CN111826540A - MAX phase metal ceramic injection molding process - Google Patents
MAX phase metal ceramic injection molding process Download PDFInfo
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- CN111826540A CN111826540A CN202010704456.1A CN202010704456A CN111826540A CN 111826540 A CN111826540 A CN 111826540A CN 202010704456 A CN202010704456 A CN 202010704456A CN 111826540 A CN111826540 A CN 111826540A
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- injection molding
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- 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
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- 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
- B22F1/103—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing an organic binding agent comprising a mixture of, or obtained by reaction of, two or more components other than a solvent or a lubricating agent
-
- 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
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- 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
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- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses an MAX phase metal ceramic injection molding process, which comprises the following steps: mixing powder: the addition amount of the binder accounts for 25-45% of the total volume of the mixed powder, and the binder is prepared from the following raw materials in parts by weight: 25-35 parts of cellulose acetate butyrate, 60-80 parts of polyethylene glycol, 1-3 parts of stearic acid and 0.4-0.6 part of phenothiazine, wherein when the kneader is heated to a preset temperature, the binder and MAX phase powder are poured into the kneader to be fully mixed; preparing granular feed by a granulator, and performing injection molding by using an injection molding machine to obtain a green body; putting the green body into distilled water, degreasing, and removing part of the binder; drying the green body, and removing the residual binder by a thermal degreasing method; and solidifying the metal ceramic green body by a high-temperature pressureless sintering method, and cooling to room temperature to obtain a finished product. The binder disclosed by the invention is water-soluble, good in fluidity and dispersibility, and capable of being uniformly mixed with MAX phase powder, and has the characteristics of uniform blank molding, low injection molding cost, short degreasing time, high efficiency, no pollution and the like.
Description
Technical Field
The invention relates to the technical field of metal ceramic part molding, in particular to a binder for metal ceramic injection molding and an injection molding process.
Background
MAX phase cermet is a new kind of high-performance comprehensive ceramic material, besides possessing conductivity and thermal conductivity, higher Young's modulus and shear modulus, good metal characteristics such as machinability, etc., it also possesses good ceramic characteristics such as corrosion resistance, thermal stability, oxidation resistance and self-lubricity, so it is widely used in the fields of gas igniter, heat exchanger, high thrust rocket nozzle, brush wire, kiln furniture, metal smelting electrode and high-temperature sealing element, etc., MAX phase cermet needs to use binder in the course of processing, the binder adopted at present mostly belongs to water-insoluble binder, the solvent degreasing uses organic solvent, such as hexane, etc., there is certain difficulty in industrialization, its organic solvent is harmful to the staff's health, and pollute the environment; the catalytic degreasing generates a large amount of formaldehyde gas in the degreasing process, thereby polluting the environment.
Disclosure of Invention
The invention provides an MAX phase metal ceramic injection molding process according to the defects, wherein a water-soluble binder is used for metal ceramic molding, and the injection molding process is designed by combining the characteristics of the binder.
The technical scheme of the invention is as follows:
a MAX phase cermet injection molding process comprises the following steps:
s1, mixing powder: the MAX phase powder particle specification is 8-12 mu m, the addition amount of the binder accounts for 25-45% of the total volume of the mixed powder, and the binder is prepared from the following raw materials in parts by weight: 25-35 parts of Cellulose Acetate Butyrate (CAB), 60-80 parts of polyethylene glycol (PEG), 1-3 parts of stearic acid and 0.4-0.6 part of phenothiazine; when the kneader is heated to a preset temperature, the binder and the powder are poured into the kneader to be fully mixed;
s2, granulating and injection molding: after the mixed and stirred powder is cooled, preparing granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body;
s3, solvent degreasing: putting the green body into solvent degreasing equipment or a container, and performing solvent degreasing in distilled water with flow rate to remove part of the binder;
s4, thermal degreasing: drying the green body degreased by the solvent, then putting the green body into a degreasing sintering dry distillation furnace, slowly heating the green body in argon with flow velocity, and removing the residual binder by a thermal degreasing method;
s5, sintering: and solidifying the green body subjected to the two-step degreasing and binder removal by a high-temperature pressureless sintering method, and cooling to room temperature to obtain a highly compact MAX finished product.
In the invention, the cellulose acetate butyrate, the polyethylene glycol, the stearic acid and the phenothiazine which are selected as the binding agent are subjected to synergistic reaction to form the environment-friendly water-soluble base binding agent which is easy to demould and good in binding property. Wherein the cellulose acetate butyrate reduces the crystallinity of the binder, so that the binder can be degreased more quickly at a lower temperature during thermal degreasing; polyethylene glycol is soluble in water, and the dissolution and diffusion speeds are high at a certain water temperature; stearic acid is used as a lubricant, not only can play a role of a bridge between the binder and the powder particles to prevent two phases from being separated, ensure the uniformity of mixed materials, but also can play a role of lubrication between the powder particles and the die wall; phenothiazine is to prevent oxidation of polyethylene glycol during heating of the powder injection molding.
The injection molding method combines the mature powder metallurgy technology of organic polymer injection molding, has the advantages of capability of molding workpieces with complex shapes at one time, high dimensional precision of the workpieces, no need of machining, easiness in realizing high-efficiency automatic production and the like, and is particularly suitable for mass production of parts with complex shapes, high precision and high performance.
Preferably, in step S1, the kneader is set to a predetermined temperature of 160 to 180 ℃ and the mixing and stirring time is 1 to 3 hours.
Preferably, in the step S2, the injection pressure is 20 to 50MPa, and the injection temperature is 180 to 220 ℃.
Preferably, in the step S3, the temperature of the distilled water is 40-60 ℃, the flow rate is 0-20 cm/S, and the distilled water is kept for 5-10 hours.
Preferably, in the step S4, the drying time is 30-90 min, the argon flow rate is 100-200L/h, the temperature is slowly increased to 450-580 ℃ under the argon flushing, and the heat preservation time is 1-3 h.
Preferably, in the step S5, the sintering temperature is 1280-1400 ℃, and the heat preservation time is 3-6 h.
The binder in the MAX phase metal ceramic injection molding process is a water-soluble binder, and when the binder is applied, the flowability and the dispersibility of the binder are good, the binder is uniformly mixed with MAX phase powder, a blank is uniformly molded, the properties of the blank are consistent, the binder has the characteristics of low cost, short degreasing time, high efficiency, no pollution and the like, and the quality of the ceramic blank is not influenced in the discharging process.
Detailed Description
The following is a further explanation of a MAX phase cermet injection molding process, but the examples are not intended to limit the invention in any way.
Example 1, the binder for injection molding of MAX phase cermet of this example was composed of the following components in parts by weight: 25 parts of cellulose acetate butyrate, 60 parts of polyethylene glycol, 1 part of stearic acid and 0.4 part of phenothiazine. And pouring the binder accounting for 25 percent of the total volume of the mixed powder and MAX phase cermet powder into a kneader preheated to 160 ℃ for mixing uniformly for 1 hour, fully melting and mixing the components uniformly, discharging and cooling to room temperature to obtain MAX phase cermet molding feed.
And preparing the feed into granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body. The injection pressure of the injection molding machine is 20MPa, and the temperature of an injection nozzle is 180 ℃.
Soaking the green body in distilled water at 40 ℃, keeping for 5 hours, and removing polyethylene glycol; then drying the blank after solvent degreasing for 30min, putting the blank into a degreasing sintering retort, heating to 450 ℃ at a heating rate of 2 ℃/min at a gas flow rate of 100L/h under an argon atmosphere, and keeping for 1h to obtain a degreased blank; then the vacuum degree of the degreasing sintering retort is adjusted to 10- 6mbar, sintering the degreased blank body, wherein the sintering temperature is 1280 ℃, the heat preservation time is 3 hours, and cooling the MAX-phase metal ceramic part.
Example 2, the binder for injection molding of MAX phase cermet of this example was composed of the following components in parts by weight: 35 parts of cellulose acetate butyrate, 80 parts of polyethylene glycol, 3 parts of stearic acid and 0.6 part of phenothiazine. And pouring the binder accounting for 45 percent of the total volume of the mixed powder and MAX phase cermet powder into a kneader preheated to 180 ℃ for uniformly mixing for 3 hours, fully melting and uniformly mixing the components, discharging and cooling to room temperature to obtain MAX phase cermet molding feed.
And preparing the feed into granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body. The injection pressure of the injection molding machine is 50MPa, and the temperature of an injection nozzle is 220 ℃.
Soaking the green body in distilled water at 60 ℃, keeping for 10h, and removing polyethylene glycol; then drying the blank degreased by the solvent for 90min, putting the blank into a degreasing sintering retort, heating to 580 ℃ at a heating rate of 2 ℃/min at a gas flow rate of 200L/h under an argon atmosphere, and keeping for 3h to obtain a degreased blank; then the vacuum degree of the degreasing sintering retort is adjusted to 10- 6mbar, sintering the degreased blank body, wherein the sintering temperature is 1400 ℃, the heat preservation time is 6h,and cooling the MAX phase metal ceramic part.
Example 3, the binder for injection molding of MAX phase cermet of this example was composed of the following components in parts by weight: 30 parts of cellulose acetate butyrate, 70 parts of polyethylene glycol, 2 parts of stearic acid and 0.5 part of phenothiazine. And pouring the binder accounting for 35 percent of the total volume of the mixed powder and MAX phase cermet powder into a kneader preheated to 170 ℃ for mixing uniformly for 2 hours, fully melting and mixing the components uniformly, discharging and cooling to room temperature to obtain MAX phase cermet molding feed.
And preparing the feed into granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body. The injection pressure of the injection molding machine is 35MPa, and the temperature of an injection nozzle is 200 ℃.
Soaking the green body in distilled water at 50 ℃, keeping for 7h, and removing polyethylene glycol; then drying the blank after solvent degreasing for 60min, putting the blank into a degreasing sintering retort, heating to 500 ℃ at a heating rate of 2 ℃/min under the argon atmosphere at a gas flow rate of 150L/h, and keeping for 2h to obtain a degreased blank; then the vacuum degree of the degreasing sintering retort is adjusted to 10- 6mbar, sintering the degreased blank at 1350 ℃, keeping the temperature for 4h, and cooling the degreased blank to obtain the MAX-phase metal ceramic part.
Example 4, the binder for injection molding of MAX phase cermet of this example was composed of the following components in parts by weight: 25 parts of cellulose acetate butyrate, 60 parts of polyethylene glycol, 3 parts of stearic acid and 0.6 part of phenothiazine. And pouring the binder accounting for 25 percent of the total volume of the mixed powder and MAX phase cermet powder into a kneader preheated to 160 ℃ for uniformly mixing for 3 hours, fully melting and uniformly mixing the components, discharging and cooling to room temperature to obtain MAX phase cermet molding feed.
And preparing the feed into granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body. The injection pressure of the injection molding machine is 20MPa, and the temperature of an injection nozzle is 180 ℃.
Soaking the green body in 60 deg.C distilled water, maintaining for 10 hr, and removing polyethylene glycol(ii) a Then drying the blank after solvent degreasing for 30min, putting the blank into a degreasing sintering retort, heating to 580 ℃ at a heating rate of 2 ℃/min at a gas flow rate of 100L/h under an argon atmosphere, and keeping for 3h to obtain a degreased blank; then the vacuum degree of the degreasing sintering retort is adjusted to 10- 6mbar, sintering the degreased blank body, wherein the sintering temperature is 1280 ℃, the heat preservation time is 6 hours, and cooling the MAX-phase metal ceramic part.
Example 5, the binder for injection molding of MAX phase cermet of this example was composed of the following components in parts by weight: 35 parts of cellulose acetate butyrate, 80 parts of polyethylene glycol, 3 parts of stearic acid and 0.4 part of phenothiazine. And pouring the binder accounting for 25 percent of the total volume of the mixed powder and MAX phase cermet powder into a kneader preheated to 160 ℃ for uniformly mixing for 3 hours, fully melting and uniformly mixing the components, discharging and cooling to room temperature to obtain MAX phase cermet molding feed.
And preparing the feed into granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body. The injection pressure of the injection molding machine is 50MPa, and the temperature of an injection nozzle is 220 ℃.
Soaking the green body in distilled water at 60 ℃, keeping for 5h, and removing polyethylene glycol; then drying the blank after solvent degreasing for 30min, putting the blank into a degreasing sintering retort, heating to 450 ℃ at a heating rate of 2 ℃/min at a gas flow rate of 100L/h under an argon atmosphere, and keeping for 1h to obtain a degreased blank; then the vacuum degree of the degreasing sintering retort is adjusted to 10- 6mbar, sintering the degreased blank body, wherein the sintering temperature is 1400 ℃, the heat preservation time is 6h, and cooling the MAX-phase metal ceramic part.
In the above embodiment, the specification of MAX phase powder particles is 8-12 mu m.
The above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. It should be understood that any changes or modifications obvious to those skilled in the art are within the scope of the present invention.
Claims (6)
1. An MAX phase cermet injection molding process is characterized by comprising the following steps:
s1, mixing powder: the MAX phase powder particle specification is 8-12 mu m, the addition amount of the binder accounts for 25-45% of the total volume of the mixed powder, and the binder is prepared from the following raw materials in parts by weight: 25-35 parts of cellulose acetate butyrate, 60-80 parts of polyethylene glycol, 1-3 parts of stearic acid and 0.4-0.6 part of phenothiazine; when the kneader is heated to a preset temperature, the binder and the powder are poured into the kneader to be fully mixed;
s2, granulating and injection molding: after the mixed and stirred powder is cooled, preparing granular feed by a granulator or a crusher, and performing injection molding on the granular feed by using an injection molding machine to obtain a green body;
s3, solvent degreasing: putting the green body into solvent degreasing equipment or a container, and carrying out solvent degreasing in distilled water with flow rate to remove part of the binder;
s4, thermal degreasing: drying the green body degreased by the solvent, then putting the green body into a degreasing sintering dry distillation furnace, slowly heating the green body in argon with flow velocity, and removing the residual binder by a thermal degreasing method;
s5, sintering: and solidifying the green body subjected to the two-step degreasing and binder removal by a high-temperature pressureless sintering method, and cooling to room temperature to obtain a highly compact MAX finished product.
2. The MAX phase cermet injection molding process of claim 1, wherein in step S1, the kneader is set at a predetermined temperature of 160-180 ℃, and the mixing and stirring time is 1-3 h.
3. The MAX phase cermet injection molding process of claim 1, wherein, in step S2, the injection pressure is 20-50 MPa and the injection temperature is 180-220 ℃.
4. The MAX phase cermet injection molding process of claim 1, wherein, in step S3, the temperature of distilled water is 40-60 ℃, the flow rate is 0-20 cm/S, and the temperature is maintained for 5-10 h.
5. The MAX phase cermet injection molding process of claim 1, wherein in step S4, the drying time is 30-90 min, the argon flow rate is 100-200L/h, the temperature is slowly raised to 450-580 ℃ under argon flushing, and the holding time is 1-3 h.
6. The MAX phase cermet injection molding process of claim 1, wherein, in step S5, the sintering temperature is 1280-1400 ℃, and the holding time is 3-6 h.
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| CN202010704456.1A CN111826540A (en) | 2020-07-21 | 2020-07-21 | MAX phase metal ceramic injection molding process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725710A (en) * | 2020-12-18 | 2021-04-30 | 苏州欧美克合金工具有限公司 | Processing technology of mixed type metal ceramic material |
| CN117020198A (en) * | 2023-10-08 | 2023-11-10 | 华南理工大学 | Metal injection molding feed of kovar alloy |
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| CN117020198A (en) * | 2023-10-08 | 2023-11-10 | 华南理工大学 | Metal injection molding feed of kovar alloy |
| CN117020198B (en) * | 2023-10-08 | 2023-12-08 | 华南理工大学 | Metal injection molding feed of kovar alloy |
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