Plum blossom glaze porcelain and preparation method thereof

Abstract

The invention relates to the technical field of ceramic processes, in particular to plum blossom glaze porcelain and a preparation method thereof. By providing the glaze slip components of the plum-blossom glaze porcelain and the firing process control method, stable plum-blossom-shaped patterns can be formed on the surface of the porcelain, the whole technological process is controllable, finally-formed porcelain finished products are stable in output, the whole technological time is greatly shortened compared with the prior art, and the production cost is reduced. Compared with the prior art, the energy consumption in the technological process is reduced, and the method has higher technical effects of engineering and automation.

Description

Technical Field

[0001] The present invention relates to the technical field of ceramic technology, and particularly relates to a plum blossom glaze porcelain and a preparation method thereof. Background Art

[0002] Ceramic products are widely used globally, and the technology for preparing ceramics is also very mature. The traditional method of decorating the surface of ceramics is to glaze the surface of the ceramic body. The glaze layer is smooth and has a high brightness, which can not only make the appearance of ceramic products more beautiful, but also increase the mechanical strength and is easier to wash. The kiln-transformed glaze means that when the ware is fired in the kiln, due to the presence of various color-forming elements in the kiln, after oxidation or reduction, an unexpected glaze color effect appears after leaving the kiln. The traditional kiln-transformed glaze is fired at medium to high temperatures, with a firing temperature above 1300 °C and a firing time mostly above 12 hours. Its high firing temperature, long time, and rough control of the firing process lead to large energy consumption, high cost, and unstable finished products. Summary of the Invention

[0003] In order to solve the above problems, the embodiments of the present application provide a plum blossom glaze porcelain and a preparation method thereof, which can achieve a glaze surface effect similar to blooming plum blossoms through a surface glaze component, and can achieve the forming temperature of the finished product and reduce the firing cost through precise temperature control.

[0004] In order to achieve the above object, the technical solutions adopted in the embodiments of the present application are as follows:

[0005] In a first aspect, a plum blossom glaze porcelain is provided, including a body blank and a bottom glaze layer and a surface glaze layer disposed on the surface of the body blank. The bottom glaze layer and the surface glaze layer are fired in an electric kiln in a medium-temperature oxidation atmosphere at a firing temperature of 1220 - 1260 °C, and the temperature is controlled based on time in the electric kiln through adaptive temperature compensation according to a configured firing curve; the surface glaze layer includes the following components: 35 - 45 parts of potassium feldspar, 16 - 25 parts of quartz, 1 - 4 parts of kaolin, 1 - 4 parts of dolomite, 20 - 30 parts of iron oxide, 10 - 20 parts of calcined talc, 10 - 20 parts of bovine bone ash, 1 - 5 parts of calcite, and 1 - 5 parts of frit.

[0006] Further, the thickness of the bottom glaze layer is 0.3 - 0.4 mm, and the thickness of the surface glaze layer is 0.3 - 0.5 mm.

[0007] Further, the surface glaze layer includes the following components: 30 parts of potassium feldspar, 15 parts of quartz, 3 parts of kaolin, 3 parts of dolomite, 20 parts of iron oxide, 12 parts of calcined talc, 12 parts of bovine bone ash, 3 parts of calcite, and 2 parts of frit.

[0008] Further, the surface glaze layer comprises the following components: 32 parts of potassium feldspar, 14 parts of quartz, 2.5 parts of kaolin, 2.5 parts of dolomite, 20 parts of iron oxide, 12 parts of calcined talc, 11 parts of bovine bone ash, 3 parts of calcite, and 3 parts of frit.

[0009] Further, the frit comprises the following components: 53% of SiO2, 10% of Al2O3, 13.5% of CaO, 3.5% of MgO, 4.2% of K2O, 1.5% of Na2O, 10.5% of B2O3, and 1.5% of BaO.

[0010] In a second aspect, a method for preparing plum blossom glaze porcelain is provided for preparing the plum blossom glaze porcelain described in any one of the above, comprising the following steps: proportioning the components of the surface glaze layer, ball milling with water to obtain glaze slurries respectively, controlling the concentration of the glaze slurries to be 50-58 Baume degrees, and applying the glaze slurries on the underglaze layer to form a surface glaze layer with a thickness of 0.3-0.5 mm; feeding the glazed blank into an electric kiln, controlling the temperature based on time change with an oxidation atmosphere and a configured firing curve through adaptive temperature compensation, after the electric kiln reaches the firing temperature, cooling down uniformly to natural cooling, and the total firing time is 5-7 hours; the firing temperature is 1220-1260 °C.

[0011] Further, the mass ratio of material:ball:water in the wet ball milling is 1:1.5-2:0.6, and the wet ball milling time is 1 h-3 h; after wet ball milling, screening through a 100-120 mesh sieve, the fineness of the glaze slurry is 250 mesh sieve, and the residue on the sieve is 0.02%-0.1%.

[0012] Further, the moisture content of the glazed blank before entering the electric kiln is 1-2%.

[0013] Further, the adaptive temperature compensation obtains the predicted temperature at the next time point through the current temperature and a temperature prediction model, determines the temperature difference based on the predicted temperature and the standard temperature of the firing curve, determines the target output power of the electric kiln based on the temperature difference, and adjusts the current temperature based on the target output power.

[0014] Further, the temperature prediction model includes an input state estimate and an output state estimate. The input state estimate is used for estimating the state of the temperature at the next time point, and the output state estimate is used for estimating the state of the output power at the current time point; obtaining the predicted temperature at the next time point through the current temperature and the temperature prediction model includes: filtering and estimating the state vector in the input state estimate through Kalman filtering, then updating and optimizing the output matrix in the output state estimate through maximum correlation entropy, and obtaining the predicted temperature at the next time point and the target output power at the current time point based on the optimized state vector and output matrix.

[0015] In the technical solution provided by the embodiments of the present application, by providing a glaze composition for plum blossom glaze porcelain and a firing process control method, it is possible to form a stable plum blossom-shaped pattern on the surface of the porcelain, and the overall process is controllable, and the output of the finally formed porcelain products is relatively stable. The overall process time is greatly shortened compared with the prior art, the energy consumption in the process is reduced, and it has higher engineering and automation technical effects compared with the prior art. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings required for the description of the embodiments. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained according to these drawings.

[0017] Figure 1 It is a flowchart of the method for preparing plum blossom glaze porcelain provided by the embodiments of the present application.

[0018] Figure 2 It is a schematic diagram of the surface result of the plum blossom glaze porcelain provided by the embodiments of the present application. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0019] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. For those conditions not specified in the embodiments, they are carried out according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments not specified in the manufacturer are all conventional products that can be obtained through commercial purchase. The following described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art without creative efforts in combination with the embodiments of the present invention belong to the scope of protection of the present invention.

[0020] The embodiments of the present application provide a porcelain that can present a plum blossom-shaped pattern on the surface. The fired porcelain glaze has a brownish color, and a large number of red, pink, and peach blossom-like plum blossoms of different sizes are naturally formed in the brownish color, having a unique artistic effect.

[0021] Specifically, the plum blossom glaze porcelain in this embodiment includes a plain body and an underglaze layer and a top glaze layer disposed on the surface of the plain body. Among them, in this embodiment, in order to form a plum blossom-shaped pattern on the surface of the porcelain, the top glaze layer is configured, and based on the medium-temperature oxidation atmosphere, adaptive temperature compensation control is used to realize the expression of the pattern on the porcelain glaze. Among them, the adaptive temperature compensation control realizes precise control during the porcelain firing process by eliminating various system noises during the electric kiln heating process, thereby making the formation of the pattern on the top glaze layer more stable and reducing the firing cost caused by rough temperature control in the prior art firing process.

[0022] In the embodiment of the present application, the top glaze layer of the plum blossom glaze porcelain in this embodiment includes the following components by weight:

[0023] 30-45 parts of potassium feldspar, 14-25 parts of quartz, 1-4 parts of kaolin, 1-4 parts of dolomite, 20-30 parts of iron oxide, 10-20 parts of calcined talc, 10-20 parts of bovine bone ash, 1-5 parts of calcite, 1-5 parts of frit.

[0024] In this embodiment, the bovine bone ash belongs to phosphate, and the phase separation effect is achieved by introducing bovine bone ash. The structural feature of the plum blossom kiln-varied glaze in this embodiment is that isolated round crystals of different sizes, shaped like red plum blossoms, are distributed in the continuous matrix phase. Its generation mechanism is that iron oxide presents red crystallization into crystals of different sizes in the oxidation atmosphere. The number and size of these phase-separated round bodies significantly affect the artistic appearance of the ceramic glaze. Among them, in this embodiment, by adding bovine bone ash, the average size of the phase-separated isolated circles of the plum blossom kiln glaze is 10 mm, and some are less than 3 mm. By adding bovine bone ash, the display of the plum blossom-shaped pattern on the glaze surface is more vivid and three-dimensional.

[0025] Specifically, the frit in this embodiment includes the following components:

[0026] 53% of SiO2, 10% of Al2O3, 13.5% of CaO, 3.5% of MgO, 4.2% of K2O, 1.5% of Na2O, 10.5% of B2O3, 1.5% of BaO.

[0027] Among them, for the frit used in this embodiment, the proportions of boric acid and calcite are relatively high. The use of boric acid and calcite can increase the degree of vitrification of the glaze, reduce the melting temperature of the glass phase, thereby increasing the transparency of the glaze and making the glaze surface present a smooth and bright visual effect. It can improve the toughness of the glaze, make the glaze surface harder and not easily cracked. And by adding boric acid, it can promote the formation of the glass phase, increase the content of the glass phase in the glaze, thereby enhancing the toughness of the glaze surface. It can adjust the melting temperature to make the melting temperature of the glaze lower. Therefore, the addition of boric acid can effectively reduce the sintering time of the glaze.

[0028] Refer to Figure 1 , in this embodiment, for the composition of the plum blossom glaze porcelain described above, a corresponding preparation method is also provided to realize the firing of the plum blossom glaze porcelain, which specifically includes the following steps:

[0029] Step S11. Weigh the components of the surface glaze layer according to the proportion, add water and ball mill them to obtain glaze slurries respectively. Control the concentration of the glaze slurries to be 50-58 Baumé degrees, and apply the glaze slurries on the underglaze layer to form a surface glaze layer with a thickness of 0.3-0.5 mm.

[0030] In this embodiment, for the components of the surface glaze layer, i.e.: 30-45 parts of potassium feldspar, 14-25 parts of quartz, 1-4 parts of kaolin, 1-4 parts of dolomite, 20-30 parts of iron oxide, 10-20 parts of burnt talc, 10-20 parts of bovine bone ash, 1-5 parts of calcite, 1-5 parts of frit; among which the frit is: 53% of SiO2, 10% of Al2O3, 13.5% of CaO, 3.5% of MgO, 4.2% of K2O, 1.5% of Na2O, 10.5% of B2O3, 1.5% of BaO.

[0031] Since this embodiment mainly provides a porcelain product with a plum blossom-shaped glaze surface, it is only necessary to develop the components of the surface glaze layer in this embodiment. For the inner glaze layer, the existing inner glaze layer in the prior art can be directly used. Apply any inner glaze layer on the inner surface of the dried and repaired blank body, control the thickness of its glaze layer to be 0.3 mm and make its outer edge clean. Then apply the glaze slurry with the above components on the outside of the blank body and control the thickness of the surface glaze layer to be 0.45 mm.

[0032] Among them, the glaze slurries in this embodiment are obtained by ball milling with water. The mass ratio of materials, balls, and water in the ball milling with water in this embodiment is 1:1.5-2:0.6, and the wet ball milling time is 1 h-3 h. After ball milling with water, it is sieved through a 100-120 mesh sieve, and the fineness of the glaze slurry is 250 mesh sieve, and the sieve residue is 0.02%-0.1%.

[0033] Add clear water to the slurry after ball milling with water and adjust the concentration of the glaze slurry to 55.

[0034] Step S12. Send the glazed blank into an electric kiln, control the temperature based on time change with an oxidation atmosphere and a configured firing curve through adaptive temperature compensation. After the electric kiln reaches the firing temperature, cool it down evenly until natural cooling.

[0035] Before this process, it is also necessary to control the moisture content of the glazed blank before entering the kiln to ensure that the moisture content of the glazed blank entering the electric kiln is 1-2%.

[0036] Among them, regarding the firing process, in this embodiment, a medium-temperature oxidation atmosphere one-time firing process is adopted. The firing temperature is 1220 - 1260 °C, and the total firing time is 5 - 7 hours.

[0037] For ceramic finished products, the firing temperature is an important factor affecting the final color of the glaze surface, and is the main reason for the difference between yellow and brown in medium-temperature multi-color glazes. The difference between these two colors is also a key factor in the formation of plum blossom-shaped patterns. During the firing process of medium-temperature multi-color glazes, there are two key stages: the oxidation stage and the reduction stage. The starting temperature point of strong oxidation has an important impact on the final color of the porcelain glaze. If the starting temperature point of strong oxidation is relatively low and the reduction time is short, there will be more organic matter residues in the glaze. These organic matters do not undergo physical changes at high temperatures, thus affecting the shape of the glaze surface. On the contrary, if the starting temperature point of strong oxidation is too high and the reduction time is long, the glaze surface will melt, which hinders the penetration of the oxidation atmosphere into the iron oxide ions in the glaze layer, thereby affecting the final color of the glaze surface. Therefore, the effect of multi-color porcelain finished products depends not only on the composition of the surface glaze layer, but also on the temperature control during the firing process.

[0038] Therefore, in the prior art, in order to ensure that the temperature control can match the firing process, a firing curve is generally configured. The control of the electric kiln can real-time control the temperature in the kiln through the firing curve to ensure the matching of the porcelain firing process and the temperature control, so that the glaze color and pattern of the porcelain out of the kiln match the expected ones.

[0039] However, it should be noted that the temperature environment in the kiln is not an ideal fixed steady state. In actual production, the temperature in the kiln is often affected by various factors, such as raw material properties, environmental temperature, heating method, environmental conditions, etc. These factors will all generate certain random noises. Therefore, temperature control has a certain degree of difficulty. During the firing process, the generation of noise may be caused by the random fluctuations of various factors. This kind of noise may cause the temperature to deviate from the target temperature. Therefore, measures need to be taken to reduce the influence of the noise to ensure the stability and accuracy of the sintering temperature. Generally, in the prior art, the PID control logic is usually adopted. However, because the firing process is a complex process with time delay and noise, and there are complex physical and chemical reactions in the kiln during the firing process, the traditional PID is a linear controller and it is difficult to meet the requirements.

[0040] Therefore, in this embodiment, in order to accurately control the temperature during the firing process, the firing curve is optimized through an adaptive temperature compensation method, and the temperature is controlled based on time changes through a model prediction logic.

[0041] Specifically, the adaptive temperature compensation in this embodiment is to obtain the predicted temperature at the next time point through the current temperature and the temperature prediction model, and determine whether there is a difference between the predicted temperature and the standard temperature of the firing curve and the temperature difference. Based on this temperature difference, the target output power of the electric kiln at the current time point is determined, and the current temperature is adjusted based on this target output power to cause the temperature to change until the temperature at the next time point conforms to the standard temperature corresponding to the firing curve.

[0042] Among them, the temperature prediction model in this embodiment is a function model, including input state and output state estimation. Among them, the input state estimation is used to estimate the temperature at the next time point, and the output state estimation is used to estimate the state of the output power at the current time point.

[0043] For obtaining the predicted temperature at the next time point through the current temperature and the temperature prediction model, in order to ensure the accuracy of the prediction result, it is necessary to reduce the interference of noise in the environment on the result. In this embodiment, the influence of noise needs to be eliminated. Among them, the noise corresponding to the temperature in the kiln includes Gaussian noise and non-Gaussian noise according to its manifestation form. In this embodiment, the Gaussian noise is eliminated by Kalman filtering, and the non-Gaussian noise is eliminated by maximum correlation entropy.

[0044] Specifically, regarding the prediction process, first, the state vector in the input state estimation is filtered and estimated by Kalman filtering, then the output matrix in the output state estimation is updated and optimized by maximum correlation entropy, and the predicted temperature at the next time point and the target output power at the current time point are obtained through the optimized state vector and output matrix.

[0045] In this embodiment, the above temperature control process is described in detail. First, the temperature prediction model in this embodiment is represented based on the following formula: Where x(k) is the state vector at time k, x(k + 1) is the state vector at time k + 1, A is the state matrix, B is the transfer matrix, F is the covariance matrix, Δu(k) is the control increment, y(k) is the output vector, Z is the output matrix, and w(k) and v(k) are random noises following a random distribution.

[0046] Among them, the output vector refers to the predicted temperature value of the model output, the control increment refers to the control increment for controlling the current output power of the electric kiln, and the logic of this temperature prediction model is to determine the control increment by obtaining the temperature prediction value at a certain moment, and realize the temperature control of the electric kiln through this control increment.

[0047] It can be seen from this that in order to accurately determine the control increment, it is necessary to accurately obtain the temperature prediction value in the electric kiln temperature system. And because there is noise interfering with the temperature change in the system, it is necessary to exclude the interference of the noise on the prediction process when determining the temperature prediction value, so as to improve the accuracy of determining the control increment.

[0048] In this embodiment, the noise existing in the system includes Gaussian noise and non-Gaussian noise according to its distribution characteristics, and different filtering methods are used to filter the above two noises respectively.

[0049] First, the Kalman filter is used to process the Gaussian noise in the state vector noise of the input state estimation. According to the Kalman filter principle, the state x(k) is updated and filtered, and finally the updated and processed The Kalman filter uses the minimum variance estimation. By continuously extracting information from the measurement values and predicting the current state, the state is estimated. The specific processing process is to first assign initial values to the initial prediction error covariance matrix and the initial state, and calculate the optimal prediction of the state variable. Specifically, according to the optimal state value at the previous moment and the input increment Δu(k - 1), let The optimal prediction value of the state vector is expressed based on the following formula: The prediction error covariance matrix is expressed based on the following formula: p(k|k - 1) = AP(k - 1)A T +Q k , where Q k is the prediction value covariance matrix. Calculate the Kalman filter gain, error covariance, and update error respectively, and further obtain the input variable and output variable. Based on the calculation of the optimal prediction of the state variable and the covariance matrix of the prediction error, and perform the iteration of the above process to obtain the optimal estimated state value.

[0050] In this embodiment, the maximum correlation entropy is used to filter the non-Gaussian noise introduced during the firing process for updating the output matrix Z. The processing process first determines the correlation entropy threshold and initializes the weight vector, calculates the maximum correlation entropy using the current weight vector, and calculates the constraint vector when the correlation entropy reaches the maximum value under the current weight vector according to the definition of the maximum correlation entropy. According to the error vector between the current weight vector and the constraint vector, if the norm of the error vector is less than the threshold, the calculation is completed; otherwise, the weight vector is updated using the gradient descent method according to the error vector, and the iteration calculation is performed until the norm of the error vector is less than the threshold to achieve the convergence of the weight vector.

[0051] In this embodiment, through the above filtering process, the problem of inaccurate results caused by system noise during the determination of the state vector and output matrix can be eliminated. Output prediction is performed on the state vector and output matrix after filtering. Specifically, the prediction error of the temperature in the kiln in this embodiment can be defined as: e(k+i) = y p (k) - y(k), where y p (k) represents the actual measured value of the temperature at time k, and y(k) represents the predicted value of the temperature at time k. The temperature prediction error based on feedback correction is expressed based on the following formula: e(k+1) = e(k) + h i [e(k) - e(k-1)], where for h i represents the prediction time domain, and its matrix-vector expression can be expressed based on the following formula: The corrected model prediction output is: y c (k+i) = y(k+i) + h i e(k+1).

[0052] In this embodiment, a firing curve is configured in the electric kiln. In order to enable the control method to make the temperature in the kiln track the firing curve, a corresponding control reference trajectory is configured and expressed based on the following formula: y r (k+i) = α i y p (k) + (1 - α i )y s (k), where y r (k+i) is the desired control reference trajectory, y s (k) is the configured firing curve, α = exp(-T s / T r ) is the softening factor, T s is the sampling time, and T r is the time constant. The matrix form corresponding to this control reference trajectory can be expressed as: where I = [1 1 … 1] T is the model prediction error correction matrix,

[0053] Based on the above model, the state vector is updated, and the updated state vector is: X = Fx(k) + φΔu(k), where where O is a zero matrix of (2n + d), and the output matrix can be expressed as: where G = {Z1, Z2, …, Z p} is p × {(2n + d - 1) × p}. And according to the updated state vector, the prediction output is corrected, and the corrected prediction output is expressed as: Taking the partial derivative of the predicted output with respect to the target cost optimization function, the control increment can be obtained as: kΔU = M r [Y r -Y c , where M r =[φ T C T Q r Cφ + R] -1 φ T G T Q r .

[0054] For the control increment at time k in the electric kiln temperature control process, it can be expressed as: Δu(k)= -m1x(k)-m2e(k)-m3 + m4y p (k)+m5y s (k), where m1, m2, m3, m4, and m5 are each row of matrices M1, M2, M3, M4, and M5 respectively. Through the above processing, the output power control quantity for the electric kiln can finally be obtained as: u(k)= u(k - 1)+Δu(k).

[0055] In this embodiment, through the above steps S11 - S12, various types of noises in the electric kiln temperature control process can be eliminated, and precise control of the temperature inside the electric kiln can be achieved through non - minimum state - space control logic.

[0056] Refer to Figure 2 , for the porcelain product fired by controlling the above glaze layer components and firing process, the fired porcelain glaze has a brownish - red color, and a large number of red, pink, and peach - red "plum blossoms" of different sizes are naturally formed in the brownish - red color, looking like a riot of flowers, extremely beautiful, natural and crystal - clear, with a unique artistic effect.

[0057] The following specific examples are used to further illustrate the specific composition and firing process of the plum - blossom glaze porcelain of the present invention.

[0058] Example 1

[0059] A kind of plum - blossom glaze porcelain includes a body blank and a bottom glaze layer and a surface glaze layer disposed on the surface of the body blank. Among them, for the surface glaze layer, by weight, it includes the following components:

[0060] Potassium feldspar 30 parts, quartz 15 parts, kaolin 3 parts, dolomite 3 parts, iron oxide 20 parts, calcined talc 12 parts, bone ash 12 parts, calcite 3 parts, frit 2 parts.

[0061] The specific steps are as follows:

[0062] Step 1. Weigh and proportion the above weights, add water and ball mill to obtain glaze slurries respectively. The mass ratio of material:ball:water is 1:1.5 - 2:0.6 for wet ball milling for 2 hours. After ball milling, sieve through a 100-mesh sieve. The fineness of the glaze slurry is such that the residue on a 250-mesh sieve is 0.04%, and add clear water to adjust the glaze slurry concentration to 55 Baumé concentration.

[0063] Step 2. Apply an inner glaze randomly on the inner surface of the dried and trimmed ceramic blank. The thickness of the glaze layer is 0.3 mm. Wipe clean the zero glaze on the outer edge, and dip the above blank into the glaze slurry with the concentration adjusted to 55 Baumé concentration. Control the thickness of the glaze layer to be 0.45 mm and control the moisture content to be 1 - 2%.

[0064] Step 3. Send the glazed blank into an electric kiln, control the temperature based on time change with an oxidation atmosphere and through adaptive temperature compensation according to the configured firing curve. After the electric kiln reaches 1260 °C, cool down evenly until natural cooling, and control the total firing time to be 6.5 hours.

[0065] Example 2

[0066] A plum blossom glaze porcelain includes a plain blank and a bottom glaze layer and a top glaze layer disposed on the surface of the plain blank. Among them, for the top glaze layer, it includes the following components by weight:

[0067] 32 parts of potassium feldspar, 14 parts of quartz, 2.5 parts of kaolin, 2.5 parts of dolomite, 20 parts of iron oxide, 12 parts of burnt talc, 11 parts of bovine bone ash, 3 parts of calcite, 3 parts of frit.

[0068] The specific steps are as follows:

[0069] Step 1. Weigh and proportion the above weights, add water and ball mill to obtain glaze slurries respectively. The mass ratio of material:ball:water is 1:1.5 - 2:0.6 for wet ball milling for 2 hours. After ball milling, sieve through a 110-mesh sieve. The fineness of the glaze slurry is such that the residue on a 250-mesh sieve is 0.04%, and add clear water to adjust the glaze slurry concentration to 55 Baumé concentration.

[0070] Step 2. Apply an inner glaze randomly on the inner surface of the dried and trimmed ceramic blank. The thickness of the glaze layer is 0.3 mm. Wipe clean the zero glaze on the outer edge, and dip the above blank into the glaze slurry with the concentration adjusted to 55 Baumé concentration. Control the thickness of the glaze layer to be 0.45 mm and control the moisture content to be 1 - 2%.

[0071] Step 3. Send the glazed blank into an electric kiln, control the temperature based on time change with an oxidation atmosphere and through adaptive temperature compensation according to the configured firing curve. After the electric kiln reaches 1240 °C, cool down evenly until natural cooling, and control the total firing time to be 6 hours.

[0072] Example 3

[0073] A plum blossom glaze porcelain, comprising a plain body and an underglaze layer and a top glaze layer disposed on the surface of the plain body. Among them, the top glaze layer comprises the following components by weight:

[0074] 38 parts of potassium feldspar, 21 parts of quartz, 3.5 parts of kaolin, 3 parts of dolomite, 26 parts of iron oxide, 14 parts of calcined talc, 16 parts of bovine bone ash, 4 parts of calcite, and 3 parts of frit.

[0075] The specific steps are as follows:

[0076] Step 1. Weigh and proportion the above weights, and prepare glaze slurries respectively after wet ball milling with water. The mass ratio of material:ball:water is 1:1.5 - 2:0.6 for wet ball milling for 2.5 h. After ball milling, pass through a 100-mesh sieve. The fineness of the glaze slurry passes through a 250-mesh sieve with a residue of 0.04%, and add clear water to adjust the concentration of the glaze slurry to 55 Baumé.

[0077] Step 2. Apply any inner glaze on the inner surface of the dried and repaired ceramic body. The thickness of the glaze layer is 0.3 mm. Wipe clean the zero glaze at the outer edge, and dip the above blank into the glaze slurry with the concentration adjusted to 55 Baumé. Control the thickness of the glaze layer at 0.45 mm, and control the moisture content at 1 - 2%.

[0078] Step 3. Send the glazed blank into an electric kiln, and control the temperature based on time change with an oxidation atmosphere and a configured firing curve through adaptive temperature compensation. After the electric kiln reaches 1220 °C, cool down evenly to natural cooling, and control the total firing time to be 5 hours.

[0079] Example 4

[0080] A plum blossom glaze porcelain, comprising a plain body and an underglaze layer and a top glaze layer disposed on the surface of the plain body. Among them, the top glaze layer comprises the following components by weight:

[0081] 45 parts of potassium feldspar, 25 parts of quartz, 2 parts of kaolin, 2 parts of dolomite, 28 parts of iron oxide, 18 parts of calcined talc, 19 parts of bovine bone ash, 5 parts of calcite, and 4 parts of frit.

[0082] The specific steps are as follows:

[0083] Step 1. Weigh and proportion the above weights, and prepare glaze slurries respectively after wet ball milling with water. The mass ratio of material:ball:water is 1:1.5 - 2:0.6 for wet ball milling for 2 h. After ball milling, pass through a 110-mesh sieve. The fineness of the glaze slurry passes through a 250-mesh sieve with a residue of 0.04%, and add clear water to adjust the concentration of the glaze slurry to 55 Baumé.

[0084] Step 2. Apply an inner glaze on the inner surface of the dried and trimmed ceramic blank. The thickness of the glaze layer is 0.3 mm. Wipe clean the zero glaze on the outer edge of the blank, and dip the above blank into the glaze slurry with the concentration adjusted to 55 Baumé. Control the thickness of the glaze layer at 0.45 mm and control the moisture content at 1-2%.

[0085] Step 3. Send the glazed blank into an electric kiln. Control the temperature based on time change with an oxidation atmosphere and a configured firing curve through adaptive temperature compensation. After the electric kiln reaches 1250 °C, cool it down evenly until natural cooling, and control the total firing time at 6.5 hours.

[0086] Example Five

[0087] A plum blossom glaze porcelain includes a plain blank and a bottom glaze layer and a top glaze layer disposed on the surface of the plain blank. Among them, the top glaze layer includes the following components by weight:

[0088] 45 parts of potassium feldspar, 25 parts of quartz, 1 part of kaolin, 1 part of dolomite, 30 parts of iron oxide, 20 parts of calcined talc, 20 parts of bovine bone ash, 5 parts of calcite, 5 parts of frit.

[0089] The specific steps are as follows:

[0090] Step 1. Weigh and prepare the above weights, and respectively prepare glaze slurries after wet ball milling with water. The mass ratio of material:ball:water is 1:1.5-2:0.6 for wet ball milling for 2 h. After ball milling, pass through a 110-mesh sieve, and the fineness of the glaze slurry passing through a 250-mesh sieve has a residue of 0.04%, and add clear water to adjust the concentration of the glaze slurry to 55 Baumé.

[0091] Step 2. Apply an inner glaze on the inner surface of the dried and trimmed ceramic blank. The thickness of the glaze layer is 0.3 mm. Wipe clean the zero glaze on the outer edge of the blank, and dip the above blank into the glaze slurry with the concentration adjusted to 55 Baumé. Control the thickness of the glaze layer at 0.45 mm and control the moisture content at 1-2%.

[0092] Step 3. Send the glazed blank into an electric kiln. Control the temperature based on time change with an oxidation atmosphere and a configured firing curve through adaptive temperature compensation. After the electric kiln reaches 1230 °C, cool it down evenly until natural cooling, and control the total firing time at 5.5 hours.

[0093] In this embodiment, among the above embodiments, the optimal embodiments are Example One and Example Two.

[0094] Through the components of the plum blossom glaze porcelain provided by the above embodiments and the process control process, it is possible to form a plum blossom-shaped pattern on the surface of the porcelain, and the porcelain products finally formed through the process of the above embodiments are relatively stable in output, and can directly shorten the overall process time, reduce the energy consumption in the process, and have higher technical advantages in engineering and automation compared with the prior art.

[0095] The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A plum blossom glaze porcelain, comprising a plain body, an inner glaze layer disposed on the inner surface of the plain body, and a surface glaze layer on the outer surface of the plain body, characterized in that, The bottom glaze layer and the top glaze layer are fired in an electric kiln under a medium-temperature oxidation atmosphere at a firing temperature of 1220 - 1260°C, and the temperature is controlled based on time variation with a configured firing curve through adaptive temperature compensation in the electric kiln; the top glaze layer includes the following components by weight: 30 - 45 parts of potassium feldspar, 14 - 25 parts of quartz, 1 - 4 parts of kaolin, 1 - 4 parts of dolomite, 20 - 30 parts of iron oxide, 10 - 20 parts of calcined talc, 10 - 20 parts of bovine bone ash, 1 - 5 parts of calcite, 1 - 5 parts of frit.

2. The plum blossom glaze porcelain according to claim 1, characterized in that, The thickness of the bottom glaze layer is 0.3 - 0.4 mm, and the thickness of the top glaze layer is 0.3 - 0.5 mm.

3. The plum blossom glaze porcelain according to claim 1, characterized in that, The top glaze layer includes the following components: 30 parts of potassium feldspar, 15 parts of quartz, 3 parts of kaolin, 3 parts of dolomite, 20 parts of iron oxide, 12 parts of calcined talc, 12 parts of bovine bone ash, 3 parts of calcite, 2 parts of frit.

4. The plum blossom glaze porcelain according to claim 1, characterized in that, The top glaze layer includes the following components: 32 parts of potassium feldspar, 14 parts of quartz, 2.5 parts of kaolin, 2.5 parts of dolomite, 20 parts of iron oxide, 12 parts of calcined talc, 11 parts of bovine bone ash, 3 parts of calcite, 3 parts of frit.

5. The plum blossom glaze porcelain according to any one of claims 1-4, characterized in that, The frit includes the following components: 53% of SiO2, 10% of Al2O3, 13.5% of CaO, 3.5% of MgO, 4.2% of K2O, 1.5% of Na2O, 10.5% of B2O3, 1.5% of BaO.

6. A method for preparing plum blossom glaze porcelain, characterized in that, The method for preparing the plum blossom glaze porcelain according to any one of claims 1 - 5 includes the following steps: Weigh the components of the top glaze layer according to the ratio, add water and ball mill them respectively to obtain glaze slurries, control the concentration of the glaze slurries to be 50 - 58 Baume degrees, and apply the glaze slurries on the bottom glaze layer to form a top glaze layer with a thickness of 0.3 - 0.5 mm; Send the glazed blank into the electric kiln, control the temperature based on time variation with a configured firing curve under an oxidation atmosphere through adaptive temperature compensation. After the electric kiln reaches the firing temperature, cool it down uniformly until natural cooling, and the total firing time is 5 - 7 hours; the firing temperature is 1220 - 1260°C.

7. The method for preparing plum blossom glaze porcelain according to claim 6, characterized in that, The mass ratio of the material, balls, and water in the wet ball mill is 1:1.5 - 2:0.6, and the wet ball milling time is 1 h - 3 h; after wet ball milling, pass through a 100 - 120 - mesh sieve, the fineness of the glaze slurry is 250 - mesh sieve, and the sieve residue is 0.02% - 0.1%.

8. The method for preparing plum blossom glaze porcelain according to claim 6, characterized in that, The moisture content of the glazed blank before entering the electric kiln is 1 - 2%.

9. The method for preparing plum blossom glaze porcelain according to claim 6, characterized in that, The adaptive temperature compensation obtains the predicted temperature at the next time point through the current temperature and the temperature prediction model, determines the temperature difference based on the predicted temperature and the standard temperature of the firing curve, determines the target output power of the electric kiln based on the temperature difference, and adjusts the current temperature based on the target output power.

10. The preparation method of the plum blossom glaze porcelain according to claim 9, characterized in that, The temperature prediction model includes an input state estimate and an output state estimate. The input state estimate is used for the state estimate of the temperature at the next time point, and the output state estimate is used for the state estimate of the output power at the current time point; Obtaining the predicted temperature at the next time point through the current temperature and the temperature prediction model includes: filtering and estimating the state vector in the input state estimate through Kalman filtering, and then updating and optimizing the output matrix in the output state estimate through maximum correlation entropy. Based on the optimized state vector and output matrix, the predicted temperature at the next time point and the target output power at the current time point are obtained.

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