CN102747242A - Method for preparing large-size hard alloy - Google Patents
Method for preparing large-size hard alloy Download PDFInfo
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- CN102747242A CN102747242A CN2012102610224A CN201210261022A CN102747242A CN 102747242 A CN102747242 A CN 102747242A CN 2012102610224 A CN2012102610224 A CN 2012102610224A CN 201210261022 A CN201210261022 A CN 201210261022A CN 102747242 A CN102747242 A CN 102747242A
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Abstract
The invention provides a method for preparing large-size hard alloy, which comprises the following steps of: (S1) preparing several segments of small-size hard alloy blanks by using a compression molding method; (S2) performing first vacuum sintering on each hard alloy blank to obtain a semi-finished hard alloy product; (S3) flat grinding the end face of each semi-finished hard alloy product, and successively butting the end faces; and (S4) performing second vacuum sintering on the several segments of entire butted semi-finished hard alloy products to obtain the finished large-size hard alloy product, wherein the highest temperature of second vacuum sintering is 1400-1420 DEG C, the heating speed in the second vacuum sintering process is 3-7 DEG C/min, and the temperature is maintained for 45-80 min after a liquid phase occurs during the second vacuum sintering process. The invention overcomes the limitation that the large-size hard alloy product can only be produced by isostatic pressing in the prior art. Compared with the isostatic pressing production method, the method provided by the invention has greatly reduced cost and greatly shortened production period, and the grinding amount of the product is small.
Description
Technical field
The present invention relates to the wimet preparation field, be specifically related to a kind of preparation method of large size wimet.
Background technology
At present, for the hart metal product that length is big, volume is bigger, the consistent method that adopts is that isostatic pressing production, vacuum sintering obtain both at home and abroad.When isostatic pressing was produced, have following shortcoming: 1, the product mold fabrication cycle was longer, and a cover isostatic tooling needs 15 to 20 days from being fabricated into trial production; 2, mould costs an arm and a leg, and the price of a cover isostatic tooling is generally more than 6000 yuan; 3, life cycle of the product is long.Therefore, isostatic pressing method of the prior art is general only is applied when typical products in mass production is produced.
And to the less large size hart metal product of quantity on order, valve series hard alloy product for example, if adopt isostatic pressing production, then cost is higher and the delivery cycle is longer, can not meet customer need.For example length is processed from the Mold Making to the finished product greater than the valve series hard alloy product of 150mm, need could to deliver goods more than 35 days, and its stock removal is more than 50% during employing isostatic pressing method, and Mold Making expense in addition is higher, causes production cost high.
Common press moulding mode then is difficult to produce larger-size hart metal product, mainly has a following difficult problem: (one) press stroke and pressure are not enough; (2) because product length is bigger, each several part density difference is very big during compacting, and great distortion is arranged during the product sintering; (3) because product length is bigger, product forms liquid phase during vacuum sintering, can cause product flexural deformation, even through reprocessing the product that also is difficult to guarantee to obtain the desired shape size.
Summary of the invention
The cost that isostatic pressing production large size hart metal product exists in the prior art is high, life cycle of the product is long and can not guarantee the shape of product size in order to solve in the present invention; And common press moulding mode can not prepare the technical problem of large size hart metal product, the invention provides that a kind of low production cost, production cycle significantly shorten, the preparation method of the simple large size wimet of technology.
Technical scheme of the present invention is:
A kind of preparation method of large size wimet may further comprise the steps:
S1, elder generation adopt compression-moulding methods to prepare the undersized wimet blank of plurality of sections;
S2, each wimet blank is carried out a vacuum sintering, obtain plurality of sections wimet work in-process respectively;
S3, the half-finished end face of each section wimet is carried out plain grinding, then the end face of each section wimet work in-process through plain grinding docked successively, make during butt joint that two neighboring sections wimet work in-process are set level fully, seamless contact between adjacent two end faces;
S4, the plurality of sections wimet work in-process integral body after will docking are carried out the secondary vacuum sintering, obtain the large size hard alloy finished product; Wherein, secondary vacuum agglomerating top temperature is 1400-1420 ℃, and the temperature rise rate in the secondary vacuum sintering process is 3-7 ℃/min, occurs in the secondary vacuum sintering process being incubated 45-80min after the liquid phase.
The preparation method of large size wimet provided by the invention; Earlier prepare plurality of sections small size wimet work in-process through common compression molding; Then it is docked successively, when the secondary vacuum sintering, still can bond to mutually together between the work in-process, through the concrete sintering condition of secondary vacuum agglomerating (comprising sintering temperature, temperature rise rate and soaking time) is suitably selected through bonding; Guarantee the half-finished bonding surface of two neighboring sections wimet behind the secondary vacuum sintering on the crystalline phase microstructure with normal crystalline phase microstructure basically identical; Thereby obtain large-sized hard alloy finished product, overcome the restriction that large size hart metal product in the prior art can only be produced through isostatic pressing, and with respect to the isostatic pressing working method; Method production cost provided by the invention reduces greatly; Production cycle shortens greatly, and the product stock removal is little, practices thrift man-hour and raw material.
Embodiment
The invention provides a kind of preparation method of large size wimet, may further comprise the steps:
S1, elder generation adopt compression-moulding methods to prepare the undersized wimet blank of plurality of sections;
S2, each wimet blank is carried out a vacuum sintering, obtain plurality of sections wimet work in-process respectively;
S3, the half-finished end face of each section wimet is carried out plain grinding, then the end face of each section wimet work in-process through plain grinding docked successively, make during butt joint that two neighboring sections wimet work in-process are set level fully, seamless contact between adjacent two end faces;
S4, the plurality of sections wimet work in-process integral body after will docking are carried out the secondary vacuum sintering, obtain the large size hard alloy finished product; Wherein, secondary vacuum agglomerating top temperature is 1400-1420 ℃, and the temperature rise rate in the secondary vacuum sintering process is 3-7 ℃/min, occurs in the secondary vacuum sintering process being incubated 45-80min after the liquid phase.
The preparation method of large size wimet provided by the invention; Earlier prepare plurality of sections small size wimet work in-process through common compression molding; Then it is docked successively, when the secondary vacuum sintering, still can bond to mutually together between the work in-process, through the concrete sintering condition of secondary vacuum agglomerating (comprising sintering temperature, temperature rise rate and soaking time) is suitably selected through bonding; Guarantee at the half-finished bonding surface of two neighboring sections wimet behind the secondary vacuum sintering consistent with normal crystalline phase microstructure on the crystalline phase microstructure; Thereby obtain large-sized hard alloy finished product, overcome the restriction that large size hart metal product in the prior art can only be produced through isostatic pressing, and with respect to the isostatic pressing working method; Method production cost provided by the invention reduces greatly; Production cycle shortens greatly, and the product stock removal is little, practices thrift man-hour and raw material.
Among the present invention, among the step S1, when compression molding prepared the wimet blank, compacting height should be controlled well, suppress the highly too high distortion that then is easy to generate, and suppressed highly too shortly to make that then whole prod institute segments is too many, brought difficulty to the secondary vacuum sintering.Among the present invention, the principle that compacting is highly confirmed is: when guaranteeing pressed compact, do not produce under the prerequisite of distortion through vacuum sintering for the first time, and high more good more.Contriver of the present invention finds through a large amount of experiments: the compacting height of wimet blank and the ratio of external diameter be greater than 2 o'clock, easy deformation during the product sintering; Therefore, among the present invention, ratio≤2 of the compacting of wimet blank height and external diameter.In addition, different according to the cobalt contents of the wall thickness of product and used material, compacting highly also can be carried out accommodation, and the present invention does not have particular determination.
Among the present invention, compression molding prepares the quantity of undersized wimet blank and can suitably select according to the concrete size of the required large size hart metal product of reality.For example, when the final height dimension of hard alloy finished product be 240mm, when external diameter is 50mm, can be first three sections wimet blanks that height is 80-82mm of compression molding preparation, but be not limited to this.
Among the present invention, compression molding prepares undersized wimet blank and the wimet blank is carried out the ordinary method of the method for a vacuum sintering for those skilled in the art, and the present invention does not have special stipulation.The condition that is compression molding and a vacuum sintering gets final product in the normal ranges of this area, specifically can suitably select according to the concrete composition of the wimet of being selected for use.Under the preferable case; Among the step S2, the top temperature of a vacuum sintering is 1350-1410 ℃, and the temperature rise rate in the once sintered process is 3-7 ℃/min; 320-540 ℃ of time insulation 150-250min in the vacuum sintering process, insulation 60-90 min in the time of 1350-1410 ℃.Among the step S2, after the vacuum sintering, the wimet work in-process that obtain have enough process redundancy, can obtain the product of client's desired shape size behind the assurance completion secondary vacuum sintering through following process.
Among the present invention, thereby be can complete matching realization slitless connection when guaranteeing follow-up butt joint to the purpose that the half-finished end face of each section wimet carries out plain grinding.Under the preferable case, the half-finished end face of each section wimet carried out plain grinding after, roughness is 0.8-6.4.Roughness＜0.8 o'clock, product butt joint back is easy to generate relative slippage because frictional force is too for a short time, thereby makes product can not meet the demands through concentricity behind the double sintering; Thick original text degree＞6.4 o'clock can not guarantee the work in-process slitless connection.Two sections wimet work in-process that are in end positions during butt joint when butt joint only one of them end face be used for contacting with adjacent wimet work in-process; Therefore as a kind of preferred implementation of the present invention; Among the step S3; Two sections wimet work in-process that lay respectively at end positions during butt joint only need a plain grinding one of which end face when plain grinding, and all need handle two end faces during all the other wimet work in-process plain grindings.
As a kind of preferred implementation of the present invention; Among the step S3; Can between two adjacent contact end faces, fill certain quantity of additive during the product butt joint; This additive can be a cobalt powder, also can be cobalt powder, nickel powder with the mixed uniformly mixture of certain proportioning, or other single kinds or the mixture of multiple matrix metal powder.When product being carried out second time vacuum sintering; After temperature reaches 1300 ℃; Said additive slowly forms liquid phase, and under gravity and capillary force, a part of liquid phase penetrates in the adjacent two-section product; Thereby make the more piece product to connect more closely, reach with isostatic pressing production, normal sintering after homomorphosis, large-sized hard alloy finished product of the basic indifference of performance.
As previously mentioned, contriver of the present invention finds through a large amount of experiments, among the present invention; After the butt joint of sectional wimet work in-process; Can be through control secondary vacuum agglomerating condition, guarantee the half-finished bonding surface of two neighboring sections wimet behind the secondary vacuum sintering on the crystalline phase microstructure with normal crystalline phase microstructure basically identical, thereby make between the adjacent wimet work in-process; Because the liquid phase influence that gravity, bonding form mutually can make bonding surface be firmly bonded to together.
Among the present invention,, can realize seamless contact during for the butt joint of assurance wimet, be required to be concentric butt joint when each section wimet work in-process dock among the step S3 if said wimet work in-process are cylindrical or the center has the cylindrical of through hole.For example, when said wimet was used for the valve series products, it had the cylindrical of through hole through the blank center of being that compression molding prepares.
Under the preferable case; When carrying out second time vacuum sintering; Can place ovality in the central position in the central through hole of product less than 0.2 graphite core; And antiseized boat coating and drying in the shade naturally when this graphite core periphery need be coated with one or more layers sintering, the external diameter of the graphite core after drying in the shade should equate with the endoporus of required alloy finished product, the alloy work in-process after highly will a little higher than butt joint.Produce after the vacuum sintering for the second time of product process and shrink, can tightly bind round on graphite core.Because the ovality of graphite core, makes that the product endoporus ellipse that tightly binds round on graphite core also can be less less than 0.2 (promptly not having ellipse basically).Therefore, place the situation that occurs ovalizing deflection when graphite core can effectively be avoided the product sintering.
Preparation in accordance with the present invention, the secondary vacuum sintering also can be proceeded ground finish to sintered products as required, thereby be met the elaboration of customer requirement after accomplishing.For example, the performance requriements of valve series hard alloy is not high, and being mainly wear-resisting, corrosion-resistant, high pressure resistant, general wimet can reach; Even through the secondary vacuum sintering, still guarantee to reach the performance of products requirement.Promptly adopt preparation method provided by the invention, can be applicable to the production of valve hart metal product.
With respect to the isostatic pressing working method, preparation method provided by the invention has the following advantages: 1, die cost is practiced thrift 100-200% on year-on-year basis, has cut down die cost greatly; 2, the product stock removal is below 15%, and the utmost point has reduced production cost effectively; 3, from the die sinking to delivery, only need about 17 days, the life cycle of the product that reduces by more than half.
Clearer for technical problem, technical scheme and beneficial effect that the present invention is solved, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Embodiment 1
Producing highly is 240mm, and external diameter is 50mm, and endoporus is the hard alloy finished product nozzle S1 of 30mm.By 3 sections compactings of wimet ordinary production process stempressing moulding preparation highly is that 100.5mm, pressed compact external diameter are that 62.5mm, pressed compact endoporus are the cylindrical wimet blank that the center of 37.5mm has through hole; Then respectively in vacuum sintering furnace top temperature be to carry out a vacuum sintering under 1370 ℃, its temperature rise rate is 3 ℃/min, insulation 150min in the time of 320-540 ℃, insulation 60min in the time of 1350-1370 ℃, the wimet work in-process that to obtain 3 sections height be 81mm.Then will be wherein the end face plain grinding of 2 sections wimet work in-process I, III, two end faces of other 1 section wimet work in-process II all carry out plain grinding, to the end face roughness be 3.2; According to the order of I, II, III three sections wimet work in-process are alignd, make the seamless contact of end face behind the plain grinding with one heart then; The pure cobalt powder of interpolation one deck between two contact surfaces, and integral body is respectively put into vacuum sintering furnace, and top temperature is to carry out the secondary vacuum sintering under 1400 ℃; Its temperature rise rate is 4 ℃/min; Occur being incubated 45min after the liquid phase, the cooling back through ground finish, obtains highly being the hard alloy finished product nozzle S1 of 240mm according to necessary requirement.
Embodiment 2
Producing highly is 180mm, and external diameter is 65mm, and endoporus is the hard alloy finished product nozzle S2 of 30mm
By 2 sections compactings of wimet ordinary production process stempressing moulding preparation highly is that 113mm, pressed compact external diameter are that 81.25mm, pressed compact endoporus are the cylindrical wimet blank that the center of 37.5mm has through hole; Then respectively in vacuum sintering furnace top temperature be to carry out a vacuum sintering under 1410 ℃; Its temperature rise rate is 5 ℃/min; Insulation 250min in the time of 320-540 ℃, insulation 90min in the time of 1350-1410 ℃, the wimet work in-process that to obtain 2 sections height be 91mm.An end face with 2 sections wimet work in-process I, II carries out plain grinding then, to the end face roughness be 4.0, then these two sections wimet I, II work in-process are alignd, make the seamless contact of end face behind the plain grinding with one heart; Between two contact surfaces, add one deck additive, the composition of additive is the cobalt powder of 70wt% and the nickel powder of 30wt%, and places the graphite core that scribbles 2 coatings in the work in-process central position; The graphite core external diameter is 29mm; Be 230mm highly, integral body is put into vacuum sintering furnace, top temperature is to carry out the secondary vacuum sintering under 1420 ℃; Its temperature rise rate is 7 ℃/min; Occur being incubated 60min after the liquid phase, the cooling back through ground finish, obtains highly being the hard alloy finished product nozzle S2 of 180mm according to necessary requirement.
Embodiment 3
Producing highly is 270mm, and external diameter is 35mm, and endoporus is the hard alloy finished product nozzle S3 of 20mm.By 4 sections compactings of wimet ordinary production process stempressing moulding preparation highly is that 85mm, pressed compact external diameter are that 43.75mm, pressed compact endoporus are the cylindrical wimet blank that the center of 25mm has through hole; Then respectively in vacuum sintering furnace top temperature be to carry out a vacuum sintering under 1380 ℃; Its temperature rise rate is 6 ℃/min; Insulation 180min in the time of 320-540 ℃, insulation 75min in the time of 1350-1380 ℃, the wimet work in-process that to obtain 4 sections height be 68.5mm.Then will be wherein the end face plain grinding of 2 sections wimet work in-process I, IV; Two end faces of other 2 sections wimet work in-process II, III all carry out plain grinding, to the end face roughness be 1.6, according to the order of I, II, III, IV four sections wimet work in-process are alignd, make the seamless contact of end face behind the plain grinding with one heart then; Between three contact surfaces, add one deck additive respectively; The composition of additive is the cobalt powder of 80wt% and the nickel powder of 20wt%, and integral body puts into vacuum sintering furnace, and top temperature is to carry out the secondary vacuum sintering under 1415 ℃; Its temperature rise rate is 7 ℃/min; Occur being incubated 50min after the liquid phase, the cooling back through ground finish, obtains highly being the hard alloy finished product nozzle S3 of 270mm according to necessary requirement.
Embodiment 4
Producing highly is 150mm, and external diameter is 70mm, and endoporus is the hard alloy finished product valve series products S4 of 40mm.By 2 sections compactings of wimet ordinary production process stempressing moulding preparation highly is that 96mm, pressed compact external diameter are that 89mm, pressed compact endoporus are the cylindrical wimet blank that the center of 49mm has through hole; Then respectively in vacuum sintering furnace top temperature be to carry out a vacuum sintering under 1380 ℃, its temperature rise rate is 4 ℃/min, in the time of 320-540 ℃ the insulation 120min; Insulation 75min in the time of 1350-1380 ℃, the wimet work in-process that to obtain 2 sections height be 76mm, an end face with 2 sections wimet work in-process I, II carries out plain grinding then; To the end face roughness be 6.4, then these two sections wimet I, II work in-process are alignd, make the seamless contact of end face behind the plain grinding with one heart, and place the graphite core scribble 2 coatings in the work in-process central position; The graphite core external diameter is 39mm; Be 200mm highly, integral body is put into vacuum sintering furnace, top temperature is to carry out the secondary vacuum sintering under 1200 ℃; Its temperature rise rate is 5 ℃/min; Occur being incubated 60min after the liquid phase, the cooling back through ground finish, obtains highly being the hard alloy finished product valve series products S4 of 150mm according to necessary requirement.
Comparative Examples 1
Adopt the isostatic pressing method to produce 240mm, external diameter is 50mm, and endoporus is the cylindrical hard alloy finished product DS1 that the center of 30mm has through hole.
Performance test
1, the life cycle of the product in record embodiment 1-4 and the Comparative Examples 1.
2, the products production cost in record embodiment 1-4 and the Comparative Examples 1.
3, estimate each hard alloy finished product S1-S3 and DS1 and whether occur bending and deformation, be not designated as OK if having, otherwise be designated as NG.
4, test the work-ing life of each hard alloy finished product S1-S3 and DS1, reach 10,000 hours and be designated as OK, otherwise be designated as NG.
Test result is as shown in table 1.
Table 1
| Product | Production cycle (my god) | Production cost (unit) | Product distortion situation | Work-ing life |
| S1 | 17 | 7500 | OK | OK |
| S2 | 16 | 6800 | OK | OK |
| S3 | 17 | 8400 | OK | OK |
| S4 | 18 | 8300 | OK | OK |
| DS1 | 35 | 15000 | OK | OK |
Can find out from the test result of last table 1; The large size hart metal product S1-S4 that adopts preparation method provided by the invention to obtain; The product DS1 that obtains with isostatic pressing generation method has identical form, and can both reach work-ing life more than 10,000 hours, can satisfy customer requirement; But preparation method provided by the invention shortens the production cycle greatly, and cost reduces greatly.
Above embodiment is merely preferred implementation of the present invention, should be pointed out that to those skilled in the art, and under the prerequisite that does not break away from the principle of the invention, some improvement of having done also should be regarded as protection scope of the present invention.
Claims (9)
1. the preparation method of a large size wimet is characterized in that, may further comprise the steps:
S1, elder generation adopt compression-moulding methods to prepare the undersized wimet blank of plurality of sections;
S2, each wimet blank is carried out a vacuum sintering, obtain plurality of sections wimet work in-process respectively;
S3, the half-finished end face of each section wimet is carried out plain grinding, then the end face of each section wimet work in-process through plain grinding docked successively, make seamless contact between two neighboring sections wimet work in-process complete matching, adjacent two end faces during butt joint;
S4, the plurality of sections wimet work in-process integral body after will docking are carried out the secondary vacuum sintering, obtain the large size hard alloy finished product; Wherein, secondary vacuum agglomerating top temperature is 1400-1420 ℃, and the temperature rise rate in the secondary vacuum sintering process is 3-7 ℃/min, occurs in the secondary vacuum sintering process being incubated 45-80min after the liquid phase.
2. preparation method according to claim 1 is characterized in that, among the step S1, and ratio≤2 of the compacting of the wimet blank that compression molding prepares height and external diameter.
3. preparation method according to claim 1; It is characterized in that; Among the step S2, the top temperature of a vacuum sintering is 1350-1410 ℃, and the temperature rise rate in the once sintered process is 3-7 ℃/min; 320-540 ℃ of time insulation 150-250min in the vacuum sintering process, insulation 60-90 min in the time of 1350-1410 ℃.
4. preparation method according to claim 1; It is characterized in that; Among the step S3, two sections wimet work in-process that lay respectively at end positions during butt joint only need a plain grinding one of which end face when plain grinding, all need two end faces of plain grinding during all the other wimet work in-process plain grindings.
5. according to claim 1 or 4 described preparing methods, it is characterized in that among the step S3, the roughness behind the plain grinding is 0.8-6.4.
6. according to claim 1 or 4 described preparing methods, it is characterized in that, among the step S3, also be included in the step that applies additive on two adjacent contact end faces before the butt joint; Said additive is selected from the mixture of cobalt powder or cobalt powder and nickel powder.
7. according to claim 1 or 4 described preparing methods, it is characterized in that said wimet work in-process are that the center has the cylindrical of through hole, is butt joint with one heart when each section wimet work in-process dock among the step S3.
8. preparation method according to claim 7 is characterized in that, also is included in central position in the plurality of sections wimet work in-process central through hole after the butt joint and places the step of ovality less than 0.2 graphite core; The periphery of said graphite core is coated with antiseized boat coating.
9. according to claim 1 or 4 described preparing methods, it is characterized in that, also comprise the step of after the secondary vacuum sintering is accomplished sintered products being carried out ground finish.
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| CN103990907A (en) * | 2014-04-14 | 2014-08-20 | 河源普益硬质合金厂有限公司 | High-temperature vacuum hard alloy welding method |
| CN104439254A (en) * | 2014-10-31 | 2015-03-25 | 浙江恒成硬质合金有限公司 | Large scale hard alloy butting joint process |
| CN105170975A (en) * | 2015-09-29 | 2015-12-23 | 浙江恒成硬质合金有限公司 | Butt joint method for long powder metallurgy compressed billets |
| CN106180705A (en) * | 2016-07-08 | 2016-12-07 | 中铝广西有色金源稀土有限公司 | A kind of method for preparing powder metallurgy |
| CN106222475A (en) * | 2016-08-29 | 2016-12-14 | 河源富马硬质合金股份有限公司 | A kind of preparation method of Large scale alloy |
| CN108326291A (en) * | 2018-04-27 | 2018-07-27 | 西南应用磁学研究所 | A kind of preparation method of large scale material |
| CN109079146A (en) * | 2018-08-29 | 2018-12-25 | 株洲硬质合金集团有限公司 | A kind of preparation method of hard alloy long cylinder |
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| CN106222475A (en) * | 2016-08-29 | 2016-12-14 | 河源富马硬质合金股份有限公司 | A kind of preparation method of Large scale alloy |
| CN106222475B (en) * | 2016-08-29 | 2017-12-29 | 河源富马硬质合金股份有限公司 | A kind of preparation method of Large scale alloy |
| CN108326291A (en) * | 2018-04-27 | 2018-07-27 | 西南应用磁学研究所 | A kind of preparation method of large scale material |
| CN109079146A (en) * | 2018-08-29 | 2018-12-25 | 株洲硬质合金集团有限公司 | A kind of preparation method of hard alloy long cylinder |
| CN109692962A (en) * | 2018-12-29 | 2019-04-30 | 武汉新锐合金工具有限公司 | A kind of hard alloy thin-wall part production technology |
| CN111215631A (en) * | 2020-03-16 | 2020-06-02 | 济南市冶金科学研究所有限责任公司 | Tungsten-cobalt hard alloy product thermal connection method |
| CN114029491A (en) * | 2021-10-22 | 2022-02-11 | 浙江恒成硬质合金有限公司 | Method for repairing inner hole of hard alloy blank |
| CN115837465A (en) * | 2022-12-13 | 2023-03-24 | 长沙华信合金机电有限公司 | Method for eliminating stress of sintered hard alloy |
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