CN102528037A - Sintering mold and manufacturing method thereof - Google Patents

Sintering mold and manufacturing method thereof Download PDF

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Publication number
CN102528037A
CN102528037A CN2011104560189A CN201110456018A CN102528037A CN 102528037 A CN102528037 A CN 102528037A CN 2011104560189 A CN2011104560189 A CN 2011104560189A CN 201110456018 A CN201110456018 A CN 201110456018A CN 102528037 A CN102528037 A CN 102528037A
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Prior art keywords
mold
sintering
thickness
powder
internal
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CN2011104560189A
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Chinese (zh)
Inventor
姚力军
相原俊夫
大岩一彦
潘杰
王学泽
宋佳
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Ningbo Jiangfeng Electronic Material Co Ltd
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Ningbo Jiangfeng Electronic Material Co Ltd
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Priority to CN2011104560189A priority Critical patent/CN102528037A/en
Publication of CN102528037A publication Critical patent/CN102528037A/en
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Abstract

The invention relates to a sintering mold and a manufacturing method thereof. The manufacturing method of the sintering mold comprises the steps of: manufacturing an internal mold of the sintering mold, wherein the internal mold is used for fixing powder to form a sintering shape; manufacturing a carbon/carbon composite material; and manufacturing the external mold of the sintering mold by utilizing the carbon/carbon composite material, wherein the external mold is sleeved outside the internal mold. The technical scheme of the invention reduces the breakage rate of the sintering mold, and also reduces the risk brought to a sintering furnace during the use process.

Description

Sintering mold and manufacturing approach thereof
Technical field
The present invention relates to powder metallurgical technology, particularly a kind of sintering mold and manufacturing approach thereof.
Background technology
The tungsten-titanium alloy target is a kind of more typical alloy target material, and large-scale semiconductive integrated circuit, solar cell etc. all can use the tungsten-titanium alloy target to carry out the PVD plated film, forms the barrier layer.For now, the requirement of the tungsten-titanium alloy target of using for sputter is generally tungsten-titanium alloy target purity >=99.9%, relative density >=99%, and microstructure is even, the flawless defective.In the prior art, adopt powder metallurgical technique to produce tungsten-titanium alloy target base usually, tungsten titanium mixed-powder is packed in the mould, form tungsten-titanium alloy target base through moulding process and sintering process.
The mould that is used for sintering process in the prior art comprises: graphite jig and carbon carbon composite die.
Graphite jig is processed by Delanium usually; Mode according to its moulding can be divided into: isostatic pressing formed graphite, extruded anisotropic graphite, die-pressed graphite, wherein the mould of isostatic pressing formed graphite making is widely used in industries such as powder metallurgy because of its heat-resisting quantity, chemical stability etc.
Carbon carbon composite die is the mould of being processed by carbon carbon composite, and carbon carbon composite is to be that matrix and carbon fiber or graphite fibre (or its fabric) are for strengthening the composite that body is formed with carbon.It is low that carbon carbon compound die has proportion, high strength, and advantage such as high temperature resistant, for graphite jig, it has better serviceability, however the production cycle of carbon carbon composite die is longer for graphite jig, and production cost is high with respect to graphite jig.
When in the existing technology tungsten titanium mixed-powder being carried out sintering, sintering mold comprises internal mold and external mold, and interior external mold all adopts graphite jig.Yet the phenomenon of sintering mold fracture appears in regular meeting in the time of in sintering process, and the fracture of graphite jig belongs to brittle fracture, and the graphite jig of fracture may damage the inwall of sintering furnace suddenly.Therefore,, usually can pass through to increase the thickness of graphite jig in order to prevent the fracture of graphite jig, not easy to operate but the blocked up meeting of graphite jig causes.In addition, also have the interior external mold of proposition all to adopt carbon carbon composite die to make sintering mold, and interior external mold all adopt carbon carbon composite die can cause cost too high.
Therefore, how to produce the sintering mold that cost is low, breakage rate is low and become one of present problem demanding prompt solution.
The correlation technique of relevant sintering mold can also be CN201720429U referring to publication number, and name is called a kind of one Chinese patent application of powder metallurgy brake lining pressure sintering mould.
Summary of the invention
It is low that the problem that the present invention solves provides a kind of cost, the sintering mold that breakage rate is low.
For addressing the above problem, the present invention provides a kind of manufacturing approach of sintering mold, comprising:
Make the internal mold of sintering mold, said internal mold is used for fixing powder and forms sintered shape;
Make carbon carbon composite;
Utilize said carbon carbon composite to make the external mold of sintering mold, said outer die casing is in the said internal mold outside.
Optional, said making carbon carbon composite comprises:
The preparation preform;
Said preform is carried out densification;
Preform to after densified is heat-treated.
Optional, adopt the said internal mold of isostatic pressing formed graphite material.
Optional, said powder is a tungsten titanium mixed-powder, and the thickness of said internal mold is more than or equal to 15mm, and the thickness of said external mold is between 50mm to 150mm, and the height of said external mold is between 300mm to 800mm.
Optional, the manufacturing approach of said sintering mold also comprises: at said internal mold two ends compression leg is set; At least one pad is set between said compression leg.
Optional, the thickness of said pad is between 20mm to 40mm, and the thickness of said compression leg is between 100mm to 200mm.
For addressing the above problem, the present invention also provides a kind of sintering mold, comprising: be used for fixing internal mold and the external mold that is enclosed within the said internal mold outside that powder forms sintered shape, the material of said external mold is a carbon carbon composite.
Optional, said powder is a tungsten titanium mixed-powder, and the thickness of said internal mold is more than or equal to 15mm, and the thickness of said external mold is between 50mm to 150mm, and the height of said external mold is between 300mm to 800mm.
Optional, said sintering mold also comprises: be arranged on the compression leg at said internal mold two ends and be arranged at least one pad between the said compression leg.
Optional, the thickness of said pad is between 20mm to 40mm, and the thickness of said compression leg is between 100mm to 200mm.
Compared with prior art, technical scheme of the present invention has the following advantages:
Through making carbon carbon composite; And with the external mold of said carbon carbon composite as sintering mold; Can be so that in sintering process; Sintering mold has the ability of resisting material deformation preferably and enough anti-pressure abilities, and then has guaranteed that the mouldability of the material through said sintering mold sintering is better.And, adopt the external mold of carbon carbon composite as sintering mold, also reduced the thickness of whole sintering mold, make easy to operate in actual use; Because carbon carbon composite belongs to random graphits structure, therefore, easy fracture not in the use; Reduced the breakage rate of sintering mold, even and fracture, owing to there is fiber to link to each other between the external mold of fracture; Therefore, can not be damaged to the inwall of sintering furnace, and then reduce the risk of bringing to sintering furnace in the use.
Description of drawings
Fig. 1 is the flow chart of manufacturing approach of the sintering mold of embodiment of the present invention;
Fig. 2 be the embodiment of the invention removal the internal structure sketch map of sintering mold of part internal mold and external mold.
The specific embodiment
As described in the background technology; In the prior art; Sintering mold in use the time regular meeting generation of phenomenon of rupture appears; Particularly outstanding for the sintering mold of tungsten ti powder, the breakage rate of sintering mold is higher, and the sintering mold of fracture suddenly very likely can damage the inwall of sintering furnace.
The inventor is through discovering, for tungsten titanium mixed-powder, in order to make the tungsten titanium material of last acquisition more densified; In sintering process, can adopt HTHP usually, yet along with the variation of sintering temperature; Tungsten titanium material self can show series of characteristics such as thermal expansion, contraction, and when the tungsten titanium mixed-powder of the different amounts of packing in the sintering mold, the pressure that sintering mold is born in sintering process also is different; And said pressure can be far longer than forcing press applied pressure in sintering process usually; Therefore, during the tungsten titanium mixed-powder of the different amounts of sintering, the pressure that sintering mold bore is uncertain.And; For the sintering of tungsten titanium mixed-powder; Temperature during its sintering is usually less than the optimum serviceability temperature of graphite jig, so the intensity of graphite jig can not be able to real embodiment in sintering process, owing to above-mentioned 2 reasons; Caused the generation of sintering mold phenomenon of rupture in sintering process, and the sintering mold of fracture may be damaged to the inwall of sintering furnace.
So the inventor proposes; Adopt the external mold of carbon carbon composite, because carbon carbon composite intensity is higher, so can reduce the breakage rate of sintering mold as sintering mold; Even sintering mold fracture; Link to each other owing to have fiber between the carbon carbon composite, therefore, also can not be damaged to the inwall of sintering furnace.Further; The inventor is definite through long-term and unremitting studying assiduously, and the thickness of sintering mold external mold can guarantee that sintering mold is not easy fracture within the specific limits; Satisfy sintering mold anti-pressure ability and resistance to tension in actual use; Reduce the breakage rate of sintering mold, and the thickness of whole sintering mold can reduce handled easily greatly with respect to the thickness that has sintering mold now.
For make above-mentioned purpose of the present invention, feature and advantage can be more obviously understandable, does detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.
Set forth detail in the following description so that make much of the present invention.But the present invention can be different from alternate manner described here and implements with multiple, and those skilled in the art can do similar popularization under the situation of intension of the present invention.Therefore the present invention does not receive the restriction of the following disclosed specific embodiment.
See also Fig. 1, Fig. 1 is the flow chart of manufacturing approach of the sintering mold of embodiment of the present invention; As shown in Figure 1, the manufacturing approach of said sintering mold comprises:
Step S11: make the internal mold of sintering mold, said internal mold is used for fixing powder and forms sintered shape;
Step S12: make carbon carbon composite;
Step S13: utilize said carbon carbon composite to make the external mold of sintering mold, said outer die casing is in the said internal mold outside.
Execution in step S11, in this step, the internal mold of said sintering mold can adopt graphite jig, for example: isostatic pressing formed graphite mould, extruded anisotropic graphite mould, die-pressed graphite mould, preferably, adopt the isostatic pressing formed graphite mould.The shape of said internal mold specifically wants the shape of sinter molding to decide by reality, for example: can be the cuboid of torus, hollow, square etc.
Execution in step S12 makes carbon carbon composite;
In this embodiment, make said carbon carbon composite and comprise: the preparation preform; Said preform is carried out densification; Preform to after densified is heat-treated.
Particularly, before the preparation preform, need select kinds of fibers and molding mode according to the application and the working environment of the carbon carbon composite that is designed.In this embodiment, said carbon carbon composite is mainly used in the external mold of preparation sintering mold, so adopt continuous fiber, the mode of 3 D weaving prepares preform.
Because the preform behind the 3 D weaving has a lot of holes, and density is low, so can not directly use, need carry out densification to it, and carbon is deposited on said preform, fills up its hole, could form the carbon carbon composite of compact structure.
Usually said preform is carried out densification and can adopt liquid impregnation and chemical vapour deposition (CVD) dual mode.In this embodiment, adopt the mode of chemical vapour deposition (CVD) to carry out densified to said preform.
Particularly, said preform is placed the CVD stove, import hydrocarbon gas, flow and the dividing potential drop of controlling furnace temperature, gas simultaneously is with the control reacting gas and generate the diffusion of gas in hole, and then obtains depositing more uniformly.In order to prevent the too early sealing of hole, should make that also reactive deposition speed is lower than diffusion rate.And in order to improve the density of said preform, behind the deposition certain hour, can also carry out machined, remove the outer surface that has sealed, and then deposit, so repeat said preform.
Preform to after densified is heat-treated; Particularly; To placing heating furnace through the preform after densified, furnace temperature is 1650 ℃~2800 ℃ in this embodiment, so that impurity elements such as the N in the carbon carbon composite, H, O are overflowed; The lattice of carbon is changed, with the performance of the carbon carbon composite that improves final acquisition.
Behind step S12 acquisition carbon carbon composite, execution in step S13 obtains the external mold that carbon carbon composite is made sintering mold with step S12; Said external mold is generally the cylinder of hollow; Usually by the shape decision of internal mold, if internal mold is the cuboid of hollow, then said external mold hollow space is a cuboid to the shape of hollow space; If internal mold is a torus, then said external mold hollow space is a cylinder.
In the present embodiment, behind the internal mold of making sintering mold and external mold, also need compression leg be set, at least one pad is set between said compression leg at said internal mold two ends.
Manufacturing approach through above-mentioned sintering mold; The embodiment of the invention provides a kind of sintering mold; See also Fig. 2, Fig. 2 be the embodiment of the invention removal the internal structure sketch map of sintering mold of part internal mold and external mold, as shown in Figure 2: said sintering mold comprises:
Be used for fixing internal mold 1 and the external mold 2 that is enclosed within said internal mold 1 outside that powder forms sintered shape, the material of said external mold 2 is a carbon carbon composite.
As shown in Figure 2; The two ends of said sintering mold are provided with compression leg 3; Be used for compressing in the horizontal mixed-powder to be sintered, in order the agglomerated material sintering to be gone out differing heights, have a pad 4 at least between the said compression leg 3; Between said pad 4 and the said compression leg 3, has material to be sintered 5 between pad 4 and the pad 4.
In the present embodiment,, between then said pad 4 and the said compression leg 3, be tungsten titanium mixed-powder between any two pads 4 so that tungsten titanium mixed-powder is sintered to example.In the present embodiment; Consider that for the sintering mold of tungsten titanium mixed-powder because tungsten titanium mixed-powder is in sintering process, the thermal expansion of himself, shrinkage can apply certain pressure and pulling force to sintering mold; Consider that simultaneously forcing press is to the cost of said sintering mold institute's applied pressure and making sintering mold in the sintering process; So in the present embodiment, the thickness of said internal mold is more than or equal to 15mm, for example: 16mm, 17mm, 18mm, 19mm; The thickness of said external mold is between 50mm to 150mm, for example: 50mm, 60mm, 70mm, 80mm, 90mm, 100mm, 110mm, 120mm, 130mm, 140mm, 150mm.The height of said internal mold and external mold equates, and in actual design process, has certain gradient between said internal mold and the external mold and be complementary.Particularly, the thickness of said internal mold 1 is also inhomogeneous, and the thickness of for example said internal mold 1 one ends 11 is 15mm; The thickness of the other end 12 is 17mm, and likewise, the thickness of said external mold 2 is also inhomogeneous; The thickness of for example said external mold 2 one ends 21 is 52mm, and the thickness of the other end 22 is 50mm.Having certain gradient between said internal mold 1 and the external mold 2 is complementary; Be meant that then an end 11 of said internal mold 1 is if approach a bit; 21 at one end of the said external mold 2 that then is complementary with an end 11 of said internal mold 1 is thicker; Likewise, if the other end of said internal mold 1 12 is thicker, and 22 of the other ends of the said external mold 2 that then is complementary with the other end 12 of said internal mold 1 are a little thin.Normally, the said gradient is between 1 °~5 °.
In addition, in the actual use, the height of said external mold need be considered the shrinkage ratio of material to be sintered; The height of the quantity of the height of sintered products, sintering mold Intermediate gasket and thickness and compression leg and deciding; In the present embodiment, in real process, the sintering of tungsten titanium mixed-powder; The thickness of the pad of its sintering mold is usually between 20mm to 40mm, for example: 20mm, 30mm, 40mm.The thickness of compression leg is usually between 100mm to 200mm, for example: 100mm, 120mm, 140mm, 160mm, 180mm, 200mm.The height of external mold is usually between 300mm to 800mm, for example: 300mm, 400mm, 500mm, 600mm, 700mm, 800mm.
Need to prove, be that the sintering instrument with tungsten titanium mixed-powder is that example has been carried out corresponding explanation in the present embodiment, but the sintering mold in the present embodiment not only is confined to tungsten titanium mixed-powder is carried out sintering.And the manufacturing approach of above-mentioned sintering mold also not only is confined to make the sintering mold of tungsten titanium mixed-powder, so tungsten titanium mixed-powder should be as the qualification to sintering mold of the present invention.
In sum, technical scheme of the present invention has following beneficial effect at least:
Through making carbon carbon composite; And with the external mold of said carbon carbon composite as sintering mold; Can be so that in sintering process; Sintering mold has the ability of resisting material deformation preferably and enough anti-pressure abilities, and then has guaranteed that the mouldability of the material through said sintering mold sintering is better.And, adopt the external mold of carbon carbon composite as sintering mold, also reduced the thickness of whole sintering mold, make easy to operate in actual use; Because carbon carbon composite belongs to random graphits structure, therefore, easy fracture not in the use; Reduced the breakage rate of sintering mold, even and fracture, owing to there is fiber to link to each other between the external mold of fracture; Therefore, can not be damaged to the inwall of sintering furnace, and then reduce the risk of bringing to sintering furnace in the use.
Though the present invention with preferred embodiment openly as above; But it is not to be used for limiting the present invention; Any those skilled in the art are not breaking away from the spirit and scope of the present invention; Can utilize the method and the technology contents of above-mentioned announcement that technical scheme of the present invention is made possible change and modification, therefore, every content that does not break away from technical scheme of the present invention; To any simple modification, equivalent variations and modification that above embodiment did, all belong to the protection domain of technical scheme of the present invention according to technical spirit of the present invention.

Claims (10)

1. the manufacturing approach of a sintering mold is characterized in that, comprising:
Make the internal mold of sintering mold, said internal mold is used for fixing powder and forms sintered shape;
Make carbon carbon composite;
Utilize said carbon carbon composite to make the external mold of sintering mold, said outer die casing is in the said internal mold outside.
2. the manufacturing approach of sintering mold as claimed in claim 1 is characterized in that, said making carbon carbon composite comprises:
The preparation preform;
Said preform is carried out densification;
Preform to after densified is heat-treated.
3. the manufacturing approach of sintering mold as claimed in claim 1 is characterized in that, adopts the said internal mold of isostatic pressing formed graphite material.
4. the manufacturing approach of sintering mold as claimed in claim 1; It is characterized in that said powder is a tungsten titanium mixed-powder, the thickness of said internal mold is more than or equal to 15mm; The thickness of said external mold is between 50mm to 150mm, and the height of said external mold is between 300mm to 800mm.
5. the manufacturing approach of sintering mold as claimed in claim 1 is characterized in that, also comprises: at said internal mold two ends compression leg is set; At least one pad is set between said compression leg.
6. the manufacturing approach of sintering mold as claimed in claim 5 is characterized in that, the thickness of said pad is between 20mm to 40mm, and the thickness of said compression leg is between 100mm to 200mm.
7. a sintering mold is characterized in that, comprising: be used for fixing internal mold and the external mold that is enclosed within the said internal mold outside that powder forms sintered shape, the material of said external mold is a carbon carbon composite.
8. sintering mold as claimed in claim 7 is characterized in that, said powder is a tungsten titanium mixed-powder, and the thickness of said internal mold is more than or equal to 15mm, and the thickness of said external mold is between 50mm to 150mm, and the height of said external mold is between 300mm to 800mm.
9. sintering mold as claimed in claim 7 is characterized in that, also comprises: be arranged on the compression leg at said internal mold two ends and be arranged at least one pad between the said compression leg.
10. sintering mold as claimed in claim 9 is characterized in that, the thickness of said pad is between 20mm to 40mm, and the thickness of said compression leg is between 100mm to 200mm.
CN2011104560189A 2011-12-30 2011-12-30 Sintering mold and manufacturing method thereof Pending CN102528037A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115301949A (en) * 2022-07-05 2022-11-08 华中科技大学 Sintering box and application thereof, and tungsten-copper pseudo-binary alloy powder injection molding method

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0353006A (en) * 1989-07-19 1991-03-07 Mitsubishi Kasei Corp Double hollow cylindrical body
JPH0648831A (en) * 1992-07-30 1994-02-22 Sumitomo Durez Co Ltd Carbon-carbon composite molded body
CN1778490A (en) * 2005-10-13 2006-05-31 福州大学 Bed die of large thermal-pressure mould and its production thereof
CN101530916A (en) * 2009-04-15 2009-09-16 中南大学 Method for controlling the defect of sintering expansion of powder metallurgy material and products thereof and mold
CN101747071A (en) * 2009-12-15 2010-06-23 王占双 Preparation of carbon/carbon mould for hot-pressed sintering furnace
CN102009178A (en) * 2010-11-26 2011-04-13 王东伟 Method for producing large-size metal powder filter tube

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0353006A (en) * 1989-07-19 1991-03-07 Mitsubishi Kasei Corp Double hollow cylindrical body
JPH0648831A (en) * 1992-07-30 1994-02-22 Sumitomo Durez Co Ltd Carbon-carbon composite molded body
CN1778490A (en) * 2005-10-13 2006-05-31 福州大学 Bed die of large thermal-pressure mould and its production thereof
CN101530916A (en) * 2009-04-15 2009-09-16 中南大学 Method for controlling the defect of sintering expansion of powder metallurgy material and products thereof and mold
CN101747071A (en) * 2009-12-15 2010-06-23 王占双 Preparation of carbon/carbon mould for hot-pressed sintering furnace
CN102009178A (en) * 2010-11-26 2011-04-13 王东伟 Method for producing large-size metal powder filter tube

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115301949A (en) * 2022-07-05 2022-11-08 华中科技大学 Sintering box and application thereof, and tungsten-copper pseudo-binary alloy powder injection molding method

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Application publication date: 20120704