CN1256458C - A method for preparing powder tool steel by vacuum hot pressing - Google Patents
A method for preparing powder tool steel by vacuum hot pressing Download PDFInfo
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- CN1256458C CN1256458C CN 200410021159 CN200410021159A CN1256458C CN 1256458 C CN1256458 C CN 1256458C CN 200410021159 CN200410021159 CN 200410021159 CN 200410021159 A CN200410021159 A CN 200410021159A CN 1256458 C CN1256458 C CN 1256458C
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- 239000000843 powder Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229910001315 Tool steel Inorganic materials 0.000 title claims abstract description 26
- 238000007731 hot pressing Methods 0.000 title claims abstract description 25
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 8
- 239000010439 graphite Substances 0.000 claims abstract description 8
- 229910000997 High-speed steel Inorganic materials 0.000 claims description 17
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 229910000822 Cold-work tool steel Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims 4
- 229910000831 Steel Inorganic materials 0.000 claims 3
- 239000010959 steel Substances 0.000 claims 3
- 238000009413 insulation Methods 0.000 claims 1
- 238000005204 segregation Methods 0.000 abstract description 15
- 239000002245 particle Substances 0.000 abstract description 14
- 238000000280 densification Methods 0.000 abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 238000004663 powder metallurgy Methods 0.000 abstract description 3
- 150000001247 metal acetylides Chemical class 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 229910000725 T1 high speed steel Inorganic materials 0.000 description 2
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009966 trimming Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
本发明涉及用于粉末冶金制备工具钢领域,具体为一种用真空热压法制备粉末工具钢的方法,以得到全致密无碳化物偏析的粉末工具钢。将雾化合金粉末置于石墨模具中,放入真空热压室,在真空度为8×10-1~8×10-3Pa下加热至固相线温度以下5~40℃时保温,然后加压1~10MPa,当应变速率达1×10-3/min以下时停止加压。在上述温度下塑性变形抗力已明显降低,因而采用较低压力即可实现致密化,得到相对密度99.8%以上的工件,其中无碳化物偏析,碳化物粒度3~7μm,氧含量小于100ppm。本发明解决了碳化物偏析和结构不致密等问题,可用于制备全致密、无碳化物偏析的粉末工具钢。The invention relates to the field of preparing tool steel by powder metallurgy, in particular to a method for preparing powder tool steel by vacuum hot pressing to obtain fully dense powder tool steel without carbide segregation. Put the atomized alloy powder in a graphite mold, put it into a vacuum hot-press chamber, heat it at a vacuum degree of 8×10 -1 ~ 8×10 -3 Pa to a temperature below the solidus line of 5 ~ 40°C, and then keep it warm. Pressurize at 1-10 MPa, and stop pressurizing when the strain rate reaches below 1×10 -3 /min. At the above temperature, the plastic deformation resistance has been significantly reduced, so lower pressure can be used to achieve densification, and a workpiece with a relative density of more than 99.8% can be obtained, in which there is no carbide segregation, the carbide particle size is 3-7μm, and the oxygen content is less than 100ppm. The invention solves the problems of carbide segregation and non-dense structure, etc., and can be used to prepare fully dense powder tool steel without carbide segregation.
Description
技术领域technical field
本发明涉及用于制备粉末冶金工具钢领域,具体为一种用真空热压法制备粉末工具钢的方法。The invention relates to the field of preparing powder metallurgy tool steel, in particular to a method for preparing powder tool steel by vacuum hot pressing.
背景技术Background technique
工具钢是最重要的工具材料之一,它可以制成各种复杂形状的刀具和模具,如铣刀、滚齿刀、剃齿刀、拉刀、纵剪刀、切边模、压模和挤压模等,用于各种形式的机械加工过程,工具钢中含有大量的合金元素,以保证其红硬性,但同时带来碳化物偏析问题,采用粉末冶金法则可从根本克服偏析缺陷,使其机械性能和使用寿命得以提高。Tool steel is one of the most important tool materials. It can be made into various complex shapes of knives and molds, such as milling cutters, gear hobbing cutters, gear shaving cutters, broaching knives, slitting cutters, trimming dies, compression dies and extrusion dies. Compression dies, etc., are used in various forms of mechanical processing. Tool steel contains a large amount of alloying elements to ensure its red hardness, but at the same time it brings the problem of carbide segregation. The use of powder metallurgy can fundamentally overcome the segregation defect, so that Its mechanical properties and service life are improved.
目前采用热等静压工艺是在高温(≥1100℃)和高压(100~150MPa)下使金属粉末制品成型及致密化,其密度接近理论密度,再热变形,使工具钢性能大幅度上升,但该方法所用冷、热等静压设备十分昂贵、制造成本甚高。在文献P.Hellman,et al.,Metal Powder Report,32:79-83,1977;35:254-256,1980;,47:25-29,1992和G.Hoyle的书′Highspeed steels′,1988,London,Butterworths中均有此法介绍。另外,采用超固相液相烧结法制备粉末工具钢,但烧结窗口较窄,即温度波动必须很小,因而工艺难于稳定,烧结后会形成网状碳化物,文献C.S.Wright et al.,PowderMetall.,36:213-,1993;38:221-,1995对此有详细说明。At present, the hot isostatic pressing process is used to form and densify metal powder products at high temperature (≥1100°C) and high pressure (100-150MPa), and its density is close to the theoretical density. Reheating deformation greatly improves the performance of tool steel. But the used cold and hot isostatic pressing equipment of this method is very expensive, and the manufacturing cost is very high. In the literature P.Hellman, et al., Metal Powder Report, 32:79-83, 1977; 35:254-256, 1980;, 47:25-29, 1992 and G.Hoyle's book 'Highspeed steels', 1988 , London, and Butterworths have introduced this method. In addition, powder tool steel is prepared by supersolid liquid phase sintering method, but the sintering window is narrow, that is, the temperature fluctuation must be small, so the process is difficult to stabilize, and network carbides will be formed after sintering. Literature C.S.Wright et al., PowderMetall ., 36: 213-, 1993; 38: 221-, 1995 are detailed.
发明内容Contents of the invention
本发明的目的在于提供一种用真空热压法制备粉末工具钢的方法,能够同时解决碳化物偏析和结构不致密等问题。The object of the present invention is to provide a method for preparing powder tool steel by vacuum hot pressing, which can solve the problems of carbide segregation and non-compact structure at the same time.
本发明的技术方案是将60~325目合金工具钢粉末置于石墨模具中,将工具钢合金粉末在真空度为8×10-1~8×10-3Pa下加热至固相线温度以下5~40℃时保温,然后加压1~10MPa,当应变速率达到1×10-3/min以下时停止加压,待致密完成后随炉冷却。The technical solution of the present invention is to place 60-325 mesh alloy tool steel powder in a graphite mold, and heat the tool steel alloy powder below the solidus temperature at a vacuum degree of 8×10 -1 to 8×10 -3 Pa Keep warm at 5-40°C, then pressurize at 1-10MPa, stop pressurizing when the strain rate reaches below 1×10 -3 /min, and cool with the furnace after the densification is completed.
所述加压较好为2~6MPa;所述合金工具钢可以为钼系高速钢,如M2(Fe-0.9C-6W-5Mo-4Cr-2V)、M4(Fe-1.3C-6W-5Mo-4Cr-4V)、M50(0.8C-4Mo-4Cr-1V)和M42(Fe-1.1C-1.5W-10Mo-8Co-4Cr-1V);所述合金工具钢还可以为钨系高速钢,如T1(Fe-0.8C-18W-4Cr-1V)、T15(Fe-1.5C-12W-1Mo-5Co-4Cr-5V);所述合金工具钢还可以为冷作工具钢,如Cr12MoV(Fe-12Cr-1Mo-0.5V)。The pressure is preferably 2-6MPa; the alloy tool steel can be molybdenum-based high-speed steel, such as M2 (Fe-0.9C-6W-5Mo-4Cr-2V), M4 (Fe-1.3C-6W-5Mo -4Cr-4V), M50 (0.8C-4Mo-4Cr-1V) and M42 (Fe-1.1C-1.5W-10Mo-8Co-4Cr-1V); the alloy tool steel can also be tungsten high-speed steel, Such as T1 (Fe-0.8C-18W-4Cr-1V), T15 (Fe-1.5C-12W-1Mo-5Co-4Cr-5V); the alloy tool steel can also be cold work tool steel, such as Cr12MoV (Fe -12Cr-1Mo-0.5V).
本发明的原理是将水雾化或气雾化的工具钢粉末加热至该材料的固相线温度以下,此时尚未出现液相,因而不可能出现晶界网状碳化物,但此时材料的表观屈服应力已较低,采用较低的热压压力,如1~10MPa,即可产生粉末材料的塑性流动和粘性流动,并因此而消除空洞,实现致密化,得到相对密度大于99.8%的工件,其中碳化物无偏析,碳化物的粒度3~7μm,由于整个过程在真空中进行,粉末材料的氧含量降低至100ppm以下。The principle of the present invention is to heat the water-atomized or gas-atomized tool steel powder below the solidus temperature of the material. At this time, the liquid phase has not yet appeared, so it is impossible to appear grain boundary network carbides, but at this time the material The apparent yield stress of the powder is already low, and the plastic flow and viscous flow of the powder material can be produced by using a lower hot pressing pressure, such as 1-10MPa, and thus the void can be eliminated, the densification can be achieved, and the relative density can be greater than 99.8%. The workpiece has no segregation of carbides, and the particle size of carbides is 3-7μm. Since the whole process is carried out in vacuum, the oxygen content of the powder material is reduced to below 100ppm.
本发明采用石墨为模具,以同时承受高温和压力,并得到所需工件的形状,在接近于工件的模具内设置热电偶,以求准确测量工件的温度,保证其加热过程接近但不超过固相线温度。The present invention uses graphite as the mould, so as to withstand high temperature and pressure at the same time, and obtain the shape of the required workpiece. Thermocouples are arranged in the mold close to the workpiece, in order to accurately measure the temperature of the workpiece, and ensure that the heating process is close to but not exceeding the solid state. phase temperature.
本发明采用中国专利申请(申请号为01114076.3,申请日为2001年6月15日)中所述的温度、应力和应变速率控制方法,通过在真空热压装置中设置应变传感器,控制应变速率,以测量粉末体的致密化过程,所述热压测控程序具体流程为:首先设定热压温度T设、热压压力P和终止热压应变速率,设终止热压应变速率设为1×10-3/min;开始加热,读取实际热压温度值T,判断实际热压温度T是否大于等于设定热压温度T设(低于固相线温度5~40℃),如大于等于此值,则进行恒温操作,否则继续加热;在恒温控制的同时加压,读取热压压力值,并保持压力P;读取实际应变数据,判断应变速率是否小于等于终止热压应变速率设定值,若是肯定结果,则停止加热自动卸压,冷却后可取出热压样品。The present invention adopts the temperature, stress and strain rate control method described in the Chinese patent application (the application number is 01114076.3, and the application date is June 15, 2001), by setting the strain sensor in the vacuum hot pressing device, the strain rate is controlled, To measure the densification process of the powder body, the specific flow of the hot-pressing measurement and control program is as follows: firstly, set the hot-pressing temperature T , the hot-pressing pressure P, and the termination hot-pressing strain rate , and set the termination hot-pressing strain rate to be 1 ×10 -3 /min; start heating, read the actual hot-pressing temperature T, and judge whether the actual hot-pressing temperature T is greater than or equal to the set hot-pressing temperature T (5-40°C lower than the solidus temperature), if greater than If it is equal to this value, perform constant temperature operation, otherwise continue heating; pressurize while controlling the constant temperature, read the hot pressing pressure value, and maintain the pressure P; read the actual strain data, and judge whether the strain rate is less than or equal to the termination of hot pressing strain Speed setting value , if the result is confirmed, the heating will be stopped and the pressure will be relieved automatically, and the hot-pressed sample can be taken out after cooling.
本发明的有益效果是:The beneficial effects of the present invention are:
1.可得到全致密无偏析的工具材料,本发明是采用真空热压法制备粉末工具钢,同时解决了碳化物偏析和结构不致密等问题,将工具钢合金粉末加热至固相线温度以下5~40℃时保温,在真空度为8×10-1~8×10-3Pa下,加压1~10MPa,应变速率达1×10-3/min时停止加压,可产生粉末材料的塑性流动和粘性流动,并因此而消除空洞,实现致密化,得到相对密度大于99.8%的工件,其中碳化物无偏析,碳化物的粒度3~7μm。1. The tool material with full density and no segregation can be obtained. The present invention adopts the vacuum hot pressing method to prepare powder tool steel, and at the same time solves the problems of carbide segregation and non-dense structure, and heats the tool steel alloy powder below the solidus temperature Keep warm at 5-40°C, pressurize at 1-10MPa at a vacuum of 8× 10-1-8 × 10-3 Pa, stop pressurizing when the strain rate reaches 1× 10-3 /min, and produce powder materials The plastic flow and viscous flow of the workpiece, and thus eliminate the cavity, achieve densification, and obtain a workpiece with a relative density greater than 99.8%, in which the carbide has no segregation, and the particle size of the carbide is 3 to 7 μm.
2.成本低,传统的热等静压工艺在高温(≥1100℃)和高压(100~150MPa)下使金属粉末制品成型及致密化,所用冷、热等静压设备十分昂贵,从而导致成本甚高,而本发明采用真空热压法,工件的所受压力1~10MPa,压力可降低1~2个数量级,设备简单,成本大幅度降低。2. Low cost. The traditional hot isostatic pressing process forms and densifies metal powder products at high temperature (≥1100°C) and high pressure (100-150MPa). The cold and hot isostatic pressing equipment used is very expensive, resulting in cost Very high, but the present invention adopts the vacuum hot pressing method, the pressure on the workpiece is 1-10 MPa, the pressure can be reduced by 1-2 orders of magnitude, the equipment is simple, and the cost is greatly reduced.
3.利用本发明可以制备大型复杂零件毛坯,如带孔和法兰等,材料利用率高。3. The present invention can be used to prepare large complex part blanks, such as holes and flanges, etc., and the material utilization rate is high.
附图说明Description of drawings
图1为本法制备的粉末高速钢锯片照片。Fig. 1 is the photo of the powder high-speed steel saw blade prepared by this method.
图2为本法制备粉末高速钢锯片时的致密化曲线。Fig. 2 is the densification curve when the powder high-speed steel saw blade is prepared by this method.
图3为本法制备的粉末高速钢剃齿刀照片。Fig. 3 is the photo of the powder high-speed steel gear shaving cutter prepared by this method.
图4为本法制备粉末高速钢剃齿刀时的致密化曲线。Fig. 4 is the densification curve when the powder high-speed steel gear shaving cutter is prepared by this method.
图5为本法制备的粉末高速钢纵剪刀照片。Figure 5 is a photo of powder high speed steel slitting shears prepared by this method.
图6为本法制备粉末高速钢纵剪刀时的致密化曲线。Fig. 6 is the densification curve when powder high-speed steel slitting shears are prepared by this method.
图7为本法制备之粉末高速钢纵剪刀的显微组织。Fig. 7 is the microstructure of powder high-speed steel slitting shears prepared by this method.
具体实施方式Detailed ways
实施例1真空热压M2粉末高速钢锯片
锯片的几何尺寸为φ外262mm、φ内孔18mm、h3.5mm,如图1。采用M2水雾化合金粉末成分为:Fe-0.9%C-5.5%W-4.5%Mo-4.4%Cr-2.2%V-0.04%O,该钼系高速钢的固相线温度约为1242℃。粉末的粒度为80~325目,粒度分布见表1。The geometric dimensions of the saw blade are φ262mm , φ18mm , h3.5mm, as shown in Figure 1. The composition of M2 water atomized alloy powder is: Fe-0.9%C-5.5%W-4.5%Mo-4.4%Cr-2.2%V-0.04%O, and the solidus temperature of the molybdenum-based high-speed steel is about 1242°C . The particle size of the powder is 80-325 mesh, and the particle size distribution is shown in Table 1.
表1M2水雾化合金粉末的粒度分布
将M2合金粉末置于石墨模具中,放入真空热压室,在真空度为5×10-2Pa下加热至1225~1235℃,然后加压1.3MPa,保温时间80分钟,应变速率达5×10-4/min时停止加压,取出工件后,测得其相对密度为99.8%,其中碳化物无偏析,碳化物粒度3~7μm,氧含量60ppm。Put the M2 alloy powder in a graphite mold, put it into a vacuum hot-press chamber, heat it to 1225-1235°C under a vacuum degree of 5×10 -2 Pa, then pressurize it to 1.3 MPa, keep it for 80 minutes, and strain rate up to 5 Pressurization was stopped at ×10 -4 /min, and after the workpiece was taken out, its relative density was measured to be 99.8%, in which there was no segregation of carbides, the particle size of carbides was 3-7μm, and the oxygen content was 60ppm.
该工件的致密化曲线见图2。The densification curve of the workpiece is shown in Figure 2.
实施例2真空热压M4粉末高速剃齿刀Example 2 Vacuum hot pressing M4 powder high-speed gear shaving cutter
与实施例1不同之处是:The difference from Example 1 is:
剃齿刀的几何尺寸为:φ外128mm、φ内70mm、φ孔31mm、h22mm,见图3。The geometric dimensions of the shaving cutter are: φ outside 128mm, φ inside 70mm, φ hole 31mm, h22mm, see Figure 3.
采用水雾化M4合金粉末,其成分为:Fe-1.25%C-6.5%W-4.5%Mo-4.2%Cr-4.2%V-0.05%O,该钼系高速钢的固相线温度约为1240℃,粉末的粒度为80~325目,粒度分布见表2。Water atomized M4 alloy powder is used, its composition is: Fe-1.25%C-6.5%W-4.5%Mo-4.2%Cr-4.2%V-0.05%O, the solidus temperature of the molybdenum-based high-speed steel is about 1240°C, the particle size of the powder is 80-325 mesh, and the particle size distribution is shown in Table 2.
表2 M4水雾化合金粉末的粒度分布
将M4合金粉末置于石墨模具中,放入真空热压室,在真空度为8×10-2Pa下加热至1210~1230℃,然后加压4.5MPa,时间50分钟,应变速率达2.5×10-4/min时停止加压,取出工件后,测得相对密度为99.9%,其中碳化物无偏析,碳化物粒度3~6μm,氧含量90ppm。Put the M4 alloy powder in a graphite mold, put it into a vacuum hot-press chamber, heat it to 1210-1230°C under a vacuum degree of 8×10 -2 Pa, then pressurize at 4.5MPa for 50 minutes, and the strain rate reaches 2.5× Stop pressurization at 10 -4 /min. After taking out the workpiece, the measured relative density is 99.9%, in which there is no segregation of carbides, the particle size of carbides is 3-6μm, and the oxygen content is 90ppm.
该工件的致密化曲线见图4。The densification curve of the workpiece is shown in Figure 4.
实施例3真空热压M4粉末高速钢纵剪刀Example 3 Vacuum hot pressing M4 powder high-speed steel slitting shears
与实施例1不同之处是:The difference from Example 1 is:
纵剪刀的几何尺寸为φ外276mm、φ内200mm、h25mm,见图5。所用粉末原料同实施例2。The geometric dimensions of the longitudinal scissors are 276mm outside φ, 200mm inside φ, and h25mm, see Figure 5. Used powder raw material is with embodiment 2.
将合金粉末置于石墨模具中,在真空度为8×10-3Pa下加热至1210~1235℃,加压2.3MPa,保温时间55分钟,应变速率达5×10-4/min时停止加压,取出工件后,测得到相对密度为99.85%,其中碳化物无偏析,碳化物粒度3~7μm,氧含量70ppm。该工件的致密化曲线见图6,其显微组织见图7。Put the alloy powder in a graphite mold, heat to 1210-1235°C under a vacuum of 8×10 -3 Pa, pressurize at 2.3MPa, hold for 55 minutes, and stop heating when the strain rate reaches 5×10 -4 /min After taking out the workpiece, the measured relative density is 99.85%, in which the carbides have no segregation, the carbide particle size is 3-7μm, and the oxygen content is 70ppm. The densification curve of the workpiece is shown in Figure 6, and its microstructure is shown in Figure 7.
实施例4真空热压T1粉末高速钢试样Example 4 Vacuum hot-pressed T1 powder high-speed steel sample
与实施例1不同之处是:The difference from Example 1 is:
试样的几何尺寸为φ50×h20mm,采用水雾化钨系T1高速钢合金粉末,其成分为Fe-0.8%C-18%W-4%Cr-1%V-0.05%O,该合金固相线温度约为1290℃,粉末的粒度为80~325目。将T1高速钢合金粉末置于石墨模具中,放入真空热压室,在真空度为6×10-1Pa下加热至1260~1280℃,然后加压9MPa,时间30分钟,应变速率达2×10-4/min时停止加压,取出工件后,测得相对密度为99.9%,其中碳化物无偏析,碳化物粒度3~6μm,氧含量90ppm。The geometric size of the sample is φ50×h20mm, and the water atomized tungsten-based T1 high-speed steel alloy powder is used, and its composition is Fe-0.8%C-18%W-4%Cr-1%V-0.05%O. The phase line temperature is about 1290°C, and the particle size of the powder is 80-325 mesh. Put the T1 high-speed steel alloy powder in a graphite mold, put it into a vacuum hot-press chamber, heat it to 1260-1280°C at a vacuum degree of 6×10 -1 Pa, then pressurize at 9 MPa for 30 minutes, and the strain rate reaches 2 Pressurization was stopped at ×10 -4 /min, and after the workpiece was taken out, the relative density was measured to be 99.9%, in which the carbides had no segregation, the carbide particle size was 3-6μm, and the oxygen content was 90ppm.
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