Tin sphene crystal glaze and preparation method thereof

Abstract

The invention belongs to the technical field of crystal glaze, and discloses tin sphene crystal glaze and a preparation method thereof. The tin sphene crystal glaze is prepared from the following components in percentage by mass: 50 percent to 57 percent of SiO2, 18 percent to 25 percent of CaO, 5 percent to 8 percent of ZnO, 4 percent to 9 percent of Al2O3, 3 percent to 6 percent of K2O, 8 percent to 12.5 percent of SnO2 and 0 percent to 1 percent of Cr2O3. The method comprises the following steps: uniformly mixing the raw materials and the dispersing agent, carrying out wet ball milling to obtain glaze slip, glazing on a ceramic body, and sintering to obtain the tin sphene crystal glaze. The tin sphene crystal glaze is successfully obtained, the one-time sintering process is adopted, the colors such as pink, red, dark red and purple red can be shown, crystal distribution is uniform, the colors are easy to regulate and control, the preparation process is simple, and the tin sphene crystal glaze is suitable for large-scale industrial application.

Description

Technical Field

[0001] The invention belongs to the technical field of ceramic glazes, and in particular relates to a tinstenite crystal glaze and a preparation method thereof. Background Art

[0002] Crystalline glaze is a thin glassy layer covering the surface of ceramic products. During the firing process, since the glaze contains sufficient crystalline substances, it is in a saturated state after melting, and crystallization is formed during the slow cooling process. The precipitated crystals can change the properties of the glaze, giving the glaze layer wear resistance, transparency / opaqueness, conductivity, photocatalysis and other properties. In addition, it can form beautiful crystalline patterns on the glaze surface, greatly improving the artistic effect. Tin sphene (CaSnSiO5) is a mineral belonging to the monoclinic system. It is composed of SiO4 tetrahedrons connected to SnO6 octahedrons at the same angle, and Ca ions occupy disordered positions. It is usually used as a pigment matrix or made into microwave dielectric ceramics. There are also studies on it as a fluorescent carrier. Cr-doped tin sphene is widely used as a red pigment in colorants. It has low raw material cost and good stability at high temperatures. Yu Kangtai et al. synthesized a tin sphene ceramic, the main crystal phase is tin sphene, and there are also tricalcium tin silicate and tin oxide phases, and the firing temperature is 1300℃ (Yu Kangtai, Fang Guiqin. Research on the synthesis mechanism of agate red high-temperature ceramic pigment [J]. Journal of Ceramics, 1998, 019(004): 204-208). Escardino A et al. added tin sphene pigment to different glaze formulas and found that its color would be affected by the formula. Different crystals precipitated in different glazes would change or cover the color of the pigment. In addition, phase separation of the glaze layer would also affect its color (Escardino A, Mestre S, Feliu C, et al. Stability of (Cr)CaO.SnO2.SiO2 pink pigment in ceramic frits [J]. British Ceramic Transactions, 2013, 101(5): 213-220).

[0003] Although it is mentioned above that the tin sphene crystal phase can be obtained by high temperature, it is difficult to obtain tin sphene crystal glaze by mixing the raw materials of tin sphene crystal glaze with the raw materials of base glaze. This is because the solubility of tin oxide in many high-temperature silicate melts is very low and it is not easy to melt. In the cooled glaze, tin oxide is still fine suspended particles, which makes the glaze opaque and is usually used to make the glaze white. Moreover, tin sphene crystal glaze cannot be obtained by any arbitrary raw material ratio. In addition, the existing tin sphene glaze is prepared by preparing a colorant of tin sphene crystal phase at high temperature and then adding it to the base glaze. That is, tin sphene crystals are first synthesized (usually kept at 1300-1400℃ for more than 2h) and then added to the glaze. Multiple steps are required. At the same time, the base glaze sometimes destroys the structure of the tin sphene crystals, affects the color, and is prone to uneven color.

[0004] At present, there is little research on tin sphene crystalline glaze. Developing the preparation of tin sphene (CaSnSiO5) crystalline glaze and studying its properties and application value, thereby expanding the types of crystalline glazes, is of great significance to the development of ceramic crystalline glazes. Summary of the invention

[0005] In order to overcome the shortcomings and deficiencies of the prior art, the object of the present invention is to provide a tin sphene crystalline glaze and a preparation method thereof.

[0006] The technical solution adopted by the present invention is:

[0007] A tinstenite crystalline glaze comprises the following components in percentage by mass:

[0008] SiO2: 50%~57%

[0009] CaO: 18%~25%

[0010] ZnO: 5%~8%

[0011] Al2O3: 4%~9%

[0012] K2O: 3%~6%

[0013] SnO2: 8%~12.5%

[0014] Cr2O3:0%~1%.

[0015] Preferably

[0016] SiO2: 50%~55%

[0017] CaO: 19%~23%

[0018] ZnO: 5%~7%

[0019] Al2O3: 4%~8%

[0020] K2O: 3%~5.5%

[0021] SnO2: 9%~12%

[0022] Cr2O3: 0.2%~1%.

[0023] More preferably:

[0024] SiO2: 50~52%,

[0025] CaO: 20-22%,

[0026] ZnO: 6-7%,

[0027] Al2O3: 7-8%,

[0028] K2O: 4-5%,

[0029] SnO2: 9-10%,

[0030] Cr2O3: 0.4~0.6%.

[0031] The method for preparing the tin sphene crystal glaze comprises the following steps: mixing a glaze material and a dispersant, and performing wet ball milling to prepare a glaze slurry; applying the glaze on a ceramic body; and firing the tin sphene crystal glaze.

[0032] Preferably, the dispersant is at least one of carboxymethyl cellulose, sodium carboxymethyl cellulose and sodium tripolyphosphate.

[0033] The raw materials of the glaze include potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide, tin oxide, and chromium oxide. The mixing of the glaze and the dispersant refers to mixing potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide, tin oxide, chromium oxide and the dispersant; or mixing potassium feldspar, calcined kaolin, wollastonite, quartz and zinc oxide to form a frit, and then mixing the frit, chromium oxide and the dispersant.

[0034] The firing process is a one-time firing process.

[0035] The added amount of the dispersant is 0.3% to 0.8% of the total mass of the glaze.

[0036] The wet ball milling time is 60 min to 120 min.

[0037] The glazing method is one of spraying glaze, dipping glaze and pouring glaze.

[0038] The firing is carried out at 1180° C. to 1225° C., and the heat preservation time is 5 min to 15 min.

[0039] Further preferably, the specific operation of the sintering is: heating to 1180°C to 1225°C at a heating rate of 10°C / min to 20°C / min, and then keeping the temperature for 5min to 15min.

[0040] The beneficial effects of the present invention are as follows: the tinstenite crystal glaze of the present invention adopts a one-time firing process, can present colors such as pink, red, dark red, purple red, etc., has uniform crystal distribution, is easy to control in color, and has a simple preparation process, and is suitable for large-scale industrial applications.

[0041] Specifically:

[0042] 1) The present invention adjusts the ratio of CaO, SnO2 and SiO2 (CaO: SiO2: SnO2 = 18-25: 50-57: 8-12) to design a crystalline glaze formula, thereby successfully preparing a tin sphene crystalline glaze. The crystalline glaze of the present invention only contains a tin sphene (CaSnSiO5) crystalline phase; the preparation and firing process of the present invention is simple, and there is no need to strictly control the firing system to precipitate the tin sphene, and the tin sphene can be flexibly adapted to the industrial firing system.

[0043] 2) Based on the above glaze, the present invention prepares a tin chrome red crystalline glaze by adding a certain amount of Cr2O3. The coloring principle is that Cr ions are dissolved in the tin sphene (CaSnSiO5) crystals in the glaze. 4+ Substituting Sn in the tin sphene lattice 4+ The [SnO6] octahedron is deformed, making the glaze appear red; the color can be controlled by the amount of Cr added.

[0044] 3) The present invention directly precipitates Cr-doped tin sphene (CaSnSiO5) crystals from the glaze to prepare the tin chrome red crystalline glaze in one step, instead of adding tin chrome red material to the formula of the basic glaze. The crystalline glaze is easy to control, has uniform color, deep and bright color, and has excellent decorative effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 is the X-ray diffraction pattern of the tin sphene crystalline glaze of Example 1;

[0046] Figure 2 is a SEM image of the tin sphene crystalline glaze of Example 1;

[0047] Figure 3 : is the reflection spectrum of the tin sphene crystal glaze surface of Examples 2, 3, and 4;

[0048] Figure 4 The actual photos of the tin sphene crystal glazes of Examples 1, 2, 3, and 4;

[0049] Figure 5 The X-ray diffraction pattern of the glaze prepared in Comparative Example 1;

[0050] Figure 6 This is an optical image of the glaze prepared in Comparative Example 2;

[0051] Figure 7 This is an optical image of the glaze prepared in Comparative Example 3. DETAILED DESCRIPTION

[0052] The present invention is further explained and illustrated below in conjunction with specific examples, but the embodiments of the present invention are not limited thereto. In the present invention, the weight parts of the raw materials potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide, and tin oxide are (22-28), (45-50), (2-3.5), (2-3), (5-8), (9-12), preferably (25-27), (46-48), (2.5-3), (2.2-2.8), (6.5-7.5), (9.5-10.5), respectively; the weight part of chromium oxide is 0-1 part, preferably 0.2-1 part, and more preferably 0.4-0.6 part.

[0053] Embodiment 1:

[0054] The invention discloses a method for preparing a tin sphene crystal glaze, comprising the following steps: by weight, 25 parts of potassium feldspar, 48 parts of wollastonite, 3 parts of calcined kaolin, 2.5 parts of quartz, 7 parts of zinc oxide, 10.5 parts of tin oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 60 minutes to prepare a glaze slurry; glazing is then performed on a bisque-fired ceramic body by spraying glaze, and then drying is performed; and then the ceramic body is placed in a box-type electric furnace and heated to 1180°C at a heating rate of 10°C / min, and then kept warm for 5 minutes and cooled to obtain the tin sphene crystal glaze.

[0055] The mass percentages in this embodiment are measured by XRF:

[0056] SiO2: 50.7%,

[0057] CaO: 22.9%,

[0058] ZnO: 6.3%,

[0059] Al2O3: 4.8%,

[0060] K2O: 4.7%,

[0061] SnO2: 10.5%.

[0062] The X-ray diffraction pattern of the tin sphene crystal glaze prepared in this example is as follows: Figure 1 shown.

[0063] Depend on Figure 1 It can be seen that the appearance of only tin sphene peaks indicates that there is only tin sphene crystal phase in the glaze, and no other impurities.

[0064] The surface of the tin sphene glaze prepared in this example (the cross section was etched with a 2 vol% hydrofluoric acid solution for 45 seconds and then tested) is shown in the scanning electron microscope (SEM) image. Figure 2 shown.

[0065] Depend on Figure 2It can be seen that the precipitated CaSnSiO5 crystals are square in shape, evenly distributed in the glaze, and have an average particle size of 2.1um.

[0066] The actual photo of the tin sphene crystal glaze prepared in this example is as follows: Figure 4 shown.

[0067] Depend on Figure 4 It can be seen that the color of the tinselite crystal glaze is light pink, the glaze surface has good gloss, and is smooth and flat.

[0068] Embodiment 2:

[0069] The invention discloses a method for preparing a tinstenite crystalline glaze, comprising the following steps: by weight, 22.5 parts of potassium feldspar, 50 parts of wollastonite, 3 parts of calcined kaolin, 2.5 parts of quartz, 5 parts of zinc oxide, 12 parts of tin oxide, 0.2 parts of chromium oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 120 minutes to obtain a glaze slurry; the glazing is then applied on a bisque-fired ceramic body by spraying glaze, and the glazing is then performed, and the tinstenite crystalline glaze is obtained by placing the ceramic body into a box-type electric furnace and heating the ceramic body to 1220°C at a heating rate of 10°C / min, and then the tinstenite crystalline glaze is obtained by heat preservation for 5 minutes and cooling.

[0070] The mass percentage in this embodiment is measured by XRF:

[0071] SiO2: 54.9%,

[0072] CaO: 19.7%,

[0073] ZnO: 5.4%,

[0074] Al2O3: 4.4%,

[0075] K2O: 3.3%,

[0076] SnO2: 12.1%,

[0077] Cr2O3:0.2%.

[0078] The reflectance spectrum of the tin sphene crystal glaze prepared in this example is as follows: Figure 3 shown.

[0079] Depend on Figure 3 It can be seen that the reflectivity curve of the glaze surface forms a broad absorption peak between 520nm-550nm, which indicates that there is reflected light in the red range.

[0080] The actual photo of the tin sphene crystal glaze prepared in this example is as follows: Figure 4 shown.

[0081] Depend on Figure 4It can be seen that the tin sphene crystals in the tin sphene crystal glaze are red, the crystals are evenly distributed in the glaze layer, the glaze surface has good gloss and is smooth.

[0082] Embodiment 3:

[0083] The invention discloses a method for preparing a tinstenite crystalline glaze, comprising the following steps: by weight, 26 parts of potassium feldspar, 47 parts of wollastonite, 2.9 parts of calcined kaolin, 2.5 parts of quartz, 7 parts of zinc oxide, 10 parts of tin oxide, 0.5 parts of chromium oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 120 minutes to obtain a glaze slurry; the glazing is then applied on a bisque-fired ceramic body by spraying glaze, and the glazing is then performed; the tinstenite crystalline glaze is then placed in a box-type electric furnace and heated to 1220°C at a heating rate of 10°C / min, and the mixture is kept warm for 10 minutes and cooled to obtain the tinstenite crystalline glaze.

[0084] The chemical composition was measured by XRF, and the mass percentage of the tin sphene crystal glaze in this embodiment was:

[0085] SiO2: 50.9%,

[0086] CaO: 20.4%,

[0087] ZnO: 6.5%,

[0088] Al2O3: 7.4%,

[0089] K2O: 4.9%,

[0090] SnO2: 9.4%,

[0091] Cr2O3:0.5%.

[0092] The reflectance spectrum of the tin sphene crystal glaze prepared in this example is as follows: Figure 3 shown.

[0093] Depend on Figure 3 It can be seen that the reflectivity curve of the glaze surface forms a broad absorption peak between 520nm-550nm, which indicates that there is reflected light in the red range.

[0094] The actual photo of the tin sphene crystal glaze prepared in this example is as follows: Figure 4 shown.

[0095] Depend on Figure 4 It can be seen that the color of the tinselite crystal glaze is dark red, the glaze surface has good gloss, and is smooth and flat.

[0096] Embodiment 4:

[0097] The invention discloses a method for preparing a tinstenite crystalline glaze, comprising the following steps: by weight, 28 parts of potassium feldspar, 45 parts of wollastonite, 3 parts of calcined kaolin, 2 parts of quartz, 7 parts of zinc oxide, 10 parts of tin oxide, 1 part of chromium oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 120 minutes to obtain a glaze slurry; the glazing is then applied on a bisque-fired ceramic body by spraying glaze, and the glazing is then performed; the tinstenite crystalline glaze is then placed in a box-type electric furnace and heated to 1220°C at a heating rate of 10°C / min, and then kept warm for 15 minutes and cooled to obtain the tinstenite crystalline glaze.

[0098] The mass percentages in this embodiment are measured by XRF:

[0099] SiO2: 50.6%,

[0100] CaO: 20.1%,

[0101] ZnO: 6.4%,

[0102] Al2O3: 6.6%,

[0103] K2O: 5.3%,

[0104] SnO2: 10%,

[0105] Cr2O3:1%.

[0106] The reflectance spectrum of the tin sphene crystal glaze prepared in this example is as follows: Figure 3 shown.

[0107] Depend on Figure 3 It can be seen that the reflectivity curve of the glaze surface forms a broad absorption peak between 520nm-550nm, which indicates that there is reflected light in the red range.

[0108] The actual photo of the tin sphene crystal glaze prepared in this example is as follows: Figure 4 shown.

[0109] Depend on Figure 4 It can be seen that the color of the tinselite crystal glaze is purple-red, the glaze surface has good gloss, and is smooth and flat.

[0110] Embodiment 5:

[0111] The preparation method of a tin sphene crystal glaze of the present invention comprises the following steps: by weight, 28 parts of potassium feldspar, 45 parts of wollastonite, 3 parts of calcined kaolin, 2 parts of quartz and 7 parts of zinc oxide are mixed evenly, and the mixture is placed in a box-type electric furnace and heated to 1400°C to form a frit. 85 parts of the frit, 10 parts of tin oxide, 1 part of chromium oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet ball milled for 120 minutes to form a glaze slurry, and then glaze is applied on a bisque-fired ceramic body by spraying glaze, and then the glaze is dried, and then the ceramic body is placed in a box-type electric furnace and heated to 1220°C at a heating rate of 10°C / min, and then the temperature is kept for 15 minutes and cooled to obtain the tin sphene crystal glaze.

[0112] The mass percentages in this embodiment are measured by XRF:

[0113] SiO2: 50.6%;

[0114] CaO: 20.1%,

[0115] ZnO: 6.4%,

[0116] Al2O3: 6.6%,

[0117] K2O: 5.3%,

[0118] SnO2: 10%,

[0119] Cr2O3:1%.

[0120] The reflectivity curve of the surface of the tin sphene crystal glaze layer prepared in this embodiment forms a broad absorption peak between 520nm-550nm, which can indicate that there is reflected light in the red range.

[0121] The tin sphene crystal glaze prepared in this embodiment is purple-red in color, and has a good glossiness and is flat and smooth.

[0122] Comparative Example 1 The content of CaO is different

[0123] A method for preparing a crystalline glaze comprises the following steps: by weight, 34.8 parts of potassium feldspar, 45 parts of wollastonite, 3 parts of calcined kaolin, 2 parts of quartz, 7 parts of zinc oxide, 10 parts of tin oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 120 minutes to obtain a glaze slurry; the glazing is then applied on a bisque-fired ceramic body by spraying the glaze, and the glazing is then performed; the ceramic body is then placed in a box-type electric furnace and heated to 1220°C at a heating rate of 10°C / min, and then kept warm for 15 minutes and cooled to obtain a tinstenite crystalline glaze.

[0124] According to XRF measurement, the mass percentage of SiO2 in this embodiment is 63.8%, and the mass percentage of CaO is 13.9%.

[0125] The X-ray diffraction pattern of the glaze of this comparative example is as follows Figure 5 As shown in Figure 1. Wuxi sphene crystal phase.

[0126] Comparative Example 2 without ZnO

[0127] The invention discloses a method for preparing a tin sphene crystal glaze, comprising the following steps: according to the following weight parts, 26 parts of potassium feldspar, 47 parts of wollastonite, 2.9 parts of calcined kaolin, 2.5 parts of quartz, 10 parts of tin oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 120 minutes to prepare a glaze slurry; glazing is then applied on a bisque-fired ceramic body by spraying glaze, and then drying is performed; and then the ceramic body is placed in a box-type electric furnace and heated to 1220°C at a heating rate of 10°C / min, and then kept warm for 10 minutes and cooled to obtain the tin sphene crystal glaze.

[0128] Figure 6 This is an optical image of the glaze prepared in Comparative Example 2.

[0129] After removing zinc oxide, the firing temperature of the glaze increased (the theoretical firing temperature increased, but the actual firing temperature was 1220℃, resulting in the melting point of the glaze layer not being reached and it did not melt into glass), and the glaze layer did not melt into glass.

[0130] Comparative Example 3

[0131] The invention discloses a method for preparing a tinstenite crystalline glaze, comprising the following steps: by weight, 100 parts of potassium feldspar, wollastonite, calcined kaolin, quartz, zinc oxide, tin oxide and chromium oxide and 0.375 parts of carboxymethyl cellulose are mixed and wet-milled for 120 minutes to obtain a glaze slurry; the glazing is then applied on a bisque-fired ceramic body by spraying glaze, and the glazing is then performed; the tinstenite crystalline glaze is then placed in a box-type electric furnace and heated to 1220°C at a heating rate of 10°C / min, and then the temperature is kept for 15 minutes and cooled to obtain the tinstenite crystalline glaze.

[0132] The mass percentage of each component in this embodiment is measured by XRF:

[0133] SiO2: 44.8%,

[0134] CaO: 27.9%,

[0135] ZnO: 4%,

[0136] Al2O3: 5%,

[0137] K2O: 6%,

[0138] SnO2: 11.8%,

[0139] Cr2O3: 0.5%.

[0140] Figure 7 This is an optical image of the glaze prepared in Comparative Example 3. There is too much calcium oxide, and the white substance on the surface is wollastonite.

[0141] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A tin sphene crystal glaze, characterized in that: The following components are included in mass percentage: SiO2: 50%~57% CaO: 18%~25% ZnO: 5%~8% Al2O3: 4%~9% K2O: 3%~6% SnO2: 8%~12.5% Cr2O3:0%~1%.

2. The tin sphene crystalline glaze according to claim 1, characterized in that: The following components are included in mass percentage: SiO2: 50%~55% CaO: 19%~23% ZnO: 5%~7% Al2O3: 4%~8% K2O: 3%~5.5% SnO2: 9%~12% Cr2O3: 0.2%~1%.

3. The tin sphene crystalline glaze according to claim 2, characterized in that: The following components are included in mass percentage: SiO2: 50~52%, CaO: 20-22%, ZnO: 6-7%, Al2O3: 7-8%, K2O: 4-5%, SnO2: 9-10%, Cr2O3: 0.4~0.6%.

4. The method for preparing the tin sphene crystalline glaze according to claim 1, characterized in that: The following steps are involved: The glaze and dispersant are mixed and wet-milled to form a glaze slurry, which is then applied to the ceramic body and fired to obtain the tinstenite crystal glaze.

5. The method for preparing the tin sphene crystalline glaze according to claim 4, characterized in that: The dispersant is at least one of carboxymethyl cellulose, sodium carboxymethyl cellulose and sodium tripolyphosphate; The raw materials of the glaze include: potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide, tin oxide and chromium oxide.

6. The method for preparing the tin sphene crystal glaze according to claim 5, characterized in that: The amounts of potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide and tin oxide are 22-28 parts, 45-50 parts, 2-3.5 parts, 2-3 parts, 5-8 parts and 9-12 parts by weight respectively; the amount of chromium oxide is 0-1 part by weight.

7. The method for preparing the tin sphene crystal glaze according to claim 6, characterized in that: The amounts of potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide and tin oxide are 25-27 parts, 46-48 parts, 2.5-3 parts, 2.2-2.8 parts, 6.5-7.5 parts and 9.5-10.5 parts by weight respectively; the amount of chromium oxide is 0.4-0.6 parts by weight.

8. The method for preparing the tin sphene crystal glaze according to claim 4, characterized in that: The mixing of the glaze and the dispersant refers to mixing potassium feldspar, calcined kaolin, wollastonite, quartz, zinc oxide, tin oxide, chromium oxide and the dispersant; or mixing potassium feldspar, calcined kaolin, wollastonite, quartz and zinc oxide to form a frit, and then mixing the frit, chromium oxide and the dispersant.

9. The method for preparing the tin sphene crystal glaze according to claim 4, characterized in that: The amount of the dispersant added is 0.3% to 0.8% of the total mass of the glaze; The wet ball milling time is 60min to 120min; The glazing method is one of spraying glaze, dipping glaze and pouring glaze; The firing is carried out at 1180° C. to 1225° C., and the heat preservation time is 5 min to 15 min.

10. The method for preparing the tin sphene crystal glaze according to claim 9, characterized in that: The specific operation of the firing is: heating the temperature to 1180° C. to 1225° C. at a heating rate of 10° C. / min to 20° C. / min, and then keeping the temperature for 5 min to 15 min.

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