CN115745635B - Production method of combined ceramic wire drawing crucible - Google Patents
Production method of combined ceramic wire drawing crucible Download PDFInfo
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- CN115745635B CN115745635B CN202211528277.2A CN202211528277A CN115745635B CN 115745635 B CN115745635 B CN 115745635B CN 202211528277 A CN202211528277 A CN 202211528277A CN 115745635 B CN115745635 B CN 115745635B
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Abstract
The invention discloses a production method of a combined ceramic wire drawing crucible, which belongs to the technical field of wire drawing equipment and comprises the following steps of preparing raw materials in the first step, mixing the raw materials in the second step, molding and drying in the third step, sintering a product in the fourth step and sintering a product in the fifth step; the invention cures and sinters the embedded body with anti-scouring fluid holes and the high thermal shock main body into a whole to obtain the combined ceramic wire-drawing crucible product with high thermal shock resistance, high anti-scouring property and long service life, which can be well applied to the glass fiber and metal wire-drawing fields.
Description
Technical Field
The invention belongs to the technical field of wire drawing equipment, and is mainly applied to the field of glass fiber and metal wire drawing, in particular relates to a production method of a combined ceramic wire drawing crucible.
Background
Glass fiber and metal fiber are used as an important material, and are widely applied to various technical fields such as science and technology, national defense and civil industry, electronic technology, semiconductors, optics, new energy and the like, for example, blades of wind power generation, lightweight components of aerospace equipment, platinum wires of temperature measuring thermocouples, optical fiber wires, electric insulation materials, heat insulation materials, circuit substrates and the like; at present, the glass fiber or metal wiredrawing process mostly uses a vertical self-flow method for cooling and molding, and the service life of the bottom leak hole of the crucible carrier directly determines the production efficiency, the production quality and the production cost.
The crucible carrier for carrying the glass solution or the metal solution is widely made of clay or platinum, and the crucible carrier is of an integrated structure with a bottom leak hole, but because the temperature of the glass solution or the metal solution is above 1350 ℃, and the crucible carrier for continuously heating the solution is required to be supplied with the temperature, the crucible carrier is easy to deform, crack, have short service life, pollute the solution and other objective factors influencing the quality of the final product in the use process, and the platinum crucible has very high price and very high use cost.
When the glass fiber and the metal wire are scoured and eroded to a certain extent or eroded due to high-temperature active chemical reaction, a new crucible carrier needs to be replaced by stopping production, so that the cost is high, the loss of stopping production and maintenance is huge, and huge cost difficulties and production troubles are caused for glass fiber and metal wire manufacturing enterprises.
Disclosure of Invention
The invention provides a production method of a combined ceramic wire drawing crucible, which optimizes the formula and the proportion of raw materials, adjusts the working procedures and parameters of a process, and uses wire drawing heads with different densities and a crucible body for combined molding so as to solve the defects described in the prior art.
The technical scheme adopted by the invention is as follows:
the production method of the combined ceramic wire drawing crucible is characterized by comprising the following steps of:
step one, raw material preparation:
weighing the component formula of the first part of crucible main body for standby, wherein the weight percentage of the component formula comprises the following components in percentage by mass: 67% or more zirconium dioxide material Zr02 or less than 79%, 1% or less yttrium oxide material Y203 or less than 3%, 10% or less zirconium mullite material Azs or less than 15%, 6% or less kyanite Al2[ SIO4] O or less than 8%, 3% or less corundum material alpha-Al 2O3 or less than 5%, 1% or less alumina powder material alpha-Al 2O3 or less than 2%;
weighing the component formula of the second part of embedded body for standby, wherein the weight percentage of the component formula comprises the following components in percentage by mass: zirconium dioxide material Zr02 is more than or equal to 94% and less than or equal to 96.8%, silicon dioxide material SiO2 is more than or equal to 0.2% and less than or equal to 1%, yttrium oxide material Y203 is more than or equal to 3% and less than or equal to 5%;
step two, mixing raw materials:
the two raw materials for standby in the weighing step are distinguished, polyurethane mixing dispersion balls are additionally added according to the proportion of 7% -12% of the total mass of the mixed materials in each part, the polyurethane mixing dispersion balls are fed into three-dimensional mixing equipment for mixing respectively, the mixing time is 10-16 hours, and the two raw materials are taken out for standby after being mixed respectively;
step three, molding and drying:
dividing the second step to obtain two mixed materials, respectively adding polyvinyl alcohol binder solution according to the proportion of 1% -8% of the total mass of the mixed materials to prepare a pug, respectively filling the pug into corresponding forming dies, pressurizing in the die cavity, performing pressure on the device with the pressure tonnage not less than 500 tons, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out a semi-finished green body; finally, placing the obtained semi-finished green body in a high-temperature drying box for drying, uniformly heating the semi-finished green body for 10 hours at the temperature of 0-200 ℃, keeping the temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying;
step four, sintering the product:
sintering by using an electric heating closed kiln or a gas heating kiln, respectively placing the semi-finished product green body of the first part and the semi-finished product green body of the second part into different sintering equipment for sintering, wherein the sintering temperature of the first part is 1650+/-3 ℃ and the sintering temperature of the second part is 1750+/-3 ℃, naturally cooling the kiln to room temperature after the sintering is completed, and taking out the product to respectively obtain a crucible main body corresponding to the first part and an embedded body corresponding to the second part;
step five, sintering the product:
smearing a first part of pug on the outer surface of the embedded body, plugging the pug into a reserved hole at the bottom of the crucible main body, after the embedded body is plugged into all reserved holes, placing the two parts of products which are combined into a sintering furnace again for sintering, wherein the sintering temperature is 1300 ℃, the temperature rising curve is between room temperature and 1300 ℃ and is not higher than 5 ℃ per minute, carrying out composite integrated sintering, bonding the solid micro liquid phase of which the bonding surface is sintered at high temperature into a whole by utilizing high temperature, keeping the 1300 ℃ for 6 hours after the temperature reaches 1300 ℃, and naturally cooling to the room temperature by closing the heating power to obtain the combined ceramic wire drawing crucible.
Further, in the second step, the polyurethane mixed dispersion balls are polyurethane round balls with diameters of 1-8 mm.
Preferably, in the method for preparing the pug in the third step, 10% polyvinyl alcohol solution is additionally added according to the proportion of 1% -8% of the total mass of the mixed materials, and then spray drying is carried out by using ceramic spray drying granulation equipment to prepare particles with unequal 0.1-0.2 mm and water content less than 0.5%.
As a preferable method for preparing pug in the third step, 10% polyvinyl alcohol solution is additionally added according to the proportion of 1% -8% of the total mass of the mixed material, the mixed material is placed in a stainless steel stirrer, the stirring is carried out for more than or equal to 1 hour, after the polyvinyl alcohol binder and the raw materials are fully and uniformly stirred, the raw materials are placed in a drying box with the temperature of 30-80 ℃ for drying for not less than 10 hours until the water content of the raw materials is less than 0.5%.
Further, in the fourth step, the sintering temperature corresponding to the first part is 1650±3 ℃, the sintering curve is started from 0 ℃, and the sintering curve is increased to 1650 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; and after the temperature reaches 1650 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the crucible main body.
Further, in the fourth step, the sintering temperature corresponding to the second part is 1750+/-3 ℃, the sintering curve starts from 0 ℃, and the sintering curve is increased to 1750 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; and after the temperature reaches 1750 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the embedded body.
Further, in the fourth step and the fifth step, the crucible body is a rectangular concave groove, wherein the melt cavity is a U-shaped lower groove, and a cylindrical preformed hole is formed on the cavity wall of the melt cavity, particularly on the lower part of the cavity wall.
Preferably, the insert body in the fourth and fifth steps is cylindrical, and a fluid hole is formed through the center of the insert body.
Preferably, the insert body in the fourth and fifth steps is cone-shaped, and a fluid hole is formed through the center of the insert body.
Further, the liquid flowing hole comprises a conical liquid inlet part and a straight tube wire drawing part, and a small-diameter through hole of the conical liquid inlet part is smoothly connected with the straight tube wire drawing part.
The invention has the beneficial effects that:
1. the invention adopts a production method that two parts of ceramic bodies with different material proportions and different densities are integrally combined, the produced combined ceramic bushing product can be applied to the fields of glass fiber and metal wire drawing, and the adverse effects of production interruption, quality pollution and the like caused by the factors of deformation, scouring, erosion, cracking and the like of the bushing product in use at high temperature can be effectively reduced; compared with the traditional clay wire drawing and platinum wire drawing crucible, the use temperature is higher, the long-term safe use temperature can reach 1700 ℃, compared with the traditional material, the thermal shock resistance performance is greatly improved, the pollution probability to the solution is almost zero, the probability of deformation cracking in the use process is reduced by more than 90% compared with the crucible made of the original material, the liquid flow hole of the high-density zirconia ceramic enables the anti-scouring performance to be improved by 5 times compared with the original material, and the manufacturing cycle cost of glass fiber and metal wire drawing enterprises and the product qualification rate are greatly improved.
2. On the basis of taking a zirconium dioxide material as a matrix material, dividing a product design into two parts of ceramic products with different densities according to the use characteristics of a wire drawing crucible, wherein the first part is to prepare a ceramic crucible main body by matching with a component with low density of 4.3-4.5 g/cm < 3 > and high thermal shock resistance, and reserving a bottom liquid hole site; the second part is to embed the ceramic embedded body with the high density of 5.3-5.5 g/cm < 3 > of flushing-resistant fluid holes in the preformed holes at the bottom of the crucible main body in a sinking manner; the embedded body designed by the invention is used as a melt outflow part, and has the advantages of high-temperature scouring resistance, erosion resistance and long service life due to high density, small volume and small heated volume change rate, so that the problem of volume stress cracking of the high-density zirconia ceramic with poor thermal shock resistance is alleviated.
3. The method comprises the steps of compounding and forming a first part of raw materials, drying the first part of raw materials by moisture, sintering the first part of raw materials at 1650 ℃ to form a crucible main body, drying the second part of raw materials by moisture through dry pressing and sintering the second part of raw materials at 1750 ℃ to form an embedded body, respectively manufacturing the first part of raw materials and the second part of raw materials into products, embedding and combining the two ceramic products with different densities due to different raw material components into a whole, performing 1300 ℃ co-sintering, and curing and sintering the embedded body with a fluid hole and the high-thermal-shock main body into a whole to obtain the combined ceramic wire-drawing crucible product with high thermal shock resistance and high anti-scouring property and long service life, thereby being well applied to the fields of glass fibers and metal wire drawing.
4. According to the crucible main body of the first part, the zirconium-based composite high thermal shock resistance low-density material is adopted, the defect of aging fading of the stabilization rate of stabilized zirconium is avoided, the zirconium content reaches 60-75% in a micron and particle powder combination mode, the purpose that the temperature resistance reaches 1700 ℃ for long-term use is achieved, the continuous heating thermal shock resistance working condition and high-temperature creep use working condition of a long-term constant glass solution and a metal solution on the crucible main body are solved, and the high-temperature use problems such as cracking deformation and the like are avoided.
5. The embedded body of the second part is made of high-purity high-content zirconia raw materials, and is sintered at high temperature to form compact ceramic, wherein the fluid hole structure is formed by connecting a conical fluid inlet part with a straight cylinder wire drawing part, the function of the embedded body is to alleviate the problem of short service life caused by friction and scouring of fluid holes in the wire drawing process, and the embedded body has small volume and small heated volume change rate, thereby alleviating the problem of volume stress cracking of the compact zirconia ceramic with poor thermal shock resistance, and having the advantages of high-temperature scouring resistance, erosion resistance and long service life of the compact zirconia ceramic, and higher functional design.
Drawings
FIG. 1 is a schematic view of a structure of a crucible body according to the present invention;
FIG. 2 is a schematic view of a cylindrical insert according to the present invention;
FIG. 3 is a schematic view of a conical insert according to the present invention;
wherein, 1-crucible main part, 2-melt chamber, 3-preformed hole, 4-embedding body, 5-liquid flowing hole, 51-toper feed liquor portion, 52-straight section of thick bamboo wire drawing portion.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the scope of the present invention by equally replacing or changing the technical solutions and the inventive concepts thereof within the scope of the present invention.
The invention provides a method for producing a combined ceramic wire-drawing crucible, wherein the design of the material association formula and the proportion of a product is that the ceramic wire-drawing crucible is made of zirconium dioxide materialOn the basis of a base material, the design of a product is divided into two parts with different densities according to the use characteristics of a wire drawing crucible to be combined, wherein the first part is to match a ceramic crucible main body with low density of 4.3-4.5 g/cm 3 The components with high thermal shock resistance are manufactured and the holes of the bottom liquid flow holes are reserved; the second part is to make the preformed hole at the bottom of the crucible main body have a high density of 5.3-5.5 g/cm 3 The ceramic embedded body of the flushing-resistant fluid hole is embedded in a sinking manner; finally, the combined ceramic wire drawing crucible formed by two parts with different densities is obtained.
The crucible body of the first part of the present invention comprises the following components: zirconium dioxide material Zr0 2 Yttria material Y 2 0 3 Zirconium mullite material Azs, kyanite Al 2 [SIO 4 ]alpha-Al of O, corundum material 2 O 3 alpha-Al of alumina powder material 2 O 3 。
The zirconium dioxide material Zr0 2 The monoclinic zirconium powder with the purity of not less than 98 percent has the D50 granularity of 20-30 um.
The yttrium oxide material Y 2 0 3 The purity is not lower than 98 percent, and the D50 granularity is in the range of 10um to 15 um.
The purity of the zirconium mullite material Azs is not lower than 98%, and the D50 granularity of the zirconium mullite material is in the range of 1-20 um;
the kyanite Al 2 [SIO 4 ]O is the purity of not less than 98%, and the D50 granularity is in the range of 15-20 um;
the purity of the corundum material alpha-Al 2O3 is not lower than 98%, and the D50 granularity of the corundum material alpha-Al 2O3 is in the range of 15-20 um;
the purity of the alumina powder material alpha-Al 2O3 is not lower than 98%, and the D50 granularity is in the range of 1 um-3 um.
The material is used as a component formula of the first part of crucible main body, and the material comprises the following components in percentage by mass: 67% or more zirconium dioxide material Zr02 or less than 79%, 1% or less yttrium oxide material Y203 or less than 3%, 10% or less zirconium mullite material Azs or less than 15%, 6% or less kyanite Al2[ SIO4] O or less than 8%, 3% or less corundum material alpha-Al 2O3 or less than 5%, 1% or less alumina powder material alpha-Al 2O3 or less than 2%;
the crucible body produced by the first part production further comprises: titanium oxide, iron oxide, aluminum oxide, hafnium oxide.
The insert of the second part of the invention comprises the following components: zirconium dioxide material Zr0 2 SiO of silicon dioxide material 2 Yttria material Y 2 0 3 。
The zirconium dioxide material Zr0 2 The monoclinic zirconium powder with the purity of not less than 98 percent has the D50 granularity of 20-30 um.
The silicon dioxide material SiO 2 The purity is not lower than 98%, and the D50 granularity is in the range of 1-20 um. The yttrium oxide material Y 2 0 3 The purity is not lower than 98 percent, and the D50 granularity is in the range of 10um to 15 um.
The material is used as a component formula of the second part of embedded body, and the material comprises the following components in percentage by mass:
zirconium dioxide material Zr0 with the content of 94 percent or less 2 96.8% or less, 0.2% or less of SiO as a silica material 2 Yttrium oxide material Y less than or equal to 1%, 3% 2 0 3 ≤5%。
The invention provides a production method of a combined ceramic wire-drawing crucible, wherein regarding the design of product technology related procedures and parameters, the component materials of a first part of crucible main body are compounded and then are molded by a pressure molding method, moisture is dried, and then sintered at 1650 ℃ for later use, the component materials of a second part of embedded body are compounded and then are molded by pressure, then are dried by moisture, and then sintered at 1750 ℃ for later use, the two different parts of materials are singly manufactured into ceramic products, the ceramic products made of the two different material components are embedded and combined into a whole, the 1300 ℃ co-sintering is carried out, and the high-impact-resistance embedded body and the high-impact-resistance crucible main body are solidified and sintered into a whole, so that a high-service-life ceramic product with high thermal shock resistance and high scouring resistance is obtained, and the method is better applied to the fields of glass fiber and metal wire drawing.
The production method of the combined ceramic wire drawing crucible comprises the following steps: step one, preparing raw materials; step two, mixing raw materials; step three, molding and drying; step four, sintering the product; and fifthly, sintering the product.
The preparation method of the raw materials comprises the following specific steps:
the first part of the crucible main body comprises raw material components, zirconium dioxide material Zr0 2 Yttria material Y 2 0 3 Zirconium mullite material Azs, kyanite Al 2 [SIO 4 ]O, corundum material alpha-Al 2O3 and alumina powder material alpha-Al 2O3 are weighed according to a formula for standby.
The second part of the embedded body comprises a raw material component, a zirconium dioxide material Zr0 2 SiO of silicon dioxide material 2 Yttria material Y 2 0 3 Weighing according to a formula for standby.
The raw materials are selected as follows:
the zirconium dioxide material Zr0 2 The monoclinic zirconium powder with the purity of not less than 98 percent has the D50 granularity of 20-30 um.
The yttrium oxide material Y 2 0 3 The purity is not lower than 98 percent, and the D50 granularity is in the range of 10um to 15 um.
The purity of the zirconium mullite material Azs is not lower than 98%, and the D50 granularity of the zirconium mullite material is in the range of 1-20 um.
The kyanite Al 2 [SIO 4 ]O is the purity not lower than 98%, and the D50 granularity is 15-20 um.
The purity of the corundum material alpha-Al 2O3 is not lower than 98%, and the D50 granularity of the corundum material alpha-Al 2O3 is 15-20 um.
The purity of the alumina powder material alpha-Al 2O3 is not lower than 98%, and the D50 granularity is in the range of 1 um-3 um.
The silicon dioxide material SiO 2 The purity is not lower than 98%, and the D50 granularity is in the range of 1-20 um.
The specific method for mixing the raw materials is as follows:
dividing two spare raw materials, adding polyurethane mixing dispersion balls into the three-dimensional mixing equipment for mixing according to the proportion of 7-12% of the total mass of the mixed raw materials, taking the mass percentage as 100 units, and taking out the two spare raw materials after the two spare raw materials are mixed respectively, wherein the mixing time is 10-16 hours;
the polyurethane mixed dispersion balls are polyurethane round balls with diameters of 1-8 mm.
The specific method for forming and drying is as follows:
and (3) distinguishing the mixed material of the first part and the mixed material of the second part obtained in the step (II), firstly, respectively adding a polyvinyl alcohol binder solution according to the proportion of 1% -8% of the total mass of the mixed material of the first part/the second part, and drying until the moisture content is less than 0.5%, so as to form the mud material for forming.
And then, separating pugs of the first part and the second part, respectively loading the pugs into corresponding forming dies, floating pressurizing by adopting a cold isostatic press or a four-column hydraulic press or vibration forming, pressurizing in a die cavity, pressurizing by adopting pressure equipment with the pressure tonnage not less than 500 tons, maintaining the pressure at more than or equal to 200 megapascals for 200 seconds, and demoulding to take out a semi-finished green body.
And finally, placing the obtained semi-finished green body in a high-temperature drying box for drying, uniformly heating the drying curve to 0-200 ℃ for 10 hours, keeping the constant temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying.
The specific method for sintering the product is as follows:
the green body of the first part and the green body of the second part are sintered by adopting a sintering method: sintering by using an electric heating closed kiln or a gas heating kiln, sintering by using the electric heating closed kiln or the gas heating kiln, respectively placing the first part of semi-finished green body and the second part of semi-finished green body in different sintering equipment for sintering, wherein the sintering temperature of the first part is 1650+/-3 ℃, the sintering temperature of the second part is 1750+/-3 ℃, taking out the product after the kiln is naturally cooled to room temperature after the sintering is finished, the product obtained by sintering the green body of the first part is a crucible main body, and the product obtained by sintering the green body of the second part is an embedded body.
Step five, the specific method for sintering the product is as follows:
smearing a first part of pug on the outer surface of an embedded body, plugging the pug into a reserved hole at the bottom of a crucible main body, after all the embedded bodies are plugged into all the reserved holes, putting the two products which are combined into a sintering furnace again for sintering, wherein the sintering temperature is 1300 ℃, the temperature rising curve is between room temperature and 1300 ℃ and is not higher than 5 ℃ per minute, carrying out composite integrated sintering, bonding the solid micro liquid phase of the bonding surface which is sintered at high temperature into a whole by utilizing high temperature, keeping the 1300 ℃ for 6 hours after the temperature reaches 1300 ℃, and naturally cooling to the room temperature by closing heating power to obtain the integrated ceramic fiber drawing crucible which has high thermal shock property, flow Kong Gaokang scouring property and overall long service life.
Example 1
The production process of the combined ceramic bushing includes the following steps:
step one, raw material preparation, the specific method is as follows:
weighing the raw material components of the first part of crucible main body for standby, wherein the raw material components comprise the following components in percentage by mass: zirconium dioxide material Zr0 2 67% yttrium oxide material Y 2 0 3 3 percent of zirconium mullite material Azs percent of 15 percent, kyanite Al 2 [SIO 4 ]O is 8%, corundum material alpha-Al 2O3 is 5%, and alumina powder material alpha-Al 2O3 is 2%.
Weighing the raw material components included in the second part of embedded body for standby, wherein the raw material components comprise the following components in percentage by mass: zirconium dioxide material Zr0 2 94% of silicon dioxide material SiO 2 1% of yttrium oxide material Y 2 0 3 5%.
The specific method for mixing the raw materials is as follows:
polyurethane pellets with the diameter of 1-8 mm are additionally added according to the proportion of 7% of the total mass of the first part of mixing, enter three-dimensional mixing equipment, and are mixed for 10-16 hours, and then the first part of mixed materials are taken out for standby.
And (3) adding polyurethane pellets with the diameter of 1-8 mm into the three-dimensional mixing equipment according to the proportion of 7% of the total mass of the second part of the mixed materials, mixing for 10-16 hours, and taking out the second part of the mixed materials for standby.
Step three, molding and drying, wherein the specific method is as follows:
and (3) adding a 10% polyvinyl alcohol solution into the first part of mixed material according to the proportion of 8% of the total mass, placing the mixed material into a stainless steel stirrer, fully stirring for more than or equal to 1 hour, placing the pug into a drying box with the temperature of 30-80 ℃ for drying for not less than 10 hours after the polyvinyl alcohol binder and the mixed material are fully and uniformly stirred until the water content of the first part of pug is less than 0.5%.
And then loading the first part of pug into a corresponding crucible main body forming die, floating and pressurizing by using a cold isostatic press, pressurizing in a die cavity, performing pressure tonnage of no less than 500 tons of pressure equipment, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out the crucible main body green compact.
And adding a 10% polyvinyl alcohol solution into the second part of mixed material according to the proportion of 1% of the total mass, and performing spray drying by using ceramic spray drying granulation equipment to prepare the granular pug with unequal 0.1-0.2 mm and less than 0.5% of water content.
And then loading the second part of pug into a corresponding embedded body forming die, floating and pressurizing by using a cold isostatic press, pressurizing in a die cavity, performing pressure tonnage of no less than 500 tons of pressure equipment, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out the embedded body green compact.
And finally, placing the obtained crucible main body green compact and the obtained embedded body green compact into a high-temperature drying box for drying, uniformly heating the drying curve to 0-200 ℃ for 10 hours, keeping the constant temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying.
Step four, sintering the product, wherein the specific method is as follows:
placing the crucible main body green compact obtained in the step three into an electric heating closed kiln for sintering, wherein the sintering temperature is 1650+/-3 ℃, the sintering curve starts from 0 ℃, and the temperature is increased to 1650 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; after 1650 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the product to obtain a crucible main body shown in figure 1; as shown in fig. 1, the crucible main body 1 is a rectangular concave groove, wherein the melt cavity 2 is a U-shaped lower groove, and a cylindrical preformed hole 3 is arranged on the cavity wall of the melt cavity 2, particularly on the lower part of the cavity wall for embedding the embedded body 4.
Placing the embedded body green compact obtained in the step three into an electric heating closed kiln for sintering, wherein the sintering temperature is 1750+/-3 ℃, the sintering curve starts from 0 ℃, and the temperature is increased to 1750 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; after 1750 ℃ is reached, maintaining the constant temperature for 18-24 hours, then closing the heating power, naturally cooling the kiln to room temperature, and taking out the product to obtain the embedded body shown in fig. 2; as shown in fig. 2, the embedded body 4 is cylindrical, a conical liquid flowing hole 5 is formed in the center of the embedded body in a penetrating manner, the conical liquid flowing hole 5 comprises a conical liquid inlet portion 51 and a straight tube drawing portion 52, and a small-diameter through hole of the conical liquid inlet portion is smoothly connected with the straight tube drawing portion.
Step five, sintering the product, wherein the specific method is as follows:
smearing a first part of pug on the outer surface of an embedded body, plugging the pug into reserved holes at the bottom of a main body of a first part of crucible, after all the embedded bodies are plugged into all the reserved holes, placing the two combined products in a sintering furnace again for sintering at 1300 ℃, carrying out composite integral sintering at a temperature rising curve of between room temperature and 1300 ℃ and not higher than 5 ℃ per minute, bonding the solid micro liquid phase sintered at a high temperature on the bonding surface into a whole by utilizing high temperature, keeping the temperature of 1300 ℃ for 6 hours after the temperature reaches 1300 ℃, and naturally cooling to the room temperature by closing heating power to obtain the integrated ceramic fiber drawing crucible which has high thermal shock property, flow Kong Gaokang property and overall long service life and is used for glass fiber and metal drawing.
Example 2
The production process of the combined ceramic bushing includes the following steps:
step one, raw material preparation, the specific method is as follows:
weighing the raw material components of the first part of crucible main body for standby, wherein the raw material components comprise the following components in percentage by mass: zirconium dioxide material Zr02 is 79%, yttrium oxide material Y203 is 1%, zirconium mullite material Azs is 10%, kyanite Al2 SIO 4O is 6%, corundum material alpha-Al 2O3 is 3%, alumina powder material alpha-Al 2O3 is 1%.
Weighing the raw material components included in the second part of embedded body for standby, wherein the raw material components comprise the following components in percentage by mass: the zirconium dioxide material Zr02 was 96.8%, the silicon dioxide material SiO2 was 0.2%, and the yttrium oxide material Y203 was 3%.
Step two, mixing raw materials, wherein the specific method is as follows:
polyurethane pellets with the diameter of 1-8 mm are additionally added according to the proportion of 10% of the total mass of the first part of mixing, enter three-dimensional mixing equipment, and are mixed for 10-16 hours, and then the first part of mixed materials are taken out for standby.
And (3) adding polyurethane pellets with the diameter of 1-8 mm into the three-dimensional mixing equipment according to the proportion of 10% of the total mass of the second part of the mixed materials, mixing for 10-16 hours, and taking out the second part of the mixed materials for standby.
Step three, molding and drying, wherein the specific method is as follows:
adding 10% polyvinyl alcohol solution into the mixture of the first part according to the proportion of 6% of the total mass, placing the mixture into a stainless steel stirrer, fully stirring for more than or equal to 1 hour, placing the pug into a drying box with the temperature of 30-80 ℃ for drying for not less than 10 hours after the polyvinyl alcohol binder solution and the mixture are fully and uniformly stirred until the water content of the pug is less than 0.5%.
In the same mud material preparation method, the mixed material of the second part is additionally added with 10% polyvinyl alcohol solution according to the proportion of 6% of the total mass of the mixed material, the mixed material is placed in a stainless steel stirrer, the stirring is carried out for more than or equal to 1 hour, after the polyvinyl alcohol binder and the mixed material are fully and uniformly stirred, the mud material is placed in a drying box with the temperature of 30-80 ℃ for drying for not less than 10 hours until the water content of the mud material is less than 0.5%.
And then loading the first part of pug into a corresponding crucible main body forming die, floating and pressurizing by utilizing a four-column hydraulic press, pressurizing in a die cavity, performing pressure tonnage of no less than 500 tons of pressure equipment, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out the crucible main body green compact.
And (3) placing the obtained crucible main body green body into a high-temperature drying box for drying, uniformly heating the drying curve to 0-200 ℃ for 10 hours, keeping the constant temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying.
And then loading the second part of pug into a corresponding embedded body forming die, floating and pressurizing by utilizing a four-column hydraulic press, pressurizing in a die cavity, performing pressure tonnage of no less than 500 tons of pressure equipment, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out the embedded body green compact.
And (3) placing the obtained embedded green body in a high-temperature drying box for drying, uniformly heating the drying curve to 0-200 ℃ for 10 hours, keeping the constant temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying.
Step four, sintering the product, wherein the specific method is as follows:
placing the crucible main body green body obtained in the step three into a gas heating kiln for sintering, wherein the sintering temperature is 1650+/-3 ℃, the sintering curve starts from 0 ℃, and the temperature is increased to 1650 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; after 1650 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the product to obtain a crucible main body shown in figure 1; as shown in fig. 1, the crucible main body 1 is a rectangular concave groove, wherein the melt cavity 2 is a U-shaped lower groove, and a cylindrical preformed hole 3 is arranged on the cavity wall of the melt cavity 2, particularly on the lower part of the cavity wall for embedding the embedded body 4.
Placing the embedded green body obtained in the step three into a gas heating kiln for sintering, wherein the sintering temperature is 1750+/-3 ℃, the sintering curve starts from 0 ℃, and the temperature is increased to 1750 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; after 1750 ℃ is reached, maintaining the constant temperature for 18-24 hours, then closing the heating power, naturally cooling the kiln to room temperature, and taking out the product to obtain an embedded body shown in figure 3; as shown in fig. 3, the embedded body 4 is in a cone shape, a cone-shaped liquid flowing hole 5 is formed in the center of the embedded body in a penetrating manner, the cone-shaped liquid flowing hole 5 comprises a cone-shaped liquid inlet part 51 and a straight tube wire drawing part 52, and a small-diameter through hole of the cone-shaped liquid inlet part is smoothly connected with the straight tube wire drawing part.
Step five, sintering the product, wherein the specific method is as follows:
smearing a first part of pug on the outer surface of an embedded body, plugging the pug into a reserved hole at the bottom of a crucible main body, after all the embedded bodies are plugged into all the reserved holes, putting the two products which are combined into a sintering furnace again for sintering, wherein the sintering temperature is 1300 ℃, the temperature rising curve is between room temperature and 1300 ℃ and is not higher than 5 ℃ per minute, carrying out composite integral sintering, bonding the solid micro liquid phase of the bonding surface which is sintered at high temperature into a whole by utilizing high temperature, keeping the temperature at 1300 ℃ for 6 hours after the temperature reaches 1300 ℃, and naturally cooling the heating power to the room temperature state to obtain the integrated ceramic fiber drawing crucible which is used for drawing glass fiber and metal and has high thermal shock property, fluid Kong Gaokang scouring property and overall long service life.
Example 3
The production process of the combined ceramic bushing includes the following steps:
step one, raw material preparation, the specific method is as follows:
weighing the raw material components of the first part of crucible main body for standby, wherein the raw material components comprise the following components in percentage by mass: the zirconium dioxide material Zr02 is 73%, the yttrium oxide material Y203 is 2%, the zirconium mullite material Azs is 12.5%, the kyanite Al2 SIO 4O is 7%, the corundum material alpha-Al 2O3 is 4%, and the alumina powder material alpha-Al 2O3 is 1.5%.
Weighing the raw material components included in the second part of embedded body for standby, wherein the raw material components comprise the following components in percentage by mass: the zirconium dioxide material Zr02 was 95.4%, the silicon dioxide material SiO2 was 0.6%, and the yttrium oxide material Y203 was 4%.
Step two, mixing raw materials, wherein the specific method is as follows:
polyurethane pellets with the diameter of 1-8 mm are additionally added according to the proportion of 12% of the total mass of the first part of mixing, enter three-dimensional mixing equipment, and are mixed for 10-16 hours, and then the first part of mixed materials are taken out for standby.
Polyurethane pellets with the diameter of 1-8 mm are additionally added according to the proportion of 12% of the total mass of the second part of the mixture, the polyurethane pellets enter three-dimensional mixing equipment, and the second part of the mixture is taken out for standby after 10-16 hours of mixing.
The specific method for forming and drying is as follows:
and adding 10% polyvinyl alcohol solution into the first part of mixed material according to the proportion of 4% of the total mass, and performing spray drying by using ceramic spray drying granulation equipment to prepare particles with unequal 0.1-0.2 mm and water content less than 0.5%.
According to the same pug preparation method, the second part of mixed material is additionally added with 10% polyvinyl alcohol solution according to the proportion of 4% of the total mass of the mixed material, and spray drying is carried out by using ceramic spray drying granulation equipment to prepare particles with unequal 0.1-0.2 mm and less than 0.5% of moisture content.
And then loading the first part of pug into a corresponding crucible main body forming die, floating and pressurizing by using a vibration forming machine, pressurizing in a die cavity, performing pressure tonnage of no less than 500 tons of pressure equipment, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out the crucible main body green compact.
Synchronously loading the second part of pug into a corresponding embedded body forming die, floating and pressurizing by using a vibration forming machine, pressurizing in a die cavity, performing pressure tonnage of no less than 500 tons of pressure equipment, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out the embedded body green compact.
And finally, placing the obtained crucible main body green compact and the obtained embedded body green compact into a high-temperature drying box for drying, uniformly heating the drying curve to 0-200 ℃ for 10 hours, keeping the constant temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying.
Step four, sintering the product, wherein the specific method is as follows:
placing the crucible main body green compact obtained in the step three into an electric heating closed kiln for sintering, wherein the sintering temperature is 1650+/-3 ℃, the sintering curve starts from 0 ℃, and the temperature is increased to 1650 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; after 1650 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the product to obtain a crucible main body shown in figure 1; as shown in fig. 1, the crucible main body 1 is a rectangular concave groove, wherein the melt cavity 2 is a U-shaped lower groove, and a cylindrical preformed hole 3 is arranged on the cavity wall of the melt cavity 2, particularly on the lower part of the cavity wall for embedding the embedded body 4.
Placing the embedded body green compact obtained in the step three into an electric heating closed kiln for sintering, wherein the sintering temperature is 1750+/-3 ℃, the sintering curve starts from 0 ℃, and the temperature is increased to 1750 ℃ at a uniform heating rate of not lower than 30 ℃ per hour; after 1750 ℃ is reached, maintaining the constant temperature for 18-24 hours, then closing the heating power, naturally cooling the kiln to room temperature, and taking out the product to obtain an embedded body shown in figure 3; as shown in fig. 3, the embedded body 4 is in a cone shape, a cone-shaped liquid flowing hole 5 is formed in the center of the embedded body in a penetrating manner, the cone-shaped liquid flowing hole 5 comprises a cone-shaped liquid inlet part 51 and a straight tube wire drawing part 52, and a small-diameter through hole of the cone-shaped liquid inlet part is smoothly connected with the straight tube wire drawing part.
Step five, sintering the product, wherein the specific method is as follows:
smearing the pug of the first part before drying on the outer surface of the embedded body, plugging the pug into reserved holes at the bottom of the main body of the first part, after all the embedded bodies are plugged into all the reserved holes, putting the two combined products into a sintering furnace again for sintering, wherein the sintering temperature is 1300 ℃, the temperature rising curve is between room temperature and 1300 ℃ and not higher than 5 ℃ per minute, carrying out composite integral sintering, bonding the solid micro liquid phase of the bonding surface of the integrated products subjected to high-temperature sintering into a whole by utilizing high temperature, keeping the temperature of 1300 ℃ for 6 hours after the temperature reaches 1300 ℃, and naturally cooling the heating power to the room temperature state to obtain the integrated ceramic fiber drawing crucible which is integrated and has high thermal shock property, fluid Kong Gaokang scouring property and overall long service life.
The combined ceramic wire drawing crucible finally obtained through the three embodiments is used in the fields of glass fiber and metal wire drawing, compared with the traditional clay wire drawing and platinum wire drawing crucible, the service temperature is higher, the long-term safe service temperature can reach 1700 ℃, compared with the traditional material, the thermal shock resistance is greatly improved, the pollution probability to the solution is almost zero, the probability of deformation cracking in the use process is reduced by more than 90% compared with the crucible made of the original material, the liquid flow hole of the high-density zirconia ceramic enables the anti-scouring performance to be improved by 5 times compared with the original material, and the manufacturing cycle cost of glass fiber and metal wire drawing enterprises and the improvement of the product qualification rate are greatly improved.
In the description of the present specification, reference to the terms "one embodiment," "example," "specific example," and the like, means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Claims (10)
1. The production method of the combined ceramic wire drawing crucible is characterized by comprising the following steps of:
step one, raw material preparation:
weighing the component formula of the first part of crucible main body for standby, wherein the weight percentage of the component formula comprises the following components in percentage by mass: zirconium dioxide material ZrO of 67% or less 2 Yttrium oxide material Y less than or equal to 79% and less than or equal to 1% 2 O 3 Less than or equal to 3 percent, less than or equal to 10 percent of zirconium mullite material Azs less than or equal to 15 percent, and less than or equal to 6 percent of kyanite Al 2 [SiO 4 ]O is less than or equal to 8 percent, and the corundum material alpha-Al is more than or equal to 3 percent 2 O 3 Less than or equal to 5 percent, 1 percent or less of alumina powder material alpha-Al 2 O 3 ≤2%；
Weighing the component formula of the second part of embedded body for standby, wherein the weight percentage of the component formula comprises the following components in percentage by mass: zirconium dioxide material ZrO of which the content is more than or equal to 94 percent 2 96.8% or less, 0.2% or less of SiO as a silica material 2 Yttrium oxide material Y less than or equal to 1%, 3% 2 O 3 ≤5%；
Step two, mixing raw materials:
the two raw materials for standby weighing in the first step are distinguished, polyurethane mixing dispersion balls are additionally added according to the proportion of 7% -12% of the total mass of the mixed materials in each part, the polyurethane mixing dispersion balls are fed into three-dimensional mixing equipment for mixing respectively, the mixing time is 10-16 hours, and the two raw materials are taken out for standby after being mixed respectively;
step three, molding and drying:
dividing the second step to obtain two mixed materials, respectively adding polyvinyl alcohol binder solution according to the proportion of 1% -8% of the total mass of the mixed materials to prepare a pug, respectively filling the pug into corresponding forming dies, pressurizing in the die cavity, performing pressure on the device with the pressure tonnage not less than 500 tons, performing demoulding after the pressure is more than or equal to 200 megapascals and the pressure is maintained for 200 seconds, and taking out a semi-finished green body; finally, placing the obtained semi-finished green body in a high-temperature drying box for drying, uniformly heating the semi-finished green body for 10 hours at the temperature of 0-200 ℃, keeping the temperature of 200 ℃ for 12-18 hours, and naturally cooling to room temperature after drying;
step four, sintering the product:
sintering by using an electric heating closed kiln or a gas heating kiln, respectively placing the semi-finished product green body of the first part and the semi-finished product green body of the second part into different sintering equipment for sintering, wherein the sintering temperature of the first part is 1650+/-3 ℃ and the sintering temperature of the second part is 1750+/-3 ℃, naturally cooling the kiln to room temperature after the sintering is completed, and taking out the product to respectively obtain a crucible main body corresponding to the first part and an embedded body corresponding to the second part;
step five, sintering the product:
smearing a first part of pug on the outer surface of the embedded body, plugging the pug into a preformed hole at the bottom of the main body of the crucible, arranging a liquid flowing hole in the center of the embedded body in a penetrating way, after the embedded body is plugged into all the preformed holes, placing the two parts of products which are combined into a sintering furnace again for sintering, wherein the sintering temperature is 1300 ℃, the temperature rising curve is between room temperature and 1300 ℃ and is not higher than 5 ℃ per minute, carrying out composite integrated sintering, bonding the solid micro-liquid phase of which the bonding surface is sintered at high temperature into a whole by utilizing high temperature, keeping the temperature at 1300 ℃ for 6 hours after the temperature reaches 1300 ℃, and closing the heating power to naturally cool to the room temperature state, thus obtaining the combined ceramic wire drawing crucible.
2. The method for producing a composite ceramic bushing according to claim 1, wherein the polyurethane mixed dispersion balls in the second step are polyurethane round balls with diameters of 1-8 mm.
3. The method for producing a composite ceramic bushing according to claim 1, wherein the slurry is prepared in the third step by adding 10% polyvinyl alcohol solution in an amount of 1% -8% of the total mass of the mixture, and spray-drying the slurry by using ceramic spray-drying granulation equipment to obtain particles with a water content of 0.1-0.2 mm and less than 0.5%.
4. The method for producing a composite ceramic bushing according to claim 1, wherein the method for preparing pug in the third step is characterized in that 10% polyvinyl alcohol solution is additionally added according to the proportion of 1% -8% of the total mass of the mixed material, the mixed material is placed in a stainless steel stirrer, the stirring is carried out for more than or equal to 1 hour, after the polyvinyl alcohol binder and the raw materials are fully and uniformly stirred, the raw materials are placed in a drying box with the temperature of 30 ℃ -80 ℃ for drying for more than 10 hours until the water content of the raw materials is less than 0.5%.
5. The method of producing a composite ceramic bushing according to claim 1, wherein the sintering temperature corresponding to the first part in the fourth step is 1650±3 ℃, the sintering curve is started from 0 ℃, and the sintering curve is increased to 1650 ℃ at a uniform temperature increase rate of not less than 30 ℃ per hour; and after the temperature reaches 1650 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the crucible main body.
6. The method for producing a composite ceramic bushing according to claim 1, wherein the sintering temperature corresponding to the second part in the fourth step is 1750±3 ℃, the sintering curve is started from 0 ℃, and the sintering curve is increased to 1750 ℃ at a uniform temperature increase rate of not lower than 30 ℃ per hour; and after the temperature reaches 1750 ℃, maintaining the constant temperature for 18-24 hours, closing the heating power, naturally cooling the kiln to room temperature, and taking out the embedded body.
7. The method according to claim 1, wherein in the fourth step and the fifth step, the crucible body is a rectangular concave groove, the melt cavity is a U-shaped lower groove, and a cylindrical preformed hole is provided on the wall of the melt cavity.
8. The method of claim 1, wherein the insert in the fourth and fifth steps is cylindrical and has a fluid hole extending through the center thereof.
9. The method of claim 1, wherein the insert in step four and step five is tapered and has a fluid hole extending through the center thereof.
10. The method of claim 8 or 9, wherein the fluid flow hole comprises a tapered fluid inlet portion and a straight tube drawing portion, and the small diameter through hole of the tapered fluid inlet portion is smoothly connected with the straight tube drawing portion.
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