishing solution and preparation method and application thereof Download PDF

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CN114774003A
CN114774003A CN202210588044.5A CN202210588044A CN114774003A CN 114774003 A CN114774003 A CN 114774003A CN 202210588044 A CN202210588044 A CN 202210588044A CN 114774003 A CN114774003 A CN 114774003A
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modified layer
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mechanical polishing
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CN114774003B (en
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赖涛
徐超
彭小强
胡皓
刘俊峰
李煌
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National University of Defense Technology
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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
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • G—PHYSICS
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Abstract

The invention discloses a chemical mechanical polishing solution for a NiP modified layer, and a preparation method and application thereof, wherein the polishing solution comprises the following components in percentage by mass: 15-30% of polishing abrasive, 1-10% of oxidant, 1-5% of complexing agent, 1-5% of surfactant and the balance of water, wherein the polishing abrasive is silicon dioxide, and the pH value of the polishing solution is 6.5-7.5. The preparation method comprises the steps of mixing the polishing abrasive, the complexing agent, the surfactant and water, adding the oxidant and adjusting the pH value to a set value. The chemical mechanical polishing solution for the NiP modified layer can realize the balance of chemical corrosion and mechanical removal, can be used for chemically and mechanically polishing the NiP modified layer, can realize high-precision processing of the NiP modified layer, can obtain a high-quality processed surface, and enables the NiP modified layer to meet various requirements.

Description

NiP modified layer chemical mechanical polishing solution and preparation method and application thereof
Technical Field
The invention belongs to the technical field of optical element processing, and relates to a chemical mechanical polishing solution for a NiP modified layer, and a preparation method and application thereof.
Background
At present, the typical range of the micro roughness of the surface of the mirror material manufactured by the conventional processing technology, such as metal material, is from RMS 2nm to RMS 10nm, and at this time, the mirror material can only meet the use requirement of infrared spectrum generally, but is difficult to meet the use requirement of visible light and shorter wavelength range. In addition, the micro roughness of the surface of the reflector material is better than RMS 1nm to meet the use requirement in the visible spectrum range; in particular, in the field of hard X-ray mirror applications, higher demands are made on the microroughness of the mirror material surface, which demands microroughness better than RMS 0.3 nm. Therefore, how to effectively reduce the surface roughness of the reflector material is of great significance for improving the wide application of the reflector material in the optical field.
The modification of the surface of the substrate is a common method for improving the optical performance of the mirror surface of the reflector, for example, the NiP modified layer is deposited on the mirror surface of the reflector, which can improve the surface defects of the substrate, and simultaneously, the high-quality metal optical element is obtained by processing the NiP modified layer. However, in the existing processing method of the NiP modified layer, the first process is single-point diamond turning, and although the surface meeting the infrared imaging quality requirement can be directly obtained by the single-point diamond turning technology, the single-point diamond turning precision is limited by a machine tool, and the processing can generate periodic turning lines, so that diffraction and stray light are caused, the light flux loss is increased, the reflectivity and the imaging quality of the mirror surface are reduced, and the optical performance of the mirror surface is affected. Therefore, after single-point diamond turning, the NiP modified layer needs to be further processed to meet higher use requirements.
The chemical mechanical polishing is a surface finishing process, and the existing chemical mechanical polishing process for processing the NiP modified layer mostly has the following defects: (1) the curved surface element can not be processed; (2) the control of surface scratch damage still cannot meet the use requirement of high precision; (3) most of the used polishing solutions contain toxic and harmful chemical agents, such as Benzotriazole (BTA), Ethylene Diamine Tetraacetic Acid (EDTA) and other toxic substances, and the addition of the toxic agents can not only influence the health of processing operators, but also cause harm to the environment. In addition, during the practical research process of the inventor of the present application, it is also found that: the polishing solution for polishing the surface of the metal substrate is not suitable for polishing the NiP modified layer, and the possible reasons are that the abrasive material and the pH value of the existing chemical mechanical polishing solution can cause immeasurable damage to the NiP modified layer, for example, when aluminum oxide is used as the abrasive material, a large number of scratches can be caused on the surface of the NiP modified layer, and meanwhile, under the condition of lower pH value, the chemical reaction is severe, and pitting caused by acid etching can be easily generated on the surface of the NiP modified layer.
Therefore, the chemical mechanical polishing solution suitable for processing the NiP modified layer is obtained, and has very important significance for realizing high-precision processing of the NiP modified layer.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a chemical mechanical polishing solution for a NiP modified layer, a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the chemical mechanical polishing solution for the NiP modified layer comprises the following components in percentage by mass:
Figure BDA0003666622860000021
the polishing abrasive is silicon dioxide; the pH value of the chemical mechanical polishing solution for the NiP modified layer is 6.5-7.5.
The chemical mechanical polishing solution for the NiP modified layer is further improved and comprises the following components in percentage by mass:
Figure BDA0003666622860000022
the polishing abrasive is silicon dioxide; the pH value of the NiP modified layer chemical mechanical polishing solution is 6.8-7.2.
In the chemical mechanical polishing solution for the NiP modified layer, the average grain diameter of the silicon dioxide is 35nm or 50 nm.
In the chemical mechanical polishing solution for the NiP modified layer, the oxidizing agent is hydrogen peroxide.
In the chemical mechanical polishing solution for the NiP modified layer, the complexing agent is at least one of oxalic acid, citric acid, glycine, alanine and triethanolamine; the surfactant is at least one of sodium stearate, potassium stearate and sodium dodecyl benzene sulfonate.
As a general technical concept, the present invention also provides a preparation method of the above-mentioned NiP modified layer chemical mechanical polishing solution, comprising the following steps:
s1, mixing the polishing abrasive, the complexing agent, the surfactant and water, and stirring to obtain a mixed solution A;
s2, adding an oxidant into the mixed solution A to obtain a mixed solution B;
and S3, adding a pH regulator into the mixed solution B, and regulating the pH value to a set value to obtain the NiP modified layer chemical mechanical polishing solution.
In a further improvement of the above preparation method, in step S3, the pH adjusting agent is at least one of phosphoric acid, citric acid, potassium hydroxide, and sodium hydroxide.
In the preparation method, the further improvement is that in step S1, the stirring speed is 300r/min to 600 r/min; the stirring time is 5 min-10 min.
As a general technical concept, the invention also provides application of the chemical mechanical polishing solution for the NiP modified layer or the chemical mechanical polishing solution for the NiP modified layer prepared by the preparation method in processing the NiP modified layer.
The application is further improved, and the application is to adopt the chemical mechanical polishing solution of the NiP modified layer to carry out chemical mechanical polishing on the processed NiP modified layer; the chemical mechanical polishing process parameters are as follows: manufacturing a polishing disk by using asphalt, wherein the rotating speed of the polishing disk is controlled to be 60-120 rpm, the polishing pressure is controlled to be 0.02-0.05 MPa, and the feeding speed is 80-150 mm/min; the equipment adopted in the chemical mechanical polishing is a small grinding head polishing machine tool.
Compared with the prior art, the invention has the advantages that:
(1) aiming at the defects that the existing chemical mechanical polishing solution contains a large amount of toxic and harmful components and is difficult to meet the use requirement of high precision, the invention creatively provides the chemical mechanical polishing solution for the NiP modified layer, and the balance between the chemical corrosion effect and the mechanical removal effect can be realized by optimizing the components and the content of each component, so that when the polishing solution is used for chemically and mechanically polishing the NiP modified layer, the high-precision processing of the NiP modified layer can be realized, the high-quality processing surface can be obtained, and finally the NiP modified layer can meet various requirements; meanwhile, the chemical mechanical polishing solution for the NiP modified layer has no toxic chemical reagent, is harmless to the health of operators, has a pH value of 6.5-7.5, and cannot damage and corrode equipment.
(2) The invention also provides a preparation method of the chemical mechanical polishing solution for the NiP modified layer, which comprises the steps of mixing polishing abrasive, complexing agent, surfactant and water, adding oxidant under the action of the surfactant to facilitate avoiding agglomeration of the polishing abrasive, and finally adjusting the pH value to a set value by utilizing the pH regulator to obtain the chemical mechanical polishing solution for the NiP modified layer with stable properties. The preparation method has the advantages of simple process, convenient operation and the like, is suitable for large-scale preparation, and is beneficial to industrial application.
(3) The invention also provides application of the chemical mechanical polishing solution for the NiP modified layer in processing the NiP modified layer, in particular to the application of the chemical mechanical polishing solution for the NiP modified layer in chemical mechanical polishing of the NiP modified layer, which can process the NiP modified layer with high quality by balancing the mechanical removal effect and the chemical reaction effect in the polishing process, has high use value and good application prospect and has important significance in promoting the wide application of the NiP modified layer in the optical field.
Drawings
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
FIG. 1 is a schematic diagram of the chemical reaction of the NiP modified layer during polishing in the present invention.
FIG. 2 is a schematic diagram of the mechanical removal of the NiP modified layer of the present invention.
Fig. 3 is a schematic view of the cmp slurry for the NiP-modified layer in example 1 of the present invention polishing the NiP-modified layer.
FIG. 4 is a graph showing the surface quality test results of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 1 of the present invention.
FIG. 5 is a graph showing the surface quality test results of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 2 of the present invention.
FIG. 6 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 3 of the present invention.
FIG. 7 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 4 of the present invention.
FIG. 8 is a three-dimensional topography of the surface of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 4 of the present invention.
FIG. 9 is a graph showing the results of the surface quality test of the NiP modified layer using the NiP modified layer CMP slurry in example 5 of the present invention.
FIG. 10 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with a pH 4 NiP modified layer CMP slurry in example 6 of the present invention.
FIG. 11 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with pH 7 CMP slurry in example 6 of the present invention.
FIG. 12 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with a pH 10 NiP modified layer CMP slurry in example 6 of the present invention.
FIG. 13 is a graph showing the results of surface quality tests on NiP modified layers of concave spherical surfaces after polishing with a chemical mechanical polishing solution for NiP modified layers with silicon dioxide as the polishing abrasive in example 7 of the present invention.
FIG. 14 is a graph showing the results of surface quality tests on NiP modified layers of concave spherical surfaces after polishing with a chemical mechanical polishing solution for NiP modified layers with alumina as the polishing abrasive in example 7 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
As shown in fig. 1, the chemical reaction of the NiP modification layer in the polishing solution is:
Ni+H2O2→NiO+H2O
NiO+H2O2→Ni2O3+H2O
P+H2O2→P2O3+H2O
as can be seen from the above reaction formula, NiO and Ni are generated on the surface of the NiP modified layer under the action of the oxidizing agent (hydrogen peroxide)2O3And P2O3The oxide film of (3). NiO and Ni in the polishing solution2O3And P2O3The following reaction with water will continue to take place:
P2O3+H2O→H3PO3
Figure BDA0003666622860000051
Figure BDA0003666622860000052
in the above reaction, Ni is formed2+、Ni3+Can generate complex reaction with added complex in the solution, can accelerate the oxidation reaction and realize the dissolution of the polishing product. In addition, the bonding force between the generated oxide film and the NiP modified layer is smaller than that between molecular layers in the NiP modified layer, so that the oxide film is easier to remove. Meanwhile, the micro-morphology of the surface of the NiP modified layer is in a rugged state, the material removal rate at a high point is high during polishing, and the material removal rate at a low point is low, so that an oxide film at the low point can play a role in protection, and the surface is prevented from being excessively scratched. Therefore, the use of the oxidizing agent and the complexing agent can improve the polishing efficiency of the NiP modified layer and is beneficial to obtaining the ultra-smooth surface of the workpiece.
As shown in fig. 2, the Preston equation is a classical equation of a mathematical model for the removal of chemical mechanical polishing material, and it is considered that the material removal rate is mainly linearly proportional to the pressure applied by the polishing and the relative velocity of the polishing interface. However, more factors, particularly consumables such as polishing pads and polishing solutions composed of nano-sized abrasives, also have a great influence on material removal. In view of this, the material removal model mentioned by Luo and Dornfeld was chosen to explain the mechanical removal effect in ultra-smooth polishing of NiP coatings.
Figure BDA0003666622860000053
Wherein MRR is the material removal rate; phi is a standard normal distribution function; p0Is a down force; v is relative speed; c2、C3To be a undetermined coefficient, C3The values depend on the following formula.
Figure BDA0003666622860000054
Figure BDA0003666622860000055
In the formula, C1Is a undetermined coefficient; rhoωIs the density of the sample; a. the0Is the nominal contact area; k is 1+3 sigma/xavg(σ is the standard deviation of a normal distribution); dsThe dilution ratio of the polishing solution (volume ratio of the polishing solution to water); ρ is a unit of a gradientsIs the density of the polishing solution; m iss-aIs the concentration of the abrasive in the polishing solution; dsumThe density of protrusions per unit area of the polishing pad in contact with the surface of the sample; a is the average area of the individual asperities before deformation of the polishing pad; l is the height of the asperities before deformation of the polishing pad; rhoaThe density of the abrasive; x is the number ofavgIs the average particle size of the abrasive; epIs the modulus of elasticity of the polishing pad; hωIs the hardness of the sample; b is a mixture of1The value of (d) depends on the following formula:
Figure BDA0003666622860000061
wherein R is the radius of the top of the convex body of the polishing pad. C2The value of (c) depends on the following formula:
Figure BDA0003666622860000062
in the formula, HpIs the hardness of the polishing pad. The model mainly explores a solid-solid contact wear mechanism from a mechanical angle and more comprehensively describes a mechanical removal effect in machining.
In the chemical mechanical polishing process of the NiP modified layer, it is most important to achieve a balance between the mechanical removal action and the chemical reaction action during polishing to obtain a high-quality processed surface. Therefore, the invention mainly aims to realize the balance between the mechanical removal effect and the chemical reaction effect in the polishing process so as to optimize the formula of the polishing solution and the processing technological parameters.
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The chemical mechanical polishing solution for the NiP modified layer comprises the following components in percentage by mass:
Figure BDA0003666622860000063
in this example, the polishing abrasive is silica and has an average particle diameter of 50 nm.
In this example, the pH of the cmp slurry for the NiP modification layer was 6.5.
In this example, the oxidizing agent is hydrogen peroxide; in the invention, the hydrogen peroxide is used as an oxidant, has stable property in the use process, does not belong to hazardous chemicals, has extremely low danger and is more suitable for green manufacture.
In this embodiment, the complexing agent is oxalic acid, and may be any one of citric acid, glycine, and alanine;
in this example, the surfactant is sodium stearate, and potassium stearate may also be used.
A method for preparing the above chemical mechanical polishing solution for the NiP modification layer in this embodiment includes the following steps:
s1, mixing the polishing abrasive, the complexing agent, the surfactant and the deionized water, and stirring at the rotating speed of 300-600 r/min for 5-10 min to obtain a mixed solution A.
And S2, adding an oxidant into the mixed solution A, and uniformly mixing to obtain a mixed solution B.
And S3, adding a pH regulator into the mixed solution B, regulating the pH value to 6.5, and uniformly mixing to obtain the NiP modified layer chemical mechanical polishing solution. In the step, according to the actual situation, the pH regulator is selected from one of phosphoric acid, citric acid, potassium hydroxide and sodium hydroxide, and the pH value is directly regulated to 6.5.
An application of the above-described chemical mechanical polishing solution for the NiP modification layer prepared in this embodiment in processing the NiP modification layer is used for performing chemical mechanical polishing on the NiP modification layer with the surface roughness greater than RMS 2nm, a sample is a mirror with a diameter of 100mm, the NiP modification layer is plated on Al6061, the thickness of the NiP modification layer is 100 μm, the Ni content in the NiP modification layer is 88 wt%, the P content is 12 wt%, the sample is subjected to ultra-precision turning, and the initial micro roughness is RMS 2.326 nm.
The polishing equipment is a numerical control small grinding head machine tool, the polishing time is 18min, the used polishing disc is an asphalt disc with the diameter of 20mm, the polishing schematic diagram is shown in figure 3, and the polishing parameters are shown in table 1.
TABLE 1 polishing parameters in example 1
Pressure (Mpa) Rotational speed/(rpm) Feed speed/(mm/min)
0.05 120 150
The surface morphology of the NiP modified layer after polishing was measured under a 20 × lens using a white light interferometer (Zygo NewView 700), and the results are shown in fig. 4. FIG. 4 is a graph showing the surface quality test results of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 1 of the present invention. As can be seen from FIG. 4, the surface micro-roughness of the NiP modified layer after polishing with the chemical mechanical polishing solution for NiP modified layers of the present invention was RMS 1.374 nm.
Example 2
The chemical mechanical polishing solution for the NiP modified layer comprises the following components in percentage by mass:
Figure BDA0003666622860000071
in this example, the polishing abrasive is silica and has an average particle diameter of 50 nm.
In this example, the pH of the cmp slurry for the NiP modification layer was 6.8.
In this example, the oxidizing agent is hydrogen peroxide.
In this embodiment, the complexing agent is oxalic acid, and may be any one of citric acid, glycine, and alanine;
in this example, the surfactant is sodium stearate, and potassium stearate may also be used.
A method for preparing the above chemical mechanical polishing solution for the NiP modification layer in this embodiment includes the following steps:
s1, mixing the polishing abrasive, the complexing agent, the surfactant and the deionized water, and stirring at the rotating speed of 600r/min for 5min to obtain a mixed solution A.
And S2, adding an oxidant into the mixed solution A, and uniformly mixing to obtain a mixed solution B.
And S3, adding a pH regulator into the mixed solution B, regulating the pH value to 6.8, and uniformly mixing to obtain the NiP modified layer chemical mechanical polishing solution. In the step, according to the actual situation, the pH regulator is selected from one of phosphoric acid, citric acid, potassium hydroxide and sodium hydroxide, and the pH value is directly regulated to 6.8.
The application of the chemical mechanical polishing solution for the NiP modified layer prepared in the embodiment in processing the NiP modified layer is to perform chemical mechanical polishing on the sample processed in embodiment 1 (the surface roughness of the NiP modified layer is between RMS 1nm and RMS 2nm), wherein the used polishing equipment is a numerical control small grinding head machine tool, the polishing is performed once for 22.5min, the used polishing disc is an asphalt disc with the diameter of 20mm, the polishing schematic diagram is shown in fig. 3, and the polishing parameters are shown in table 2. In the actual operation process, the constant pressure is kept during processing, but the pressure is applied by adopting air pressure during processing, the unit is pressure intensity, so that the diameter of the polishing disc corresponds to the pressure intensity, and if polishing discs with other sizes are adopted, the pressure intensity can be adjusted according to the actual situation along with the change of the pressure intensity.
Table 2 polishing parameters in example 2
Pressure intensity (Mpa) Rotational speed/(rpm) Feed speed/(mm/min)
0.04 100 120
The surface morphology of the NiP modified layer after polishing was measured under a 20 Xlens using a white light interferometer (Zygo NewView 700) and the results are shown in FIG. 5. FIG. 5 is a graph showing the results of the surface quality test of the NiP modified layer after polishing with the NiP modified layer CMP slurry in example 2 of the present invention. As can be seen from FIG. 5, the surface of the NiP modified layer after polishing with the chemical mechanical polishing solution for NiP modified layer of the present invention had a microroughness of RMS 0.584 nm.
Example 3
The chemical mechanical polishing solution for the NiP modified layer comprises the following components in percentage by mass:
Figure BDA0003666622860000081
in this example, the polishing abrasive is silica and has an average particle diameter of 50 nm.
In this example, the pH of the cmp slurry for the NiP modification layer was 7.2.
In this example, the oxidizing agent is hydrogen peroxide; the complexing agent is triethanolamine; surfactant sodium dodecyl benzene sulfonate.
A method for preparing the above chemical mechanical polishing solution for the NiP modification layer in this embodiment includes the following steps:
s1, mixing the polishing abrasive, the complexing agent, the surfactant and the deionized water, and stirring at the rotating speed of 600r/min for 5min to obtain a mixed solution A.
And S2, adding an oxidant into the mixed solution A, and uniformly mixing to obtain a mixed solution B.
And S3, adding the pH regulator into the mixed solution B, regulating the pH value to 7.2, and uniformly mixing to obtain the chemical mechanical polishing solution for the NiP modified layer. In the step, according to the actual situation, the pH regulator is selected to be one of phosphoric acid, citric acid, potassium hydroxide and sodium hydroxide, and the pH value is directly regulated to be 7.2.
An application of the above-mentioned chemical mechanical polishing solution for the NiP modified layer prepared in this embodiment in processing the NiP modified layer is to perform chemical mechanical polishing on the sample processed in embodiment 2 (the surface roughness of the NiP modified layer is between RMS 0.5nm and RMS 1nm), wherein the polishing device used is a numerical control small grinding head machine tool, the polishing is performed once for 27min, the used polishing disc is an asphalt disc with a diameter of 20mm, the polishing schematic diagram is shown in fig. 3, and the polishing parameters are shown in table 3.
Table 3 polishing parameters in example 3
Pressure (Mpa) Speed of rotation/(rpm) Feed speed/(mm/min)
0.03 80 100
The surface morphology of the NiP modified layer after polishing was measured under a 20 Xlens using a white light interferometer (Zygo NewView 700) and the results are shown in FIG. 6. FIG. 6 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with the chemical mechanical polishing solution for the NiP modified layer in example 3 of the present invention. As can be seen from FIG. 6, the surface of the NiP modified layer after polishing with the chemical mechanical polishing solution for NiP modified layer of the present invention had a microroughness of RMS 0.291 nm.
Example 4
The chemical mechanical polishing solution for the NiP modified layer comprises the following components in percentage by mass:
Figure BDA0003666622860000091
in this example, the polishing abrasive is silica and has an average particle diameter of 35 nm.
In this example, the pH of the cmp slurry for the NiP modification layer was 7.5.
In this example, the oxidizing agent is hydrogen peroxide; the complexing agent is triethanolamine; surfactant sodium dodecyl benzene sulfonate.
A method for preparing the above chemical mechanical polishing solution for the NiP modification layer in this embodiment includes the following steps:
s1, mixing the polishing abrasive, the complexing agent, the surfactant and the deionized water, and stirring for 5min at the rotating speed of 600r/min to obtain a mixed solution A.
And S2, adding an oxidant into the mixed solution A, and uniformly mixing to obtain a mixed solution B.
And S3, adding a pH regulator into the mixed solution B, regulating the pH value to 7.5, and uniformly mixing to obtain the NiP modified layer chemical mechanical polishing solution. In the step, according to the actual situation, the pH regulator is selected to be one of phosphoric acid, citric acid, potassium hydroxide and sodium hydroxide, and the pH value is directly regulated to 7.5.
The application of the chemical mechanical polishing solution for the NiP modified layer prepared in this embodiment in processing the NiP modified layer is to perform chemical mechanical polishing on the sample processed in embodiment 3 (the surface roughness of the NiP modified layer is less than 0.5nm RMS), wherein the used polishing equipment is a numerical control small grinding head machine tool, the polishing takes 33min for one time, the used polishing disc is an asphalt disc with the diameter of 20mm, the polishing schematic diagram is shown in fig. 3, and the polishing parameters are shown in table 4.
Table 4 polishing parameters in example 3
Pressure (Mpa) Speed of rotation/(rpm) Feed speed/(mm/min)
0.02 60 80
The surface morphology of the NiP modified layer after polishing was measured under a 20 × lens using a white light interferometer (Zygo new view 700), and the results are shown in fig. 7 and 8.
FIG. 7 is a graph showing the results of the surface quality test of the NiP modified layer after polishing with the NiP modified layer CMP slurry in example 4 of the present invention. As can be seen from fig. 7, the surface of the NiP modified layer after being polished by the NiP modified layer chemical mechanical polishing solution of the invention has a micro roughness RMS of 0.223nm, and fig. 8 is a three-dimensional topography of the surface of the NiP modified layer after being polished by the NiP modified layer chemical mechanical polishing solution in example 4 of the invention. As can be seen from fig. 7 and 8, the NiP modified layer having high surface quality can be obtained after the NiP modified layer is polished by the cmp slurry.
Example 5
The polishing effect of the chemical mechanical polishing solution for the NiP modified layer on the NiP modified layer of the curved surface element is examined, the sample piece used in the embodiment is a concave spherical mirror with the diameter of 75mm and the NiP modified layer plated on Al6061, the curvature radius is 95mm, the thickness of the NiP modified layer is 100 micrometers, the Ni content in the NiP modified layer is 88 wt%, the P content in the NiP modified layer is 12 wt%, and the microroughness of the sample piece is RMS 1.206 nm. The used polishing equipment is a numerical control small grinding head machine tool, polishing is carried out twice, the time is about 60min, the used polishing disk is an asphalt disk, the diameter is 10mm, and the polishing parameters are shown in table 5.
Table 5 polishing parameters in example 1
Serial number Pressure intensity (Mpa) Rotational speed/(rpm) Feed speed/(mm/min)
1 0.01 100 120
2 0.075 80 100
In this example, the formula of the polishing solution in the first polishing was the same as that in example 2, and the formula of the polishing solution in the second polishing was the same as that in example 3.
The surface morphology of the NiP modified layer after polishing was measured under a 20 Xlens using a white light interferometer (Zygo NewView 700) and the results are shown in FIG. 9. FIG. 9 is a graph showing the results of the surface quality test of the NiP modified layer after polishing with the NiP modified layer CMP slurry in example 5 of the present invention. As can be seen from FIG. 9, the surface of the NiP modified layer after polishing with the chemical mechanical polishing solution for NiP modified layer of the present invention had a microroughness of 0.297nm RMS.
Example 6
The polishing effect of the chemical mechanical polishing solution for the NiP modified layer with different pH values on the NiP modified layer is examined, the surface roughness of the adopted workpiece is RMS 1.177nm which is between RMS 1nm and RMS 2nm, so the polishing solution and the processing parameters are basically the same as those in the embodiment 2, and the difference is only that: the pH values of the chemical mechanical polishing solution of the NiP modified layer are 4, 7 and 10 in sequence.
The surface morphology of the NiP modified layer after polishing with the NiP modified layer chemical mechanical polishing solution of different pH values was measured under a 20 Xlens using a white light interferometer (Zygo NewView 700), and the results are shown in FIGS. 10-12.
FIG. 10 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with a pH 4 NiP modified layer CMP slurry in example 6 of the present invention. As can be seen from fig. 10, the reason why the pits are formed on the surface of the NiP modification layer after polishing may be that the NiP modification layer is polished under acidic conditions, and the chemical reaction is severe, so that the pits are easily formed by acid etching.
FIG. 11 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with pH 7 CMP slurry in example 6 of the present invention. As can be seen from fig. 11, the surface of the NiP modified layer after polishing had no significant processing defects.
FIG. 12 is a graph showing the results of surface quality tests of the NiP modified layer after polishing with a pH 10 NiP modified layer CMP slurry in example 6 of the present invention. As can be seen from fig. 12, the surface of the NiP modified layer after polishing has a lot of scratches, which may be caused by that the NiP modified layer is polished under alkaline conditions, the polishing solution has crystallization, and the grain size is much larger than that of the polishing abrasive grains, so that scratches are easily generated by the sliding of the grains on the surface during polishing.
From the results of fig. 10 to 12, it can be seen that the chemical mechanical polishing solution for NiP modified layers of the present invention is more advantageous for obtaining NiP modified layers with higher processing precision when the pH value is neutral.
Example 7
The polishing effect of the chemical mechanical polishing solution for the NiP modified layer of different polishing abrasive materials on the NiP modified layer is inspected, the adopted workpiece surface roughness is RMS 1.153nm which is between RMS 1nm and RMS 2nm, so the polishing solution and the processing parameters are basically the same as those of the embodiment 2, and the difference is only that: the polishing abrasive of the chemical mechanical polishing solution of the NiP modified layer sequentially comprises silicon dioxide and aluminum oxide. The hardness of the silica, alumina and NiP modified layers is shown in table 6.
TABLE 6 hardness values for different polishing abrasives and NiP in example 6
Material NiP Silicon dioxide Alumina oxide
Mohs hardness 5.6 7 9
The surface morphology of the NiP modified layer after polishing with the NiP modified layer chemical mechanical polishing solution of different polishing abrasives was measured with a white light interferometer (Zygo NewView 700) under a 20 × lens, and the results are shown in fig. 13-14.
FIG. 13 is a graph showing the results of the surface quality test of the NiP modified layer on the concave spherical surface after polishing with the chemical mechanical polishing solution for the NiP modified layer in which the polishing abrasive is silicon dioxide in example 7 of the present invention. As can be seen from fig. 13, when silicon dioxide is used as the polishing abrasive, the surface of the NiP modified layer after polishing has no scratch damage, and the polishing quality is good.
FIG. 14 is a graph showing the results of surface quality tests on NiP modified layers of concave spherical surfaces after polishing with a chemical mechanical polishing solution for NiP modified layers with alumina as the polishing abrasive in example 7 of the present invention. As can be seen from fig. 14, using alumina as a polishing abrasive, a large number of scratches were generated on the surface of the NiP modified layer after polishing.
From the results of the above examples, it can be seen that the NiP modified layer chemical mechanical polishing solution and the processing technology developed by the present invention can obtain a NiP modified layer with high surface quality, and meet the high-level application requirements.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and adaptations to those skilled in the art without departing from the principles of the present invention should also be considered as within the scope of the present invention.

Claims (10)

1. The chemical mechanical polishing solution for the NiP modified layer is characterized by comprising the following components in percentage by mass:
Figure FDA0003666622850000011
the polishing abrasive is silicon dioxide; the pH value of the chemical mechanical polishing solution for the NiP modified layer is 6.5-7.5.
2. The chemical mechanical polishing solution for the NiP modified layer according to claim 1, which comprises the following components in percentage by mass:
Figure FDA0003666622850000012
the polishing abrasive is silicon dioxide; the pH value of the NiP modified layer chemical mechanical polishing solution is 6.8-7.2.
3. The chemical mechanical polishing solution for a NiP modification layer according to claim 1 or 2, wherein the average particle size of the silica is 35nm or 50 nm.
4. The chemical mechanical polishing solution for a NiP modification layer according to claim 1 or 2, wherein the oxidizing agent is hydrogen peroxide.
5. The chemical mechanical polishing solution for the NiP modified layer according to claim 1 or 2, wherein the complexing agent is at least one of oxalic acid, citric acid, glycine, alanine and triethanolamine; the surfactant is at least one of sodium stearate, potassium stearate and sodium dodecyl benzene sulfonate.
6. A method for preparing the chemical mechanical polishing solution for the NiP modified layer according to any one of claims 1 to 5, which comprises the following steps:
s1, mixing the polishing abrasive, the complexing agent, the surfactant and water, and stirring to obtain a mixed solution A;
s2, adding an oxidant into the mixed solution A to obtain a mixed solution B;
and S3, adding a pH regulator into the mixed solution B, and regulating the pH value to a set value to obtain the NiP modified layer chemical mechanical polishing solution.
7. The method according to claim 6, wherein in step S3, the pH adjuster is at least one of phosphoric acid, citric acid, potassium hydroxide, and sodium hydroxide.
8. The method according to claim 6 or 7, wherein in step S1, the rotation speed of the stirring is 300r/min to 600 r/min; the stirring time is 5 min-10 min.
9. Use of the chemical mechanical polishing solution for a NiP modified layer according to any one of claims 1 to 5 or the chemical mechanical polishing solution for a NiP modified layer prepared by the preparation method according to any one of claims 6 to 8 in processing a NiP modified layer.
10. The use of claim 9, wherein the use is chemical mechanical polishing of a processed NiP modified layer with a NiP modified layer chemical mechanical polishing slurry; the chemical mechanical polishing process parameters are as follows: manufacturing a polishing disk by using asphalt, wherein the rotating speed of the polishing disk is controlled to be 60-120 rpm, the polishing pressure is controlled to be 0.02-0.05 MPa, and the feeding speed is 80-150 mm/min; the equipment adopted in the chemical mechanical polishing is a small grinding head polishing machine tool.
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