CN108841329B - Method for preparing nano-colloid organic composite polishing solution and application thereof - Google Patents
Method for preparing nano-colloid organic composite polishing solution and application thereof Download PDFInfo
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- CN108841329B CN108841329B CN201810669839.2A CN201810669839A CN108841329B CN 108841329 B CN108841329 B CN 108841329B CN 201810669839 A CN201810669839 A CN 201810669839A CN 108841329 B CN108841329 B CN 108841329B
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
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Abstract
The embodiment of the invention discloses a method for preparing a nano-colloid organic composite polishing solution, which is prepared from the following raw materials in parts by weight: ethylene glycol ethyl ester: 80 parts by weight; nano silicon dioxide: 5 parts by weight; surfactant (b): m parts by weight; dispersing agent: 1 part by weight; deionized water: n weight portions; a stabilizer: 2 parts by weight; pH regulator: 5 parts by weight; wherein M is 2-6, N is 1-5, and the raw materials are allowed to have an error within 0.1 weight part. The embodiment of the invention also discloses a method for polishing the thallium-doped cesium iodide crystal by using the nano colloid organic composite polishing solution prepared by the method, so that the thallium-doped cesium iodide crystal with the surface roughness of less than 10nm can be obtained.
Description
Technical Field
The invention relates to the technical field of polishing solution, in particular to a method for preparing nano colloidal organic composite polishing solution and a method for polishing thallium-doped cesium iodide crystals by using the nano colloidal organic composite polishing solution prepared by the method.
Background
The thallium-doped cesium iodide crystal CsI (TI) belongs to a typical inorganic scintillation crystal, can emit ultraviolet rays or visible light after absorbing the energy of X-rays, gamma-rays or other high-energy particles, has an emission spectrum matched with a silicon photodiode, is high in light yield, short in irradiation length and good in mechanical property, is an excellent and practical scintillation crystal material, is particularly suitable for detecting medium and low energy particles, and is widely applied to the aspect of X-ray detection.
The Mohs hardness of thallium-doped cesium iodide crystal is 2, and the density is 3.67g/cm3The refractive index of 1.84 is soft, fragile, high in temperature sensitivity coefficient and water-soluble, and is one of soft and brittle crystal materials which are generally recognized to be difficult to polish, so that many mature conventional polishing methods cannot be applied to the polishing process of thallium-doped cesium iodide crystals. At present, the main polishing methods include ultra-precision grinding technology, single-point diamond cutting technology and traditional grinding and polishing. The surface roughness of the thallium-doped cesium iodide crystal polished by the method is generally 20-70 nm, and the application requirement is difficult to meet.
Accordingly, a technical solution is desired to overcome or at least alleviate the above-mentioned drawbacks of the prior art.
Disclosure of Invention
The embodiment of the invention aims to provide a method for preparing a nano colloidal organic composite polishing solution and a method for polishing thallium-doped cesium iodide crystals by using the nano colloidal organic composite polishing solution prepared by the method, so as to improve the smoothness of the thallium-doped cesium iodide crystals after polishing.
In order to achieve the above object, an embodiment of the present invention provides a method for preparing a nano-colloid organic composite polishing solution, which is prepared from the following raw materials in parts by weight:
ethylene glycol ethyl ester: 80 parts by weight of a water-soluble polymer,
nano silicon dioxide: 5 parts by weight of a reaction product of (B),
surfactant (b): m is the weight portion of the compound (I),
dispersing agent: 1 part by weight of a reaction product of (B),
deionized water: n is the weight portion of N,
a stabilizer: 2 parts by weight of a reaction product of (B),
pH regulator: 5 parts by weight of a reaction product of (B),
wherein M is 2-6, N is 1-5, and the raw materials are allowed to have an error within 0.1 weight part.
Preferably, M is 5 and N is 2.
Preferably, the nano-silica is a particle having an average particle diameter of 50 nm.
Preferably, the surfactant comprises M/2 parts by weight of potassium hexametaphosphate and M/2 parts by weight of sodium chloride.
Preferably, the stabilizer is 2 parts by weight of acrylic polyester copolymer resin.
Preferably, the pH adjuster is 2.5 parts by mass of a sodium hydroxide solution and 2.5 parts by mass of a dilute hydrochloric acid solution.
Preferably, the nano-colloid organic composite polishing solution is prepared by the following steps:
(1) surface activation: placing the surfactant M in parts by weight into the nano silicon dioxide 5 in parts by weight for ultrasonic dispersion, and standing for more than 10 hours; (2) mixing organic solvents: adding 80 parts by weight of organic solvent of ethylene glycol ethyl ester into the nano silicon dioxide after surface activation, and performing ultrasonic dispersion for more than 30 minutes; (3) and (3) stabilizing and curing: sequentially adding 1 part by weight of dispersant and 2 parts by weight of stabilizer into the solution obtained in the step of mixing the organic solvent; (4) adjusting the pH value: adjusting the pH value of the solution after the stabilizing and curing step to 8.5-8.8 by using 5 parts by weight of pH regulator; (5) adding a polishing agent: adding N parts by weight of deionized water serving as a polishing agent into the solution after the pH adjustment step; (6) and (3) filtering: and repeatedly filtering the solution after the step of adding the polishing agent for more than 3 times, wherein the solution obtained after filtering is the nano colloid organic composite polishing solution.
Preferably, the method for preparing a nano-colloid organic composite polishing solution provided by the embodiment of the invention further comprises the step (7) of sealing: and storing the nano colloid organic composite polishing solution obtained after the filtering step in a PE plastic bucket for sealing and storage.
Preferably, the dispersion method in the step (1) and the step (2) is ultrasonic vibration dispersion, and the ultrasonic vibration frequency is 270 KHz.
The embodiment of the invention also provides a method for polishing thallium-doped cesium iodide crystals by using the nano colloidal organic composite polishing solution prepared by the method, which comprises the following steps:
and (3) polishing the thallium-doped cesium iodide crystal by using the nano colloid organic composite polishing solution, wherein the polishing pressure is set to be 0.05MP, and the polishing time is set to be 10min, so that the thallium-doped cesium iodide crystal with the surface roughness of less than 10nm is obtained.
The novel nano-colloid organic composite polishing solution can be prepared based on the method provided by the embodiment of the invention, and when the nano-colloid organic composite polishing solution is used for polishing the thallium-doped cesium iodide crystal, the thallium-doped cesium iodide crystal with the surface roughness of less than 10nm can be obtained, so that the problem of overlarge surface roughness after the thallium-doped cesium iodide crystal in the prior art is solved.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a nano-colloid organic composite polishing solution according to an embodiment of the present invention.
Fig. 2 shows the surface morphology of a thallium-doped cesium iodide crystal obtained after polishing the thallium-doped cesium iodide crystal with the polishing solution prepared in example 1 of the present invention.
Detailed Description
In the drawings, the same or similar reference numerals are used to denote the same or similar elements or elements having the same or similar functions. Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
In the description of the present invention, the terms "central", "longitudinal", "lateral", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and therefore, should not be construed as limiting the scope of the present invention.
The embodiment of the invention provides a method for preparing a nano-colloid organic composite polishing solution, which is prepared from the following raw materials in parts by weight:
ethylene glycol ethyl ester: 80 parts by weight of a water-soluble polymer,
nano silicon dioxide: 5 parts by weight of a reaction product of (B),
surfactant (b): m is the weight portion of the compound (I),
dispersing agent: 1 part by weight of a reaction product of (B),
deionized water: n is the weight portion of N,
a stabilizer: 2 parts by weight of a reaction product of (B),
pH regulator: 5 parts by weight of a reaction product of (B),
wherein M is 2-6, N is 1-5, and the raw materials are allowed to have an error within 0.1 weight part.
As shown in fig. 1, the method for preparing the nano-colloid organic composite polishing solution by using the raw materials comprises the following steps:
Preferably, the method further comprises a step 107 of sealing: and storing the nano colloid organic composite polishing solution obtained after the filtering step in a PE plastic bucket for sealing and storage.
The embodiment of the invention also provides a method for polishing thallium-doped cesium iodide crystals by using the nano-colloid organic composite polishing solution prepared by the method shown in fig. 1, which comprises the following steps:
and (3) polishing the thallium-doped cesium iodide crystal by using the nano colloid organic composite polishing solution, wherein the polishing pressure is set to be 0.05MP, and the polishing time is set to be 10min, so that the thallium-doped cesium iodide crystal with the surface roughness of less than 10nm is obtained.
The method provided by the invention is further described below by means of specific examples.
Example 1
In the method for preparing a nano-colloid organic composite polishing solution provided in this example, the following raw materials are used: 80 parts of ethylene glycol ethyl ester, 5 parts of nano silicon dioxide, 5 parts of surfactant, 1 part of dispersant, 2 parts of deionized water, 2 parts of stabilizer and 5 parts of pH regulator.
Specifically, the raw material preparation work includes: 800g of ethylene glycol ethyl ester, 50g of nano silicon dioxide, 25g of surfactant sodium hexametaphosphate, 25g of potassium chloride, 10g of dispersant acrylic polyester copolymer resin, 20g of deionized water, 20g of stabilizer, 25g of pH regulator 5% sodium hydroxide solution and 25g of 5% hydrochloric acid solution are weighed for later use.
The method for preparing the nano-colloid organic composite polishing solution provided by the embodiment comprises the following steps:
(1) surface activation: placing 25g of surfactant sodium hexametaphosphate and 25g of potassium chloride in 50g of nano silicon dioxide, ultrasonically dispersing for 0.5h, and standing for 15 h.
(2) Mixing organic solvents: adding 800g of ethylene glycol ethyl ester into the nano silicon dioxide after surface activation, and performing ultrasonic dispersion, wherein the ultrasonic vibration time is more than 30 minutes.
(3) And (3) stabilizing and curing: 10g of dispersant acrylic polyester copolymer resin and 20g of stabilizer are added to the solution obtained in the step (2) in sequence.
(4) Adjusting the pH value: and (3) adjusting the pH value of the solution obtained in the step (3) to 8.5-8.8 by using 25g of a pH adjusting agent 5% sodium hydroxide solution and 25g of a 5% hydrochloric acid solution.
(5) Polishing agent (water): to the solution obtained in (4), 20g of deionized water was added.
(6) And (3) filtering: repeatedly filtering the solution obtained in the step (5) for more than 3 times.
(7) Sealing and storing: and (4) taking the solution obtained by filtering in the step (6) as nano-colloid organic composite polishing solution, sealing and storing in a PE plastic barrel, wherein the polishing solution is the nano-colloid organic composite polishing solution which can be used for ultra-smooth dissolution and polishing of thallium-doped cesium iodide crystals.
The rice colloid organic composite polishing solution prepared by the embodiment has the advantages of uniform appearance, good dispersibility, difficult aggregation of particles, and difficult sedimentation after long-term storage.
Fig. 2 is a surface topography of a thallium-doped cesium iodide crystal obtained by polishing a thallium-doped cesium iodide crystal with the polishing solution prepared in this example. Wherein, each expression has the following corresponding meaning:
surface Map: surface topography map
3D Model: three-dimensional topography map
PV: peak to valley value
rms: root mean square value
Ra: roughness of
Size X: dimension in X direction
Size Y: dimension in Y direction
Removed: removal of the item Plane: least squares fitting plane
Trimming: de-bounding
Filter High wavelet: upper cut-off wavelength
Filter Low wavelet: lower cut-off wavelength
Surface Profile: line cutting diagram
Height: height
Profile State: transversal state
Intensity Map: and (6) actually measuring the light intensity distribution diagram.
As can be seen from FIG. 2, the roughness Ra of the polished surface of the thallium-doped cesium iodide crystal was 8.759 nm. Compared with the polishing by using the common polishing solution, the defects on the surface of the thallium-doped cesium iodide crystal are effectively removed, no new surface defects are introduced, and the surface roughness is superior to 10 nm.
Example 2
In the method for preparing a nano-colloid organic composite polishing solution provided in this example, the following raw materials are used: 80 parts of ethylene glycol ethyl ester, 5 parts of nano silicon dioxide, 6 parts of surfactant, 1 part of dispersant, 1 part of deionized water, 2 parts of stabilizer and 5 parts of pH regulator.
Specifically, the raw material preparation work includes: 800g of ethylene glycol ethyl ester, 50g of nano silicon dioxide, 30g of surfactant sodium hexametaphosphate, 30g of potassium chloride, 10g of dispersant acrylic polyester copolymer resin, 10g of deionized water, 20g of stabilizer, 25g of pH regulator 5% sodium hydroxide solution and 25g of 5% hydrochloric acid solution are weighed for later use.
The method for preparing the nano-colloid organic composite polishing solution provided by the embodiment comprises the following steps:
(1) surface activation: 30g of sodium hexametaphosphate as a surfactant and 30g of potassium chloride are placed in 50g of nano silicon dioxide, ultrasonic dispersion is carried out for 0.5h, and standing is carried out for 15 h.
(2) Mixing organic solvents: adding 800g of ethylene glycol ethyl ester into the nano silicon dioxide after surface activation, and performing ultrasonic dispersion, wherein the ultrasonic vibration time is more than 30 minutes.
(3) And (3) stabilizing and curing: 10g of dispersant acrylic polyester copolymer resin and 20g of stabilizer are added to the solution obtained in the step (2) in sequence.
(4) Adjusting the pH value: and (3) adjusting the pH value of the solution obtained in the step (3) to 8.5-8.8 by using 25g of a pH adjusting agent 5% sodium hydroxide solution and 25g of a 5% hydrochloric acid solution.
(5) Polishing agent (water): to the solution obtained in (4), 10g of deionized water was added.
(6) And (3) filtering: repeatedly filtering the solution obtained in the step (5) for more than 3 times.
(7) Sealing and storing: and (4) taking the solution obtained by filtering in the step (6) as nano-colloid organic composite polishing solution, sealing and storing in a PE plastic barrel, wherein the obtained polishing solution is the nano-colloid organic composite polishing solution which can be used for ultra-smooth dissolving and polishing of thallium-doped cesium iodide crystals.
When the polishing solution prepared by the embodiment is used for polishing the thallium-doped cesium iodide crystal, the defects on the surface of the thallium-doped cesium iodide crystal are effectively removed, no new surface defects are introduced, and the surface roughness can be better than 10 nm.
Example 3
In the method for preparing a nano-colloid organic composite polishing solution provided in this example, the following raw materials are used: 80 parts of ethylene glycol ethyl ester, 5 parts of nano silicon dioxide, 2 parts of surfactant, 1 part of dispersant, 5 parts of deionized water, 2 parts of stabilizer and 5 parts of pH regulator.
Specifically, the raw material preparation work includes: 800g of ethylene glycol ethyl ester, 50g of nano silicon dioxide, 10g of surfactant sodium hexametaphosphate, 10g of potassium chloride, 10g of dispersant acrylic polyester copolymer resin, 50g of deionized water, 20g of stabilizer, 25g of pH regulator 5% sodium hydroxide solution and 25g of 5% hydrochloric acid solution are weighed for later use.
The method for preparing the nano-colloid organic composite polishing solution provided by the embodiment comprises the following steps:
(1) surface activation: 10g of sodium hexametaphosphate as a surfactant and 10g of potassium chloride are placed in 50g of nano silicon dioxide, ultrasonic dispersion is carried out for 0.5h, and standing is carried out for 15 h.
(2) Mixing organic solvents: adding 800g of ethylene glycol ethyl ester into the nano silicon dioxide after surface activation, and performing ultrasonic dispersion, wherein the ultrasonic vibration time is more than 30 minutes.
(3) And (3) stabilizing and curing: 10g of dispersant acrylic polyester copolymer resin and 20g of stabilizer are added to the solution obtained in the step (2) in sequence.
(4) Adjusting the pH value: and (3) adjusting the pH value of the solution obtained in the step (3) to 8.5-8.8 by using 25g of a pH adjusting agent 5% sodium hydroxide solution and 25g of a 5% hydrochloric acid solution.
(5) Polishing agent (water): to the solution obtained in (4), 50g of deionized water was added.
(6) And (3) filtering: repeatedly filtering the solution obtained in the step (5) for more than 3 times.
(7) Sealing and storing: and (4) taking the solution obtained by filtering in the step (6) as nano-colloid organic composite polishing solution, sealing and storing in a PE plastic barrel, wherein the obtained polishing solution is the nano-colloid organic composite polishing solution which can be used for ultra-smooth dissolving and polishing of thallium-doped cesium iodide crystals.
When the polishing solution prepared by the embodiment is used for polishing the thallium-doped cesium iodide crystal, the defects on the surface of the thallium-doped cesium iodide crystal are effectively removed, no new surface defects are introduced, and the surface roughness can be better than 10 nm.
Finally, it should be pointed out that: the above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Those of ordinary skill in the art will understand that: modifications can be made to the technical solutions described in the foregoing embodiments, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The method for preparing the nano-colloid organic composite polishing solution is characterized by preparing the nano-colloid organic composite polishing solution from the following raw materials in parts by weight:
ethylene glycol ethyl ester: 80 parts by weight of a water-soluble polymer,
nano silicon dioxide: 5 parts by weight of a reaction product of (B),
surfactant (b): m is the weight portion of the compound (I),
dispersing agent: 1 part by weight of a reaction product of (B),
deionized water: n is the weight portion of N,
a stabilizer: 2 parts by weight of a reaction product of (B),
pH regulator: 5 parts by weight of a reaction product of (B),
wherein M is 2-6, N is 1-5, and the raw materials are allowed to have an error within 0.1 weight part;
the nano colloid organic composite polishing solution is prepared by the following steps:
(1) surface activation: placing the surfactant M in parts by weight into the nano silicon dioxide 5 in parts by weight for ultrasonic dispersion, and standing for more than 10 hours; (2) mixing organic solvents: adding 80 parts by weight of organic solvent of ethylene glycol ethyl ester into the nano silicon dioxide after surface activation, and performing ultrasonic dispersion for more than 30 minutes; (3) and (3) stabilizing and curing: sequentially adding 1 part by weight of dispersant and 2 parts by weight of stabilizer into the solution obtained in the step of mixing the organic solvent; (4) adjusting the pH value: adjusting the pH value of the solution after the stabilizing and curing step to 8.5-8.8 by using 5 parts by weight of pH regulator; (5) adding a polishing agent: adding N parts by weight of deionized water serving as a polishing agent into the solution after the pH adjustment step; (6) and (3) filtering: and repeatedly filtering the solution after the step of adding the polishing agent for more than 3 times, wherein the solution obtained after filtering is the nano colloid organic composite polishing solution.
2. The method of preparing a nanocolloid organic composite polishing solution according to claim 1, wherein M is 5 and N is 2.
3. The method of preparing a nano-colloidal organic composite polishing solution according to claim 1, wherein the nano-silica is a particle having an average particle diameter of 50 nm.
4. The method of preparing a nanocolloid organic composite polishing solution according to claim 1, wherein the surfactant comprises M/2 parts by weight of potassium hexametaphosphate and M/2 parts by weight of sodium chloride.
5. The method of preparing a nano-colloidal organic composite polishing solution according to claim 1, wherein the stabilizer is 2 parts by weight of acrylic polyester copolymer resin.
6. The method of preparing a nano-colloidal organic composite polishing solution according to claim 1, wherein the pH adjustor is 2.5 parts by mass of a sodium hydroxide solution and 2.5 parts by mass of a dilute hydrochloric acid solution.
7. The method for preparing a nano-colloidal organic composite polishing solution according to claim 1, further comprising the step of (7) sealing: and storing the nano colloid organic composite polishing solution obtained after the filtering step in a PE plastic bucket for sealing and storage.
8. The method for preparing a nano-colloid organic composite polishing solution according to claim 1, wherein the dispersion method in the step (1) and the step (2) is ultrasonic vibration dispersion, and the ultrasonic vibration frequency is 270 KHz.
9. A method for polishing thallium-doped cesium iodide crystals using the nanocolloid organic composite polishing solution prepared by the method for preparing a nanocolloid organic composite polishing solution according to claim 1, comprising:
and (3) polishing the thallium-doped cesium iodide crystal by using the nano colloid organic composite polishing solution, wherein the polishing pressure is set to be 0.05MP, and the polishing time is set to be 10min, so that the thallium-doped cesium iodide crystal with the surface roughness of less than 10nm is obtained.
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| CN1858134A (en) * | 2006-05-31 | 2006-11-08 | 河北工业大学 | Chemical and mechanical water-free polishing liquid for lithium-cessium borate crystal and leveling method |
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| CN1858134A (en) * | 2006-05-31 | 2006-11-08 | 河北工业大学 | Chemical and mechanical water-free polishing liquid for lithium-cessium borate crystal and leveling method |
| CN107129762A (en) * | 2017-05-12 | 2017-09-05 | 江南大学 | A kind of polishing fluid of carborundum chemically mechanical polishing and preparation method thereof |
| CN107987731A (en) * | 2017-12-19 | 2018-05-04 | 北京航天赛德科技发展有限公司 | A kind of polishing fluid for sapphire 3D polishings and preparation method thereof |
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