CN110480016B - Method for preparing functional ceramic part with complex structure by adopting powder injection molding - Google Patents
Method for preparing functional ceramic part with complex structure by adopting powder injection molding Download PDFInfo
- Publication number
- CN110480016B CN110480016B CN201910875210.8A CN201910875210A CN110480016B CN 110480016 B CN110480016 B CN 110480016B CN 201910875210 A CN201910875210 A CN 201910875210A CN 110480016 B CN110480016 B CN 110480016B
- Authority
- CN
- China
- Prior art keywords
- degreasing
- temperature
- blank
- injection molding
- functional ceramic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/54—Producing shaped prefabricated articles from the material specially adapted for producing articles from molten material, e.g. slag refractory ceramic materials
Abstract
The invention relates to a method for preparing a functional ceramic part with a complex structure by adopting powder injection molding, which is characterized by comprising the following steps: s1, feed preparation: uniformly mixing functional ceramic powder and a binder to form a feed; s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank; s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank; s5, sintering: and (4) placing the thermal degreasing blank prepared in the step (S4) into a sintering furnace, and sintering in an air atmosphere to obtain a sintered blank. According to the invention, the volume ratio range of the functional ceramic powder and the binder is set, so that the functional ceramic powder can be completely wrapped by the binder, and a defect-free injection blank can be easily obtained.
Description
Technical Field
The invention relates to the field of preparation of a functional ceramic part with a complex structure, in particular to a method for preparing the functional ceramic part with the complex structure by adopting powder injection molding.
Background
Ceramic materials are widely applied to parts requiring special electromagnetic functions due to their special dielectric properties, temperature characteristics, and extremely high corrosion resistance, strength, and hardness. With the development of electronic communication and automation industries, the structure of the functional ceramic part is increasingly complex. The functional ceramics refer to a novel material with special functions, and the performance of the functional ceramics is extremely sensitive to the content of impurity elements and the porosity.
At present, the functional ceramic part is prepared by a method of powder pressing formingAnd, its disadvantages are: 1) the blank obtained by press forming has low dimensional accuracy and simple structure, and a large amount of machining is needed to ensure the structure and dimensional accuracy of the product; 2) the characteristics of the pressing forming method are influenced, the density/compactness of the product along the thickness direction is inconsistent, the product performance is influenced, and the deformation of the product is large in the sintering process; 3) the ceramic powder is required to have higher flowability in the press forming process, i.e. the powder has a larger particle size, and generally D is required50Not less than 4 μm, therefore, the sintering temperature of the product is greatly improved. In summary, the following steps: the functional ceramic parts prepared by press forming have poor control on aspects such as product size control, structure complexity, product size consistency and the like, and are not beneficial to batch preparation of the functional ceramic parts with complex structures.
Although some patents disclose methods for preparing ceramics by powder injection molding, in summary, the following disadvantages are mainly observed in the patents: 1) most of the wax-based binder systems used for the selection of the binder type have the disadvantage that the degreasing time required is extremely long, requiring more than 72 hours. The plastic-based binder system is selected individually, but because the catalytic degreasing process is researched coarsely and shallowly, a relatively precise degreasing process cannot be provided, and the degreasing process can be verified only by experience, the binder is easy to be removed incompletely, and the defects of binder residue or sintering holes and the like are formed in the functional ceramic product, so that the product performance is influenced; 2) the volume ratio of the binder and the ceramic powder is not studied in place, and the volume ratio range of the binder and the ceramic powder cannot be accurately given; 3) the selected ceramic powder usually has very fine particle size, D50Less than or equal to 0.3 mu m, the cost of the powder is greatly increased; 4) the wax-based binder has low molecular weight, low decomposition temperature, poor strength of injection blank and poor shape retention, and is not beneficial to the preparation of high-precision products.
Disclosure of Invention
The invention aims to provide a method for preparing a functional ceramic part with a complex structure by adopting powder injection molding, which can ensure the dimensional precision and consistency of parts, does not need to reserve the dimensional allowance of subsequent processing or only needs to reserve few allowance, and has high utilization rate of raw materials. And simultaneously, the defect that the ceramic part is prepared by powder injection molding in Western Europe can be overcome.
The technical scheme for realizing the purpose of the invention is as follows: the invention comprises the following steps:
s1, feed preparation: uniformly mixing functional ceramic powder and a binder to form a feed material, wherein the volume of the functional ceramic powder is V1And volume V of binder2The following relationship is satisfied:
where ρ is1Is the tap density of the functional ceramic powder;
ρ2is the theoretical density of the functional ceramic powder;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity with a complex structure under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the flow of the catalyst in the catalytic degreasing is 0.8-10 ml/min, the catalytic temperature is 80-140 ℃, and the catalytic degreasing time t is more than or equal to (600+ 120H) min; wherein H is the maximum wall thickness of the part and the unit is mm;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank, wherein the maximum temperature of the thermal degreasing is 900 ℃, and the heating rate is controlled to be 1-3 ℃/min;
s5, sintering: placing the hot degreased blank prepared in the step S4 in a sintering furnace, sintering in an air atmosphere to obtain a sintered blank, wherein the sintering temperature T is controlled to be 1300-1650 ℃, and the heat preservation time is 3-6 hours;
the main components of the binder used in the step S1 are 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
In the step S2, the material for the powder injection molding machine is filledThe temperature of the cylinder is 160-200 ℃, the temperature of the nozzle is 180-3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
In the step S3, the catalyst is nitric acid or oxalic acid, and the specific degreasing process is divided into 4 stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing, the temperature is 85-100 ℃, the time is 90min, the acid introducing amount is 0.8-1.5 ml/min, the third stage is a main degreasing stage, the temperature is 100-140 ℃, the time is t ≥ 390+ 120H min, the acid introducing amount is 3.0-10.0 ml/min, and the fourth stage is post-washing, the heating and the acid introducing are stopped, and the residual acid on the surface of the product is cleaned for 45 min.
The thermal degreasing process in the step S4 is: the heating rate is controlled to be 1-3 ℃/min, the temperature is kept for 3-6 hours within the temperature range of 300-500 ℃, and the highest heating temperature is less than or equal to 900 ℃.
As an optimization design, the grain diameter D of the functional ceramic powder is selected50The range is as follows: 0.5 to 4.0 μm.
The following steps can be added according to the use requirements of the parts:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
The functional ceramic parts required to be prepared include but are not limited to ceramic dielectric filters, ceramic dielectric resonators, piezoelectric ceramic sensors and the like.
The invention has the positive effects that:
(1) the invention adopts a plastic-based binder system (the main elements are carbon, hydrogen and oxygen), and through deep research on the decomposition mechanism of the binder system, the invention ensures that other types except the skeleton agent in the binder can be rapidly removed at a proper temperature through a catalyst of nitric acid or oxalic acid, and then the skeleton agent in the binder is removed by matching with a reasonable thermal degreasing process, so that the prepared product can be ensured to have no binder residue and impurity elements, and the problem of performance reduction of the product caused by the preparation of functional ceramics by traditional powder injection molding is greatly improved.
(2) For a specific functional ceramic powder, the higher the tap density is, the lower the specific surface area of the functional ceramic powder is, and thus the lower the binder proportion required for completely and uniformly wrapping the functional ceramic powder is, and vice versa; meanwhile, the feeding material can obtain good fluidity only on the premise that the functional ceramic powder is completely and uniformly wrapped by the binding agent, so that a defect-free injection blank can be easily obtained, and meanwhile, the injection pressure and the equipment load can be reduced. The invention sets the volume ratio range of the binder and the functional ceramic powder according to the principle, thereby uniformly wrapping the functional ceramic powder by the binder and finally obtaining a defect-free injection blank more easily. The upper limit of the binder proportion is that excessive binder proportion can cause the formation of cavities and collapse in the product during the degreasing and sintering process, and the product performance is affected.
(3) The grain size D50 range of the functional ceramic powder selected in the invention is 0.5-4 μm, which is beneficial to the preparation of the functional ceramic powder on one hand, and the tap density of the functional ceramic powder in the grain size range is suitable for adopting a plastic-based binder system, and is beneficial to catalytic degreasing on the other hand.
(4) The invention adopts catalytic degreasing, has short degreasing period, good degreasing effect and little environmental pollution.
(5) The invention is beneficial to completely removing the binder of the product by adjusting the degreasing time of the nitric acid for the products with different wall thicknesses.
(6) The invention adopts the injection molding method to prepare the functional ceramic part with the complex structure, the obtained functional ceramic part can realize various structural characteristics (such as holes, steps, grooves and the like), has high dimensional precision and high density, and is beneficial to improving the product quality, reducing the machining amount, lowering the cost and improving the productivity.
Detailed Description
(example 1)
When the alumina ceramic product with the wall thickness of 2mm is prepared by powder injection molding, the invention comprises the following steps:
s1, feed preparation: uniformly mixing alumina ceramic powder and binder to form feed material, wherein the volume V of the alumina ceramic powder1And volume V of binder2Has a ratio of
Tap density rho of alumina-based ceramic powder1Is 1.82g/cm3Theoretical density of alumina-based ceramic powder ρ0Is 3.96g/cm3(ii) a Particle diameter D of alumina-based ceramic powder50Comprises the following steps: 2.3 μm;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the catalyst is nitric acid, and the specific degreasing process is divided into four stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing at 90 ℃ for 90min, the acid introduction amount is 0.9ml/min, the third stage is a main degreasing stage at 110 ℃ for 660min, the acid introduction amount is 3.5ml/min, the fourth stage is post-washing, the heating and the acid introduction are stopped, and residual acid on the surface of the product is cleaned for 45 min;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank; controlling the heating rate at 1.5 ℃/min during thermal degreasing, and preserving the heat for 3.5 hours at the temperature of 300-500 ℃, wherein the highest heating temperature is 600 ℃;
s5, sintering: and (4) placing the thermal degreasing blank prepared in the step (S4) into a sintering furnace, sintering in an air atmosphere to obtain a sintered blank, wherein the sintering temperature T is controlled at 1600 ℃, and the heat preservation time is 3.5 hours.
The density of the sintered product can reach 98.1%.
The binder used in the step S1 mainly comprises 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
In the step S2, the temperature of the material barrel of the powder injection molding machine is 160-200 ℃, the temperature of the nozzle is 180-3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
The method also comprises the following steps as required:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
The dielectric constant of the product obtained by the method is 9.3; the dielectric loss was 0.0018.
(example 2)
When the alumina ceramic product with the wall thickness of 4mm is prepared by powder injection molding, the invention comprises the following steps:
s1, feed preparation: uniformly mixing alumina ceramic powder and binder to form feed material, wherein the volume V of the alumina ceramic powder1And volume V of binder2Has a ratio of
The tap density rho 1 of the alumina-based ceramic powder was 1.62g/cm3The theoretical density rho 0 of the alumina-based ceramic powder is 3.96g/cm3(ii) a Particle diameter D of alumina-based ceramic powder50Comprises the following steps: 0.62 μm;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the catalyst is nitric acid, and the specific degreasing process is divided into four stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing at 85 ℃ for 90min, the acid amount is 1ml/min, the third stage is a main degreasing stage at 105 ℃ for 900min, the acid amount is 6.8ml/min, the fourth stage is post-washing, the heating and the acid introduction are stopped, and the residual acid on the surface of the product is cleaned for 45 min;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank; controlling the heating rate at 1.3 ℃/min during thermal degreasing, and keeping the temperature for 3 hours at the temperature of 300-500 ℃, wherein the highest heating temperature is 750 ℃;
s5, sintering: and (4) placing the thermal degreasing blank prepared in the step (S4) into a sintering furnace, sintering in an air atmosphere to obtain a sintering blank, controlling the sintering temperature T to be 1580 ℃, and keeping the temperature for 3 hours.
The density of the sintered product can reach 98.3 percent.
The binder used in the step S1 mainly comprises 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
In the step S2, the temperature of the material barrel of the powder injection molding machine is 160-200 ℃, the temperature of the nozzle is 180-3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
The method also comprises the following steps as required:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
The dielectric constant of the product obtained by the method is 9.25; the dielectric loss was 0.0015.
(example 3)
When the zirconia ceramic product with the wall thickness of 3.5mm is prepared by powder injection molding, the method comprises the following steps:
s1, feed preparation: uniformly mixing zirconia ceramic powder and a binder to form a feed material, wherein the volume V of the zirconia ceramic powder1And volume V of binder2Has a ratio of
Tap density rho of zirconia-based ceramic powder1Is 2.89g/cm3Theoretical Density of zirconia-based ceramic powder ρ0Is 6.01g/cm3(ii) a Particle diameter D of zirconia-based ceramic powder50Comprises the following steps: 1.85 μm;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the catalyst is nitric acid, and the specific degreasing process is divided into four stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing at 95 ℃ for 90min, the acid amount is 1.2ml/min, the third stage is a main degreasing stage at 115 ℃ for 850min, the acid amount is 5ml/min, the fourth stage is post-washing, the heating and the acid introduction are stopped, and the residual acid on the surface of the product is cleaned for 45 min;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank; controlling the heating rate at 1 ℃/min during thermal degreasing, and keeping the temperature for 4 hours within the temperature range of 300-500 ℃, wherein the highest heating temperature is 900 ℃;
s5, sintering: and (4) placing the hot degreasing blank prepared in the step (S4) into a sintering furnace, sintering in an air atmosphere to obtain a sintered blank, controlling the sintering temperature T to be 1480 ℃, and keeping the temperature for 4 hours.
The density of the sintered product can reach 99.2%.
The binder used in the step S1 mainly comprises 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
In the step S2, the temperature of the material barrel of the powder injection molding machine is 160-200 ℃, the temperature of the nozzle is 180-25～200cm3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
The method also comprises the following steps as required:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
The dielectric constant of the product obtained by the method is 4.3; the dielectric loss was 0.0008.
(example 4)
When the titanium-zirconium-tin ceramic product with the wall thickness of 5mm is prepared by powder injection molding, the method comprises the following steps:
s1, feed preparation: uniformly mixing titanium-zirconium-tin ceramic powder and binder to form feed material, wherein the volume V of the titanium-zirconium-tin ceramic powder1And volume V of binder2Has a ratio of
Tap density rho of titanium-zirconium-tin ceramic powder1Is 2.41g/cm3Theoretical density of titanium-zirconium-tin series ceramic powder rho0Is 5.18g/cm3(ii) a Particle diameter D of titanium-zirconium-tin ceramic powder50Comprises the following steps: 0.71 μm;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the catalyst is oxalic acid, and the specific degreasing process comprises four stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing at 100 ℃ for 90min, the acid introduction amount is 1.5ml/min, the third stage is a main degreasing stage at 130 ℃ for 950min, the acid introduction amount is 10ml/min, the fourth stage is post-washing, the heating and the acid introduction are stopped, and residual acid on the surface of the product is cleaned for 45 min;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank; controlling the heating rate at 3 ℃/min during thermal degreasing, and keeping the temperature for 6 hours at the temperature of 300-500 ℃, wherein the highest heating temperature is 650 ℃;
s5, sintering: and (4) placing the hot degreased blank prepared in the step (S4) into a sintering furnace, sintering in an air atmosphere to obtain a sintered blank, wherein the sintering temperature T is controlled at 1340 ℃, and the heat preservation time is 6 hours.
The density of the sintered product can reach 98.7%.
The binder used in the step S1 mainly comprises 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
In the step S2, the temperature of the material barrel of the powder injection molding machine is 160-200 ℃, the temperature of the nozzle is 180-3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
The method also comprises the following steps as required:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
The dielectric constant of the product obtained by the method is 38.2; the dielectric loss was 0.0002.
(example 5)
When the titanium-magnesium-calcium ceramic product with the wall thickness of 4.6mm is prepared by powder injection molding, the method comprises the following steps:
s1, feed preparation: mixing Ti-Mg-Ca ceramic powder with adhesive to obtain feed material, the volume of Ti-Mg-Ca ceramic powder is V1And volume V of binder2Has a ratio of
Tap density rho of titanium-magnesium-calcium ceramic powder1Is 1.98g/cm3Of titanium-magnesium-calcium based ceramic powdersTheoretical density ρ0Is 3.74g/cm3(ii) a Particle diameter D of titanium-magnesium-calcium ceramic powder50Comprises the following steps: 3.5 μm;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the catalyst is oxalic acid, and the specific degreasing process comprises four stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing at 90 ℃ for 90min, the acid introduction amount is 0.8ml/min, the third stage is a main degreasing stage at 140 ℃ for 990min, the acid introduction amount is 7.5ml/min, the fourth stage is post-rinsing, heating and acid introduction are stopped, and residual acid on the surface of the product is cleaned for 45 min;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank; controlling the heating rate at 2.5 ℃/min during thermal degreasing, and keeping the temperature for 5 hours within the temperature range of 300-500 ℃, wherein the highest heating temperature is 800 ℃;
s5, sintering: and (4) placing the thermal degreasing blank prepared in the step (S4) into a sintering furnace, sintering in an air atmosphere to obtain a sintered blank, wherein the sintering temperature T is controlled to be 1360 ℃, and the heat preservation time is 4.5 hours.
The density of the sintered product can reach 99.5 percent.
The binder used in the step S1 mainly comprises 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
In the step S2, the temperature of the material barrel of the powder injection molding machine is 160-200 ℃, the temperature of the nozzle is 180-3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
The method also comprises the following steps as required:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
The dielectric constant of the product obtained by the method is 21.1; the dielectric loss was 0.0003.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for preparing a functional ceramic part with a complex structure by adopting powder injection molding; the method is characterized by comprising the following steps:
s1, feed preparation: uniformly mixing functional ceramic powder and a binder to form a feed material, wherein the volume of the functional ceramic powder is V1And volume V of binder2The following relationship is satisfied:
where ρ is1Is the tap density of the functional ceramic powder;
ρ0is the theoretical density of the functional ceramic powder;
s2, injection molding: placing the feed prepared in the step S1 in a powder injection molding machine, and injecting the feed into a mold cavity under the conditions of injection pressure of 80-200MPa and injection temperature of 160-200 ℃ to form an injection blank;
s3, degreasing: carrying out catalytic degreasing on the injection blank prepared in the step S2 to form a catalytic degreasing blank; the flow of the catalyst in the catalytic degreasing is 0.8-10 ml/min, the catalytic temperature is 80-140 ℃, and the catalytic degreasing time t is more than or equal to (600+ 120H) min; wherein H is the maximum wall thickness of the part and the unit is mm;
s4, thermal degreasing: carrying out thermal degreasing on the catalytic degreasing blank prepared in the step S3 to obtain a thermal degreasing blank, wherein the maximum temperature of the thermal degreasing is 900 ℃, and the heating rate is controlled to be 1-3 ℃/min;
s5, sintering: and (4) placing the hot degreasing blank prepared in the step (S4) into a sintering furnace, sintering in an air atmosphere to obtain a sintered blank, controlling the sintering temperature T to be 1300-1650 ℃, and keeping the temperature for 3-6 hours.
2. The method for preparing the functional ceramic part with the complicated structure by the powder injection molding according to claim 1, wherein the method comprises the following steps: the binder used in the step S1 mainly comprises 60-70% of polyformaldehyde, 20-25% of a skeleton binder, 5-10% of a dispersing agent, 5-10% of a lubricating agent and 1-3% of an antioxidant.
3. The method for preparing the functional ceramic part with the complicated structure by the powder injection molding according to claim 1, wherein the method comprises the following steps: in the step S2, the temperature of the material barrel of the powder injection molding machine is 160-200 ℃, the temperature of the nozzle is 180-3And/s, the injection peak pressure is 80-200MPa, and the pressure is maintained for 2s after the injection is finished, wherein the pressure maintaining pressure is 60-140 MPa.
4. The method for preparing the functional ceramic part with the complicated structure by the powder injection molding according to claim 1, wherein the method comprises the following steps: in the step S3, the catalyst is nitric acid or oxalic acid, and the specific degreasing process is divided into four stages: the first stage is pre-washing and pre-heating, the temperature is 70-80 ℃, the time is 75min, and the acid introducing amount is 0; the second stage is fine degreasing, the temperature is 85-100 ℃, the time is 90min, the acid introducing amount is 0.8-1.5 ml/min, the third stage is a main degreasing stage, the temperature is 100-140 ℃, the time t is more than or equal to (390+120 x H) min, the acid introducing amount is 3.0-10.0 ml/min, and the fourth stage is post-washing, the heating and the acid introducing are stopped, and the residual acid on the surface of the product is cleaned for 45 min.
5. The method for preparing the functional ceramic part with the complicated structure by the powder injection molding according to claim 1, wherein the method comprises the following steps: the thermal degreasing process in the step S4 is: the heating rate is controlled to be 1-3 ℃/min, the temperature is kept for 3-6 hours within the temperature range of 300-500 ℃, and the highest heating temperature is less than or equal to 900 ℃.
6. A method for preparing a functional ceramic part with a complex structure by using powder injection molding according to claim 1, 2 or 3, wherein: particle size D of selected functional ceramic powder50The range is as follows: 0.5 to 4.0 μm.
7. The method for preparing the functional ceramic part with the complicated structure by the powder injection molding according to claim 6, further comprising the steps of:
s6, post-processing: and carrying out post-treatment on the sintered blank, wherein the post-treatment comprises one or more of grinding, surface metallization, laser etching and surface coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910875210.8A CN110480016B (en) | 2019-09-17 | 2019-09-17 | Method for preparing functional ceramic part with complex structure by adopting powder injection molding |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910875210.8A CN110480016B (en) | 2019-09-17 | 2019-09-17 | Method for preparing functional ceramic part with complex structure by adopting powder injection molding |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110480016A CN110480016A (en) | 2019-11-22 |
| CN110480016B true CN110480016B (en) | 2021-11-05 |
Family
ID=68558252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910875210.8A Active CN110480016B (en) | 2019-09-17 | 2019-09-17 | Method for preparing functional ceramic part with complex structure by adopting powder injection molding |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110480016B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110976857B (en) * | 2019-12-26 | 2022-08-05 | 西安铂力特增材技术股份有限公司 | Degreasing method for indirect additive manufacturing |
| CN111136275A (en) * | 2020-01-20 | 2020-05-12 | 江苏精研科技股份有限公司 | Method for preparing large-area thin-wall part by injection molding |
| CN111548145A (en) * | 2020-05-30 | 2020-08-18 | 张保林 | Injection molding method of microwave dielectric ceramic filter and ceramic filter thereof |
| CN111826540A (en) * | 2020-07-21 | 2020-10-27 | 丽水学院 | MAX phase metal ceramic injection molding process |
| CN111872398B (en) * | 2020-08-11 | 2022-06-28 | 江苏精研科技股份有限公司 | Method for preventing product from adhering to mould in powder injection moulding |
| CN112010640A (en) * | 2020-09-03 | 2020-12-01 | 东莞信柏结构陶瓷股份有限公司 | Powder for injection, plastic-based binder, process and ceramic filter |
| CN112276095A (en) * | 2020-10-16 | 2021-01-29 | 苏州敏发科精密电子科技有限公司 | Metal injection molding catalytic degreasing method |
| CN112408952B (en) * | 2020-12-03 | 2022-07-15 | 厦门钨业股份有限公司 | High-thermal-conductivity thin-wall ceramic tube and manufacturing method thereof |
| CN113245549B (en) * | 2021-04-02 | 2022-01-14 | 北京钢研高纳科技股份有限公司 | High-temperature alloy regulator and preparation method thereof |
| CN113387691A (en) * | 2021-07-20 | 2021-09-14 | 东莞市华研新材料科技有限公司 | Ceramic plastic-based feed with high catalytic degreasing rate and preparation method thereof |
| CN115321968A (en) * | 2022-08-14 | 2022-11-11 | 浙江昶科陶瓷新材料有限公司 | POM (polyoxymethylene) based formula system for injection molding of superfine alumina ceramic powder and application thereof |
| CN115353371A (en) * | 2022-08-14 | 2022-11-18 | 浙江昶科陶瓷新材料有限公司 | ZTA ceramic powder catalytic degreasing type injection feed for large-size thick-wall injection molding and preparation method thereof |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5996201A (en) * | 1982-11-22 | 1984-06-02 | Sumitomo Electric Ind Ltd | Treatment of superhard powder |
| CN101698613A (en) * | 2009-06-05 | 2010-04-28 | 西安交通大学 | Degreasing method used for transparent alumina ceramic injection molding product |
| CN101797645A (en) * | 2010-04-12 | 2010-08-11 | 长沙学院 | Binder for micro-powder injection molding and application method thereof |
| CN102115606A (en) * | 2010-12-06 | 2011-07-06 | 常州精研科技有限公司 | Adhesive and method for preparing metal powder injection molding feedstock from same |
| CN102355967A (en) * | 2009-03-16 | 2012-02-15 | 株式会社Ihi | Injection molding composition |
| DE102011117764A1 (en) * | 2011-11-07 | 2013-05-08 | Technische Universität Bergakademie Freiberg | Pressure slip casting method for deagglomerated slip based on ceramic or metallic powder having specific particle size, comprises using pressure slip castable porous molds that are temporarily coated with flocculating agent |
| CN105108154A (en) * | 2015-09-21 | 2015-12-02 | 深圳艾利门特科技有限公司 | Method for preparing special-shaped complex part through powder injection molding technology |
| CN106735195A (en) * | 2017-03-28 | 2017-05-31 | 江苏精研科技股份有限公司 | The degreasing sintered tools of MIM and degreasing sintered technique |
| CN107052346A (en) * | 2016-12-28 | 2017-08-18 | 江苏精研科技股份有限公司 | The preparation technology of powder injection forming tungsten-nickel hard alloy |
| CN107089824A (en) * | 2017-06-01 | 2017-08-25 | 内蒙古科技大学 | A kind of alundum (Al2O3) boron carbide composite ceramic pellet and preparation method thereof |
| CN107324801A (en) * | 2017-06-21 | 2017-11-07 | 东莞华晶粉末冶金有限公司 | A kind of ceramic injection forming material and preparation method thereof |
| CN109650853A (en) * | 2019-02-27 | 2019-04-19 | 湖南英捷高科技有限责任公司 | A kind of preparation method of crystalline ceramics locking bracket |
| CN109848419A (en) * | 2019-03-15 | 2019-06-07 | 江苏精研科技股份有限公司 | A method of nickel base superalloy complex parts are prepared using powder injection-molded |
| CN110106396A (en) * | 2019-06-14 | 2019-08-09 | 重庆文理学院 | A kind of excellent in mechanical performance titanium alloy and preparation method thereof |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004300528A (en) * | 2003-03-31 | 2004-10-28 | Taiheiyo Cement Corp | Sliding parts and brake disc rotor |
| US7798201B2 (en) * | 2007-08-24 | 2010-09-21 | General Electric Company | Ceramic cores for casting superalloys and refractory metal composites, and related processes |
| KR20150137172A (en) * | 2014-05-28 | 2015-12-09 | 한국생산기술연구원 | Binder composition, feedstock for powder metallurgy and method of debinding the binder composition |
| CN105131508B (en) * | 2015-09-28 | 2017-08-25 | 王有才 | A kind of adhesive for powder injection forming, preparation method and applications method |
| CN105482752B (en) * | 2015-12-10 | 2018-09-14 | 翁廷 | Modeling based binder and its method for being used to prepare powder injection forming green body |
| CN106977184A (en) * | 2017-03-14 | 2017-07-25 | 深圳市星迪伟业科技有限公司 | A kind of ceramic part and its production technology |
| CN109382507B (en) * | 2017-08-03 | 2020-01-31 | 全亿大科技（佛山）有限公司 | Preparation method of powder injection molding feed |
| CN108941572A (en) * | 2018-06-26 | 2018-12-07 | 深圳市鑫迪科技有限公司 | The preparation method of feeding for metal powder injection molding |
-
2019
- 2019-09-17 CN CN201910875210.8A patent/CN110480016B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5996201A (en) * | 1982-11-22 | 1984-06-02 | Sumitomo Electric Ind Ltd | Treatment of superhard powder |
| CN102355967A (en) * | 2009-03-16 | 2012-02-15 | 株式会社Ihi | Injection molding composition |
| CN101698613A (en) * | 2009-06-05 | 2010-04-28 | 西安交通大学 | Degreasing method used for transparent alumina ceramic injection molding product |
| CN101797645A (en) * | 2010-04-12 | 2010-08-11 | 长沙学院 | Binder for micro-powder injection molding and application method thereof |
| CN102115606A (en) * | 2010-12-06 | 2011-07-06 | 常州精研科技有限公司 | Adhesive and method for preparing metal powder injection molding feedstock from same |
| DE102011117764A1 (en) * | 2011-11-07 | 2013-05-08 | Technische Universität Bergakademie Freiberg | Pressure slip casting method for deagglomerated slip based on ceramic or metallic powder having specific particle size, comprises using pressure slip castable porous molds that are temporarily coated with flocculating agent |
| CN105108154A (en) * | 2015-09-21 | 2015-12-02 | 深圳艾利门特科技有限公司 | Method for preparing special-shaped complex part through powder injection molding technology |
| CN107052346A (en) * | 2016-12-28 | 2017-08-18 | 江苏精研科技股份有限公司 | The preparation technology of powder injection forming tungsten-nickel hard alloy |
| CN106735195A (en) * | 2017-03-28 | 2017-05-31 | 江苏精研科技股份有限公司 | The degreasing sintered tools of MIM and degreasing sintered technique |
| CN107089824A (en) * | 2017-06-01 | 2017-08-25 | 内蒙古科技大学 | A kind of alundum (Al2O3) boron carbide composite ceramic pellet and preparation method thereof |
| CN107324801A (en) * | 2017-06-21 | 2017-11-07 | 东莞华晶粉末冶金有限公司 | A kind of ceramic injection forming material and preparation method thereof |
| CN109650853A (en) * | 2019-02-27 | 2019-04-19 | 湖南英捷高科技有限责任公司 | A kind of preparation method of crystalline ceramics locking bracket |
| CN109848419A (en) * | 2019-03-15 | 2019-06-07 | 江苏精研科技股份有限公司 | A method of nickel base superalloy complex parts are prepared using powder injection-molded |
| CN110106396A (en) * | 2019-06-14 | 2019-08-09 | 重庆文理学院 | A kind of excellent in mechanical performance titanium alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110480016A (en) | 2019-11-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110480016B (en) | Method for preparing functional ceramic part with complex structure by adopting powder injection molding | |
| CN110540424B (en) | Feed for zirconia ceramic injection molding and preparation method thereof | |
| CN109848419B (en) | Method for preparing nickel-based high-temperature alloy complex part by adopting powder injection molding | |
| CN107573061B (en) | The manufacturing method and its application of honeycomb blind hole toughened zirconium oxide ceramic shell | |
| CN106977200A (en) | A kind of method for manufacturing zirconium oxide ceramic false tooth | |
| CN102717081A (en) | Method for preparing miniature mold by powder micro injection forming method | |
| CN107398559A (en) | A kind of powder injection-molded method of large parts for support of arranging in pairs or groups | |
| WO2010135859A1 (en) | Accurate shaping method for metal ceramic material | |
| CN105921752A (en) | Method for preparing invar alloy resonance bar | |
| CN111668579A (en) | Semi-finished product of 5G communication filter dielectric ceramic part and forming method thereof | |
| CN111205094A (en) | Preparation method of 3D color ceramic backboard | |
| CN105236963A (en) | Zirconium oxide ceramic ferrule workblank production process | |
| CN114349519A (en) | Slurry formula and production process of gel-casting ceramic filter | |
| CN113084718B (en) | Forming and sintering process of metal bond diamond grinding head | |
| CN110655405A (en) | Preparation method of ceramic matrix composite structure | |
| CN114101678A (en) | Preparation method of high-performance metal-ceramic composite material | |
| CN112676566B (en) | High-strength wear-resistant high-temperature-resistant automobile blade and preparation method thereof | |
| CN105060896A (en) | Preparation method of silicon carbide ceramic precision device | |
| CN108620574B (en) | Forming agent, feed and preparation method thereof, green body and preparation method thereof | |
| CN109994235B (en) | Preparation method of UO2 fuel pellet | |
| CN111112569B (en) | Processing technology of metal-based ceramic composite material part | |
| CN110540410B (en) | Feed for alumina ceramic injection molding and preparation method thereof | |
| CN110483051B (en) | Preparation method of density-controllable B10-rich boron carbide ceramic | |
| CN114702315A (en) | Hot-bending ceramic and preparation method thereof | |
| CN108856713B (en) | SUS201 stainless steel injection molding feed and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |