KR101981065B1 - Translucent celadon composition and manufacturing method of the same - Google Patents

Abstract

The present invention provides a translucent ceramic composition. In one embodiment of the present invention, the substrate comprises 17 to 31 wt% of SiO2, 8 to 10 wt% of Al2O3, 0.1 to 0.3 wt% of Fe2O3, 0.05 to 0.12 wt% of TiO2, 27 to 35 wt% of CaO, 0.1 to 0.5 wt% 0.5 to 1.1% by weight of K2O, 0.1 to 0.5% by weight of Na2O, and 20 to 27% by weight of P2O5.

Description

TECHNICAL FIELD [0001] The present invention relates to a transparent translucent ceramics composition,

The present invention relates to a ceramic article, and more particularly, to a translucent ceramic composition which can be used as a transparent material for illumination and a method for producing the same.

Generally, ceramics are manufactured from pottery, bottles, pollen, etc. using clay having excellent plasticity. Recently, there have been various demands based on the environment-friendly characteristics of ceramics.

Particularly, attempts have been made to make lighting products using ceramics. In recent years, with the development of LED lighting, development of lighting ceramics having physical properties corresponding thereto has been demanded.

Therefore, ceramics products are being developed, in which holes are made in the ceramics to make light distribution through holes, or ceramics are formed in a thickness of 2 to 3 mm to allow light to pass through.

However, such a configuration is not compatible with various three-dimensional structures of the lighting product, and there is a problem that the durability is remarkably deteriorated due to the thin thickness of the ceramic product. Thus, as described in Korean Patent No. 10-1651354, a technique for securing the strength of ceramics in order to maintain a thin thickness of ceramics has been developed, but there is still no technique for expressing the translucency of ceramics itself.

In other words, the general structure of ceramics is mostly composed of mullite phase and quartz phase in order to secure physical properties such as strength, surface roughness, oil level hardness and thermal shock resistance related to the use thereof.

[Prior Art Literature]

Korean Registered Patent No. 10-1651354 (Aug. 25, 2016)

It is an object of the present invention to provide a porcelain composition which can secure transparency by itself.

The present invention solves the above problems by providing a light transmitting translucent ceramic composition in which the TCP (Tricalcium Phosphate, Ca3 (PO4) 2) crystal phase is the predominant crystal phase.

In one embodiment of the present invention, the TCP crystal phase of the present invention is characterized in that it is formed by mixing natural ash (Ca10 (PO4) 6 (OH) 2) and synthetic ash (CaHPO4.2H2O). In other words, although the crystal structure of general ceramics is composed of mullite and quartz, it does not have translucency, but inhibits crystal formation of mullite and quartz and promotes crystal formation of TCP (Tricalcium phosphate, Ca3 (PO4) 2) And the optimum ratio of TCP crystal formation was achieved by varying the blending ratio of natural ash (Ca10 (PO4) 6 (OH) 2) and synthetic ash (CaHPO4.2H2O).

In one embodiment of the present invention, the substrate comprises 17 to 31 wt% SiO2, 8 to 10 wt% Al2O3, 0.1 to 0.3 wt% Fe2O3, 0.05 to 0.12 wt% TiO2, 27 to 35 wt% CaO, 0.1 to 0.5 wt% 0.5 to 1.1% by weight of K2O, 0.1 to 0.5% by weight of Na2O, and 20 to 27% by weight of P2O5.

In one embodiment of the present invention, the natural bone ash (Ca10 (PO4) 6 (OH) 2) and the synthetic base ash (CaHPO4.2H2O) are contained in the base in an amount of 45 to 50% by weight. Therefore, the moldability was maintained by maintaining the contents of other active ingredients limestone, feldspar, feldspar, T-stones, core, N.K, A.k, W clay, B and K as a certain level.

At this time, it is preferable that the mixing ratio of the weight% of the synthetic ash to the weight% of the coke oven ash for the generation of the TCP crystal phase is 0.4 to 1.2. In this range, it was confirmed that the desired light transmittance was obtained while keeping the strength and formability of the ceramics. At this time, it was confirmed that the formation of mullite phase and quartz phase was suppressed and TCP formation was smoothly performed. In this case, the content ratio of CaO to P2O5 is 1.2 to 1.33.

Meanwhile, in one embodiment of the present invention, the mullite crystal phase or the Kurtz crystal phase may exist in a sub-crystalline phase, in order to prevent moldability and strength deterioration of the ceramic composition.

The present invention also relates to a process for producing a slip for a molding, comprising the steps of blending a raw material, producing a base cake, aging a base cake, adding water to the base cake and stirring to prepare a molding slip, By weight based on the total weight of the composition.

In an embodiment of the present invention, in the step of mixing the raw materials, a primary raw material is added, followed by ball milling, followed by ball milling with a secondary raw material.

In one embodiment of the present invention, the step of producing the molding slip is aged in a low-speed stirring state after the agitation. Thereafter, calcination is performed at 1250 to 1270 deg. C for 30 minutes to 1 hour 30 to complete the preparation of the ceramic composition.

The translucent ceramic composition according to the present invention has a light transmittance capable of functioning as a housing for illumination by forming a TCP crystalline phase by optimally mixing natural bone ash (Ca10 (PO4) 6 (OH) 2) with synthetic ash (CaHPO4.2H2O) Respectively.

Further, in the present invention, the optimal blending ratio and ratio of the natural ash and the synthetic ash were derived, and the light transmittance was secured and the formability of the ceramics was maintained at the same time.

In addition, the present invention maintains the strength of the ceramics while ensuring the transparency.

1 is a graph showing the results of the whiteness evaluation.
2 is a graph showing the results of strength evaluation.
3 is a graph showing the results of the light transmittance evaluation.
4 is a graph showing the experimental composition and formability of TCP.
5 is a photograph showing a process of preparing a cake by blending raw materials.
6 is a graph showing the RHK temperature curve in the sintering process.
Fig. 7 is a photograph showing the firing step.
FIG. 8 is an XRD graph and a tissue photograph showing the appearance of the TCP crystallization phase. FIG.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, This is possible. Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.

1. Ratio adjustment test of natural ash and synthetic ash

As shown in the following Tables 1 and 2, each component of the substrate was compounded and a ratio adjustment test was carried out. At this time, the whiteness and the intensity for acting as the housing of the illumination were measured.

 Mixing ratio Natural bone Synthetic bone Limestone I feldspar T Stone Main wave N.K A.k W clay B Stone S.K Sum A1 46 0 0 4.6 6.5 9.9 4.5 7.2 11.8 4.5 5.0 100 A2 35 11 5.3 4.2 5.9 8.9 4.1 6.5 10.6 4.0 4.5 100 A3 25 21 10.1 3.8 5.3 8.0 3.7 5.8 9.6 3.7 4.0 100 A4 15 31 14.9 3.4 4.7 7.2 3.3 5.2 8.5 3.3 3.5 100 A5 5 41 19.8 2.9 4.1 6.3 2.8 4.5 7.5 2.9 3.2 100 A6 0 46 22.2 2.7 3.8 5.9 2.6 4.2 7.0 2.6 3.0 100

 Chemical composition analysis SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O P2O5 Ig.loss A1 30.61 13.81 0.28 0.11 27.04 0.61 1.04 0.48 20.35 5.65 A2 27.50 12.45 0.25 0.10 28.77 0.50 0.94 0.40 21.91 7.16 A3 24.71 11.21 0.23 0.09 30.33 0.41 0.85 0.33 23.33 8.52 A4 21.87 9.96 0.20 0.08 31.91 0.31 0.76 0.26 24.77 9.88 A5 18.98 8.72 0.17 0.07 33.53 0.21 0.66 0.18 26.19 11.29 A6 17.53 8.12 0.16 0.06 34.32 0.16 0.61 0.14 26.91 11.97

At this time, the content of the natural ash and the synthetic ash was adjusted to be 45 to 50% by weight. When the content is less than 44 wt%, the formation of the TCP crystal phase is not promoted. When the content is more than 55 wt%, the formability is deteriorated and it is difficult to form the appearance of the lighting device.

The whiteness for A1 to A6 is shown in Fig. 1 and the intensity is shown in Fig. Referring to the drawings, the translucent ceramic composition according to an embodiment of the present invention has a slight decrease in whiteness from A1 to A6, but the whiteness is not significantly reduced because it is not significantly reduced.

However, in the case of strength, the decrease in strength was observed in A4, A5, and A6, so that it was more preferable that the contents of A1 to A3 were favorable.

2. TCP content adjustment test

In this experiment, as shown in Tables 3 and 4, a test was conducted to adjust the TCP content including the content of the natural ash and the synthetic ash of less than 45% by weight and the case of exceeding 50% by weight.

 TCP content adjustment test Natural bone Synthetic bone Limestone I feldspar T Stone Main wave N.K A.k W clay B Stone S.K Sum B1 17.8 15.0 7.2 5.2 7.3 11.0 5.0 8.0 13.1 5.0 5.4 100 B2 25 21 10.1 3.8 5.3 8.0 3.7 5.8 9.6 3.7 4.0 100 B3 31.2 26.3 12.5 2.6 3.6 5.5 2.5 4.0 6.5 2.5 2.8 100 B4 35.7 30.0 14.3 1.7 2.4 3.7 1.6 2.7 4.4 1.6 1.9 100

 Chemical composition analysis SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O P2O5 Ig.loss B1 33.39 15.28 0.30 0.12 23.07 0.34 1.16 0.37 17.74 8.24 B2 24.71 11.21 0.23 0.09 30.33 0.41 0.85 0.33 23.33 8.52 B3 17.19 7.68 0.16 0.06 36.60 0.46 0.59 0.30 28.24 8.71 B4 11.77 5.14 0.12 0.04 41.13 0.51 0.39 0.28 31.73 8.89

In the case of B3 and B4, the content of the natural ash and the synthetic ash exceeded 50% by weight, and the decrease in the formability was observed as in Fig. Further, in the case of B1, the transmittance was observed to decrease. Accordingly, it was found that the content of the natural ash and the synthetic ash required for the formation of the TCP crystal phase was more preferably 45 to 50 wt%.

3. TCP content increase test

In this experiment, as shown in Tables 5 and 6, the content of the natural ash and the synthetic ash was fixed at 50% by weight, and the mixing ratio of both was changed.

 TCP content increase test Natural bone Synthetic bone Limestone I feldspar T Stone N.K A.k W clay Sum C1 30.0 20.0 11.0 5.8 12.1 9.7 4.8 6.6 100.0 C2 25.0 25.0 12.1 5.8 11.0 9.7 4.8 6.6 100.0 C3 20.0 30.0 12.8 5.8 10.3 9.7 4.8 6.6 100.0 C4 15.0 35.0 13.5 5.8 9.6 9.7 4.8 6.6 100.0

 Chemical composition analysis SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O P2O5 Ig.loss C1 25.03 9.98 0.18 0.06 30.89 0.44 0.92 0.40 23.11 8.98 C2 24.03 9.84 0.18 0.06 31.06 0.39 0.91 0.37 23.92 9.24 C3 23.35 9.75 0.17 0.06 31.02 0.34 0.90 0.34 24.72 9.35 C4 22.67 9.66 0.17 0.06 30.97 0.28 0.90 0.32 25.52 9.46

The transmittance according to this experiment is shown in Fig. Referring to the drawings, the transmittance was observed favorably in the order of C3, C2, and C4, and in the case of B4 described above, it was confirmed that the transmittance was also decreased in addition to the reduction in the moldability described above. This is a very significant result confirming that the TCP crystallization phase of B4 grows beyond the threshold value and the transmittance is lowered. That is, in order to realize a preferable transmittance, the mixing ratio of the ash ash to the synthetic ash is 0.4 to 1.2, but in the case of B4, the light transmittance is decreased to 1.5.

As described above, the TCP experimental composition in Experiments 1 to 3 is shown in Fig. Referring to FIG. 4, it can be seen that the content ratio of CaO to P2O5 in the substrate is in the range of 1.2 to 1.33. In this range, the transmittance is most preferably observed, and more preferably, Is limited to 0.4 to 1.2.

4. Transparent base manufacturing process

Hereinafter, the manufacturing process of the light transmitting substrate will be described. The process for producing a light transmitting base includes the steps of mixing the raw materials, preparing the base cake, aging the base cake, adding water to the base cake and stirring to prepare a molding slip, .

1) Transparent base material mixing process.

As shown in Table 7, the raw material is put into a ball mill and ball milled for 12 hours, followed by addition of secondary raw materials and further milling for 3 hours. The pulverized slurry is agitated in a stirring tank and pressed to produce a ground cake state. Cake ripening is aged 3-5 days.

 Light Transmissible Organic Compounding Table Primary (12 hours) Second (3 hours) Raw material name Remarks Raw material name Remarks T-stones Moisture 5% Natural Bone Esh Moisture 14% B NZ.K Moisture 4% I feldspar W clay Moisture 5% Limestone AKW.K Moisture 10% Natural Bone Esh Moisture 14% SSP.K Moisture 8% Synthetic bosh water Based on 50% moisture of slurry Main wave Moisture 2% water Based on 45% moisture of slurry

As shown in FIG. 5, the raw materials thus prepared are ball-milled, mixed, de-ironed, sieved, filtered and compressed to form a base cake.

2) Molding process

After adding the appropriate amount of water and agitating agent to the prepared base cake, the mixture was agitated for 4 hours at high speed, aged for 1 day under low speed stirring, and then used as slip for molding after adjusting to the specification of the drain slip combination ratio shown in Table 8.

 Drain slip combination ratio table
Jun Viscosity 4.5 to 5.5 Poise (standard used: 8 ± 1) importance 1.920 ~ 1.925 g / cc (use standard: 1.91 ± 0.03) moisture 25.7 ~ 26.2% (standard used: 26 ± 1.0) Combination amount 1.370kg combination time
(cake moisture 21%) (2 pallets) 2.055 kg combination
(cake moisture 21%) (3 pallets) Volume 92kg 137kg Sodium silicate (0.2%) 2.2 kg 3.3kg CF-44 (0.2%) 1.73kg 2.6kg

3)

Referring to FIG. 6 and FIG. 7, the molded product is sintered in RHK, which is a primary sintering furnace, and sintering time is 4 to 6 hours, soaking temperature is 1265 ° C, and soaking time is 1 hour.

As described above, it is possible to develop TCP as an environment-friendly ceramics lighting which can replace the plastic by promoting the formation of TCP crystal phase in the ceramic substrate and improving the transparency of the impermeable ceramics material.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be appreciated by those skilled in the art that numerous changes and modifications can be made to the invention. And all such modifications and changes as fall within the scope of the present invention are therefore to be regarded as being within the scope of the present invention.

Claims (15)

The TCP (Tricalcium Phosphate, Ca3 (PO4) 2) crystal phase contains a major crystal phase,
The TCP crystal phase is formed by combining natural bone ash (Ca10 (PO4) 6 (OH) 2) with synthetic ash (CaHPO4.2H2O)
Wherein the natural base ash (Ca10 (PO4) 6 (OH) 2) and the synthetic base ash (CaHPO4.2H2O) are contained in the base in an amount of 45 to 50% by weight.
delete delete delete The method according to claim 1,
Wherein the mixing ratio of the natural bone ash to the synthetic ash in the above-mentioned substrate is 0.4 to 1.2.
delete The method according to claim 1,
Wherein the substrate is a mullite crystal phase or a Kurtz crystal phase is a subcrystalline phase.
Blending the raw material;
Preparing a base cake;
Aging the base cake;
Adding water to the base cake and stirring to prepare a molding slip; And
And firing the molding slip,
In the step of blending the raw materials, the main crystalline phase of the compounded raw material is composed of TCP (Tricalcium Phosphate, Ca3 (PO4) 2)
The TCP crystal phase is formed by combining natural bone ash (Ca10 (PO4) 6 (OH) 2) with synthetic ash (CaHPO4.2H2O)
Wherein the natural base ash (Ca10 (PO4) 6 (OH) 2) and the synthetic base ash (CaHPO4.2H2O) are contained in the base in an amount of 45 to 50 wt%.
delete delete delete delete 9. The method of claim 8,
Wherein the step of blending the raw material is a step of ball milling with a first raw material, followed by ball milling, followed by ball milling with a second raw material.
9. The method of claim 8,
Wherein the step of preparing the molding slip is aged in a low-speed stirring state after the agitation and stirring.
9. The method of claim 8,
Wherein the baking is performed at a temperature of 1250 to 1270 deg. C for 30 minutes to 1 hour and 30 hours.

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