CN102617188A

CN102617188A - Method for preparing split-phase black fancy glaze by utilizing industrial slag

Info

Publication number: CN102617188A
Application number: CN2012100871003A
Authority: CN
Inventors: 王毅; 刘子建; 高黎
Original assignee: Shaanxi University of Science and Technology
Current assignee: JIANGSU FANXIANG BUILDING MATERIALS TECHNOLOGY Co.,Ltd.
Priority date: 2012-03-28
Filing date: 2012-03-28
Publication date: 2012-08-01
Anticipated expiration: 2032-03-28
Also published as: CN102617188B

Abstract

A method for preparing split-phase black fancy glaze by utilizing industrial slag includes evenly grinding slag coarse materials in a mortar, filling the ground slag coarse materials into a crucible, roasting the materials in a high temperature furnace to 1000 DEG C, conducting heat preservation for 60 minutes, enabling the materials to be naturally cooled, conducting ball grinding after cooling, conducting screening through a 80-mesh screen to prepare fine slag, mixing feldspar, quartz, calcite, talc, calcium phosphate, fine slag, sodium tripolyphosphate and CMC, conducting fine grinding to 250 meshes, modulating glaze slip to be 1.7g/cm<3>, evenly spreading the glaze slip on a base, heating the glaze slip to 1180 DEG C to 1250 DEG C, conducting heat preservation for 20 to 50 minutes, and then conducting natural cooling. Split mechanism and slag coloring oxide generated by a melt in the roasting process of the glaze slip are combined to conduct coloring and enable a little color oxide to generate strong coloring capability. The preparation method of the black fancy glaze is low in cost, high in stability and abundant in decorative pattern. Further, colorant content of the black fancy glaze is 30% to 50% of color material content in common glaze.

Description

A kind of preparation method who utilizes industrial slag to carry out phase-splitting black fancy glaze

Technical field

The present invention relates to a kind of preparation method who utilizes industrial slag to carry out phase-splitting black fancy glaze, be specifically related to a kind of preparation method who can be used for construction sanitary ceramic, domestic ceramics, the art pottery and the ceramic black fancy glaze of other high, medium and low temperature.

Background technology

The black glaze is a kind of famous and precious glaze.Decorating porcelain in China with black glaze is a kind of ancient traditional method, the black glaze of Deqing ware of the black glaze in the Shangyu of the Eastern Han Dynasty and the Eastern Jin Dynasty, and with dignified, solemn, steady color sensation characteristics, extremely people like always.These black glaze burn till under reducing atmosphere with ferruginous clay and make, and its colour generation is extremely unstable, and firing process is difficult to grasp.Along with the development of ceramic industry in modern age, the normal Co that adopts in the production ₂O ₃, Fe ₂O ₃, Cr ₂O ₃, Mn ₂O ₃Be prepared into colorant earlier Deng MOX, join again and make black glaze in the parent glaze.Though the glaze firing of this kind mode is not influenced by atmosphere, but need in not zinciferous lime glaze, use, and colorant receives Co ₂O ₃Etc. the influence of the prices of raw and semifnished materials, cost is very high.

Some scholars process Fe-Cr-Mn-Ni system black material and the black material (Sun Chen of Fe-Cr-Cu-Ni system of no Co in recent years; Yin Shujian, the army of wearing, Dong Bo; Zhang Yuhong. the application of no cobalt black colorant and attention problem. advanced ceramics and technology; 1998 (2): 41-44.), be colorant but the black glaze of this kind still belongs to a kind of isomorphous mixed type spinel, and Fe ₂O ₃, Mn ₂O ₃Higher etc. painted oxide content; Need through the synthetic in advance colorant of technologies such as calcining, pickling, elutriation, technological process relative complex and energy consumption are high, pollution is big, and relative cost is as the same higher; Do not meet the needs of current international community energy-saving and emission-reduction, demand technological improvement urgently and improve.

Summary of the invention

The object of the present invention is to provide that to utilize a kind of industrial slag to prepare cheap, blackness is high, and colour generation is pure, the method for the phase-splitting black fancy glaze of stable performance.

For achieving the above object, the technical scheme that the present invention adopts is:

1) meticulous scoriaceous preparation:

After in mortar, grinding industrial slag evenly, put into crucible and be fired to 1000 ℃, and be incubated 60 minutes, carry out ball milling after cooling, take out the back and cross 80 mesh sieves in High Temperature Furnaces Heating Apparatus, get final product meticulous slag;

2) preparation of glaze slip:

By mass percentage with the feldspar of 50-70%, the quartz of 10-20%, the calcite of 2-10%; The talcum of 0-5%; The calcium phosphate of 1-8%, the meticulous slag of 10-25% mix mixture, in mixture, add the tripoly phosphate sodium STPP of mixture quality 0.4% and 1% CMC again and mix; Be finely ground to 250 orders, modulation glaze slip proportion is 1.6-1.7g/cm ³

3) glaze slip is executed equably applied on base substrate, be warming up to 1180-1250 ℃, be incubated 20-50 minute naturally cooling and promptly obtain phase-splitting black fancy glaze.

The rotating speed of the ball mill that described ball milling adopts is 900r/h, and the ball milling time is 30 minutes.

The industrial slag of multiple metallic element is rich in utilization of the present invention, through the prescription modulation, utilizes the parvafacies mechanism that melt produces in the glaze sintering process to carry out painted.And research and analyse through means of testing such as XRD, reflection spectrum analyses and to show that the mechanism that black glaze according to the invention presents black is to realize (the Fe Mg that promptly forms through solid state reaction through industrial slag according to the mixing principle of losing lustre of color _0.05) ₂Mg _0.05O ₃Magnesium ferriferous oxide, SiO ₂, Mg ₂SiO ₄, painted oxide compound such as alkali tirodite, introduce in the glaze, these sosoloid carry out selectivity to the visible light of different-waveband and absorb, the visible light of 380～780nm section all absorbs and is rendered as the black glaze the most at last.

The color glaze colourity of the present invention preparation is pure, glaze is bright and bright-coloured; And can be according to consumption and firing temperature different; Make glaze form the decorative pattern of different colours such as blueness, redness; And the higher microfacies of degree of staining is posted one deck black film and makes whole glass show black the same because of light transmission, the whole glaze layer of refraction action as glass.This type of black glaze improves colour stability because of microfacies to painted ionic package action, and colorant content is merely the 30%-50% of common glaze colorant consumption.This kind raw materials of slag source is wide, cheap, and blackness is high, pure, the stable performance of colour generation, and the black glaze that can be widely used in all kinds of ceramic products is decorated.Thereby produce the black fancy glaze of a kind of low cost, high stability.

Description of drawings

Fig. 1 is that the present invention implements the scoriaceous XRD figure in calcining back;

Fig. 2 is the sample photo of the embodiment of the invention 1, and wherein Fig. 2 a is the optical micro analysis photo, and Fig. 2 b is a stereoscan photograph;

Fig. 3 is the sample photo of the embodiment of the invention 2.

Embodiment

Below in conjunction with embodiment the present invention is done further explain.

Embodiment 1:

1) meticulous scoriaceous preparation:

After in mortar, grinding industrial slag evenly, putting into crucible and be fired to 1000 ℃ in High Temperature Furnaces Heating Apparatus, and naturally cooling after being incubated 60 minutes, is ball milling 30 minutes under the 900r/h at rotating speed after cooling, takes out the back and crosses 80 mesh sieves, get final product meticulous slag;

2) preparation of glaze slip:

By mass percentage with 50% feldspar, 10% quartz, 10% calcite; 2% talcum; 3.0% calcium phosphate, 25% meticulous slag mix mixture, in mixture, add the tripoly phosphate sodium STPP of mixture quality 0.4% and 1% CMC again and mix; Be finely ground to 250 orders, modulation glaze slip proportion is 1.7g/cm ³

3) glaze slip is executed equably applied on base substrate, be warming up to 1250 ℃, be incubated 50 minutes naturally cooling and promptly obtain phase-splitting black fancy glaze.

Table one is the test result parameter of embodiment 1;

Can find out that by table 1 in the international luminouslighting council (CIE) chromaticity diagram, the distributed points of color is in black-and-blue zone.

As can be seen from Figure 1 this slag contains color development composition iron and compound thereof in forming, and explains that pigmentation element is mainly from red stone;

By the photo of Fig. 2 can find out the present invention prepared for phase-splitting black fancy glaze.

Embodiment 2:

1) meticulous scoriaceous preparation:

After in mortar, grinding industrial slag evenly, put into crucible and be fired to 1000 ℃ in High Temperature Furnaces Heating Apparatus,, and naturally cooling after being incubated 60 minutes is a ball milling 30 minutes under the 900r/h at rotating speed after cooling, takes out the back and crosses 80 mesh sieves, get final product meticulous slag;

2) preparation of glaze slip:

By mass percentage with 55% feldspar; 20% quartz, 8% calcite, 2% calcium phosphate; 15% meticulous slag mix mixture; The tripoly phosphate sodium STPP of adding mixture quality 0.4% and 1% CMC mix in mixture again, are finely ground to 250 orders, and modulation glaze slip proportion is 1.7g/cm ³

3) glaze slip is executed equably applied on base substrate, be warming up to 1230 ℃, be incubated 40 minutes naturally cooling and promptly obtain phase-splitting black fancy glaze.

By the photo of Fig. 3 can find out the present invention prepared for phase-splitting black fancy glaze.

Embodiment 3:

1) meticulous scoriaceous preparation:

After in mortar, grinding industrial slag evenly, put into crucible in High Temperature Furnaces Heating Apparatus be fired to 1000 ℃ and be incubated 60 minutes after naturally cooling, be ball milling 30 minutes under the 900r/h at rotating speed after cooling, take out the back and cross 80 mesh sieves, get final product meticulous slag;

2) preparation of glaze slip:

By mass percentage with 60% feldspar, 15% quartz, 6% calcite; 5% talcum; 1.0% calcium phosphate, 13% meticulous slag mix mixture, in mixture, add the tripoly phosphate sodium STPP of mixture quality 0.4% and 1% CMC again and mix; Be finely ground to 250 orders, modulation glaze slip proportion is 1.7g/cm ³

3) glaze slip is executed equably applied on base substrate, be warming up to 1220 ℃, be incubated 40 minutes naturally cooling and promptly obtain phase-splitting black fancy glaze.

Embodiment 4:

1) meticulous scoriaceous preparation:

After in mortar, grinding industrial slag evenly, putting into crucible and be fired to 1000 ℃ in High Temperature Furnaces Heating Apparatus, and be incubated 60 minutes, is that ball milling took out the back in 30 minutes and crosses 80 mesh sieves under the 900r/h at rotating speed after cooling, get final product meticulous slag;

2) preparation of glaze slip:

By mass percentage with 65% feldspar, 10% quartz, 6% calcite; 2% talcum; 5.0% calcium phosphate, 12% meticulous slag mix mixture, in mixture, add the tripoly phosphate sodium STPP of mixture quality 0.4% and 1% CMC again and mix; Be finely ground to 250 orders, modulation glaze slip proportion is 1.6g/cm ³

3) glaze slip is executed equably applied on base substrate, be warming up to 1200 ℃, be incubated 30 minutes naturally cooling and promptly obtain phase-splitting black fancy glaze.

Embodiment 5:

1) meticulous scoriaceous preparation:

2) preparation of glaze slip:

By mass percentage with 70% feldspar; 10% quartz, 2% calcite, 8% calcium phosphate; 10% meticulous slag mix mixture; The tripoly phosphate sodium STPP of adding mixture quality 0.4% and 1% CMC mix in mixture again, are finely ground to 250 orders, and modulation glaze slip proportion is 1.6g/cm ³

3) glaze slip is executed equably applied on base substrate, be warming up to 1180 ℃, be incubated 20 minutes naturally cooling and promptly obtain phase-splitting black fancy glaze.

Claims

1. preparation method who utilizes industrial slag to carry out phase-splitting black fancy glaze is characterized in that:

1) meticulous scoriaceous preparation:

2) preparation of glaze slip:

2. the preparation method who utilizes industrial slag to carry out phase-splitting black fancy glaze according to claim 1 is characterized in that: the rotating speed of the ball mill that described ball milling adopts is 900r/h, and the ball milling time is 30 minutes.