CN114507065A - Injection molding alumina ceramic material and injection molding method thereof - Google Patents
Injection molding alumina ceramic material and injection molding method thereof Download PDFInfo
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Abstract
The invention discloses an injection molding alumina ceramic material and an injection molding method thereof, and relates to the technical field of ceramic materials. The invention discloses an injection molding alumina ceramic material which is prepared from the following raw materials in percentage by weight: 80.24-80.75% of ceramic powder, 5.03-5.15% of amorphous alpha-olefin copolymer, 4.88-5.00% of linear low density polyethylene, 1.58-2.31% of stearic acid, 3.36-4.35% of tributyl citrate, 2.45-2.53% of titanate coupling agent and 0.15-0.22% of dinaphthyl methane disulfonic acid sodium; the ceramic powder is composed of alumina powder, yttrium oxide powder and magnesium oxide powder; the invention also provides an injection molding method of the alumina ceramic material. The injection molding alumina ceramic material provided by the invention has excellent high strength and high toughness, is not easy to brittle failure, has high density and small product shrinkage rate, and can obtain a product with high dimensional precision; the invention has the advantages of easily obtained raw materials, easily controlled preparation process, short time consumption and easy, rapid and automatic mass production.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to an injection molding alumina ceramic material and an injection molding method thereof.
Background
Ceramic Injection Molding (CIM) is a branch of the modern Powder Injection Molding (PIM) technology, and is a new process for preparing ceramic parts developed by combining a polymer injection molding method with a ceramic preparation process. The forming process has the characteristics of high degree of mechanization and automation, high production efficiency, short forming period, high blank strength and the like, can accurately control the process, can form various small ceramic parts with complicated geometric shapes and special requirements in a near-net shape, and is easy to realize large-batch and large-scale production. The basic flow of the ceramic injection molding process is as follows: the ceramic powder, the adhesive, the dispersant, the lubricant and the like are uniformly mixed to form a hot melt, then the hot melt is injected into a die cavity with a part shape by an injection machine to form a blank, and the blank is degreased and sintered at high temperature to obtain the ceramic powder.
The binder is the core and key of the powder injection molding technology, and each improvement and breakthrough of the injection molding technology is accompanied with the emergence of a new binding system. In CIM, since the particle size of ceramic powder is smaller than that in metal powder injection molding, the flowability of ceramic powder itself is poor, and the gap between the powder after mixing ceramic powder and binder is very small, which causes difficulty in degreasing and affects the quality of the final product, thus making the current technology have more strict requirements for binder. There are four major binder systems that are currently mature: the first is a thermoplastic system, which has good applicability, good fluidity, easy molding, high powder loading, easy control of the injection process, but long degreasing time, complex process and higher cost; the second is a thermosetting system, the strength of an injection blank is high, the degreasing speed is high, but the injection process is not easy to control, the applicability is poor, and the defects of products are more; the third is a gel system which has less organic matters and high degreasing speed, but has low green strength and difficult degreasing; the fourth is a water soluble system which degreases quickly but with a small powder load, resulting in a lower strength product. Because the ceramic injection molding technology has strict selection requirements on ceramic powder, a binder, a dispersant and the like, a thermoplastic system binder is commonly used internationally at present, the selection types of the binder are particularly few, if the binder system is not properly selected, the problems of non-uniformity in the curing and degreasing processes before sintering, difficulty in separation of the binder and the like are easily caused, the mechanical strength of a final product is easily poor, the final product is easy to break, the production efficiency of the product is also influenced, and the development of the domestic ceramic injection molding technology is limited.
Disclosure of Invention
The invention mainly aims to provide an injection molding alumina ceramic material which has excellent high strength and high toughness, is not easy to brittle failure, has high density and small product shrinkage rate, and can obtain a product with high dimensional precision; the invention has the advantages of easily obtained raw materials, easily controlled preparation process, short time consumption and easy, rapid and automatic mass production.
In order to realize the purpose of the invention, the invention provides an injection molding alumina ceramic material which is prepared from the following raw materials in percentage by weight: 80.24-80.75% of ceramic powder, 5.03-5.15% of amorphous alpha-olefin copolymer, 4.88-5.00% of linear low density polyethylene, 1.58-2.31% of stearic acid, 3.36-4.35% of tributyl citrate, 2.45-2.53% of titanate coupling agent and 0.15-0.22% of dinaphthyl methane disulfonic acid sodium;
the titanate coupling agent is isopropyl tri (dioctyl pyrophosphato acyloxy) titanate;
the ceramic powder is prepared from the following raw materials in percentage by mass: 95.4 to 97.28% of alumina powder, 0.93 to 1.4% of yttrium oxide powder and 1.80 to 3.2% of magnesium oxide powder.
The invention also provides an injection molding method for injection molding of the alumina ceramic material, which comprises the following steps:
s1, rough mixing: weighing the raw materials according to the mass percentage, drying the ceramic powder at 200 ℃ for 2h, adding all the raw materials into a constant-temperature stirring mixer according to a proportion, and stirring at constant temperature for 2h to obtain a coarse mixed material;
s2, extruding: putting the coarse mixed material into a vacuum pug mill, and repeatedly extruding for 3 times or more to prepare a mixed material;
s3, injection molding: adding the mixed materials into an injection molding machine for injection molding to form a blank body;
s4, solvent degreasing: soaking the blank in isopropanol at the temperature of 50-60 ℃, soaking for 6-8 h at constant temperature, taking out, and then placing in a drying oven at the temperature of 100 +/-5 ℃ for 2 h;
s5, thermal degreasing and sintering: and (3) putting the blank degreased by the solvent into a sintering furnace, heating to 450-700 ℃ for thermal degreasing, continuously heating to 1200-1400 ℃ for sintering, and naturally cooling to room temperature to obtain the alumina ceramic body.
Further, the particle size of the ceramic powder is 30-60 nm.
Further, in the coarse mixing process of the step S1, the temperature of the constant-temperature stirring mixer is set to be 110 ℃, and the stirring speed is set to be 250-260 r/min.
Further, in the extruding and refining process of the step S2, the repeated extruding times of the vacuum pug mill is 4-5 times, so that the mixed material is granulated and then agglomerated without loosening.
Further, the thermal degreasing process in step S5 includes: heating to 220 ℃ at normal temperature at a speed of 3 ℃/min in a sintering furnace, and keeping the temperature for 1 h; then heating to 450 ℃ at the speed of 1 ℃/min, and preserving heat for 2 h; then heating to 700 ℃ at the speed of 2 ℃/min, and preserving heat for 4h to obtain the hot degreased blank.
Further, the sintering process of step S5 is: in a sintering furnace, directly heating the blank after thermal degreasing to 900 ℃ at the speed of 5 ℃/min at the temperature of 700 ℃, and preserving heat for 1 h; then raising the temperature to 1050 ℃ at the speed of 5 ℃/min, and preserving the temperature for 1 h; then heating to 1200 ℃ at the speed of 10 ℃/min, and preserving heat for 2 h; finally, the temperature is raised to 1400 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 h.
The invention achieves the following beneficial effects:
1. the invention adopts alumina as a base material, uses yttrium oxide and magnesium oxide as sintering aids, mixes with a binder system (amorphous alpha-olefin copolymer, linear low-density polyethylene, stearic acid, tributyl citrate and titanate coupling agent) and a dispersant, squeezes, performs injection molding, degreases in a mode of combining solvent degreasing and thermal degreasing, and then performs sintering at a lower temperature to obtain the alumina ceramic body with high density and uniformity. The yttrium oxide and the magnesium oxide are added to serve as sintering aids of the alumina ceramic, so that the sintering temperature of the alumina ceramic is remarkably reduced, the interface bonding force with other components is increased, and the compactness, the mechanical strength and the fracture toughness of the alumina ceramic are improved; the adhesive system with specific components is adopted, has moderate viscosity, small temperature fluctuation, good fluidity and better adhesive force to the ceramic powder, reduces the deformation probability of a ceramic blank and ensures that the shrinkage rate of a product is smaller; the binder system of the invention adopts the solvent for degreasing firstly and then carries out thermal degreasing, thereby reducing the degreasing time, improving the degreasing efficiency, and avoiding the defects caused by thermal stress, thereby reducing the thermal shock to the ceramic blank, reducing the defects, reducing the porosity of the alumina, further improving the density, mechanical strength and impact resistance of the binder system, and ensuring that the binder system is not easy to brittle failure.
2. The amorphous alpha-olefin copolymer (APAO) is a flexible olefin copolymer with low molecular weight, high fluidity, amorphous state and high randomness, is combined with linear low-density polyethylene, stearic acid, tributyl citrate and titanate coupling agent, has higher fluidity, keeps moderate viscosity of a binder system, and is suitable for the ceramic powder, so that the ceramic powder is uniformly dispersed, and has better bonding effect with the ceramic powder; in the degreasing process of the binder system, the solvent is firstly used for degreasing, so that components such as stearic acid, tributyl citrate and the like are dissolved out, and then the thermal degreasing is adopted, so that the degreasing time is greatly shortened, the degreasing efficiency is improved, the blank body can be kept not to deform, the shrinkage rate is reduced, and the density of the binder system is further improved.
3. The titanate coupling agent is added into the bonding system, so that the bonding effect of the bonding agent and the ceramic powder can be improved, the generated titanium oxide can enlarge the length-diameter ratio of alumina grains in the degreasing process, the titanium oxide, the magnesium oxide and the yttrium oxide act together to ensure that the length-diameter ratio of each alumina grain is basically consistent, the density of the alumina ceramic material is further improved, and the strength and the toughness of the ceramic material are improved.
4. The raw materials are easy to obtain and environment-friendly, the preparation method is simple and easy to operate, the materials are squeezed and mixed for more than 3 times (preferably 4-5 times), the mixing effect of the mixed materials is good, the mixing efficiency is high, the mixed materials are blocked and are not easy to break, and the generation of air holes in injection molding green bodies is reduced; the preparation process of the invention is easy to control, short in time, low in sintering temperature and easy for rapid automatic mass production.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The titanate coupling agent in the embodiment of the invention is isopropyl tri (dioctyl pyrophosphato acyloxy) titanate provided by a new Nanjing Feiteng material; amorphous alpha-olefin copolymers (APAO) are provided by liao chemical company ltd; linear Low Density Polyethylene (LLDPE) is supplied by medium petrochemicals, model number M2720A; the alumina powder has a particle size of 30-60nm, and is provided by Henan New material, model number is HN-L30.
The injection-molded alumina ceramic material and the injection-molding method thereof according to the present invention will be described with reference to specific examples.
Example 1:
the injection molding alumina ceramic material of the embodiment is composed of the following raw materials by weight percent: 80.24% of ceramic powder, 5.15% of APAO, 5.00% of LLDPE, 1.58% of stearic acid, 4.35% of tributyl citrate, 2.53% of titanate coupling agent and 1.15% of dinaphthyl methane disulfonic acid, wherein the ceramic powder is composed of the following raw materials in percentage by mass: 95.4% of alumina powder, 1.4% of yttrium oxide powder and 3.2% of magnesium oxide powder, and the grain size of the ceramic powder is 30-60 nm.
The injection molding method for the injection molding of the alumina ceramic material specifically comprises the following steps:
s1, rough mixing: weighing the raw materials according to the mass percentage, firstly drying the ceramic powder at 200 ℃ for 2h, then adding all the raw materials into a constant-temperature stirring mixer according to the proportion, setting the stirring speed at 260r/min, and stirring at 110 ℃ for 2h to obtain a coarse mixed material.
S2, extruding: and (3) putting the coarse mixed material into a vacuum pug mill, and repeatedly extruding for 3 times at 155 ℃ to obtain the mixed material.
S3, injection molding: and adding the mixed materials into an injection molding machine, setting the injection pressure to be 100MPa, setting the injection temperature to be 190 ℃, setting the mold temperature to be 60 ℃, and performing injection molding to form a blank.
S4, solvent degreasing: soaking the blank in isopropanol at 50 deg.C for 8 hr, taking out, and placing in a drying oven at 100 deg.C for 2 hr.
S5, thermal degreasing: putting the blank degreased by the solvent into a sintering furnace, heating to 220 ℃ at normal temperature at a speed of 3 ℃/min, and preserving heat for 1 h; then heating to 450 ℃ at the speed of 1 ℃/min, and preserving heat for 2 h; then heating to 700 ℃ at the speed of 2 ℃/min, and preserving heat for 4h to obtain the hot degreased blank.
S6, sintering: continuously heating the blank after thermal degreasing to 900 ℃ at the temperature of 700 ℃ at the speed of 5 ℃/min, and preserving the heat for 1 h; then raising the temperature to 1050 ℃ at the speed of 5 ℃/min, and preserving the temperature for 1 h; then heating to 1200 ℃ at the speed of 10 ℃/min, and preserving heat for 2 h; finally, the temperature is raised to 1400 ℃ at the speed of 10 ℃/min, and after heat preservation is carried out for 3h, the alumina ceramic body with the required shape is obtained after natural cooling to the room temperature.
Example 2:
the injection molding alumina ceramic material of the embodiment is composed of the following raw materials by weight percent: 80.75% of ceramic powder, 5.03% of APAO, 4.88% of LLDPE, 2.31% of stearic acid, 3.36% of tributyl citrate, 2.45% of titanate coupling agent and 1.22% of dinaphthyl methane disulfonic acid, wherein the ceramic powder is composed of the following raw materials in percentage by mass: 97.28% of alumina powder, 0.93% of yttrium oxide powder and 1.79% of magnesium oxide powder, and the grain size of the ceramic powder is 30-60 nm.
The specific procedure of the injection molding method for injection molding an alumina ceramic material was the same as in example 1, and specifically referring to example 1, except that in the kneading process of example 2, 4 times of repeated extrusion was carried out at 155 ℃.
Example 3:
the injection molding alumina ceramic material of the embodiment is composed of the following raw materials by weight percent: 80.36% of ceramic powder, 5.12% of APAO, 4.95% of LLDPE, 2.08% of stearic acid, 3.85% of tributyl citrate, 2.46% of titanate coupling agent and 1.18% of dinaphthyl methane disulfonic acid, wherein the ceramic powder is composed of the following raw materials in percentage by mass: 96.81% of alumina powder, 1.07% of yttrium oxide powder and 2.12% of magnesium oxide powder, and the grain size of the ceramic powder is 30-60 nm.
The specific procedure of the injection molding method for injection molding an alumina ceramic material was the same as in example 1, and with specific reference to example 1, except that in the kneading process of example 3, the kneading process was repeated at 155 ℃ for 5 times to prepare a kneaded material.
Example 3:
the injection molding alumina ceramic material of the embodiment is composed of the following raw materials by weight percent: 80.5% of ceramic powder, 5.08% of APAO, 4.92% of LLDPE, 1.65% of stearic acid, 4.2% of tributyl citrate, 2.48% of titanate coupling agent and 1.17% of dinaphthyl methane disulfonic acid, wherein the ceramic powder is composed of the following raw materials in percentage by mass: 96.27% of alumina powder, 1.18% of yttrium oxide powder and 2.55% of magnesium oxide powder, and the grain size of the ceramic powder is 30-60 nm.
The specific procedure of the injection molding method for injection molding an alumina ceramic material was the same as in example 1, and with specific reference to example 1, except that in the kneading process of example 4, 4 times of repeated extrusion was carried out at 155 ℃.
Comparative example 1
The alumina ceramic body of this comparative example was prepared in the same manner as in example 4, except that no APAO was added and the LLDPE was added in an amount of 10% in this comparative example 1, and the other components and preparation method were specifically referred to example 4.
Comparative example 2
The alumina ceramic body of this comparative example was prepared in the same manner as in example 4, except that the titanate coupling agent and tributyl citrate were not added and the amount of stearic acid added was 8.33% in this comparative example 2, and the other components and the preparation method were specifically referred to example 4.
Comparative example 3
The alumina ceramic body of this comparative example was prepared in the same manner as in example 4, except that in this comparative example 3, no titanate coupling agent was added and stearic acid was added in an amount of 5.85%, and the other components and the preparation method were specifically referred to example 4.
Comparative example 4
The method for preparing an alumina ceramic body in this comparative example was the same as in example 4, except that in the method for preparing this comparative example 4, thermal degreasing was not performed, i.e., the green body formed after solvent degreasing was directly placed in a sintering furnace and sintered, and the sintering process was: placing the blank in a sintering furnace, heating to 700 ℃ at normal temperature at a speed of 5 ℃/min, preserving heat for 4h, then heating to 900 ℃ at a speed of 5 ℃/min, and preserving heat for 1 h; then heating to 1050 ℃ at the speed of 3 ℃/min, and preserving heat for 1 h; then heating to 1200 ℃ at the speed of 3 ℃/min, and preserving heat for 2 h; finally, the temperature is raised to 1400 ℃ at the speed of 10 ℃/min, and after heat preservation is carried out for 3h, the alumina ceramic body with the required shape is obtained after natural cooling to the room temperature.
The solvent degreasing process in this comparative example 4 was: soaking the injection molding blank body in isopropanol at the temperature of 50 ℃, soaking for 24h at constant temperature, taking out, and then placing in a drying oven at the temperature of 100 ℃ for 2 h.
Comparative example 5
The method for preparing an alumina ceramic body in this comparative example was the same as in example 4, except that in the method for preparing the alumina ceramic body in this comparative example 5, solvent degreasing was not performed, that is, thermal degreasing was directly performed after injection molding a green body, and the thermal degreasing process was: placing the injection molded blank body into a sintering furnace, heating to 220 ℃ at normal temperature at a speed of 3 ℃/min, and preserving heat for 1 h; then heating to 450 ℃ at the speed of 1.5 ℃/min, and preserving heat for 2 h; then the temperature is raised to 700 ℃ at the speed of 3 ℃/min, and the temperature is preserved for 4h, thus obtaining the blank after thermal degreasing.
As compared with the alumina ceramic bodies obtained in the comparative examples 1 to 5, the alumina ceramic bodies obtained in the above examples 1 to 4 were tested for various indexes, and the specific test results are shown in Table 1 below.
TABLE 1 test result table of mechanical properties of alumina ceramic body
Remarking: the density is the relative density rhorI.e. according to the formula rhorBulk density ρsTheoretical density ρthAnd (4) calculating.
According to the comparative test results of the examples 1 to 4 and the comparative examples 1 to 5, it can be seen that compared with the comparative examples, the injection molding alumina ceramic material has higher tensile strength, compressive strength and fracture toughness, is not easy to fracture, has high density and good product quality, and is suitable for large-scale automatic production.
The technical features of the embodiments described above can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (7)
1. An injection molding alumina ceramic material is characterized by comprising the following raw materials in percentage by weight: 80.24-80.75% of ceramic powder, 5.03-5.15% of amorphous alpha-olefin copolymer, 4.88-5.00% of linear low density polyethylene, 1.58-2.31% of stearic acid, 3.36-4.35% of tributyl citrate, 2.45-2.53% of titanate coupling agent and 0.15-0.22% of dinaphthyl methane disulfonic acid sodium;
the titanate coupling agent is isopropyl tri (dioctyl pyrophosphato acyloxy) titanate;
the ceramic powder is prepared from the following raw materials in percentage by mass: 95.4 to 97.28% of alumina powder, 0.93 to 1.4% of yttrium oxide powder and 1.80 to 3.2% of magnesium oxide powder.
2. An injection molding method for injection molding of an alumina ceramic material as claimed in claim 1, comprising the steps of:
s1, rough mixing: weighing the raw materials according to the mass percentage, drying the ceramic powder at 200 ℃ for 2h, adding all the raw materials into a constant-temperature stirring mixer according to a proportion, and stirring at constant temperature for 2h to obtain a coarse mixed material;
s2, extruding: putting the coarse mixed material into a vacuum pug mill, and repeatedly extruding for more than 3 times to prepare a mixed material;
s3, injection molding: adding the mixed materials into an injection molding machine for injection molding to form a blank body;
s4, solvent degreasing: soaking the blank in isopropanol at the temperature of 50-60 ℃, soaking for 6-8 h at constant temperature, taking out, and then placing in a drying oven at the temperature of 100 +/-5 ℃ for 2 h;
s5, thermal degreasing and sintering: and (3) putting the blank degreased by the solvent into a sintering furnace, heating to 450-700 ℃ for thermal degreasing, continuously heating to 1200-1400 ℃ for sintering, and naturally cooling to room temperature to obtain the alumina ceramic body.
3. The injection molding method of an alumina ceramic material as claimed in claim 2, wherein the ceramic powder has a particle size of 30 to 60 nm.
4. The injection molding method of an alumina ceramic material as claimed in claim 2, wherein in the step S1, the temperature of the thermostatic stirring mixer is set to 110 ℃, and the stirring speed is set to 250-260 r/min.
5. The injection molding method of an alumina ceramic material as claimed in claim 2, wherein in the step S2, the vacuum pug mill repeatedly extrudes 4-5 times, so that the mixture is pelletized and does not loosen.
6. The injection molding method for injection molding of alumina ceramic material as claimed in claim 2, wherein the thermal degreasing process of step S5 is: heating to 220 ℃ at normal temperature at a speed of 3 ℃/min in a sintering furnace, and keeping the temperature for 1 h; then heating to 450 ℃ at the speed of 1 ℃/min, and preserving heat for 2 h; then heating to 700 ℃ at the speed of 2 ℃/min, and preserving heat for 4h to obtain the hot degreased blank.
7. The injection molding method for injection molding of alumina ceramic material as claimed in claim 2, wherein the sintering process of step S5 is: in a sintering furnace, directly heating the blank after thermal degreasing to 900 ℃ at the speed of 5 ℃/min at the temperature of 700 ℃, and preserving heat for 1 h; then raising the temperature to 1050 ℃ at the speed of 5 ℃/min, and preserving the temperature for 1 h; then heating to 1200 ℃ at the speed of 10 ℃/min, and preserving heat for 2 h; finally, the temperature is raised to 1400 ℃ at the speed of 10 ℃/min, and the temperature is kept for 3 h.
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