CN114774003B - 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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CN114774003B
CN114774003B CN202210588044.5A CN202210588044A CN114774003B CN 114774003 B CN114774003 B CN 114774003B CN 202210588044 A CN202210588044 A CN 202210588044A CN 114774003 B CN114774003 B CN 114774003B
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modified layer
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mechanical polishing
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CN114774003A (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
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Abstract

The invention discloses a NiP modified layer chemical mechanical polishing solution, 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 polishing abrasive, complexing agent, surfactant and water, adding oxidant and adjusting pH value to a set value. The NiP modified layer chemical mechanical polishing solution can realize the balance of chemical corrosion action and mechanical removal action, can be used for chemically and mechanically polishing the NiP modified layer, can realize high-precision processing of the NiP modified layer, and can obtain a high-quality processing surface, so that the NiP modified layer can 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 processing of optical elements, and relates to a NiP modified layer chemical mechanical polishing solution, a preparation method and application thereof.
Background
At present, the typical range of micro roughness obtained on the surface of a reflector material manufactured by conventional processing technology, such as a metal material, is RMS 2nm to RMS 10nm, and the reflector material can only generally meet the use requirement of infrared spectrum, but hardly meet the use requirement of visible light and shorter wavelength range. In addition, to meet the use requirements in the visible spectrum, the microscopic roughness of the surface of the reflector material should be better than RMS 1nm; in particular, in the field of hard X-ray mirror applications, higher demands are placed on the micro-roughness of the mirror material surface, which is better than RMS 0.3nm. 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.
Modifying the surface of the substrate is a common method for improving the optical performance of the mirror surface of the mirror, for example, depositing a NiP modified layer on the mirror surface of the mirror can play a role in improving the surface defects of the substrate, and at the same time, a 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 working procedure is single-point diamond turning, although the surface meeting the infrared imaging quality requirement can be directly obtained through the single-point diamond turning technology, the single-point diamond turning precision is limited by a machine tool, periodic turning patterns can be generated during processing, diffraction and stray light are caused, the light flux loss is increased, the reflectivity and imaging quality of a mirror surface are reduced, and the optical performance of the mirror surface is influenced. Therefore, after single-point diamond turning, the NiP modified layer also needs to be further processed to meet higher use requirements.
The chemical mechanical polishing is a surface finishing process, and most of the existing chemical mechanical polishing processes for processing the NiP modified layer have the following defects: (1) failure to process curved surface elements; (2) The control of surface scratch damage still has difficulty in achieving high-precision use requirements; (3) Most of the polishing solutions used contain toxic and harmful chemical agents, such as Benzotriazole (BTA), ethylenediamine tetraacetic acid (EDTA) and other toxic substances, and the addition of the toxic agents can not only influence the physical health of processing operators, but also cause harm to the environment. In addition, during the actual research of the present inventors, it was also found that: the existing polishing solution for polishing the surface of a metal substrate is not suitable for polishing the NiP modified layer, and probably because the polishing solution is an abrasive and pH value of the existing chemical mechanical polishing solution can produce immeasurable damages to the NiP modified layer, such as a large number of scratches on the surface of the NiP modified layer caused by taking alumina as an abrasive, and meanwhile, under the condition of lower pH value, the chemical reaction is intense, and pitting caused by acid etching is easy to produce on the surface of the NiP modified layer, so that the NiP modified layer deposited on the mirror surface of a reflecting mirror still has difficulty in meeting better use requirements.
Therefore, the obtained chemical mechanical polishing solution is suitable for processing the NiP modified layer, and has great 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 provide a NiP modified layer chemical mechanical polishing solution, a preparation method and application thereof, wherein the NiP modified layer chemical mechanical polishing solution can realize the balance of chemical corrosion action and mechanical removal action, can be used for chemically and mechanically polishing a NiP modified layer, can realize high-precision processing of the NiP modified layer, can obtain a high-quality processing surface, and can meet various requirements.
In order to solve the technical problems, the invention adopts the following technical scheme:
the NiP modified layer chemical mechanical polishing solution comprises the following components in percentage by mass:
Figure BDA0003666622860000021
the polishing abrasive is silicon dioxide; the pH value of the NiP modified layer chemical mechanical polishing solution is 6.5-7.5.
The NiP modified layer chemical mechanical polishing solution 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.
The NiP modified layer chemical mechanical polishing solution is further improved, and the average particle size of the silicon dioxide is 35nm or 50nm.
The NiP modified layer chemical mechanical polishing solution is further improved, and the oxidant is hydrogen peroxide.
The NiP modified layer chemical mechanical polishing solution is further improved, 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.
As a general technical conception, the invention also provides a preparation method of the NiP modified layer chemical mechanical polishing solution, which comprises the following steps:
s1, mixing polishing abrasive, complexing agent and surfactant with 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 the above preparation method, in step S3, the pH adjuster is at least one of phosphoric acid, citric acid, potassium hydroxide and sodium hydroxide.
In the preparation method, which is further improved, in the step S1, the stirring rotating speed is 300 r/min-600 r/min; the stirring time is 5-10 min.
As a general technical concept, the invention also provides the application of the NiP modified layer chemical mechanical polishing solution or the NiP modified layer chemical mechanical polishing solution prepared by the preparation method in the processing of the NiP modified layer.
The application is further improved, wherein the application is that a NiP modified layer is subjected to chemical mechanical polishing by using a NiP modified layer chemical mechanical polishing solution; the technological parameters of the chemical mechanical polishing are as follows: manufacturing a polishing disc by using asphalt, wherein the rotating speed of the polishing disc is controlled to be 60-120 rpm, the polishing pressure is controlled to be 0.02-0.05 MPa, and the feeding speed is controlled to be 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 high-precision use requirement, the invention creatively provides the NiP modified layer chemical mechanical polishing solution, and the balance of chemical corrosion action and mechanical removal action can be realized by optimizing the components and the content of each component, so that the high-precision processing of the NiP modified layer can be realized when the polishing solution is used for chemically and mechanically polishing the NiP modified layer, the high-quality processing surface can be obtained, and finally the NiP modified layer can meet various requirements; meanwhile, the NiP modified layer chemical mechanical polishing solution 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 NiP modified layer chemical mechanical polishing solution, which comprises the steps of firstly mixing polishing abrasive, complexing agent, surfactant and water, under the action of the surfactant, facilitating the prevention of agglomeration of the polishing abrasive, further adding an oxidant, and finally regulating the pH value to a set value by utilizing a pH regulator to obtain the NiP modified layer chemical mechanical polishing solution 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 industrialized application.
(3) The invention also provides application of the NiP modified layer chemical mechanical polishing solution in processing the NiP modified layer, in particular to chemical mechanical polishing of the NiP modified layer by using the NiP modified layer chemical mechanical polishing solution, and the NiP modified layer with high quality can be obtained by processing through the mechanical removal effect and the chemical reaction effect in the balanced polishing process, so that the NiP modified layer 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.
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In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
FIG. 1 is a schematic diagram of the chemical reaction of the NiP modified layer of the present invention during polishing.
FIG. 2 is a schematic representation of the mechanical removal of the NiP modified layer of the present invention that occurs at the time.
FIG. 3 is a schematic view showing the polishing of the NiP modified layer by the NiP modified layer chemical mechanical polishing liquid in example 1 of the present invention.
FIG. 4 is a graph showing the results of surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 1 of the present invention.
FIG. 5 is a graph showing the results of surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 2 of the present invention.
FIG. 6 is a graph showing the results of surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 3 of the present invention.
FIG. 7 is a graph showing the results of surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 4 of the present invention.
FIG. 8 is a three-dimensional topography of the surface of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution in example 4 of the present invention.
FIG. 9 is a graph showing the results of surface quality test of a concave spherical NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution in example 5 of the present invention.
FIG. 10 is a graph showing the results of surface quality test of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution having a pH of 4 in example 6 of the present invention.
FIG. 11 is a graph showing the results of surface quality test of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution having a pH of 7 in example 6 of the present invention.
FIG. 12 is a graph showing the results of surface quality test of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution having a pH of 10 in example 6 of the present invention.
FIG. 13 is a graph showing the results of surface quality test of a concave spherical NiP modified layer polished with a NiP modified layer chemical mechanical polishing liquid in which polishing abrasive is silica in example 7 of the present invention.
FIG. 14 is a graph showing the results of surface quality test of a concave spherical NiP modified layer polished with a NiP modified layer chemical mechanical polishing liquid in which polishing abrasive is alumina in example 7 of the present invention.
Detailed Description
The invention is further described below in connection with the drawings and the specific preferred embodiments, but the scope of protection of the invention is not limited thereby.
As shown in fig. 1, the chemical reaction of the NiP modified layer in the polishing liquid is:
Ni+H 2 O 2 →NiO+H 2 O
NiO+H 2 O 2 →Ni 2 O 3 +H 2 O
P+H 2 O 2 →P 2 O 3 +H 2 O
as can be seen from the above reaction formula, niP modified layer surface is formed to contain NiO and Ni under the action of oxidant (hydrogen peroxide) 2 O 3 And P 2 O 3 Is formed on the substrate. In the polishing solution, niO and Ni 2 O 3 And P 2 O 3 The following reaction with water will continue to occur:
P 2 O 3 +H 2 O→H 3 PO 3
Figure BDA0003666622860000051
Figure BDA0003666622860000052
in the above reaction, ni is formed 2+ 、Ni 3+ Can carry out complex reaction with the added complex in the solution, can accelerate the oxidation reaction and realize the dissolution of the polishing product. In addition, the binding force between the generated oxide film and the NiP modified layer is smaller than that between the inside molecular layers of the NiP modified layer, so that the oxide film is easier to remove. Meanwhile, the microscopic morphology of the surface of the NiP modified layer is in a high-low uneven 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 protecting, and excessive scratching of the surface is avoided. Therefore, the polishing efficiency of the NiP modified layer can be improved by using the oxidant and the complexing agent, and the ultra-smooth workpiece surface can be obtained.
As shown in FIG. 2, the Preston equation is a classical equation for a mathematical model of chemical mechanical polishing material removal, and it is believed that the material removal rate is primarily linearly proportional to the pressure applied by 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, have a great influence on material removal. With this in mind, the material removal model mentioned by Luo and Dornfeld was chosen to explain the mechanical removal effect in the ultra-smooth polishing of NiP coatings.
Figure BDA0003666622860000053
Wherein MRR is the material removal rate; phi is a standard normal distribution function; p (P) 0 Is the downward pressure; v is the relative velocity; c (C) 2 、C 3 For undetermined coefficient, C 3 The numerical value depends on the following formula.
Figure BDA0003666622860000054
Figure BDA0003666622860000055
Wherein C is 1 Is a coefficient to be determined; ρ ω Is the density of the sample; a is that 0 Is the nominal contact area; k=1+3 σ/x avg (sigma is the standard deviation of the normal distribution); d, d s The dilution ratio of the polishing solution (the volume ratio of the polishing solution to water); ρ s Is the density of the polishing solution; m is m s-a Is the concentration of the abrasive in the polishing solution; d (D) sum The density of asperities in contact with the sample surface per unit area of the polishing pad; a is the average area of a single convex body before the polishing pad is deformed; l is the height of the convex body before the polishing pad is deformed; ρ a The density of the abrasive; x is x avg Is the average particle size of the abrasive; e (E) p Is the modulus of elasticity of the polishing pad; h ω Is the hardness of the sample; b 1 The value of (2) depends on the following formula:
Figure BDA0003666622860000061
wherein R is the radius of the top end of the convex body of the polishing pad. C (C) 2 The value of (2) depends on the following formula:
Figure BDA0003666622860000062
wherein H is p Is the hardness of the polishing pad. The model is mainly used for exploring a solid-solid contact abrasion mechanism from the mechanical point of view, and the mechanical removal effect in processing is more comprehensively described.
In the chemical mechanical polishing of NiP modified layers, it is most important to achieve a balance between mechanical removal and chemical reaction during polishing to obtain a high quality of the processed surface. Therefore, the invention mainly optimizes the formula of the polishing solution and the processing technological parameters around realizing the balance between the mechanical removal effect and the chemical reaction effect in the polishing process.
For a better illustration of the present invention, which is convenient for understanding the technical solution of the present invention, exemplary but non-limiting examples of the present invention are as follows:
example 1
The NiP modified layer chemical mechanical polishing solution comprises the following components in percentage by mass:
Figure BDA0003666622860000063
in this example, the polishing abrasive was silica with an average particle size of 50nm.
In this example, the pH of the NiP modified layer chemical mechanical polishing solution was 6.5.
In this embodiment, the oxidizing agent is hydrogen peroxide; in the invention, hydrogen peroxide is used as an oxidant, the property is stable in the using process, the hydrogen peroxide does not belong to dangerous chemicals, the danger is extremely low, and the hydrogen peroxide is more suitable for green manufacturing.
In this embodiment, the complexing agent is oxalic acid, or any one of citric acid, glycine and alanine;
in this embodiment, the surfactant is sodium stearate, and potassium stearate may be used.
The preparation method of the NiP modified layer chemical mechanical polishing solution in the embodiment comprises the following steps:
s1, mixing polishing abrasive, complexing agent, surfactant and deionized water, and stirring for 5-10 min at the rotating speed of 300-600 r/min to obtain a mixed solution A.
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 actual conditions, 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.
The application of the NiP modified layer chemical mechanical polishing solution prepared in the embodiment in the process of processing the NiP modified layer is used for performing chemical mechanical polishing on the NiP modified layer with the surface roughness larger than RMS 2nm, a sample piece is a reflector with the diameter of 100mm and the NiP modified layer plated on Al6061, the thickness of the NiP modified layer is 100 mu m, the Ni content in the NiP modified layer is 88wt%, the P content is 12wt%, the sample piece is subjected to ultra-precise turning, and the initial microscopic roughness is 2.326nm.
The polishing equipment used is a numerical control small grinding head machine tool, the polishing is carried out once for 18min, the polishing disk used is an asphalt disk, the diameter is 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 polished surface morphology of the NiP modified layer was measured under a 20 x lens using a white light interferometer (Zygo NewView 700), and the results are shown in fig. 4. FIG. 4 is a graph showing the results of surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 1 of the present invention. As can be seen from FIG. 4, the microscopic roughness of the surface of the NiP modified layer after being polished by the chemical mechanical polishing solution of the NiP modified layer of the present invention is RMS 1.374nm.
Example 2
The NiP modified layer chemical mechanical polishing solution comprises the following components in percentage by mass:
Figure BDA0003666622860000071
in this example, the polishing abrasive was silica with an average particle size of 50nm.
In this example, the pH of the NiP modified layer chemical mechanical polishing solution was 6.8.
In this embodiment, the oxidizing agent is hydrogen peroxide.
In this embodiment, the complexing agent is oxalic acid, or any one of citric acid, glycine and alanine;
in this embodiment, the surfactant is sodium stearate, and potassium stearate may be used.
The preparation method of the NiP modified layer chemical mechanical polishing solution in the embodiment comprises the following steps:
s1, mixing polishing abrasive, complexing agent, surfactant and deionized water, and stirring for 5min at the rotating speed of 600r/min to obtain a mixed solution A.
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 actual conditions, 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 above-mentioned NiP modified layer chemical mechanical polishing solution prepared in this example in the processing of the NiP modified layer is that the sample piece is the sample piece processed in example 1 (the surface roughness of the NiP modified layer is between RMS 1nm and RMS 2 nm), and chemical mechanical polishing is performed, wherein the polishing equipment used is a numerical control small grinding head machine tool, the polishing is performed once for 22.5min, the polishing disc used 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 required to be maintained, but the pressure is adopted for processing, the unit is the pressure, so the diameter of the polishing disc has a corresponding relation with the pressure, and if the polishing disc with other sizes is adopted, the pressure is changed along with the change, and the pressure can be adjusted according to the actual situation.
Table 2 polishing parameters in example 2
Pressure (Mpa) Rotational speed/(rpm) Feed speed/(mm/min)
0.04 100 120
The polished surface morphology of the NiP modified layer was measured under a 20 x lens 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 surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 2 of the present invention. As can be seen from FIG. 5, the microscopic roughness of the surface of the NiP modified layer after being polished by the chemical mechanical polishing solution of the NiP modified layer of the present invention is RMS 0.584nm.
Example 3
The NiP modified layer chemical mechanical polishing solution comprises the following components in percentage by mass:
Figure BDA0003666622860000081
in this example, the polishing abrasive was silica with an average particle size of 50nm.
In this example, the pH of the NiP modified layer chemical mechanical polishing solution was 7.2.
In this embodiment, the oxidizing agent is hydrogen peroxide; the complexing agent is triethanolamine; the surfactant sodium dodecyl benzene sulfonate.
The preparation method of the NiP modified layer chemical mechanical polishing solution in the embodiment comprises the following steps:
s1, mixing polishing abrasive, complexing agent, surfactant and deionized water, and stirring for 5min at the rotating speed of 600r/min to obtain a mixed solution A.
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 7.2, and uniformly mixing to obtain the NiP modified layer chemical mechanical polishing solution. In the step, according to actual conditions, 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 7.2.
The application of the above-mentioned NiP modified layer chemical mechanical polishing solution prepared in this example in the processing of the NiP modified layer is that the sample piece is the sample piece processed in example 2 (the surface roughness of the NiP modified layer is between 0.5nm and 1nm RMS), and chemical mechanical polishing is performed, wherein the polishing equipment used is a numerical control small grinding head machine tool, the polishing is performed once, the polishing time is 27min, the polishing disc used is an asphalt disc, the diameter is 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) Rotational speed/(rpm) Feed speed/(mm/min)
0.03 80 100
The polished surface morphology of the NiP modified layer was measured under a 20 x lens 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 test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 3 of the present invention. As can be seen from FIG. 6, the microscopic roughness of the surface of the NiP modified layer after being polished by the chemical mechanical polishing solution of the NiP modified layer of the present invention is 0.291nm in RMS.
Example 4
The NiP modified layer chemical mechanical polishing solution comprises the following components in percentage by mass:
Figure BDA0003666622860000091
in this example, the polishing abrasive was silica with an average particle size of 35nm.
In this example, the pH of the NiP modified layer chemical mechanical polishing solution was 7.5.
In this embodiment, the oxidizing agent is hydrogen peroxide; the complexing agent is triethanolamine; the surfactant sodium dodecyl benzene sulfonate.
The preparation method of the NiP modified layer chemical mechanical polishing solution in the embodiment comprises the following steps:
s1, mixing polishing abrasive, complexing agent, surfactant and deionized water, and stirring for 5min at the rotating speed of 600r/min to obtain a mixed solution A.
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 actual conditions, 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 7.5.
The application of the NiP modified layer chemical mechanical polishing solution prepared in the embodiment in the process of processing the NiP modified layer is that the sample piece is the sample piece processed in the embodiment 3 (the surface roughness of the NiP modified layer is smaller than 0.5nm RMS), chemical mechanical polishing is carried out, wherein the polishing equipment is a numerical control small grinding head machine tool, the polishing is carried out once and for 33 minutes, the 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 4.
Table 4 polishing parameters in example 3
Pressure (Mpa) Rotational speed/(rpm) Feed speed/(mm/min)
0.02 60 80
The polished surface morphology of the NiP modified layer was measured under a 20 x lens using a white light interferometer (Zygo NewView 700), and the results are shown in fig. 7 and 8.
FIG. 7 is a graph showing the results of surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 4 of the present invention. As can be seen from FIG. 7, the microscopic roughness of the surface of the NiP modified layer after being polished by the NiP modified layer chemical mechanical polishing liquid of the present invention is 0.223nm in RMS, 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 liquid in example 4 of the present invention. As can be seen from fig. 7 and 8, after the NiP-modified layer is polished with the chemical mechanical polishing liquid, a NiP-modified layer with high surface quality can be obtained.
Example 5
The effect of the NiP modified layer chemical mechanical polishing liquid on polishing the NiP modified layer on the curved surface element was examined, and the sample piece used in this example was a concave spherical mirror with a diameter of 75mm, in which the NiP modified layer was plated on Al6061, with a radius of curvature of 95mm, a thickness of the NiP modified layer of 100 μm, a Ni content of 88wt%, a P content of 12wt% and a microscopic roughness of 1.206nm in the sample piece. The polishing equipment used was a numerically controlled small grinding head machine tool, the polishing was carried out twice for about 60 minutes, the polishing disk used was an asphalt disk with a diameter of 10mm, and the polishing parameters are shown in Table 5.
Table 5 polishing parameters in example 1
Sequence number Pressure (Mpa) Rotational speed/(rpm) Feed speed/(mm/min)
1 0.01 100 120
2 0.075 80 100
In this example, the formulation of the polishing liquid at the first polishing was the same as in example 2, and the formulation of the polishing liquid at the second polishing was the same as in example 3.
The polished surface morphology of the NiP modified layer was measured under a 20 x lens 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 surface quality test of a NiP modified layer after polishing with a NiP modified layer chemical mechanical polishing solution in example 5 of the present invention. As can be seen from FIG. 9, the microscopic roughness of the surface of the NiP modified layer after being polished by the chemical mechanical polishing solution of the NiP modified layer of the present invention was 0.297nm in RMS.
Example 6
The polishing effect of the NiP modified layer chemical mechanical polishing solution with different pH values on the NiP modified layer is examined, the surface roughness of the adopted workpiece is RMS 1.177nm, and the roughness 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 that: the pH value of the NiP modified layer chemical mechanical polishing solution is sequentially 4, 7 and 10.
The surface morphology of the NiP modified layer after polishing was measured with a NiP modified layer chemical mechanical polishing solution of different pH values under a 20 Xlens using a white light interferometer (Zygo NewView 700), and the results are shown in FIGS. 10 to 12.
FIG. 10 is a graph showing the results of surface quality test of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution having a pH of 4 in example 6 of the present invention. As can be seen from FIG. 10, the surface of the NiP modified layer after polishing has pitting, which may be caused by polishing the NiP modified layer under acidic conditions, and the chemical reaction is severe, so pitting is easily formed under the action of acid etching.
FIG. 11 is a graph showing the results of surface quality test of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution having a pH of 7 in example 6 of the present invention. As can be seen from fig. 11, the surface of the NiP modified layer after polishing has no significant processing defects.
FIG. 12 is a graph showing the results of surface quality test of a NiP modified layer polished with a NiP modified layer chemical mechanical polishing solution having a pH of 10 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 large number of scratches, probably because the NiP modified layer is polished under alkaline conditions, the polishing liquid is crystallized, and the grain size is much larger than the polishing abrasive grains, so that scratches are easily generated due to the sliding of the grains on the surface during polishing.
From the results of FIGS. 10 to 12, it is understood that the NiP modified layer chemical mechanical polishing liquid of the present invention is more advantageous for obtaining a NiP modified layer with higher processing accuracy at neutral pH.
Example 7
The polishing effect of the NiP modified layer chemical mechanical polishing solution of different polishing abrasives on the NiP modified layer is examined, the surface roughness of the adopted workpiece is RMS 1.153nm and 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 that: the polishing abrasive of the NiP modified layer chemical mechanical polishing solution is silicon dioxide and aluminum oxide in sequence. The hardness of the silica, alumina and NiP modified layers is shown in table 6.
TABLE 6 different polishing abrasives and NiP hardness values in example 6
Material NiP Silica dioxide Alumina oxide
Mohs hardness of 5.6 7 9
The surface morphology of the NiP modified layer was measured with a white light interferometer (Zygo NewView 700) under a 20 x lens with different polishing abrasives using a NiP modified layer chemical mechanical polishing liquid, and the results are shown in fig. 13 to 14.
FIG. 13 is a graph showing the results of surface quality test of a concave spherical NiP modified layer polished with a NiP modified layer chemical mechanical polishing liquid in which polishing abrasive is silica in example 7 of the present invention. As can be seen from fig. 13, the surface of the NiP modified layer after polishing was free from scratch damage by using silica as a polishing abrasive, and the polishing quality was good.
FIG. 14 is a graph showing the results of surface quality test of a concave spherical NiP modified layer polished with a NiP modified layer chemical mechanical polishing liquid in which polishing abrasive is alumina 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 is known that the NiP modified layer chemical mechanical polishing solution and the processing technique 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 only 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 concept of the invention belong to the protection scope of the invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.

Claims (8)

1. The NiP modified layer chemical mechanical polishing solution for optical element processing is characterized by comprising the following components in percentage by mass:
15 to 30 percent of polishing abrasive,
1 to 10 percent of oxidant,
1 to 5 percent of complexing agent,
1% -5% of surfactant and the balance of water;
the polishing abrasive is silicon dioxide; the pH value of the NiP modified layer chemical mechanical polishing solution is 7-7.5; the oxidant is hydrogen peroxide; 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.
2. The NiP-modified layer chemical mechanical polishing liquid as recited in claim 1, comprising the following components in mass percent:
15 to 30 percent of polishing abrasive,
1 to 10 percent of oxidant,
1 to 5 percent of complexing agent,
1% -5% of surfactant and the balance of water;
the polishing abrasive is silicon dioxide; the pH value of the NiP modified layer chemical mechanical polishing solution is 7-7.2.
3. The NiP-modified-layer chemical-mechanical polishing liquid according to claim 1 or 2, characterized in that the average particle diameter of the silica is 35nm or 50nm.
4. A method for preparing the NiP-modified-layer chemical mechanical polishing liquid as set forth in any one of claims 1 to 3, comprising the steps of:
s1, mixing polishing abrasive, complexing agent and surfactant with 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.
5. The method according to claim 4, wherein in step S3, the pH adjustor is at least one of phosphoric acid, citric acid, potassium hydroxide and sodium hydroxide.
6. The method according to claim 4 or 5, wherein in step S1, the stirring speed is 300r to 600r/min; the stirring time is 5-10 min.
7. Use of the NiP-modified layer chemical-mechanical polishing liquid according to any one of claims 1 to 3 or the NiP-modified layer chemical-mechanical polishing liquid produced by the production method according to any one of claims 4 to 6 for processing a NiP-modified layer.
8. The use according to claim 7, wherein the use is chemical mechanical polishing of the processed NiP modified layer with a NiP modified layer chemical mechanical polishing solution; the technological parameters of the chemical mechanical polishing are as follows: manufacturing a polishing disc by using asphalt, wherein the rotating speed of the polishing disc 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 mm-150 mm/min; the equipment adopted in the chemical mechanical polishing is a small grinding head polishing machine tool.
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