CN104174854B - A kind of method preparing miniature tungsten-bast alloy part - Google Patents
A kind of method preparing miniature tungsten-bast alloy part Download PDFInfo
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- CN104174854B CN104174854B CN201410331988.XA CN201410331988A CN104174854B CN 104174854 B CN104174854 B CN 104174854B CN 201410331988 A CN201410331988 A CN 201410331988A CN 104174854 B CN104174854 B CN 104174854B
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Abstract
The present invention relates to the preparation method of a kind of tungsten-bast alloy part.Its mesh is to provide a kind of method preparing miniature tungsten-bast alloy part, adopts and is prone to fill type in this way, and green strength is high, conformality is good, and sintering temperature requires low, and finished product structure is fine and close.The preparation method of the present invention a kind of tungsten-bast alloy part includes feeding, composite deposite, mixing, injection moulding, green compact defat, sintering six steps, wherein the composite deposite step technique effect important to the present invention.
Description
Technical field
The present invention relates to a kind of metal injection molded technology, particularly relate to the preparation method of a kind of tungsten-bast alloy part.
Background technology
Metal injection molded (MIM) is to develop the most rapid new technology in field of powder metallurgy now, is also the new of metal forming
Technique, is referred to as " the 5th generation " metal forming method, in geometrical shape making complexity, uniform texture, high performance near net
Shape parts aspect has the advantage of uniqueness.
Tungsten base high-specific-gravity alloy (such as W-Ni-Fe, W-Ni-Cu etc.) with tungsten as primary raw material have high intensity, high density,
The performance advantage that high red hardness, low-expansion coefficient and splendid resistance to abrasion, corrosion resistance etc. are unique, therefore at the most advanced branches of science
Field, national defense industry and civilian industry have obtained application widely.Also just because of the most excellent performance of tungsten-bast alloy,
It is just considered the preferred raw materials in metal injection molded field.
The current technique using metal injection molded technology that tungsten-bast alloy carries out injecting product is the most similar, Chinese patent
Disclosed in CN103056372A, a kind of tungsten-bast alloy product technics comparing is representative, and the technique that the disclosure patent provides includes:
Get the raw materials ready, mix and join powder, prepare feeding, injection moulding, defat, sintering.Find during using this technique to carry out product
There are two problems: one, use commonsense method to carry out mixing and join powder, the dispersion of each metal dust is the most uneven, thus in order to
Making substrate phase uniform with the dispersed structure of dispersion phase, actual sintered temperature and sintering time all exceed theoretical value；Its two, due to tungsten
The surface characteristic of powder, in the feeding of preparation, metal dust content is less than 50VOI%, thus the mobility of feeding is very strong, solidifying plasticity
Poor, therefore the injection of thin pieces becomes difficulty, and when sintering, amount of contraction is excessive is easily deformed, and size Control becomes difficulty.
Summary of the invention
It is an object of the invention to provide a kind of method preparing miniature tungsten-bast alloy part, adopt and be prone to fill type in this way, raw
Base intensity is high, conformality is good, and sintering temperature requires low, and finished product structure is fine and close.
A kind of method preparing miniature tungsten-bast alloy part of the present invention, comprises the steps:
1) feeding: weigh each metal dust respectively.Wherein, each metal dust is chosen as W, Fe and Ni, and each metal dust
Mass ratio be Ni:Fe=9:1～5:5, W:(Ni+Fe)=90:10～98:2；Or each metal dust be chosen as W,
Cu and Ni, and the mass ratio of each metal dust is Ni:Cu=9:1～5:5, W:(Ni+Cu)=90:10～98:2；
2) composite deposite: in the way of composite deposite, described Fe powder/Cu powder and Ni powder are plated on W powder surface successively；Through compound
The W powder of coating stores for future use；
3) mixing: first binding agent to be added and banbury adds heat fusing, then it is dividedly in some parts the W powder through composite deposite in bonding agent
Form mixed liquor, until through the W powder of the composite deposite percent by volume in mixed liquor be 55%～60%；At 100 DEG C～
At a temperature of 180 DEG C mixing 1～2 hour；
4) injection moulding: install micro injection molding mould injection moulding on injection (mo(u)lding) machine, obtain the miniature tungstenio of required form
Alloy part green compact；
5) green compact defat: use two degreasing process, i.e. solvent degreasing and thermal debinding；First in normal heptane solvent, green compact are carried out
Defat in 1～6 hour；Carrying out thermal debinding again, thermal debinding is carried out under vacuum conditions.
6) sintering: being sintered in vacuum drying oven by the green compact after defat, sintering temperature is 1200 DEG C, and sintering time is 10 points
Clock；So far miniature tungsten-bast alloy part is obtained.
A kind of method preparing miniature tungsten-bast alloy part of the present invention, wherein said binding agent is 30PP-10PE-58PW-2SA.
A kind of method preparing miniature tungsten-bast alloy part of the present invention, injection temperature during wherein said injection moulding be 110 DEG C～
160℃。
A kind of method preparing miniature tungsten-bast alloy part of the present invention have employed compound plating technology and processed each powder, i.e.
Fe powder/copper powder and Ni powder are plated on W powder surface, for existing conventional mixing techniques, each metal dust successively
Uniformity significantly improves.Also this reason it is based on, in follow-up sintering process, it is only necessary to less than existing sintering technology
Temperature can realize green compact and quickly reach sintering densification, and required sintering time is short referring now to existing sintering technology.Additionally adopt
After processing each powder with compound plating technology, the surface characteristic of metal powder granulates is improved, and then binding agent dress
The ability carrying metal dust is increased dramatically, thus the mixing feeding mobility obtained is less, thus more conducively tungsten alloy thin-walled
The injection moulding of part, substantially increases the yield rate of product.
The method of preparing miniature tungsten-bast alloy part a kind of to the present invention with embodiment is described further below in conjunction with the accompanying drawings.
Accompanying drawing explanation
Fig. 1 is the structure figure of the tungsten-bast alloy part using prior art to prepare；
The structure figure of tungsten-bast alloy part prepared by the technology that Fig. 2 provides for using the present invention.
Detailed description of the invention
Embodiment one:
A kind of method preparing miniature tungsten-bast alloy part of the present invention, comprises the steps:
1) feeding: weigh each metal dust respectively.Wherein, each metal powder is chosen as W, Fe and Ni.
2) composite deposite: in the way of composite deposite, described Fe powder and Ni powder are plated on W powder surface successively；Through compound
The W powder of coating stores for future use.
3) mixing: first binding agent 30PP-10PE-58PW-2SA to be added in banbury and add heat fusing, first binding agent is added
Enter and banbury adds heat fusing, then be dividedly in some parts the W powder through composite deposite to bonding agent forming mixed liquor, directly
It is 55% to the percent by volume in mixed liquor of the W powder through composite deposite；At a temperature of 100 DEG C mixing 2
Hour.
4) injection moulding: install micro injection molding mould injection moulding on injection (mo(u)lding) machine, obtain the miniature of required form
Tungsten-bast alloy part green compact, injection temperature during described injection moulding is 110 DEG C.
5) green compact defat: use two degreasing process, i.e. solvent degreasing and thermal debinding；First to green compact in normal heptane solvent
Carry out defat in 1 hour；Carrying out thermal debinding again, thermal debinding is carried out under vacuum conditions.
6) sintering: being sintered in vacuum drying oven by the green compact after defat, sintering temperature is 1200 DEG C, and sintering time is
10 minutes.So far miniature tungsten-bast alloy part is obtained.
Wherein the second step compound plating technology in above-mentioned steps is as follows:
A) in the surface plating iron of W powder.First the mixed liquor of n-dodecane and double octyl methyl tertiary amine is heated to 100 DEG C；
W powder and Fe (CO) is added the most successively in this mixed liquor5Powder；Then mixeding liquid temperature is gradually added
Heat is to 180 DEG C, and persistently this temperature 4 hours.Finally extract W-Fe powder.
B) at W-Fe plated surface Ni.W-Fe powder previous step refined adds the NiCl of 90 DEG C26H2O、N2H4
H2O、NHCl、Na3C6H5O72H2In O mixed liquor, until the PH of mixed liquor is 9.Finally extract W-Fe-Ni
Powder.
In the present embodiment, the composition of binding agent 30PP-10PE-58PW-2SA is: by percentage to the quality, the polypropylene of 30%,
The polyethylene of 10%, the paraffin of 58%, the stearic acid of 2%.Additionally binding agent 30PP30PP-10PE-58PW-2SA can also be by
Other binding agent is replaced, such as: paraffin content is not less than the wax-based binder of 30% by percentage to the quality；Or with quality hundred
Proportion by subtraction meter ring polyacetals content is not less than the non-wax-based binder of 70%.
In order to prepare the finished product under three kinds of different metal powder mixture ratios, the proportioning situation of each metal dust selects as follows:
Proportioning one
Ni:Fe=9:1, W:(Ni+Fe)=90:10；
Proportioning two
Ni:Fe=5:5, W:(Ni+Fe)=98:2；
Proportioning three
Ni:Fe=9:5, W:(Ni+Fe)=95:5；
First with above-mentioned three kinds of metal dust mix proportion schemes, use a kind of method system preparing miniature tungsten-bast alloy part of the present invention
Standby nine miniature tungsten-bast alloy parts.
Furthermore with above-mentioned three kinds of metal dust mix proportion schemes, the existing method preparing miniature tungsten-bast alloy part is used to prepare nine
Individual miniature tungsten-bast alloy part, the so-called existing method preparing miniature tungsten-bast alloy part is exactly with Chinese patent
Preparation method disclosed in CN103056372A.
Carry out yield rate inspection by the ultrasonic nondestructive test equipment part to being prepared by two kinds of methods to find:
9 all qualified products of part prepared in the process of the present invention；
9 the part qualified products prepared in a conventional method have 7, defect ware 2.
Embodiment two
A kind of method preparing miniature tungsten-bast alloy part of the present invention, comprises the steps:
1) feeding: weigh each metal dust respectively.Wherein, each metal powder is chosen as W, Cu and Ni.
2) composite deposite: in the way of composite deposite, described Cu powder and Ni powder are plated on W powder surface successively；Through compound
The W powder of coating stores for future use.
3) mixing: first binding agent 30PP-10PE-58PW-2SA to be added in banbury and adds heat fusing, then be dividedly in some parts through
The W powder of composite deposite is to forming mixed liquor in bonding agent, until through the W powder of the composite deposite body in mixed liquor
Long-pending percentage ratio is 58%；At a temperature of 160 DEG C mixing 1.5 hours.
4) injection moulding: install micro injection molding mould injection moulding on injection (mo(u)lding) machine, obtain the miniature of required form
Tungsten-bast alloy part green compact, injection temperature during described injection moulding is 140 DEG C.
5) green compact defat: use two degreasing process, i.e. solvent degreasing and thermal debinding；First to green compact in normal heptane solvent
Carry out defat in 3 hours；Carrying out thermal debinding again, thermal debinding is carried out under vacuum conditions.
6) sintering: being sintered in vacuum drying oven by the green compact after defat, sintering temperature is 1460 DEG C, and sintering time is
18 minutes.So far miniature tungsten-bast alloy part is obtained.
Wherein the second step compound plating technology in above-mentioned steps is as follows:
A) use the mode of electroless plating at W powder plated surface Cu.By W powder, CuSO4 5H2O2, HCHO, four
Ethyl ammonium chloride mixes at a temperature of 50 DEG C, until solution PH is 13.Then W-Cu powder is extracted.
B) at W-Cu plated surface Ni.The W-Cu powder extracted in previous step is added the NiCl of 90 DEG C26H2O、
N2H4H2O、NHCl、Na3C6H5O72H2In O mixed liquor, until the PH of the mixed liquor of mixed liquor is 9.?
After extract W-Cu-Ni powder.
In the present embodiment, the composition of binding agent 30PP-10PE-58PW-2SA is: by percentage to the quality, the polypropylene of 30%,
The polyethylene of 10%, the paraffin of 58%, the stearic acid of 2%.Additionally binding agent 30PP30PP-10PE-58PW-2SA can also be by
Other binding agent is replaced, such as: paraffin content is not less than the wax-based binder of 30% by percentage to the quality；Or with quality hundred
Proportion by subtraction meter ring polyacetals content is not less than the non-wax-based binder of 70%.
In order to prepare the finished product under three kinds of different metal powder mixture ratios, the proportioning situation of each metal dust selects as follows:
Proportioning one
Ni:Cu=9:1, W:(Ni Cu)=90:10；
Proportioning two
Ni:Cu=5:5, W:(Ni Cu)=98:2；
Proportioning three
Ni:Cu=9:4, W:(Ni Cu)=95:4；
First with above-mentioned three kinds of metal dust mix proportion schemes, use a kind of method system preparing miniature tungsten-bast alloy part of the present invention
Standby nine miniature tungsten-bast alloy parts.
Furthermore with above-mentioned three kinds of metal dust mix proportion schemes, the existing method preparing miniature tungsten-bast alloy part is used to prepare nine
Individual miniature tungsten-bast alloy part, the so-called existing method preparing miniature tungsten-bast alloy part is exactly with Chinese patent
Preparation method disclosed in CN103056372A.
Carry out yield rate inspection by the ultrasonic nondestructive test equipment part to being prepared by two kinds of methods to find:
9 all qualified products of part prepared in the process of the present invention；
9 the part qualified products prepared in a conventional method have 8, defect ware 1.
Embodiment three
A kind of method preparing miniature tungsten-bast alloy part of the present invention, comprises the steps:
1) feeding: weigh each metal dust respectively.Wherein, each metal powder is chosen as W, Cu and Ni.
2) composite deposite: in the way of composite deposite, described Cu powder and Ni powder are plated on W powder surface successively；Through compound
The W powder of coating stores for future use.
3) mixing: first binding agent 30PP-10PE-58PW-2SA to be added in banbury and adds heat fusing, then be dividedly in some parts through
The W powder of composite deposite is to forming mixed liquor in bonding agent, until through the W powder of the composite deposite body in mixed liquor
Long-pending percentage ratio is 60%；At a temperature of 180 DEG C mixing 1 hour.
4) injection moulding: install micro injection molding mould injection moulding on injection (mo(u)lding) machine, obtain the miniature of required form
Tungsten-bast alloy part green compact, injection temperature during described injection moulding is 160 DEG C.
5) green compact defat: use two degreasing process, i.e. solvent degreasing and thermal debinding；First to green compact in normal heptane solvent
Carry out defat in 6 hours；Carrying out thermal debinding again, thermal debinding is carried out under vacuum conditions.
6) sintering: being sintered in vacuum drying oven by the green compact after defat, sintering temperature is 1500 DEG C, and sintering time is
20 minutes.So far miniature tungsten-bast alloy part is obtained.
Wherein the second step compound plating technology in above-mentioned steps is as follows:
A) use the mode of electroless plating at W powder plated surface Cu.By W powder, CuSO4 5H2O2, HCHO, four
Ethyl ammonium chloride mixes at a temperature of 50 DEG C, until solution PH is 13.Then W-Cu powder is extracted.
B) at W-Cu plated surface Ni.The W-Cu powder extracted in previous step is added the NiCl of 90 DEG C26H2O、
N2H4H2O、NHCl、Na3C6H5O72H2In O mixed liquor, until the PH of the mixed liquor of mixed liquor is 9.?
After extract W-Cu-Ni powder.
In the present embodiment, the composition of binding agent 30PP-10PE-58PW-2SA is: by percentage to the quality, the polypropylene of 30%,
The polyethylene of 10%, the paraffin of 58%, the stearic acid of 2%.Additionally binding agent 30PP30PP-10PE-58PW-2SA can also be by
Other binding agent is replaced, such as: paraffin content is not less than the wax-based binder of 30% by percentage to the quality；Or with quality hundred
Proportion by subtraction meter ring polyacetals content is not less than the non-wax-based binder of 70%.
In order to prepare the finished product under three kinds of different metal powder mixture ratios, the proportioning situation of each metal dust selects as follows:
Proportioning one
Ni:Cu=9:1, W:(Ni Cu)=90:10；
Proportioning two
Ni:Cu=5:5, W:(Ni Cu)=98:2；
Proportioning three
Ni:Cu=9:7, W:(Ni Cu)=93:7；
First with above-mentioned three kinds of metal dust mix proportion schemes, use a kind of method system preparing miniature tungsten-bast alloy part of the present invention
Standby nine miniature tungsten-bast alloy parts.
Furthermore with above-mentioned three kinds of metal dust mix proportion schemes, the existing method preparing miniature tungsten-bast alloy part is used to prepare nine
Individual miniature tungsten-bast alloy part, the so-called existing method preparing miniature tungsten-bast alloy part is exactly with Chinese patent
Preparation method disclosed in CN103056372A.
Carry out yield rate inspection by the ultrasonic nondestructive test equipment part to being prepared by two kinds of methods to find:
9 all qualified products of part prepared in the process of the present invention；
9 the part qualified products prepared in a conventional method have 7, defect ware 2.
The miniature tungsten-bast alloy part that an application present invention makes is randomly drawed from embodiment one, embodiment two and embodiment three kinds
Structure inspection is made with a miniature tungsten-bast alloy part applying existing technique to prepare.The structure checked such as Fig. 1,
Shown in Fig. 2.As can be seen from Figure 1 the miniature tungsten-bast alloy part composition dispersion applying existing technique to prepare is uneven, from figure
Can be seen that in 2 that the miniature tungsten-bast alloy part composition dispersion that the application present invention makes is more uniform.Thus the method that the present invention provides
It is more conducive to the production of miniature tungsten-bast alloy part
Integrated embodiment one, embodiment two and embodiment three can be seen that and use that the present invention is a kind of prepares miniature tungsten-bast alloy part
The tungsten-bast alloy finished part rate that method prepares is higher, has good application prospect.
Embodiment described above is only to be described the preferred embodiment of the present invention, not carries out the scope of the present invention
Limiting, on the premise of designing spirit without departing from the present invention, technical scheme is made by those of ordinary skill in the art
Various deformation and improvement, all should fall in the protection domain that claims of the present invention determines.
Claims (3)
1. the method preparing miniature tungsten-bast alloy part, comprises the steps:
1) feeding: weighing each metal dust respectively, wherein, each metal dust is chosen as W, Fe and Ni, and the mass ratio of each metal dust is Ni:Fe=9:1～5:5, W:(Ni+Fe)=90:10～98:2；Or each metal dust is chosen as W, Cu and Ni, and the mass ratio of each metal dust is Ni:Cu=9:1～5:5, W:(Ni+Cu)=90:10～98:2；
2) composite deposite: in the way of composite deposite, described Fe powder/Cu powder and Ni powder are plated on W powder surface successively；Store for future use through the W powder of composite deposite；
3) mixing: first binding agent to be added and banbury adds heat fusing, then be dividedly in some parts the W powder through composite deposite to binding agent is formed mixed liquor, until through the W powder of the composite deposite percent by volume in mixed liquor be 55%～60%；At a temperature of 100 DEG C～180 DEG C mixing 1～2 hour；
4) injection moulding: install micro injection molding mould injection moulding on injection (mo(u)lding) machine, obtain the miniature tungsten-bast alloy part green compact of required form；
5) green compact defat: use two step degreasing process, i.e. solvent degreasing and thermal debinding；First green compact are carried out defat in 1～6 hour in normal heptane solvent；Carrying out thermal debinding again, thermal debinding is carried out under vacuum conditions；
6) sintering: being sintered in vacuum drying oven by the green compact after defat, sintering temperature is 1200 DEG C, and sintering time is 10 minutes；So far miniature tungsten-bast alloy part is obtained.
A kind of method preparing miniature tungsten-bast alloy part the most according to claim 1, it is characterised in that: described binding agent is 30PP-10PE-58PW-2SA.
A kind of method preparing miniature tungsten-bast alloy part the most according to claim 1, it is characterised in that: injection temperature during described injection moulding is 110 DEG C～160 DEG C.
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| CN105154700A (en) * | 2015-09-24 | 2015-12-16 | 瑞声精密制造科技(常州)有限公司 | Heavy-density tungsten alloy |
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| CN110172598A (en) * | 2018-12-13 | 2019-08-27 | 苏州赛特锐精密机械配件有限公司 | A kind of method of co-injection preparation bi-component tungsten-copper alloy |
| CN110527886A (en) * | 2019-09-02 | 2019-12-03 | 广州市华司特合金制品有限公司 | A kind of clock and watch are again vertical and preparation method thereof |
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