CN105084375A - Submicron bismuth silicate powder for glass printing ink and preparation method - Google Patents
Submicron bismuth silicate powder for glass printing ink and preparation method Download PDFInfo
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- CN105084375A CN105084375A CN201510557585.1A CN201510557585A CN105084375A CN 105084375 A CN105084375 A CN 105084375A CN 201510557585 A CN201510557585 A CN 201510557585A CN 105084375 A CN105084375 A CN 105084375A
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- silicate powder
- bismuth silicate
- ball milling
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- submicron
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Abstract
The invention discloses submicron bismuth silicate powder for glass printing ink and a preparation method. The preparation method is characterized in that the powder is prepared from raw materials, namely, bismuth oxide (alpha-Bi2O3) and amorphous silica (SiO2), and the two raw materials are mechanically alloyed through high-energy ball milling. The particle size of the prepared bismuth silicate powder is in the submicron level, the bismuth silicate powder and raw materials such as boron oxide, lithium oxide and the like are further mechanically alloyed, then the mixture is mixed with an industrial pigment, and the high-quality bismuth silicate-based pigment for digital glass ink-jetting can be prepared. With the adoption of the preparation method of the bismuth silicate powder, the energy consumption is low, the emission is low, the pollution is avoided, and the product purity is high. The bismuth silicate powder can be applied to the field of digital glass ink-jetting and has broad application prospect in multiple fields such as the photovoltaic field, the information field, the environment field, the biomedicine field, the national defense field, the aviation field, the aerospace field and the like.
Description
Technical field
The invention belongs to glass ink-jet printing technology field, particularly a kind of glass ink submicron bismuth silicate powder and preparation method thereof.
Background technology
Bismuth silicate is a kind of broad-band gap, non-ferroelectric cube of semi-insulator of high resistivity, there is electric light simultaneously, photoconduction, Preset grating, piezoelectricity, acousto-optic, optically-active, the effects such as Faraday rotation, of many uses, can be used for preparing luminescent material, scintillation material, dielectric substance, photochromic glass, electronic ceramics, high-performance optical Photorefractive, high-temperature superconductor, a series of new high-tech material such as high-selectivity catalyst, can be applicable to general industry, information, environment, biomedical, national defence, aviation, multiple field such as space flight, it is the very promising multifunctional material of one.
Glass numerial code spray drawing printing technique as a kind of newly contactless, without pressure, printing technology without forme, pushed current glass fashion, personalization, art up, short run, multi-color, low-carbon environment-friendly development trend to a new height undoubtedly.But, a gordian technique of glass numerial code spray drawing printing technique is exactly the preparation of ink, the colorant of the glass ink on domestic market mainly tinbase, antimony base and zirconium base, also there is no the colorant of bismuthino, the application of colorant in glass ink field of bismuthino, what can make the more abundant image of glass shows concavo-convex texture, skin texture true to nature, soft texture, the ice-cold impression of breaking glass, form stereoscopic sensation, allow people experience more marvellous texture from vision and sense of touch.
For the preparation of bismuth silicate, CN10038071C provides one and prepares high purity bismuth silicate nano powder, first bismuth salt is dissolved in organic solvent, form bismuth-containing solution, silicoorganic compound are joined in bismuth-containing solution, abundant stirring, form uniform solution, atmospheric evaporation or negative pressure evaporation are adopted to colloidal sol, obtain dry precursor powder, finally in the environment of aerobic, precursor powder is sintered, in lower temperature with prepare purity and the good bismuth silicate nano powder of degree of crystallinity in the shorter time.But its shortcoming is that usual whole sol-gel process required time is longer, in normal needs a few week, is unfavorable for a large amount of production, and in gel, there is a large amount of micropore, will overflow again in drying process much gas and organism, and produce contraction.Patent CN102351202B also discloses a kind of preparation method of bismuth silicate powder, this method take dehydrated alcohol as ball-milling medium, by bismuth oxide and silicon oxide 6: 1 ~ 2: 3 ball milling 5 hours in molar ratio, be ball-milling medium again with dehydrated alcohol, by KCl and K2CO3 3: 5 ~ 5: 3 ball milling 5 hours in molar ratio, obtain KCl-K2CO3 composite salt; Then, by the bismuth oxide of drying and the compound of silicon oxide and KCl-K2CO3 composite salt with mass ratio 1: 4 ~ 4: 1 hand in mortar grind 30min again hand is ground after admixtion put into retort furnace, be incubated 0.5 ~ 5 hour under 630 DEG C ~ 750 DEG C conditions, take out, be cooled to room temperature; Finally, by the sample washed with de-ionized water post-drying of cooling, bismuth silicate powder is obtained, although this method employs the method for ball milling, but only serve the effect of mixing at mechanical milling process, raw material unrealized alloying, alloy process obtains by being incubated in retort furnace, and the impurity wherein contained needs to clean with deionized water, completely impurity can not be gone totally, and this preparation process program is loaded down with trivial details, energy consumption is high, cost is high, is unwell to batch production.
Summary of the invention
The object of the invention is the problem that bismuth silicate powder preparation is complicated, cost is high existed to overcome prior art, inventing the preparation method of the glass ink submicron bismuth silicate powder that a kind of speed is fast, cost is low.
One of technical scheme of the present invention is:
A preparation method for glass ink submicron bismuth silicate powder, is characterized in that raw materials is bismuth oxide (α-type Bi
2o
3) and amorphous silica (SiO
2), wherein, bismuth oxide (α-type Bi
2o
3) mass percent be 65 ~ 75%, silicon oxide (SiO
2) mass percent be 25 ~ 35%, make two kinds of raw material mechanical alloyings by the mode of high-energy ball milling, form a kind of submicron bismuth silicate powder being applicable to glass ink.
Two of technical scheme of the present invention is:
A preparation method for glass ink submicron bismuth silicate powder, is characterized in that it comprises the following steps:
1) each raw material and bismuth oxide (the α-type Bi of colorant is weighed by proportioning
2o
3), amorphous silica (SiO
2), mix;
2) raw material prepared is placed in high energy ball mill and carries out high-energy ball milling, for dissimilar ball mill, the corresponding change of ball milling parameter;
3) powder after ball milling is taken out, grind at least 30 minutes, namely obtain glass ink submicron bismuth silicate powder of the present invention.
Described each raw material and bismuth oxide (α-type Bi
2o
3) and silicon oxide (SiO
2) maximum particle diameter all need to be less than 1 μm.
The established standards of described ball milling parameter is Ball-milling Time is 48 ~ 60h, ball milling parameter for attritor mill is generally set as: per minute rotating speed 250 ~ 400n/min, ratio of grinding media to material setting 8-12:1, for preventing temperature in ball grinder too high, ball mill program setting is ball milling 30-45min, stop 10-15min, so circulate; For preventing ball milling from luming, within every 10-15 hour, powder being taken out, agglomerated powders is pulverized.
The invention has the beneficial effects as follows:
(1) the bismuth silicate powder particle diameter prepared of the present invention is in submicron rank.
(2) bismuth silicate powder that prepared by the present invention is particularly useful for the preparation of colorant in glass ink, this bismuth silicate powder and the raw material such as boron oxide, Lithium Oxide 98min are carried out further mechanical alloying, more high-quality glass numerial code spray drawing bismuth silicate primary colours material can be prepared with industrial coloring material for mixing.
(3) preparation method of bismuth silicate powder provided by the present invention, can not introduce any impurity substances in preparation process, and the product purity of preparation is high.
(4) preparation method of bismuth silicate powder provided by the present invention, without the need to the technological process of the high energy consumptions such as heating and cleaning, maximum discharge, high pollution, not only energy-saving and emission-reduction, also greatly reduce production cost.
Accompanying drawing explanation
Fig. 1 is the glass ink submicron bismuth silicate powder utilizing embodiment 1 to prepare.
Fig. 2 is the SEM figure of the glass ink submicron bismuth silicate powder utilizing embodiment 1 to prepare.
Fig. 3 is the EDS spectrogram of the glass ink submicron bismuth silicate point group utilizing embodiment 1 to prepare.
Fig. 4 is the glass ink submicron bismuth silicate powder utilizing embodiment 2 to prepare.
Fig. 5 is the SEM figure of the glass ink submicron bismuth silicate powder utilizing embodiment 2 to prepare.
Fig. 6 is the EDS spectrogram of the glass ink submicron bismuth silicate point group utilizing embodiment 2 to prepare.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Embodiment one.
As Figure 1-3.
A kind of glass ink submicron bismuth silicate powder, it is prepared from by following methods:
First, for 500ml ball grinder, be once suitable for grinding 25g bismuth silicate powder, by bismuth oxide (α-type Bi
2o
3) 65% and silicon oxide (SiO
2) 35% mass percent, calculate each raw materials quality required for ball milling 25g submicron bismuth silicate powder, bismuth oxide 16.25 grams and silicon oxide 8.75 grams, then weigh according to calculation result;
Secondly, load weighted each raw material is placed in beaker, stirs, then weigh 250g agate ball according to the ratio of grinding media to material of 10:1;
Finally; above-mentioned raw materials and agate ball are poured in ball grinder together; with ball milling 30min; the mode of stopping 10min starts ball milling, and in mechanical milling process, every 12h shuts down once; open ball grinder the powder of caking is pulverized; ensure the uniform mechanical alloying of powder in mechanical milling process, after ball milling 60h, stop ball milling.Bismuth silicate powder after ball milling is ground 30min with shredder again, namely obtains required glass ink submicron bismuth silicate powder.
The bismuth silicate powder that the present embodiment obtains, as shown in Figure 1, uniform particle sizes, as shown in Fig. 2 EDS figure, the particle diameter major part of bismuth silicate powder is less than 1 μm, the particle that minority particle diameter is greater than 1 μm, Fig. 3 is the spectrogram obtained the particle analysis of in powder with EDS, find to contain Si and Bi and O element in a particle, the mechanical alloying fully of each raw material is described, defines submicron bismuth silicate powder.
Embodiment two.
Roughly the same, difference is that the mass percent shared by raw material is different for the present embodiment and embodiment one experimental technique.According to bismuth oxide (α-type Bi
2o
3) 75%, silicon oxide (SiO
2) 25% mass percent, calculate each raw materials quality required for ball milling 25g submicron bismuth silicate powder, bismuth oxide 18.75 grams and silicon oxide 6.25 grams, then weigh according to calculation result, step below and embodiment 1 completely the same.
The submicron bismuth silicate powder that the present embodiment obtains, as shown in Figure 4, uniform particle sizes, as shown in Fig. 5 EDS figure, the particle diameter major part of bismuth silicate powder is less than 1 μm, the particle that minority particle diameter is greater than 1 μm, Fig. 6 is the spectrogram obtained powder analysis with EDS, find to contain Si and Bi and O element in a particle, the mechanical alloying fully of each raw material is described, defines submicron bismuth silicate powder.
Embodiment three.
A kind of glass ink submicron bismuth silicate powder, it is prepared from by following methods:
First, for 500ml ball grinder, be once suitable for grinding 25g bismuth silicate powder, by bismuth oxide (α-type Bi
2o
3) 70% and silicon oxide (SiO
2) 30% mass percent, calculate each raw materials quality required for ball milling 25g submicron bismuth silicate powder, bismuth oxide 17.5 grams and silicon oxide 7.5 grams, then weigh according to calculation result;
Secondly, load weighted each raw material is placed in beaker, stirs, then weigh 300g agate ball according to the ratio of grinding media to material of 12:1;
Finally; above-mentioned raw materials and agate ball are poured in ball grinder together; with ball milling 45min; the mode of stopping 15min starts ball milling, and in mechanical milling process, every 10h shuts down once; open ball grinder the powder of caking is pulverized; ensure the uniform mechanical alloying of powder in mechanical milling process, after ball milling 48h, stop ball milling.Bismuth silicate powder after ball milling is ground 40min with shredder again, namely obtains required glass ink submicron bismuth silicate powder.
The bismuth silicate powder that the present embodiment obtains, to Fig. 1,4 similar, uniform particle sizes, EDS figure is similar to Fig. 2,5, the particle diameter major part of bismuth silicate powder is less than 1 μm, the particle that minority particle diameter is greater than 1 μm, the spectrogram obtained the particle analysis of in powder with EDS and Fig. 3,6 similar, each raw material is mechanical alloying fully, defines submicron bismuth silicate powder.
Embodiment four.
A kind of glass ink submicron bismuth silicate powder, it is prepared from by following methods:
First, for 500ml ball grinder, be once suitable for grinding 25g bismuth silicate powder, by bismuth oxide (α-type Bi
2o
3) 60% and silicon oxide (SiO
2) 40% mass percent, calculate each raw materials quality required for ball milling 25g submicron bismuth silicate powder, bismuth oxide 15 grams and silicon oxide 10 grams, then weigh according to calculation result;
Secondly, load weighted each raw material is placed in beaker, stirs, then weigh 200g agate ball according to the ratio of grinding media to material of 8:1;
Finally; above-mentioned raw materials and agate ball are poured in ball grinder together; with ball milling 35min; the mode of stopping 12min starts ball milling, and in mechanical milling process, every 15h shuts down once; open ball grinder the powder of caking is pulverized; ensure the uniform mechanical alloying of powder in mechanical milling process, after ball milling 50h, stop ball milling.Bismuth silicate powder after ball milling is ground 60min with shredder again, namely obtains required glass ink submicron bismuth silicate powder.
The bismuth silicate powder that the present embodiment obtains, also to Fig. 1,4 similar, uniform particle sizes, EDS figure is also similar to Fig. 2,5, the particle diameter major part of bismuth silicate powder is less than 1 μm, the particle that minority particle diameter is greater than 1 μm, the spectrogram particle analysis of in powder obtained with EDS also to Fig. 3,6 similar, each raw material is mechanical alloying fully, defines submicron bismuth silicate powder.
Below be only enumerated part formulation, in actual applications, the mass percent of each raw material of filling a prescription can change within the specific limits, coordinates the variation of Ball-milling Time, all can produce glass ink submicron bismuth silicate powder.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.
Claims (4)
1. a glass ink submicron bismuth silicate powder, is characterized in that: it by 65 ~ 75% bismuth oxide (α-type Bi
2o
3) and 25 ~ 35% amorphous silica (SiO
2) formed by high-energy ball milling machinery alloying.
2. the preparation method of glass ink submicron bismuth silicate powder according to claim 1, is characterized in that it comprises the following steps:
1) each raw material and bismuth oxide (the α-type Bi of colorant is weighed by proportioning
2o
3) and amorphous silica (SiO
2), mix;
2) raw material prepared is placed in high energy ball mill and carries out high-energy ball milling, for dissimilar ball mill, the corresponding change of ball milling parameter;
3) powder after ball milling is taken out, grind at least 30 minutes, namely obtain glass ink submicron bismuth silicate powder.
3. method according to claim 2, is characterized in that: each raw material described in step 1) and bismuth oxide (α-type Bi
2o
3) and silicon oxide (SiO
2) maximum particle diameter all need to be less than 1 μm.
4. the preparation method of glass ink submicron bismuth silicate powder according to claim 2, it is characterized in that: step 2) established standards of described ball milling parameter is ball milling 48 ~ 60h, the ball milling parameter of attritor mill is generally set as: per minute rotating speed 250 ~ 400n/min, ratio of grinding media to material setting 8-12:1, for preventing temperature in ball grinder too high, ball mill program setting is ball milling 30-45min, stops 10-15min, so circulates; For preventing ball milling from luming, within every 10-15 hour, powder being taken out, after being pulverized by agglomerated powders, carries out ball milling.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017215099A1 (en) * | 2016-06-16 | 2017-12-21 | 江苏大学 | Bismuth-silicon-boron-based low-melting-point nano glass powder suspension for glass jet drawing and preparation method |
| CN112125517A (en) * | 2019-06-24 | 2020-12-25 | 湖南衡义材料科技有限公司 | Anti-sticking shielding silver paste ink for high-acid-resistance automobile rear windshield and preparation method thereof |
Citations (3)
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|---|---|---|---|---|
| CN101792181A (en) * | 2010-02-09 | 2010-08-04 | 陕西科技大学 | Preparation method of bismuth silicate nanocrystalline |
| CN102351203A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Method for preparing flaky bismuth silicate powder |
| CN102351202A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Preparation method of bismuth silicate powder |
-
2015
- 2015-09-02 CN CN201510557585.1A patent/CN105084375A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| CN101792181A (en) * | 2010-02-09 | 2010-08-04 | 陕西科技大学 | Preparation method of bismuth silicate nanocrystalline |
| CN102351203A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Method for preparing flaky bismuth silicate powder |
| CN102351202A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Preparation method of bismuth silicate powder |
Non-Patent Citations (2)
| Title |
|---|
| I.F.VASCONCELOS ET AL.: "Bismuth silicon oxide (Bi12SiO20-BSO) and bismuth titanium oxide(Bi12TiO20-BTO) obtained by mechanical alloying", 《JOURNAL OF MATERIALS SCIENCE LETTERS》 * |
| 张争光等: "硅酸铋粉体的制备与表征", 《硅酸盐通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017215099A1 (en) * | 2016-06-16 | 2017-12-21 | 江苏大学 | Bismuth-silicon-boron-based low-melting-point nano glass powder suspension for glass jet drawing and preparation method |
| CN112125517A (en) * | 2019-06-24 | 2020-12-25 | 湖南衡义材料科技有限公司 | Anti-sticking shielding silver paste ink for high-acid-resistance automobile rear windshield and preparation method thereof |
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Application publication date: 20151125 |