CN109014214B - Preparation method of HK30 material based on MIM molding and HK30 blade - Google Patents

Preparation method of HK30 material based on MIM molding and HK30 blade Download PDF

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CN109014214B
CN109014214B CN201811020109.6A CN201811020109A CN109014214B CN 109014214 B CN109014214 B CN 109014214B CN 201811020109 A CN201811020109 A CN 201811020109A CN 109014214 B CN109014214 B CN 109014214B
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stainless steel
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CN109014214A (en
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何浩
李益民
刘晨
陈永志
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Guangxi Metallurgical Research Institute Co ltd
Guangxi University of Science and Technology
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GUANGXI RESEARCH INSTITUTE OF METALLURGY
Guangxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/22Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps

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Abstract

The invention discloses a preparation method of an HK30 material based on MIM molding, which comprises the following steps: (1) uniformly mixing HK30 stainless steel powder and titanium powder to obtain HK30-Ti composite powder; (2) mixing the HK30-Ti composite powder obtained in the step (1) with a binder, then mixing, and granulating to obtain granular feed; (3) injecting the granular feed obtained in the step (2) on an injection molding machine to obtain an injection green body; (4) and (4) degreasing and vacuum sintering the injection green body obtained in the step (3) to obtain the HK30 material. The invention also provides an HK30 blade prepared by the HK30 material. According to the invention, Ti is added into the HK30 stainless steel powder, so that the sintering temperature is effectively increased, and the high-temperature mechanical property is further improved.

Description

Preparation method of HK30 material based on MIM molding and HK30 blade
Technical Field
The invention belongs to the field of powder metallurgy, and particularly relates to a preparation method of an HK30 material and an HK30 blade.
Background
HK30 belongs to high-chromium nickel austenitic stainless steel, and has been widely used in the fields of automobiles, chemical engineering, engineering machinery and the like due to its excellent corrosion resistance and oxidation resistance at high temperature. However, the austenitic stainless steel HK30 is seriously stuck when being processed, and the machining method is difficult to prepare small and medium-sized HK30 parts with complex shapes. The HK30 prepared by the metal injection molding method (MIM process) has the advantages of high material utilization rate, low cost, uniform structure and the like. However, in the MIM process, the two steps of adding the binder and degreasing easily cause the fluctuation of the carbon content of the final product, so that the sintering window is narrow, the product is easy to over-burn or under-burn, and the size fluctuation of the product is large. Generally, the standard deviation of the sample size at a sintering temperature of 1310 ℃ is greater than 0.04.
The related literature shows that HK30 has improved high-temperature bending strength with the increase of sintering temperature during sintering, but the problem of overburning and underburning is easy to occur during sintering due to the narrow sintering window, the sintering temperature is generally about 1310 ℃, and the high-temperature (800 ℃) tensile strength is about 420 MPa. Therefore, how to increase the sintering temperature to sinter the powder at a higher temperature and further obtain higher high-temperature mechanical properties is a hot research problem at present.
Disclosure of Invention
The invention aims to solve the technical problems of overcoming the defects and shortcomings in the background technology and providing a preparation method of HK30 material based on MIM molding and HK30 blades, wherein the HK30 material prepared by the preparation method has excellent high-temperature mechanical property and the obtained product has high yield. In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of HK30 material based on MIM molding comprises the following steps:
(1) uniformly mixing HK30 stainless steel powder and titanium powder to obtain HK30-Ti composite powder;
(2) mixing the HK30-Ti composite powder obtained in the step (1) with a binder, then mixing, and granulating to obtain granular feed;
(3) injecting the granular feed obtained in the step (2) on an injection molding machine to obtain an injection green body;
(4) and (4) degreasing and vacuum sintering the injection green body obtained in the step (3) to obtain the HK30 material.
In the above preparation method, preferably, the titanium powder is hydrogenated dehydrotitanium powder, and the amount of the hydrogenated dehydrotitanium powder is 0.4-1.2% of the total amount of the HK30-Ti composite powder.
In the above manufacturing method, preferably, the components of the HK30 stainless steel powder include the following components: 0.25-0.35% of C, 23-27% of Cr, 19-22% of Ni, 1.2-1.5% of Nb, and the balance of iron and inevitable impurities; the hydrogenated dehydrogenated titanium powder comprises the following components: 0.005% of C, 0.16% of O, 0.04% of Fe, 0.021% of N and the balance of titanium.
In the above manufacturing method, preferably, the HK30 stainless steel powder has a median particle size of 20 μm, and the hydrogenated titanium dehydrogenated powder has a median particle size of 17 μm.
In the above preparation method, it is preferable that the HK30-Ti composite powder is mixed with the binder in an amount of 57% of the loading amount of the HK30-Ti composite powder.
In the above production method, in the step (2), the kneading temperature is preferably 155 ℃ and the kneading time is preferably 180 min.
In the above preparation method, preferably, in the step (3), the injection temperature is 120-165 ℃, the injection pressure is 60-120MPa, and the mold temperature is 30-60 ℃ during injection molding.
In the above preparation method, the degreasing preferably includes: firstly, placing the injection green body in a dichloromethane solvent, and dissolving paraffin and vegetable oil components in the injection green body; and then putting the dried injection green body into a vacuum degreasing furnace, heating to 180 ℃ at a speed of 4 ℃/min under the protection of argon, preserving heat for 180min, heating to 350 ℃ at a speed of 4 ℃/min, preserving heat for 180min, and removing residual organic matters in the blank.
In the preparation method, preferably, during the vacuum sintering, the sintering temperature is controlled to be 1310-1350 ℃, and the furnace is cooled after the temperature is kept for 6 hours.
As a general technical concept, the invention also provides an HK30 blade, and the HK30 blade is prepared from the HK30 material obtained by the preparation method.
The invention takes HK30 stainless steel powder as a basic raw material, mixes Ti powder (cheap hydrogenated dehydrogenated titanium powder is adopted as the Ti powder) with different proportions by a dry mixing method, and prepares the HK30 material by an injection molding technology. During the sintering process of HK30, in order to obtain higher mechanical properties, the sintering temperature needs to be increased as much as possible so as to increase the sintering compactness. However, excessive sintering temperatures may produce a liquid phase, which may provide rapid diffusion paths and capillary forces for rapid densification. However, when the liquid phase is too much, it may cause uneven shrinkage or even collapse of the part, which is more serious especially when the part (vane) of complicated shape has a cantilever portion. According to the invention, Ti and carbon form relatively stable carbide in the sintering process by adding Ti, so that the content of carbon combined with Fe is reduced, the occurrence of liquid phase in the sintering process is delayed, the sintering temperature is effectively increased, and the high-temperature mechanical property is further improved. Meanwhile, the addition of Ti stabilizes the fluctuation of C element in the matrix, widens the sintering window of the matrix, and can greatly improve the yield of the injection molding HK30 product.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, Ti is added into the HK30 stainless steel powder, so that Ti and carbon form relatively stable carbide in the sintering process, the content of carbon combined with Fe is reduced, the occurrence of liquid phase in the sintering process is delayed, the sintering temperature is effectively increased, and the high-temperature mechanical property is improved.
2. In the invention, the addition of Ti stabilizes the fluctuation of C element in the matrix, widens the sintering window of the matrix, and can greatly improve the yield of the injection molded HK30 product.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a pictorial representation of the HK30 material prepared in example 1.
Fig. 2 is a physical diagram of HK30 leaf in example 1.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
a preparation method of HK30 material based on MIM molding comprises the following steps:
(1) mixing HK30 stainless steel powder and hydrogenated titanium hydride powder for 5h by using a four-pot mixer to obtain HK30-Ti composite powder; wherein the median particle size of the HK30 stainless steel powder is 20 μm, and the median particle size of the hydrogenated titanium hydride powder is 17 μm; the dosage of the hydrogenated and dehydrogenated titanium powder accounts for 1.2 percent of the total amount of the HK30-Ti composite powder; the compositions of the HK30 stainless steel powder and titanium powder are shown in tables 1 and 2 below;
(2) mixing the HK30-Ti composite powder obtained in the step (1) with a binder, then mixing, and granulating to obtain granular feed; wherein the dosage of the binder is controlled to be 57 percent of the loading capacity of the HK30-Ti composite powder, the mixing temperature is 155 ℃, and the mixing time is 180 min;
(3) injecting the granular feed obtained in the step (2) on a 40-ton injection molding machine to obtain an injection green body; controlling the injection temperature to be 120-165 ℃, the injection pressure to be 60-120MPa and the mold temperature to be 30-60 ℃;
(4) putting the injection green body obtained in the step (3) into a dichloromethane solvent, and dissolving paraffin and vegetable oil components in the injection green body; then putting the dried blank into a vacuum degreasing furnace, heating to 180 ℃ at a speed of 4 ℃/min under the protection of argon, preserving heat for 180min, heating to 350 ℃ at a speed of 4 ℃/min, preserving heat for 180min, and removing residual organic matters in the blank;
(5) and (3) putting the degreased green body into a vacuum sintering furnace for sintering, heating at the speed of 5 ℃/min, keeping the sintering temperature at 1350 ℃, and cooling along with the furnace after keeping the temperature for 6 hours to obtain the HK30 material in the embodiment.
Table 1: chemical composition of HK30 stainless steel powder
Figure BDA0001787101710000031
Figure BDA0001787101710000041
The HK30 material prepared in this example is shown in FIG. 1, and tested, its high temperature tensile strength (800 deg.C) is over 500MPa, and its relative density is 97.5%.
The HK30 blades processed by using the HK30 material prepared in the embodiment are shown in FIG. 2.
Example 2:
a preparation method of HK30 material based on MIM molding comprises the following steps:
(1) mixing HK30 stainless steel powder and hydrogenated titanium hydride powder for 5h by using a four-pot mixer to obtain HK30-Ti composite powder; wherein the median particle size of the HK30 stainless steel powder is 20 μm, and the median particle size of the hydrogenated titanium hydride powder is 17 μm; the dosage of the hydrogenated and dehydrogenated titanium powder accounts for 0.4 percent of the total amount of the HK30-Ti composite powder; the composition of the HK30 stainless steel powder and titanium powder was the same as in example 1;
(2) mixing the HK30-Ti composite powder obtained in the step (1) with a binder, then mixing, and granulating to obtain granular feed; wherein the dosage of the binder is controlled to be 57 percent of the loading capacity of the HK30-Ti composite powder, the mixing temperature is 155 ℃, and the mixing time is 180 min;
(3) injecting the granular feed obtained in the step (2) on a 40-ton injection molding machine to obtain an injection green body; controlling the injection temperature to be 120-165 ℃, the injection pressure to be 60-120MPa and the mold temperature to be 30-60 ℃;
(4) putting the injection green body obtained in the step (3) into a dichloromethane solvent, and dissolving paraffin and vegetable oil components in the injection green body; then putting the dried blank into a vacuum degreasing furnace, heating to 180 ℃ at a speed of 4 ℃/min under the protection of argon, preserving heat for 180min, heating to 350 ℃ at a speed of 4 ℃/min, preserving heat for 180min, and removing residual organic matters in the blank;
(5) and (3) putting the degreased green body into a vacuum sintering furnace for sintering, heating at the speed of 5 ℃/min, keeping the sintering temperature at 1350 ℃, and cooling along with the furnace after keeping the temperature for 6 hours to obtain the HK30 material in the embodiment.
The HK30 material prepared in this example was tested to be excellent in high temperature tensile strength (800 ℃). The HK30 blade processed by the HK30 material prepared in the embodiment is subjected to a dimensional fluctuation test, wherein the dimensional fluctuation test method comprises the following steps: the width data of a single sintered sample is collected, and the standard deviation of each group of samples is obtained in a fitting mode, the collection number of each sample is 200, and the result shows that the standard deviation of the sample is about 0.01793 and is greatly improved compared with the standard deviation of the original HK30 blade of about 0.04.

Claims (5)

1.一种基于MIM成型的HK30材料的制备方法,其特征在于,包括以下步骤:1. a preparation method based on the HK30 material of MIM molding, is characterized in that, comprises the following steps: (1)将HK30不锈钢粉末与钛粉混合均匀得到HK30-Ti复合粉;(1) Mix HK30 stainless steel powder and titanium powder uniformly to obtain HK30-Ti composite powder; (2)将步骤(1)中得到的HK30-Ti复合粉与粘结剂混合后进行混炼,再制粒得到粒状喂料;(2) mixing the HK30-Ti composite powder obtained in step (1) with a binder, and then kneading, and then granulating to obtain granular feed; (3)将步骤(2)中得到的粒状喂料在注射成形机上注射得到注射生坯;(3) injecting the granular feed obtained in step (2) on an injection molding machine to obtain an injection green body; (4)将步骤(3)中得到的注射生坯进行脱脂与真空烧结,即得到HK30材料;(4) degreasing and vacuum sintering the injection green body obtained in step (3) to obtain HK30 material; 其中,所述HK30不锈钢粉末中位粒径为20μm,所述钛粉为氢化脱氢钛粉,所述氢化脱氢钛粉的用量占HK30-Ti复合粉总量的0.4-1.2%,所述氢化脱氢钛粉的中位粒径为17μm;Wherein, the median particle size of the HK30 stainless steel powder is 20 μm, the titanium powder is hydrogenated and dehydrogenated titanium powder, and the amount of the hydrogenated and dehydrogenated titanium powder accounts for 0.4-1.2% of the total amount of HK30-Ti composite powder. The median particle size of the hydrodehydrogenated titanium powder is 17 μm; 所述真空烧结时,控制烧结温度为1310-1350℃,保温6h后随炉冷却;During the vacuum sintering, the sintering temperature is controlled to be 1310-1350° C., and the temperature is kept for 6 hours and then cooled with the furnace; 所述HK30不锈钢粉末的成分包括以下组分:0.25-0.35%的C、23-27%的Cr、19-22%的Ni、1.2-1.5%的Nb、余量为铁及不可避免的杂质;所述氢化脱氢钛粉的成分包括以下组分:0.005%的C、0.16%的O、0.04%的Fe、0.021%的N、余量为钛;The composition of the HK30 stainless steel powder includes the following components: 0.25-0.35% C, 23-27% Cr, 19-22% Ni, 1.2-1.5% Nb, and the balance is iron and inevitable impurities; The composition of the hydrodehydrogenation titanium powder includes the following components: 0.005% C, 0.16% O, 0.04% Fe, 0.021% N, and the balance is titanium; 所述脱脂时,包括以下步骤:首先将注射生坯置于二氯甲烷溶剂中,溶解其中的石蜡和植物油组分;然后将干燥后的注射生坯放入真空脱脂炉中,在氩气保护下,以4℃/min加热至180℃,保温180min,再以4℃/min加热至350℃,保温180min,脱除坯件内部的剩余有机物。The degreasing process includes the following steps: first, placing the injection green body in a dichloromethane solvent to dissolve the paraffin and vegetable oil components therein; Under the temperature, heat to 180°C at 4°C/min, hold for 180min, then heat to 350°C at 4°C/min, hold for 180min, and remove the remaining organic matter inside the blank. 2.根据权利要求1所述的制备方法,其特征在于,所述HK30-Ti复合粉与粘结剂混合时,粘结剂的用量控制为HK30-Ti复合粉的装载量的57%。2. preparation method according to claim 1 is characterized in that, when described HK30-Ti composite powder is mixed with binder, the consumption of binder is controlled to be 57% of the loading capacity of HK30-Ti composite powder. 3.根据权利要求1或2所述的制备方法,其特征在于,所述步骤(2)中,混炼温度为155℃,混炼时间为180min。3 . The preparation method according to claim 1 or 2 , wherein, in the step (2), the mixing temperature is 155° C. and the mixing time is 180 min. 4 . 4.根据权利要求1或2所述的制备方法,其特征在于,所述步骤(3)中, 注射成形时,注射温度为120-165℃,注射压力为60-120MPa,模温30-60℃。The preparation method according to claim 1 or 2, characterized in that, in the step (3), during injection molding, the injection temperature is 120-165°C, the injection pressure is 60-120MPa, and the mold temperature is 30-60°C °C. 5.一种HK30叶片,其特征在于,所述HK30叶片由权利要求1-4中任一项所述的制备方法得到的HK30材料制备而成。5. a HK30 blade, is characterized in that, described HK30 blade is prepared from the HK30 material that the preparation method described in any one of claim 1-4 obtains.
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