CN103145453A - Praseodymium yellow material for ceramic ink and preparation method thereof - Google Patents
Praseodymium yellow material for ceramic ink and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a praseodymium yellow material for ceramic ink. The preparation method comprises the following steps of: 1) preparing crystal seeds: uniformly mixing 50-60 parts by weight of zirconium oxide, 25-35 parts by weight of quartz powder, 3-8 parts by weight of praseodymium oxide and 1-5 parts by weight of mineralizer to obtain a mixture; mixing 100 parts by weight of the mixture with 450-550 parts by weight of agate ball stone and 54-66 parts by weight of water, grinding till the particle size achieves D90 which is not more than 5mu m, further drying and screening the mixture after grinding, then replenishing the mineralizer accounting for 3%-5% of the total weight, uniformly mixing, and then calcining, grinding and drying to obtain the crystal seeds; and 2) preparing a pigment: uniformly mixing the zirconium oxide, the quartz powder and the praseodymium oxide according to the molar ratio of (0.9-1.1): (0.9-1.1): (0.03-0.15), further adding the crystal seeds accounting for 1%-5% of the total weight and the mineralizer accounting for 3%-5% of the total weight, uniformly mixing, and then calcining, grinding and drying to obtain the praseodymium yellow material. The praseodymium yellow material disclosed by the invention has high coloring intensity and high product stability, and can achieve the requirement of the coloring intensity; and simultaneously, the process is simple and convenient, and the requirements for operation conditions are not high.
Description
Technical field
The present invention relates to be applied to the preparation method of the pr-yellow material of ceramic ink, relate in particular to a kind of ceramic ink with pr-yellow material and preparation method thereof.
Background technology
The traditional method of the praseodymium yellow pigments that the preparation ceramic ink is used is solid reaction process, and it is mixed in proportion with ground zirconium white, silicon-dioxide, Praseodymium trioxide, and directly high temperature sintering obtains.But because this method need to be carried out under high temperature (temperature〉1600 ℃), and high temperature can make the diameter of particle of acquisition excessive, and toner high temperature, poor chemical stability, and coloring intensity is also inadequate.In prior art, in order to improve the coloring intensity of colorant after levigate, some investigators and manufacturer study on synthetic method and attempt, but these synthetic methods technically or operational condition on requirement all very high, some needs specific equipment, perhaps needs very strict synthesis condition, and the industrialization aim of " easy and simple to handle; that cost is low, efficient is high " that follow this and this area is not inconsistent.
This shows how to carry out technological improvement, a kind of ceramic ink preparation method with pr-yellow material be provided, to operational condition require low, and the ceramic ink that obtains with pr-yellow material after post-production, can keep coloring intensity preferably.
Summary of the invention
The object of the invention is to, the preparation method of a kind of ceramic ink with pr-yellow material is provided, simple process, the ceramic ink that makes after the processing in later stage, can keep coloring intensity preferably with pr-yellow material.Based on this, the present invention also provides a kind of ceramic ink pr-yellow material.
For solving above technical problem, technical scheme of the present invention is:
A kind of ceramic ink comprises the steps: with the preparation method of pr-yellow material
1) crystal seed preparation
The zirconium white of 50～60 weight parts, the silica powder of 25～35 weight parts, the Praseodymium trioxide of 3～8 weight parts, the mineralizer of 1～5 weight part are mixed, obtain mixture; The mixture of 100 weight parts is mixed, grinds with the agate ballstone of 450～550 weight parts, the water of 54～66 weight parts, until particle diameter reaches D90≤5 μ m, mixture after grinding again carries out drying, sieves, then replenish and add the mineralizer mixing that accounts for gross weight 3%～5%, then calcine, grind, drying, obtain crystal seed;
2) colorant preparation
With zirconium white, silica powder, Praseodymium trioxide (0.9～1.1) in molar ratio: (0.9～1.1): (0.03-0.15) mix, the mineralizer mixing that adds again the crystal seed that accounts for gross weight 1%-5% and account for gross weight 3%～5%, then calcine, grind, drying, and get final product.
Preferably, step 2) in, zirconium white, silica powder, Praseodymium trioxide first process before mixing to fineness be 5 μ m-10 μ m.
Preferably, the mixture in step 1) is dry in the environment of 150 ℃ of following temperature, and makes dried mixture water ratio＜0.5%.
Preferably, described mineralizer is halogenide.
Preferably, described mineralizer is any one or the two or more mixture in lithium fluoride, sodium-chlor, Repone K, Sodium Fluoride.
Preferably, the processing condition of calcining in step 1) are: calcining temperature rises to 300 ℃, intensification 2H from 25 ℃; Calcining temperature rises to 600 ℃, intensification 2H from 300 ℃; Calcining temperature rises to 960 ℃, intensification 4H from 600 ℃; Then calcining temperature lowers the temperature naturally at 960 ℃ of lower constant temperature 4H.
Preferably, step 2), the processing condition of calcining are: calcining temperature rises to 300 ℃, intensification 2H from 25 ℃; Calcining temperature rises to 600 ℃, intensification 2H from 300 ℃; Calcining temperature rises to 960 ℃, intensification 4H from 600 ℃; Then calcining temperature lowers the temperature naturally at 960 ℃ of lower constant temperature 4H.
Preferably, in step 1), the crystal seed that obtains after calcining is ground, make fineness to 3 μ m～5 μ m.
Preferably, in step 1), grind to be specially and use ball mill ball milling 70～82 hours.
A kind of ceramic ink pr-yellow material of the present invention is made by aforesaid preparation method.
The ceramic ink of the present invention preparation method of pr-yellow material, owing to selecting the tiny raw material that possesses the crystallite phase of particle, make the colorant that obtains after post-production, coloring intensity improves, product stability improves, and can reach the coloring intensity requirement of ceramic ink; Owing to first making crystal seed, the crystal seed that making is obtained mixes to synthesize colorant with raw material, and institute is so that simple process, and the synthetic difficulty of colorant is low, less demanding to operational condition, and the operating speed of whole technique is fast.
Embodiment
In order to make those skilled in the art understand better technical scheme of the present invention, the present invention is described in further detail below by specific embodiment.
In view of existing ceramic ink colorant preparation method, its raw material situation that color development can shoal after levigate processing, the invention provides a kind of ceramic ink crystallite synthesis preparation method of pr-yellow material, by adopting the tiny starting material that possess microlitic structure of particle to come synthesize ceramic ink colorant, adopt crystal seed to introduce technology, guarantee resultant velocity and high-temperature stability with this.
At first, preparation is during crystal seed, fineness activity and the mixture homogeneity of the mode feed change by the ball milling refinement.Because be to be difficult to evenly spread in system go less than the material that accounts for gross weight 1% when pressed powder mixes, the material such as praseodymium compound is evenly distributed the mode by the ball milling refinement and fineness reaches refinement.According to solid state reaction mechanism, high temperature solid state reaction more easily occurs through calcining in the uniform material of altitude distribution, so more easily form aspidelite type carrier, the praseodymium compound enters in lattice more and goes simultaneously, product after calcining makes particle diameter D90 reach 3 μ m～5 μ m through refinement, as crystal seed.
secondly, in the time of the preparation colorant, adopt fineness D90 to reach the raw material of 5 μ m-10 μ m, material fineness is enough thin, be conducive to the abundant mixing of solid powder, and during the raw material pyrolytic decomposition, can form more defect lattice, defective raw material lattice reactive behavior is very high, dissolve in for the synthetic and praseodymium compound of carrier that to form stable crystal in carrier highly beneficial, along with the praseodymium compound constantly is added in carrier, the color development of mineral constantly strengthens, stability also progressively improves (the zirconium silicate carrier is synthetic that more complete high thermal resistance is better), yellow value degree is higher, colour generation is just more stable.
Particularly, crystallite of the present invention is combined to ceramic ink and comprises two large steps with the preparation method of pr-yellow material, i.e. the preparation of synthetic, the colorant of crystal seed is specific as follows:
1, crystal seed preparation
The zirconium white of 50～60 weight parts, the silica powder of 25～35 weight parts, the Praseodymium trioxide of 3～8 weight parts, the mineralizer of 1～5 weight part are mixed, obtain mixture; The mixture of 100 weight parts is mixed, grinds with the agate ballstone of 450～550 weight parts, the water of 54～66 weight parts, until particle diameter reaches D90≤5um, mixture after grinding again carries out drying, sieves, then replenish and add the mineralizer mixing that accounts for gross weight 3%～5%, then calcine, grind, drying, obtain crystal seed;
The mineralizer here can adopt halogenide, can as lithium fluoride, sodium-chlor, Repone K, Sodium Fluoride etc.;
2, colorant preparation
With zirconium white, silica powder, Praseodymium trioxide (0.9～1.1) in molar ratio: (0.9～1.1): (0.03-0.15) mix, the mineralizer mixing that adds again the crystal seed that accounts for gross weight 1%-5% and account for gross weight 3%～5%, then calcine, grind, drying, and get final product.
By the ceramic ink pr-yellow material that above preparation method makes, its chemical formula is:
ZrO
2SiO
2Pr
6O
11, and have following characteristic:
Outward appearance: yellow powder;
Lightness: 35≤L≤52;
Form and aspect: 26≤a≤32;
Form and aspect: 20≤b≤55.
Be elaborated by the following examples:
Embodiment one
The ceramic ink of the present embodiment comprises the steps: with the preparation method of pr-yellow material
1, crystal seed preparation:
1) the 55:30:5:2 preparation by weight percentage of zirconium white, silica powder, Praseodymium trioxide, lithium fluoride is mixed, obtain mixture;
2) step 1) is obtained mixture and mix by weight 100:500:60 with agate ballstone, water, inserted the ball mill ball milling approximately 72 hours, after ball milling, particle diameter reaches D90≤5 μ m;
3) with step 2) mixture that obtains after ball milling is dry in the temperature environment below 150 ℃, makes dried mixture water ratio＜0.5%; Dry thing is crossed 325 eye mesh screens;
4) being 99% lithium fluoride micro mist with the mixture after above-mentioned sieving and mass concentration mixes and stirs by the mass ratio of 96.5:3.5;
5) said mixture is packed into potcal pot calcination, the processing condition of calcining are: 25 ℃-300 ℃, intensification 2H; 300 ℃-600 ℃, intensification 2H; 600 ℃-960 ℃, intensification 4H; 960 ℃ of constant temperature 4H, cooling naturally;
6) with above-mentioned calcined material ball milling, particle diameter D90 reaches 3 μ m-5 μ m, and dry (≤150 ℃) cross 325 eye mesh screens, are the crystal seed finished product, and are standby;
2, colorant preparation:
1) with matrix material: zirconium white, silica powder, Praseodymium trioxide 1:1:0.03 in molar ratio mix;
2) add crystal seed and the lithium fluoride that step 1 makes to mix, after mixing, crystal seed accounts for 2% of mixture total weight amount again, and lithium fluoride accounts for 3% of mixture total weight amount;
3) said mixture is packed into potcal pot calcination, the technique of calcining is: 25 ℃-300 ℃, intensification 2H; 300 ℃-600 ℃, intensification 2H; 600 ℃-960 ℃, intensification 4H; 960 ℃ of constant temperature 4H, cooling is unloaded below 200 ℃ naturally;
4) with above-mentioned calcined material ball milling, particle diameter D90 is controlled at 16 μ m～18 μ m, and dry (≤150 ℃) cross 250 eye mesh screens, namely get the pr-yellow material that ceramic ink is used.
The pr-yellow material that the above ceramic ink that obtains is used carries out fineness and color development detection, and detected result is as follows:
1, fineness test
The test the data obtained: the fineness of the pr-yellow material that ceramic ink is used is D90:17.35 μ m.
2, color development comparison and detection
The basic glaze formula of the glaze colours that the pr-yellow material that ceramic ink is used uses:
0.276K
2O 0.003Fe
2O
3 3.5SiO
2
0.066Na
2O 0.522Al
2O
3 0.658CaO
Add massfraction in the parent glaze and be the pr-yellow material that 5% ceramic ink of the present invention do not add crystal seed to make with pr-yellow material and prior art and do the color development contrast, be labeled as respectively A and B, temperature of glaze firing is 1100 ℃, and firing time is 60 minutes, soaking time 15-30 minute, the test color difference:
Test the data obtained: A sample: L:49.33 a:27.35 b:27.78
Test the data obtained: B sample: L:50.28 a:22.86 b:19.45
Dark by the pr-yellow material color development that adds crystal seed preparation in above data declaration the present embodiment, yellow value degree is high, and quality improves approximately 20%.
Embodiment two
The ceramic ink of the present embodiment comprises the steps: with the preparation method of pr-yellow material
1, crystal seed preparation:
1) the 50:35:7:3 preparation by weight percentage of zirconium white, silica powder, Praseodymium trioxide, lithium fluoride is mixed, obtain mixture;
2) press said mixture and mix by weight the weight ratio of 100:520:64 with agate ballstone and water, then used the ball mill ball milling approximately 78 hours, after ball milling, particle diameter reaches D90≤5 μ m;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio＜0.5%; Dry thing is crossed 325 eye mesh screens;
4) being 99% boric acid with the mixture after above-mentioned sieving and concentration mixes and stirs by the mass ratio of 95:5;
5) said mixture is packed into potcal pot calcination, the processing condition of calcining are: 25 ℃-300 ℃, intensification 2H; 300 ℃-600 ℃, intensification 2H; 600 ℃-960 ℃, intensification 4H; 960 ℃ of constant temperature 4H, cooling naturally;
6) with above-mentioned calcined material ball milling, particle diameter D90 reaches 3-5 μ m, and dry (≤150 ℃) cross 325 eye mesh screens, are the crystal seed finished product, and are standby;
2, colorant preparation:
1) with matrix material: zirconium white, silica powder, Praseodymium trioxide 1:1:0.1 in molar ratio mix;
2) crystal seed and the Sodium Fluoride that add step 1 to make add rear crystal seed gross weight to account for 4% of gross weight again.Sodium Fluoride accounts for 3% of gross weight;
3) said mixture is packed into potcal pot calcination: the processing condition of calcining are: 25 ℃-300 ℃, and intensification 2H; 300 ℃-600 ℃, intensification 2H; 600 ℃-960 ℃, intensification 4H; 960 ℃ of constant temperature 4H, cooling discharging below 200 ℃ naturally;
4) with above-mentioned calcined material ball milling, particle diameter D90 is controlled at 16 μ m～18 μ m, and dry (≤150 ℃) cross 250 eye mesh screens, namely get pr-yellow material.
The above ceramic ink that obtains is carried out fineness and color development detection with pr-yellow material, and detected result is as follows:
1, fineness test
The test the data obtained: the fineness of pr-yellow material is D90:17.35 μ m.
2, color development comparison and detection
The basic glaze formula of the glaze colours that pr-yellow material uses:
0.216K
2O 0.003Fe
2O
3 3.5SiO2
0.036Na
2O 0.622Al
2O
3 0.658CaO
The ceramic ink that adds massfraction in the parent glaze and be the present embodiment of 5% is with pr-yellow material and do not add the pr-yellow material of the prior art preparation of crystal seed to do the color development contrast, be labeled as respectively C and D, temperature of glaze firing is 1200 ℃, firing time is 60 minutes, soaking time 15-30 minute, the test color difference:
Test the data obtained: C sample: L:49.36 a:27.85 b:27.78.
Test the data obtained: D sample: L:53.89 a:15.75 b:28.31.
The pr-yellow material that above data declaration the present embodiment is used by the ceramic ink that adds the crystal seed preparation can be stablized color development in the applied at elevated temperature situation, synthesize more completely zirconium base pr-yellow material, resistance to elevated temperatures is good, and does not add the D sample color development of crystal seed preparation to fade in prior art, the color development poor stability.
Embodiment three
The ceramic ink of the present embodiment comprises the steps: with the preparation method of pr-yellow material
1, crystal seed preparation:
1) the 58:28:6:2 preparation by weight percentage of zirconium white, silica powder, Praseodymium trioxide, lithium fluoride is mixed;
2) press said mixture and agate ballstone and water and mix by the mass ratio of 100:450:56, with ball mill ball milling approximately 80 hours, after ball milling, particle diameter reached D90≤5 μ m;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio＜0.5%; Dry thing is crossed 325 eye mesh screens;
4) being 99% Sodium Fluoride with the mixture after above-mentioned sieving and concentration mixes and stirs by the mass ratio of 97:3;
5) said mixture is packed into potcal pot calcination, the processing condition of calcining are: 25 ℃-300 ℃, intensification 2H; 300 ℃-600 ℃, intensification 2H; 600 ℃-960 ℃, intensification 4H; 960 ℃ of constant temperature 4H, cooling naturally;
6) with above-mentioned calcined material ball milling, particle diameter D90 reaches 3-5 μ m, and dry (≤150 ℃) cross 325 eye mesh screens, are the crystal seed finished product, and are standby;
2, colorant preparation:
1) with matrix material: zirconium white, silica powder, Praseodymium trioxide 1:1:0.1 in molar ratio mix;
2) crystal seed and the sodium-chlor that add step 1 to make add rear crystal seed to account for 2% of gross weight again, and sodium-chlor accounts for 4% of gross weight;
3) said mixture is packed into 25 ℃-300 ℃ of potcal pot calcinations, intensification 2H; 300 ℃-600 ℃, intensification 2H; 600 ℃-960 ℃, intensification 4H; 960 ℃ of constant temperature 4H, cooling is unloaded below 200 ℃ naturally;
4) with above-mentioned calcined material ball milling, particle diameter D90 is controlled at 16 μ m～18 μ m, and dry (≤150 ℃) cross 250 eye mesh screens, namely get the ceramic ink pr-yellow material.
The above ceramic ink that obtains is carried out fineness and color development detection with pr-yellow material, and detected result is as follows:
1, fineness test
The test the data obtained: ceramic ink is D90:17.35 μ m with the fineness of pr-yellow material.
2, color development detects
The basic glaze formula of glaze colours that ceramic ink uses with pr-yellow material:
0.206K
2O 0.003Fe
2O
3 3.2SiO
2 0.712ZnO
0.036Na
2O 0.42Al
2O
3 0.621CaO
Adding massfraction in the parent glaze and be ceramic ink that ceramic ink that the present embodiment of 5% obtains makes with pr-yellow material (being labeled as E) and experimental example one does color development with pr-yellow material A and contrasts, temperature of glaze firing is 1100 ℃, firing time is 60 minutes, soaking time 15-30 minute, the test color difference:
Test the data obtained: E sample: L:47.18 a:28.36 b:36.54.
Test the data obtained: A sample: L:49.33 a:27.35 b:27.78
Can be found out by the color development data, the pr-yellow material that the preparation method of the present embodiment makes makes color development darker due to the consumption that has increased Praseodymium trioxide, can stablize color development under high-temperature condition, and color development is limpid simultaneously, yellow value degree is high.
Be below only the preferred embodiment of the present invention, should be pointed out that above-mentioned preferred implementation should not be considered as limitation of the present invention, protection scope of the present invention should be as the criterion with the claim limited range.For those skilled in the art, without departing from the spirit and scope of the present invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the preparation method of a ceramic ink use pr-yellow material, is characterized in that, comprises the steps:
1) crystal seed preparation
The zirconium white of 50～60 weight parts, the silica powder of 25～35 weight parts, the Praseodymium trioxide of 3～8 weight parts, the mineralizer of 1～5 weight part are mixed, obtain mixture; The mixture of 100 weight parts is mixed, grinds with the agate ballstone of 450～550 weight parts, the water of 54～66 weight parts, until particle diameter reaches D90≤5 μ m, mixture after grinding again carries out drying, sieves, then replenish and add the mineralizer mixing that accounts for gross weight 3%～5%, then calcine, grind, drying, obtain crystal seed;
2) colorant preparation
With zirconium white, silica powder, Praseodymium trioxide (0.9～1.1) in molar ratio: (0.9～1.1): (0.03-0.15) mix, the mineralizer mixing that adds again the crystal seed that accounts for gross weight 1%-5% and account for gross weight 3%～5%, then calcine, grind, drying, and get final product.
2. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that step 2) in, zirconium white, silica powder, Praseodymium trioxide first process before mixing to fineness be 5 μ m-10 μ m.
3. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that, the mixture in step 1) is dry in the environment of 150 ℃ of following temperature, and makes dried mixture water ratio＜0.5%.
4. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that, described mineralizer is halogenide.
5. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that, described mineralizer is any one or the two or more mixture in lithium fluoride, sodium-chlor, Repone K, Sodium Fluoride.
6. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that, the processing condition of calcining in step 1) are: calcining temperature rises to 300 ℃, intensification 2H from 25 ℃; Calcining temperature rises to 600 ℃, intensification 2H from 300 ℃; Calcining temperature rises to 960 ℃, intensification 4H from 600 ℃; Then calcining temperature lowers the temperature naturally at 960 ℃ of lower constant temperature 4H.
7. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that step 2) in the processing condition of calcining be: calcining temperature rises to 300 ℃, intensification 2H from 25 ℃; Calcining temperature rises to 600 ℃, intensification 2H from 300 ℃; Calcining temperature rises to 960 ℃, intensification 4H from 600 ℃; Then calcining temperature lowers the temperature naturally at 960 ℃ of lower constant temperature 4H.
8. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that, in step 1), the crystal seed that obtains after calcining is ground, and makes fineness to 3 μ m～5 μ m.
9. ceramic ink according to claim 1 with the preparation method of pr-yellow material, is characterized in that, in step 1), grinds to be specially and uses ball mill ball milling 70～82 hours.
10. a ceramic ink pr-yellow material, is characterized in that, made by the preparation method of claim 1～9 any one.
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| CN105198493A (en) * | 2015-10-09 | 2015-12-30 | 秦威 | Yellow pigment composition of ceramic ink and preparation method thereof |
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| CN109161227A (en) * | 2018-08-23 | 2019-01-08 | 佛山市三水区康立泰无机合成材料有限公司 | A kind of preparation method of the reddish brown colorant of ceramic ink jet |
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Application publication date: 20130612 |