CN110256969B - Blue glass fine polishing solution and preparation method thereof - Google Patents

Abstract

The invention discloses a blue glass fine polishing solution and a preparation method thereof, relating to the technical field of blue glass polishing material preparation; comprises the following components, by weight, 10-30 parts of zirconia slurry, 20-40 parts of zirconium carbonate slurry, 10-20 parts of silicon dioxide slurry, 1-2 parts of speed increasing agent, 0.5-1 part of surface modifier, 0.5-1 part of pH regulator, 0.5-4 parts of colorant, 0.5-1 part of suspending agent and 1-57 parts of water; the preparation steps are as follows: A. grinding the slurry; B. filtering the slurry; C. primary dispersion; D. and dispersing again. The polishing solution has the characteristics of good polishing effect, high polishing efficiency, no pollution to the environment and the like, and can be used for polishing sapphire wafers and also can be used for polishing in the fields of metal, ceramics, glass, resin, painted surfaces and the like.

Description

Blue glass fine polishing solution and preparation method thereof

Technical Field

The invention relates to the technical field of blue glass polishing material preparation, in particular to a blue glass fine polishing solution and a preparation method thereof.

Background

The demand of the current market on optical blue glass products is increased day by day, the requirement on blue glass polishing solution is higher and higher, the polishing solution needs to be environment-friendly, heavy metals cannot exceed the standard, and the blue glass has color requirements, and meanwhile, the blue glass needs to be scratched without scuffing, corrosion pits, white spots, white mist and the like on the surface, so that the abrasive mainly used for polishing the blue glass in the current market is cerium oxide, zirconium oxide, cerium zirconium composite abrasive and the like. Because the domestic zirconium oxide polishing solution is added with heavy metal iron powder as toner, the problems of serious environmental pollution and the like are caused, and other reasons, most of the domestic existing zirconium oxide polishing solution can not meet the processing requirements on blue glass; although the products imported from the United states and Japan can meet the requirements, the products are expensive, and the economic burden of enterprises is increased.

Chinese patent CN103450813A discloses a method for preparing iron-doped zirconia polishing solution, which is prepared from water-soluble inorganic zirconium salt, soluble ferric salt, alkali, zirconium carbonate, an auxiliary agent and a pH value regulator, and the preparation steps comprise: preparing materials, preparing symbiotic solution, preparing symbiotic precipitate, washing, drying, calcining, grinding, stirring and dispersing; the iron-doped zirconia polishing solution prepared by the method is suitable for the processing field of high-grade optical instruments, and particularly can be used for polishing soft glass.

Chinese patent CN103450815A discloses a zirconia polishing solution for processing optical glass and a preparation method thereof, wherein the polishing solution is prepared by mixing grinding particles, an inorganic additive, a pH regulator, an organic additive and deionized water in certain parts by weight. The polishing agent disclosed by the invention has the advantages that through reasonable matching of the zirconium oxide, the zirconium carbonate, the iron oxide and the inorganic additive, the polishing efficiency is improved, and meanwhile, the mechanical action of the grinding particles on the optical material is weakened, so that the polishing agent is particularly suitable for polishing soft materials.

Chinese patent CN104152054A discloses a method for preparing zirconia-based soft glass polishing solution, which comprises the following steps: (1) calcination, (2) specific surface test, (3) grinding, (4) screening, (5) solid content test, and (6) batching.

Chinese patent CN101649183 discloses a production process of zirconia grinding fluid, which comprises the following steps: adding zirconia powder into high-speed dispersed water according to the weight portion, then adding wetting dispersant, grinding aid, mixed lipid and alcohol, fully dispersing, then sending into a high-speed sand mill for sand milling, grinding the water caltrops of the zirconia powder into round spheres, and then adding iron powder for color adjustment.

Disclosure of Invention

The invention aims to provide a blue glass fine polishing solution which has good polishing effect, high polishing efficiency and no pollution to the environment, and a preparation method thereof.

In order to achieve the technical purpose, the invention adopts the technical scheme that the blue glass fine polishing solution comprises the following components in parts by weight:

zirconia slurry 10-30 zirconium carbonate slurry 20-40 silica slurry 10-20

Accelerator 1-2 surface modifier 0.5-1 pH regulator 0.5-1

Colorant 0.5-4 suspending agent 0.5-1 water 1-57.

The content of the zirconia slurry is 40%, the particle size is 100-900 nm, and the slurry is in a monoclinic crystal form.

The content of the zirconium carbonate slurry is 40%, the particle size is 100-900 nm, and the zirconium carbonate slurry is in an amorphous crystal form.

The silicon dioxide slurry is prepared by catalyzing, hydrolyzing and concentrating Tetraethoxysilane (TEOS), the content of the silicon dioxide slurry is 40%, the particle size of the silicon dioxide slurry is 120 nanometers, and the silicon dioxide slurry is in a silkworm shape.

(the method can adopt a preparation method of nano silicon dioxide disclosed in Chinese patent CN 108455620A).

The accelerator is formed by mixing one or more of molybdate, iridate, titanate and arsenate, and when the number of the accelerator is more than two, the proportion of each component is equal parts by weight.

The surface modifier is formed by mixing one or more of BTA, organic amine ester TPP, BYK-402, ethyl titanate, butyl titanate and propyl titanate, and when the number of the BTA, the organic amine ester TPP, the BYK-402, the ethyl titanate, the butyl titanate and the propyl titanate is more than two, the proportion of each component is equal parts by weight.

The pH regulator is formed by mixing one or more of glycine, citric acid, meta-aluminate, acetic acid and hydroxide, and when the pH regulator is more than two, the proportion of each component is equal parts by weight.

The colorant is prepared by mixing one or more of carmine, amaranth, beet red, monascus red and methyl red, and when the colorant is more than two, the proportion of each component is equal parts by weight.

The suspending agent is formed by mixing one or more of 5040 dispersing agent, polymerized vegetable fat PT-11, polycarboxylate, NNO dispersing agent and liquid carbomer SF-1, and when the number of the dispersing agent is more than two, the proportion of the components is equal parts by weight.

Meanwhile, a preparation method of the blue glass fine polishing solution is also provided, and the preparation method comprises the following steps:

A. grinding the slurry: firstly, grinding zirconium oxide and zirconium carbonate to obtain mixed slurry with the particle size of 100-900 nm by using a sand mill;

B. filtering the slurry: filtering the mixed slurry by adopting a 2000-mesh screen to remove large-particle impurities in the mixed slurry to obtain filtered mixed slurry;

C. primary dispersion: then placing the filtered mixed slurry into a closed high-speed dispersion tank, adding a speed increasing agent and a suspending agent, and dispersing at high speed for 20min at the rotation speed of 1200-1500 rpm;

D. and (3) re-dispersing: and sequentially adding the silicon dioxide slurry, the surface modifier, the colorant and the pH regulator into the closed high-speed dispersion tank, and continuously dispersing at the rotation speed of 1800 plus 2000rpm for 30min to obtain the blue glass fine polishing solution.

The weight units used above may be in grams, kilograms or tons, or other weight units.

The blue glass fine polishing solution and the preparation method thereof are applied to blue glass and a precise optical soft material polishing process, and the scratches caused by the grinding materials are solved by strictly controlling the particle sizes of the zirconia and the zirconium carbonate slurry. Meanwhile, the added accelerator and the silkworm-shaped silicon dioxide slurry enable the fine polishing liquid to chemically react with the surface of the blue glass in the polishing process, so that the polishing process is accelerated, and the polishing speed is improved. The added surface modifier solves the problems of surface arable ratio, corrosion pits, white spots, white fog and the like. The added natural colorant avoids the pollution of heavy metal Fe powder to the environment, improves the environmental protection problem and can meet the color requirement of customers on the polishing solution.

Detailed Description

The present invention will be further described with reference to the following examples. The following description is given by way of example, and the scope of the invention should not be limited thereto.

The blue glass fine polishing solution comprises the following components in parts by weight: 10-30 parts of zirconia slurry, 20-40 parts of zirconium carbonate slurry, 10-20 parts of silicon dioxide slurry, 1-2 parts of speed increaser, 0.5-1 part of surface modifier, 0.5-1 part of pH regulator, 0.5-4 parts of colorant, 0.5-1 part of suspending agent and 1-57 parts of water. Wherein, the content of the zirconia sizing agent is 40 percent, the grain diameter is 100-900 nanometers, and the crystal is monoclinic. The content of the zirconium carbonate slurry is 40 percent, the particle size is 100-900 nm, and the zirconium carbonate slurry is in an amorphous crystal form. The silicon dioxide slurry is prepared by catalyzing, hydrolyzing and concentrating Tetraethoxysilane (TEOS), the content of the silicon dioxide slurry is 40%, the particle size of the silicon dioxide slurry is 120 nanometers, and the silicon dioxide slurry is in a silkworm shape. The accelerator is prepared by mixing one or more of molybdate, iridate, titanate and arsenate. The surface modifier is one or more of BTA, organic amine ester TPP, BYK-402, ethyl titanate, butyl titanate or propyl titanate. The pH regulator is prepared by mixing one or more of glycine, citric acid, meta-aluminate, acetic acid and hydroxide. The colorant is prepared by mixing one or more of carmine, amaranth, beet red, red rice red and methyl red. The suspending agent is prepared by mixing one or more of 5040 dispersant, polymerized vegetable fat PT-11, polycarboxylate, NNO dispersant and liquid carbomer SF-1.

The preparation method of the blue glass fine polishing solution comprises the following steps:

A. grinding the slurry: firstly, grinding zirconium oxide and zirconium carbonate to obtain mixed slurry with the particle size of 100-900 nm by using a sand mill;

B. filtering the slurry: filtering the mixed slurry by adopting a 2000-mesh screen to remove large-particle impurities in the mixed slurry to obtain filtered mixed slurry;

C. primary dispersion: then placing the filtered mixed slurry into a closed high-speed dispersion tank, adding a speed increasing agent and a suspending agent, and dispersing at high speed for 20min at the rotation speed of 1200-1500 rpm;

D. and (3) re-dispersing: and sequentially adding the silicon dioxide slurry, the surface modifier, the colorant and the pH regulator into the closed high-speed dispersion tank, and continuously dispersing at the rotation speed of 1800 plus 2000rpm for 30min to obtain the blue glass fine polishing solution.

The following table shows the specific components (parts by weight) of each example.

The following is the polishing process conditions of the blue glass fine polishing solution prepared in the embodiment 1 of the invention, which are applied in the experimental process of polishing the appearance rate, scratch rate and removal rate of the surface of the blue glass wafer:

polishing machine: presi 1500;

polished wafer: 6 x 4cm of blue glass;

number of wafers polished: 15 pics;

unit grinding pressure: 100g/cm²；

Double-side polishing speed ratio: 10:20:5: 1;

polishing time: 5 min;

flow rate of polishing solution: 200-400 ml/min;

after polishing, the wafer is subjected to ultrasonic cleaning, drying and thickness measurement. Measuring the thickness difference of the blue glass wafer by a thickness gauge to obtain the removal rate, measuring all wafers polished by 15pics, and obtaining the average removal rate; and testing by using a strong light lamp, detecting all wafers polished by 15pics, and obtaining the appearance rate and the scratch rate of the surface arabic ratio.

The detection result shows that after the blue glass wafer is polished by the fine polishing solution, the average removal rate is 6.5 mu m/min, the surface A/L ratio occurrence rate is 0%, the surface scratch rate is 0.01%, the requirements of the blue glass polishing process are completely met, and the processing cost is greatly saved.

The effects of the remaining examples are shown in the following table:

	apparent arrobis rate of occurrence	Average removal rate	Rate of surface scratching
				Example 2	0％	6.5μm/min	0.02％
Example 3	0％	6.8μm/min	0.01％
				Example 4	0％	6.6μm/min	0％
Example 5	0％	6.4μm/min	0％
				Example 6	0％	6.3μm/min	0.01％
Example 7	0％	6.2μm/min	0.01％
				Example 8	0％	6.7μm/min	0.03％
Example 9	0％	6.6μm/min	0％
				Example 10	0％	6.9μm/min	0.02％

As can be seen from the data of the above examples, the appearance rate of the surface Arabic ratio is 0, the average removal rate is 6.2-6.9 μm/min, and the surface scratch rate is less than or equal to 0.03%. Compared with the prior art, the surface scratch rate is obviously reduced, the polishing efficiency is greatly improved, the processing cost is reduced, and the pollution of heavy metal Fe to the environment is also reduced.

The blue glass fine polishing solution is suitable for the precise polishing of optical blue glass and optical filters.

Claims (5)

1. The blue glass fine polishing solution is characterized by comprising the following components in parts by weight:

zirconia slurry 10-30 zirconium carbonate slurry 20-40 silica slurry 10-20

Accelerator 1-2 surface modifier 0.5-1 pH regulator 0.5-1

Colorant 0.5-4 suspending agent 0.5-1 water 1-57;

the silicon dioxide slurry is prepared by catalyzing, hydrolyzing and concentrating Tetraethoxysilane (TEOS), the content of the silicon dioxide slurry is 40%, the particle size of the silicon dioxide slurry is 120 nanometers, and the silicon dioxide slurry is in a silkworm shape;

the accelerator is formed by mixing one or more of molybdate, iridate and arsenate, and when the number of the accelerator is more than two, the proportion of each component is equal parts by weight;

the surface modifier is formed by mixing one or more of BTA, organic amine ester TPP, BYK-402, ethyl titanate, butyl titanate and propyl titanate, and when the number of the BTA, the organic amine ester TPP, the BYK-402, the ethyl titanate, the butyl titanate and the propyl titanate is more than two, the proportion of each component is equal parts by weight;

the pH regulator is formed by mixing one or more of glycine, citric acid, meta-aluminate and acetic acid, and when the pH regulator is more than two, the proportion of each component is equal parts by weight;

the suspending agent is formed by mixing one or more of 5040 dispersing agent, polymerized vegetable fat PT-11, NNO dispersing agent and liquid carbomer SF-1, and when the number of the dispersing agent is more than two, the proportion of each component is equal parts by weight.

2. The blue glass finishing polishing liquid according to claim 1, wherein: the content of the zirconia slurry is 40%, the particle size is 100-900 nm, and the slurry is in a monoclinic crystal form.

3. The blue glass finishing polishing liquid according to claim 1, wherein: the content of the zirconium carbonate slurry is 40%, the particle size is 100-900 nm, and the zirconium carbonate slurry is in an amorphous crystal form.

4. The blue glass finishing polishing liquid according to claim 1, wherein: the colorant is prepared by mixing one or more of carmine, amaranth, beet red, monascus red and methyl red, and when the colorant is more than two, the proportion of each component is equal parts by weight.

5. A method for preparing a blue glass finishing polishing solution according to any one of claims 1 to 4, which comprises the following steps:

A. grinding the slurry: firstly, grinding zirconium oxide and zirconium carbonate to obtain mixed slurry with the particle size of 100-900 nm by using a sand mill;

B. filtering the slurry: filtering the mixed slurry by adopting a 2000-mesh screen to remove large-particle impurities in the mixed slurry to obtain filtered mixed slurry;

C. primary dispersion: then placing the filtered mixed slurry into a closed high-speed dispersion tank, adding a speed increasing agent and a suspending agent, and dispersing at high speed for 20min at the rotation speed of 1200-1500 rpm;

D. and (3) re-dispersing: and sequentially adding the silicon dioxide slurry, the surface modifier, the colorant and the pH regulator into the closed high-speed dispersion tank, and continuously dispersing at the rotation speed of 1800 plus 2000rpm for 30min to obtain the blue glass fine polishing solution.