CN102351542B - Preparation method of hollow-structure metal or ceramic part - Google Patents

Preparation method of hollow-structure metal or ceramic part Download PDF

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CN102351542B
CN102351542B CN 201110194281 CN201110194281A CN102351542B CN 102351542 B CN102351542 B CN 102351542B CN 201110194281 CN201110194281 CN 201110194281 CN 201110194281 A CN201110194281 A CN 201110194281A CN 102351542 B CN102351542 B CN 102351542B
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degreasing
hollow
inner core
injection
ceramic component
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CN 201110194281
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CN102351542A (en
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何浩
李益民
刘攀
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中南大学
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Abstract

The invention relates to a preparation method of a hollow-structure metal or ceramic part, which comprises the following steps: selecting metal or ceramic powder as the raw material, mixing, and granulating to obtain a feed material; selecting a core material; injecting the core material into a die by co-injection molding to obtain a core in hollow shape, and injecting the metal or ceramic feed material to be completely coated on the core, thereby obtaining a green body; and carrying out solvent extraction and heating on the green body to remove the adhesive and core, and sintering to obtain the hollow-structure product. The invention implements one-step molding of the hollow metal or ceramic part; from the raw material to the product, the production cycle is short, and the automation degree of equipment is high, thereby greatly enhancing the efficiency and forming a randomly complex and completely hollow die cavity; and thus, the invention can be used for preparing a completely hollow part with no joint, greatly lowers the cost of the product, and is especially suitable for preparing hollow metal and ceramic parts.

Description

The preparation method of a kind of hollow structure metal or ceramic component

Technical field

The invention discloses the technology of preparation method of a kind of hollow metal or ceramic component, belong to common injection forming preparing technical field.

Background technology

Along with the demand of development and national economy and energy-saving and emission-reduction, the lightweight of component, multifunction have become the focus of research.Hollow metal and ceramic component not only can the implementation structure material lighting; And have economic environmental protection, advantage such as economize on resources; Can also satisfy the demand of function component such as electrostatic shielding, magneticshielding on the function, in industry-by-industry, obtain increasing application.

The method that tradition is used to make hollow metal part mainly comprises: machine-tooled methods such as (1) boring, forging and pressing, assembling; Liquid manufacturing process such as (2) investment cast, the auxilliary shaping of gas; The powder forming method of (3) ion cladding, jet deposition, belt carcass bar powder metallurgy process such as (like compacting, injection formings); The method that can be used to make the hollow ceramic component then still less.That these methods all exist is many such as the operation process, needs are made core, can not once-forming, problem such as cycle length, inefficiency, equipment cost height, expense is big.

In recent years, powder is total to injection technique and has obtained increasing concern.This method is to be combined and a novel process growing up by the common injection technique of powder injection forming technology and plastics.Powder is the injection moulding machine of two or more injecting systems of injection molding process use altogether, advances different types of powder feed while or sequential injection in the same mould, and being shaped to have the component of coating or pattern structure.Be applied at present the preparation that the core shell has the component of heterogeneity gradually.But because the complicacy of technology does not also apply to prepare the hollow component at present.The present invention proposes, and can adopt powder to be total to injection technique and prepare hollow metal and ceramic component.Injection forming method before is different altogether with powder; The present invention does not adopt two kinds of powder feed; And adopt a kind of powder feed and a kind of inner core material that removes to inject; Obtain powder feed and partially or completely coat the blank that can remove inner core, obtain hollow structure through removing inner core again, obtain product through sintering at last.

The content of invention

The objective of the invention is to overcome the deficiency of prior art and provide a kind of technology simple, weak point consuming time, the metal with complete hollow structure of once-forming and the preparation method of ceramic component help reducing the manufacturing cost of hollow component.The special-shaped hollow structure component of refractory metal and stupalith particularly can once-forming, and cost is low.

The preparation method of a kind of hollow structure metal of the present invention or ceramic component may further comprise the steps:

The first step: material chosen

The selection of case material: case material is selected metal or ceramic powder material; Said metal-powder is selected from a kind of among stainless steel, low alloy steel, Ti alloy, Cu alloy, WC-Co, the W-Ni-Fe; Said ceramic powder is selected from a kind of in zirconium white, aluminum oxide, aluminium nitride AlN, silicon oxide, silicon nitride, the silit;

The selection of inner core material: be selected from least a in the inorganics that can remove through dissolution with solvents or heating or the organism; Specifically be to be selected from a kind of in paraffin, Vilaterm, Vestolen PP 7052, polymethylmethacrylate, polyoxyethylene glycol, sodium-chlor, the Repone K;

Sticker is selected from one or more in paraffin, Vilaterm, Vestolen PP 7052, polymethylmethacrylate, polyoxyethylene glycol, vegetables oil, the Triple Pressed Stearic Acid;

Second step: injection forming

Prepare housing feeding and inner core feeding by injection molding process; At first the inner core feeding is injected core, cooling, the inner core of acquisition hollow metal or ceramic component product; Then, said inner core is transferred in the shell mould, the housing feeding is injected said shell mould coat said inner core fully; Obtain the product crude green body;

The shape of said core is similar with the hollow type cavity shape of target hollow structure metal or ceramic component, said core be of a size of target hollow structure metal or ceramic component the hollow cavity dimension 1-2 doubly;

The shape of said shell mould is similar with the shape of target hollow structure metal or ceramic component, said shell mould be of a size of target hollow structure metal or ceramic component physical dimension 1-2 doubly;

The 3rd step: remove inner core and sticker

At first, adopt solvent degreasing, place solvent to remove the part sticker of part or all of inner core and housing the second step products obtained therefrom crude green body; Then, adopt hot degreasing process, make rest parts inner core, sticker and the solvent evaporation or the decomposition and inversion that remain in the said product crude green body hollow cavity are gas molecule, in the pore channel of shell powder, discharge; Obtain the product base substrate; Said hot degreasing process is: be heated to 300-600 ℃ with 0.5-5 ℃/min speed, the speed with 0.5-5 ℃/min is heated to 750-1200 ℃ of insulation 30-600 minute then, and degreasing atmosphere is argon gas;

The 4th step: substep sintering

The product base substrate that the 3rd step was obtained is to be warming up to 800-1200 ℃ of presintering 1-5h with 5-10 ℃/min under the 0.001Pa-10MPa environment in vacuum tightness; After being warming up to 1200-1600 ℃ of sintered heat insulating 2-10h with 5-20 ℃/min then; Cool to room temperature with the furnace, obtain hollow structure metal or ceramic component.

Among the preparation method of a kind of hollow structure metal of the present invention or ceramic component, said case material and sticker be 40-65% by volume: the 60-35% batching.

Among the preparation method of a kind of hollow structure metal of the present invention or ceramic component, said feeding by case material and sticker 100-180 ℃ of mixing making.

Among the preparation method of a kind of hollow structure metal of the present invention or ceramic component; Said inner core feeding injection temperature is 60 ℃-180 ℃, and injection pressure is 40-100MPa, and injection speed is 30-60g/s; The demoulding when treating behind the injection forming that the core temperature is reduced to 20-50 ℃ obtains inner core.

Among the preparation method of a kind of hollow structure metal of the present invention or ceramic component; Said housing feeding injection temperature is 130-220 ℃; Injection pressure is 60-120MPa, and injection speed is 30-70g/s, 40-55 ℃ of mould temperature; The demoulding when treating behind the injection forming that the shell mould temperature is reduced to 20-40 ℃ obtains the product crude green body.

Among the preparation method of a kind of hollow structure metal of the present invention or ceramic component; Said solvent degreasing is the product crude green body to be extracted in the constant temperature degreasing solvent that moves to 30-50 ℃ behind the preparatory degreasing 2-8h carry out the constant temperature degreasing in 20-50 ℃ preparatory degreasing solvent, and the constant temperature degreasing time is 2-8h.

Among the preparation method of a kind of hollow structure metal of the present invention or ceramic component, said preparatory degreasing solvent is selected from least a in methylene dichloride, normal heptane, water, the alcohol; Said constant temperature degreasing solvent is selected from least a in methylene dichloride, normal heptane, water, the alcohol.

The present invention is owing to adopt above-mentioned process method; Based on powder injection molding technology altogether, obtain hollow structure metal and ceramic component, through with metal or ceramic powder and sticker through mixing, the even feeding of acquisition of granulating; Select suitable inner core material; Adopt powder injection molding technology altogether then, accomplish the injection of inner core earlier, acquisition has the inner core of the hollow metal and the needed shape of ceramic component product of sufficient intensity; Carry out the injection of shell afterwards again, the acquisition inner core is coated on the base substrate among the shell fully.Through degreasing process inner core and sticker are removed then, and the base substrate after the degreasing is carried out sintering, thereby obtain hollow structure metal and ceramic component product.The method that obtains hollow structure among the present invention is crucial, mainly considers that from the method angle once-forming, shortening cycle raise the efficiency, reduce product cost.The present invention prepares inner core earlier, adopts metal or ceramic feeding that it is coated again, and whole process is accomplished within an infusion cycles by being total to injection machine, has realized disposable shaping; Expect product from former, with short production cycle, automation degree of equipment is high, therefore can significantly raise the efficiency, and realizes volume production, can significantly reduce the cost of product.

In above-mentioned technology, the key factor that influences product performance is the selection and the removing process of inner core.Main consideration inner core removes mode, removes speed control and the control of product conformality.Inner core material can be selected pure substance or mixture; Requirement has good flowability in injection process; Be beneficial to be shaped and provide the base substrate of needed hollow shape; Inner core material and sticker do not produce the reaction that is harmful to shaping and conformality, particularly inner core material and require and can remove through dissolution with solvents or hot degreasing process; The removing process design of inner core should realize removing fast inner core, with faster production cycle and efficient.Guarantee that again inner core removes speed and combines with the effective of casing rigidity, make in the inner core subtractive process not can because of shell lack support be out of shape or subtractive process in ftracture.Organism list constituent element inner core, mixture of organic substance inner core, inorganics and mixture of organic substance inner core are chosen in the present invention's design; Intensity and the rheological property of inner core are under injecting condition, have good flowability; Has enough intensity again; Can not produce distortion in support metal and ceramic shell, destroy hollow shape; Through adjustment and solvent composition and degreasing process, in the middle of the process that inner core removes, speed control is in the certain speed scope, and shell can not produce big volume change, thereby obtains high efficient, is not easy defectives such as shell distortion, cracking.

In sum, compare with traditional machine-tooled method, liquid manufacturing process and powder forming method technology, the present invention has realized the disposable shaping of hollow metal and ceramic component; Expect product from former, with short production cycle, automation degree of equipment is high, therefore can significantly raise the efficiency, and realizes volume production, can significantly reduce the cost of product, is particularly suitable for the preparation of hollow metal and ceramic component.

Embodiment:

Below in conjunction with three instances the inventive method is further specified.

Embodiment 1:

The preparation wall thickness is 3mm, and diameter is the 17-4PH stainless steel hollow ball of 20mm.

Getting 17-4PH stainless steel iron powder is the shell material powder, and sticker is made up of 10% vegetables oil, 30% high density polyethylene(HDPE), 60% paraffin, and the volume ratio of powder and sticker is 65: 35, and powder and sticker is mixing in mixing roll; Melting temperature is 100 ℃, is prepared into feeding, and inner core adopts paraffin, is being total to injection forming on the injection machine altogether; At first inject inner core, injection temperature is 6 ℃, and injection pressure is 40MPa; Injection speed is 30g/s, treats after the shaping that the mould temperature is cooled to 20-30 ℃ and carries out the demoulding, obtains inner core; Inner core is transferred in second die cavity, the injection feeding, and injection temperature is 130 ℃; Injection pressure is 60MPa, and injection speed is 30g/s, 40 ℃ of mould temperature.The injection base of gained is degreasing 2h in 20 ℃ of Ethylene Dichloride solution; Move to then in 30 ℃ of Ethylene Dichloride constant temperature degreasing tanks and carry out fast defat 2h; Dry 1-3h is placed on and carries out hot degreasing in the atmosphere debinding furnace in 60 ℃ of loft drier again; Be heated to 300 ℃ with 0.5 ℃/min speed, be heated to 750 ℃ with the speed of 0.5 ℃/min then and carry out hot degreasing, degreasing atmosphere is argon gas.The degreasing base is warming up to 800 ℃ of sintering 1h with 5 ℃/min in vacuum 0.001Pa, is warming up to 1200 ℃ of sintered heat insulating 2h with 5 ℃/min then, cool to room temperature at last with the furnace.

Embodiment 2:

The preparation wall thickness is 6mm, and diameter is the Ti-6V-4V hollow part of 20mm.

Get atomizing Ti6Al4V powder, sticker is by 15% vegetables oil, 35% Vestolen PP 7052,30% paraffin, and 20% polymethylmethacrylate is formed; Powder and sticker that the last step mixes is mixing on mixing roll, and the powder volume ratio is 40%, and melting temperature is 180 ℃; Extrusion granulator on forcing machine makes feeding further even again, is prepared into the shell feeding; The sandwich layer fluid adopts the mixture of 50% high density polyethylene(HDPE) and 50% paraffin, and feeding is being total to injection forming on the injection machine altogether, and the inner core injection temperature is 180 ℃; Injection pressure is 100MPa, and injection speed is 60g/s, 50 ℃ of mould temperature; The shell injection temperature is 220 ℃, and injection pressure is 120MPa, and injection speed is 70g/s, and 55 ℃ of mould temperature obtain injecting base.The injection base of gained is degreasing 8h in 50 ℃ of dichloromethane solutions; Move to then and adopt normal heptane to carry out fast defat 8h in 50 ℃ of constant temperature water bath degreasing tanks; Dry 2h is placed on and carries out hot degreasing in the atmosphere debinding furnace in 60 ℃ of loft drier again; Be heated to 600 ℃ with 5 ℃/min speed, be heated to 1000 ℃ with the speed of 5 ℃/min then and carry out hot degreasing, degreasing atmosphere is argon gas.The degreasing base is warming up to 1200 ℃ of sintering 5h with 10 ℃/min in vacuum atmosphere, is warming up to 1390 ℃ of sintered heat insulating 10h with 20 ℃/min then, cool to room temperature at last with the furnace.

Embodiment 3:

The preparation wall thickness is 1mm, and diameter is α-Al of 20mm 2O 3The pottery hollow part.

Get α-Al 2O 3Ceramic powder is a sheating material, and sticker is by 10% Triple Pressed Stearic Acid, 20% high density polyethylene(HDPE), 70% polyoxyethylene glycol, and powder and sticker is mixing on mixing roll, and the powder volume ratio is 50%; Melting temperature is 150 ℃, is prepared into the shell feeding, and inner core material adopts the mixture of 30%NaCl, 30%KCl, 5% Triple Pressed Stearic Acid, 25% high density polyethylene(HDPE); Be total to injection forming on the injection machine, inner core core injection temperature is 110 ℃, and injection pressure is 100MPa; Injection speed is 70g/s, treats after the shaping that the mould temperature is cooled to 30 ℃ of die sinkings, and the shell injection temperature is 150 ℃; Injection pressure is 80MPa, and injection speed is 55g/s, and the mould temperature obtains injecting base for 40 ℃.The injection base of gained is degreasing 2h in 30 ℃ of Ethylene Dichloride solution; Room temperature degreasing 2h in zero(ppm) water again; Repeat Ethylene Dichloride degreasing and zero(ppm) water degreasing and surpass 80% to solubility constituent element degreasing rate, dry 2h is placed on and carries out hot degreasing in the atmosphere debinding furnace in 60 ℃ of loft drier again, slowly is heated to 300 ℃ of insulation 1h with 0.5 ℃/min speed; Be heated to 600 ℃ of insulation 3h with 0.5 ℃/min speed then; Be heated to 750 ℃ with 1 ℃/min then and carry out hot degreasing and remove, degreasing atmosphere is argon gas, then the degreasing base is warming up to 1200 ℃ of sintering 1h with 10 ℃/min in vacuum atmosphere; Be warming up to 1600 ℃ of sintered heat insulating 2h with 15 ℃/min then, cool to room temperature at last with the furnace.

Embodiment 4:

The preparation wall thickness is 2mm, and diameter is the W-Ni-Fe hollow part of 20mm.

Get tungsten powder, carbonyl nickel powder, carbonyl iron dust are the shell material powder, are 90: 7: 3 by weight percentage; Place four jars of blender batch mixing 2h, sticker is made up of 15% vegetables oil, 35% Vestolen PP 7052,50% paraffin, and powder and sticker that the last step mixes is mixing on mixing roll, and the powder volume ratio is 40%; Melting temperature is 180 ℃, and extrusion granulator on forcing machine makes feeding further even again, is prepared into the shell feeding; The sandwich layer fluid adopts the mixture of 50% high density polyethylene(HDPE) and 50% paraffin, and feeding is being total to injection forming on the injection machine altogether, and the inner core injection temperature is 180 ℃; Injection pressure is 100MPa, and injection speed is 60g/s, 50 ℃ of mould temperature; The shell injection temperature is 220 ℃, and injection pressure is 120MPa, and injection speed is 70g/s, and 55 ℃ of mould temperature obtain injecting base.The injection base of gained is degreasing 8h in 50 ℃ of dichloromethane solutions; Move to then and adopt normal heptane to carry out fast defat 8h in 50 ℃ of constant temperature water bath degreasing tanks; Dry 2h is placed on and carries out hot degreasing in the atmosphere debinding furnace in 60 ℃ of loft drier again; Be heated to 600 ℃ with 5 ℃/min speed, be heated to 1000 ℃ with the speed of 5 ℃/min then and carry out hot degreasing, degreasing atmosphere is argon gas.The degreasing base is warming up to 1200 ℃ of sintering 5h with 10 ℃/min in vacuum atmosphere, is warming up to 1450 ℃ of sintered heat insulating 10h with 20 ℃/min then, cool to room temperature at last with the furnace.

Embodiment 5:

The preparation wall thickness is 2mm, and diameter is the zirconium white hollow part of 12mm.

Zirconium white is the shell material powder, is 90: 7: 3 by weight percentage, places four jars of blender batch mixing 2h, and sticker is made up of 15% vegetables oil, 35% Vestolen PP 7052,50% polyoxyethylene glycol; Powder and sticker that the last step mixes is mixing on mixing roll, and the powder volume ratio is 50%, and melting temperature is 150 ℃; Extrusion granulator on forcing machine makes feeding further even again, is prepared into the shell feeding; The sandwich layer fluid adopts the mixture of 50%KCl and 50% paraffin, and feeding is being total to injection forming on the injection machine altogether, and the inner core injection temperature is 160 ℃; Injection pressure is 90MPa, and injection speed is 50g/s, 40 ℃ of mould temperature; The shell injection temperature is 200 ℃, and injection pressure is 100MPa, and injection speed is 60g/s, and 50 ℃ of mould temperature obtain injecting base.The injection base of gained is degreasing 3h in 40 ℃ of dichloromethane solutions; Move to then and adopt normal heptane to carry out fast defat 2h in 40 ℃ of constant temperature water bath degreasing tanks; Dry 2h is placed on and carries out hot degreasing in the atmosphere debinding furnace in 50 ℃ of loft drier again; Be heated to 600 ℃ with 5 ℃/min speed, be heated to 1000 ℃ with the speed of 5 ℃/min then and carry out hot degreasing, degreasing atmosphere is argon gas.The degreasing base is warming up to 1200 ℃ of sintering 5h with 10 ℃/min in vacuum atmosphere, is warming up to 1550 ℃ of sintered heat insulating 4h with 20 ℃/min then, cool to room temperature at last with the furnace.

Claims (7)

1. the preparation method of a hollow structure metal or ceramic component may further comprise the steps:
The first step: material chosen
The selection of case material: case material is selected metal or ceramic powder material; Said metal-powder is selected from a kind of among stainless steel, low alloy steel, Ti alloy, Cu alloy, WC-Co, the W-Ni-Fe; Said ceramic powder is selected from a kind of in zirconium white, aluminum oxide, aluminium nitride AlN, silicon oxide, silicon nitride, the silit;
The selection of inner core material: be selected from least a in the inorganics that can remove through dissolution with solvents or heating or the organism; Specifically be to be selected from a kind of in paraffin, Vilaterm, Vestolen PP 7052, polymethylmethacrylate, polyoxyethylene glycol, the sodium-chlor;
Sticker is selected from least a in paraffin, Vilaterm, Vestolen PP 7052, polymethylmethacrylate, polyoxyethylene glycol, vegetables oil, the Triple Pressed Stearic Acid;
Second step: injection forming
Prepare housing feeding and inner core feeding by injection molding process; At first the inner core feeding is injected core, cooling, the inner core of acquisition hollow metal or ceramic component product; Then, said inner core is transferred in the shell mould, the housing feeding is injected said shell mould coat said inner core fully; Obtain the product crude green body;
The shape of said core is similar with the hollow type cavity shape of target hollow structure metal or ceramic component, said core be of a size of target hollow structure metal or ceramic component the hollow cavity dimension 1-2 doubly;
The shape of said shell mould is similar with the shape of target hollow structure metal or ceramic component, said shell mould be of a size of target hollow structure metal or ceramic component physical dimension 1-2 doubly;
The 3rd step: remove inner core and sticker
At first, adopt solvent degreasing, place solvent to remove the part sticker of part or all of inner core and housing the second step products obtained therefrom crude green body; Then, adopt hot degreasing process, make rest parts inner core, sticker and the solvent evaporation or the decomposition and inversion that remain in the said product crude green body hollow cavity are gas molecule, in the pore channel of shell powder, discharge; Obtain the product base substrate; Said hot degreasing process is: be heated to 300-600 ℃ with 0.5-5 ℃/min speed, the speed with 0.5-5 ℃/min is heated to 750-1200 ℃ of insulation 30-600 minute then, and degreasing atmosphere is argon gas;
The 4th step: substep sintering
The product base substrate that the 3rd step was obtained is to be warming up to 800-1200 ℃ of presintering 1-5h with 5-10 ℃/min under the 0.001Pa-10MPa environment in vacuum tightness; After being warming up to 1200-1600 ℃ of sintered heat insulating 2-10h with 5-20 ℃/min then; Cool to room temperature with the furnace, obtain hollow structure metal or ceramic component.
2. the preparation method of a kind of hollow structure metal according to claim 1 or ceramic component is characterized in that: said case material and sticker be (40-65) by volume: (60-35) batching.
3. the preparation method of a kind of hollow structure metal according to claim 2 or ceramic component is characterized in that: said feeding by case material and sticker 100-180 ℃ of mixing making.
4. the preparation method of a kind of hollow structure metal according to claim 3 or ceramic component; It is characterized in that: said inner core feeding injection temperature is 60 ℃-180 ℃; Injection pressure is 40-100MPa; Injection speed is 30-60g/s, and the demoulding when treating behind the injection forming that the core temperature is reduced to 20-50 ℃ obtains inner core.
5. the preparation method of a kind of hollow structure metal according to claim 4 or ceramic component; It is characterized in that: said housing feeding injection temperature is 130-220 ℃; Injection pressure is 60-120MPa, and injection speed is 30-70g/s, 40-55 ℃ of mould temperature; The demoulding when treating behind the injection forming that the shell mould temperature is reduced to 20-40 ℃ obtains the product crude green body.
6. the preparation method of a kind of hollow structure metal according to claim 5 or ceramic component; It is characterized in that: said solvent degreasing is the product crude green body to be extracted in the constant temperature degreasing solvent that moves to 30-50 ℃ behind the preparatory degreasing 2-8h carry out the constant temperature degreasing in 20-50 ℃ preparatory degreasing solvent, and the constant temperature degreasing time is 2-8h.
7. the preparation method of a kind of hollow structure metal according to claim 6 or ceramic component is characterized in that: said preparatory degreasing solvent is selected from a kind of in methylene dichloride, normal heptane, water, the alcohol; Said constant temperature degreasing solvent is selected from a kind of in methylene dichloride, normal heptane, water, the alcohol.
CN 201110194281 2011-07-12 2011-07-12 Preparation method of hollow-structure metal or ceramic part CN102351542B (en)

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