CN114574774A - Stainless powder metallurgy high-speed steel for wet-type rotary die cutter roller and preparation method thereof - Google Patents
Stainless powder metallurgy high-speed steel for wet-type rotary die cutter roller and preparation method thereof Download PDFInfo
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Abstract
The invention relates to stainless powder metallurgy high-speed steel, in particular to stainless powder metallurgy high-speed steel for a wet-type rotary die-cutting knife roller and a preparation method thereof. When the high-speed steel is prepared, the raw material bags are used in percentage by massComprises the following steps: mo22-5% of C, 3-5% of VC, 2-5% of Co, 18-25% of Cr, 1-2% of NbC, 1-2% of WC, 0.05-0.5% of La and Y, and the balance of Fe, wherein the sum of the mass percentages of the raw materials is 100%; the Cr, the La and the Y are prepared in the form of chromium powder, lanthanum powder and yttrium powder, are subjected to ball milling, premixed and dried under the condition of containing oxygen, and are finally introduced into high-speed steel through mixing and sintering; said oxygen-containing conditions refer to conditions wherein the oxygen content is greater than 0 and less than 4 vol.%; the carbide size in high speed steel is less than 5 μm. The preparation method comprises the following steps: pretreating raw materials, ball-milling and mixing the raw materials, pressing and forming, sintering and carrying out heat treatment. The product has reasonable component design, simple and controllable preparation process, and good mechanical property and corrosion resistance; is convenient for large-scale industrial application.
Description
Technical Field
The invention relates to stainless powder metallurgy high-speed steel, in particular to stainless powder metallurgy high-speed steel for a wet-type rotary die-cutting knife roller and a preparation method thereof.
Background
The rotary die cutting is firstly applied to the printing industry, particularly the cigarette packet printing and packaging industry, is an efficient die cutting mode for replacing flat pressing and blanking processing, and has the advantages of high efficiency and low energy consumption by distributing blades with the same shape as a product on the surface of a knife roller, and continuously cutting the material into specific shapes under certain pressure in the high-speed rotating process. With the development of the rotary die cutting technology, the rotary die cutting technology is not limited to the printing industry in the current industrial production, is suitable for die cutting production of all flexible materials, and is widely applied to industries of non-woven fabrics, plastic films, paper, copper/aluminum foils, sanitary products and the like.
The linear velocity is a key parameter of rotary die cutting, the production efficiency of the die cutting is determined, the working linear velocity is continuously improved along with the continuous development of the die cutting, and at present, part of the linear velocity breaks through 300 m/min. The high line speeds place extremely high demands on the accuracy, temperature and wear resistance of the die-cutting system and the die-cutting knife roll. The main working components of rotary die cutting are a knife roller and an anvil roller, the flexible material passes through the contact surface of the knife roller and the anvil roller during working and is cut into a specific shape by the knife roller, and the knife roller needs to maintain high sharpness at high die cutting speed, so that the knife roller material needs to have extremely high wear resistance as guarantee of service life. At present, imported powder metallurgy high-speed steel or imported hard alloy is used as a knife roll material for die cutting at the linear speed of 300m/min so as to ensure the service life of the knife roll at the high linear speed. Compared with hard alloy, the powder metallurgy high-speed steel has more excellent toughness, can avoid the edge from collapsing and is suitable for more working conditions. Compared with the traditional cast-forged high-speed steel, the powder metallurgy high-speed steel named according to the preparation method has finer and more uniform carbides in the structure and excellent hardness, toughness and wear resistance, but due to the limitation of domestic technical reserves, the gas atomization-hot isostatic pressing preparation process of the powder metallurgy high-speed steel has systematic technical bottlenecks in process control and equipment, and has the problems of large investment, long flow and difficult control, and the existing high-performance powder metallurgy high-speed steel is totally dependent on import.
Wet rotary die cutting is a more severe working condition in rotary die cutting, and is often used in the die cutting process of wet tissues and wet toilet paper. The complex wet environment and additives in the liquid cause severe corrosion to the knife roll, and it is difficult to find a long-life knife roll material suitable for the working condition in the current die cutting technology. The prior commonly used high-end knife roll material imported powder metallurgy high-speed steel and hard alloy material have high sharpness and wear resistance, but the corrosion resistance is poor, the sharpness is reduced due to the abrasion of a knife tip caused by corrosion in the use process, and in addition, substances generated by corrosion can also cause pollution to products. The conventional stainless steel material can meet the corrosion resistance requirement of working conditions, but the lower hardness cannot meet the requirements on high sharpness and high wear resistance. And aiming at the problem of poor corrosion resistance of a cutter roller in wet-type rotary die cutting application, the process for preparing the novel powder metallurgy high-speed steel through the traditional gas atomization-hot isostatic pressing process has higher difficulty. On one hand, the method is limited by the highest temperature bearing limit of atomization equipment, and the preparation of new brand powder metallurgy high-speed steel with high alloy content has higher difficulty; on the other hand, the high preparation cost of the knife roll also limits the popularization of high-speed rotary die cutting, because the geometric shape of the knife roll is a hollow cylinder, the processing amount is large, and the price of imported materials is high.
To sum up, the material and the preparation cost of the knife roller hinder the technical development of wet-type rotary die cutting, limit the die cutting speed and the service life of the knife roller, increase the production cost of products, and urgently wait for the research and development of a knife roller material with high wear resistance, excellent corrosion resistance and economy and convenience.
Disclosure of Invention
The invention aims to provide a stainless powder metallurgy high-speed steel material with good wear resistance, strong corrosion resistance and high sharpness, aiming at the problem of reduced wear resistance and service life caused by poor corrosion resistance of a knife roll in wet rotary die cutting. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
According to the stainless powder metallurgy high-speed steel material for the wet rotary die-cutting knife roller, provided by the invention, through alloy element addition and a post-treatment process, the material has excellent corrosion resistance while keeping high hardness, high wear resistance and high sharpness, the service life of the knife roller for wet rotary die-cutting is prolonged, and the production cost is reduced. The stainless powder metallurgy high-speed steel material is prepared by a traditional powder metallurgy method, has short flow and low cost compared with the traditional gas atomization-hot isostatic pressing process of imported products, has the advantage of near-net-shape forming, and can reduce the processing amount and improve the material utilization rate when used for producing the rotary die-cutting knife roller in the shape of a hollow cylinder.
The invention provides a stainless powder metallurgy high-speed steel material for a wet-type rotary die-cutting knife roller, which mainly comprises elements such as Fe, W, Mo, V, Nb, Co, Cr, C and the like, wherein the size of carbide in the structure is less than 5 mu m.
According to the preferable scheme, the preparation of the stainless powder metallurgy high-speed steel material comprises the following raw materials in percentage by mass: mo22-5% of C, 3-6% of VC, 2-5% of Co, 15-25% of Cr, 0-3% of NbC, 0-5% of WC, 0.05-0.5% of La and Y, and the balance of Fe, wherein the sum of the mass percentages of the raw materials is 100%. The Cr powder, the lanthanum powder and the yttrium powder are subjected to wet ball milling and are dried under the condition of containing oxygen, and finally are introduced into the high-speed steel through mixing and sintering; said oxygen-containing conditions refer to conditions wherein the oxygen content is greater than 0 and less than 4 vol.%;
according to the preferable scheme, the preparation of the stainless powder metallurgy high-speed steel material comprises the following raw materials in percentage by mass: mo22-5% of C, 3-5% of VC, 2-5% of Co, 18-25% of Cr, 1-2% of NbC, 1-2% of WC, 0.05-0.5% of La (lanthanum) and Y (yttrium), and the balance of Fe, wherein the sum of the mass percentages of the raw materials is 100%.
In a preferable scheme, raw materials for preparing the stainless powder metallurgy high-speed steel material are high-purity (> 99.8%) and ultrafine (average grain diameter is less than 5 mu m) powder.
The invention also provides a preparation method of the stainless powder metallurgy high-speed steel material for the wet-type rotary die-cutting knife roller, which comprises the following specific steps:
(1) pretreatment of raw materials
Carrying out wet ball milling on raw materials Cr powder, La powder and Y powder for a certain time, and drying in an atmosphere A to obtain pretreated Cr powder, La powder and Y powder; said atmosphere a contains 1-3.5 vol.% oxygen;
(2) ball milling and mixing of raw materials
Weighing raw material powder with corresponding mass percentage except Cr powder, La powder and Y powder according to a formula, additionally adding carbon black and a forming agent according to a proportion, and performing ball milling and mixing for a certain time through wet ball milling to obtain mixed slurry. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the slurry, continuing to perform ball milling mixing under certain conditions, and drying the final mixed slurry in a vacuum oven to obtain a ball milling mixture;
(3) press forming
Placing the ball-milling mixture obtained in the step (2) into a die, and pressing to obtain a cold-pressed blank;
(4) sintering
Putting the cold-pressed blank obtained in the step (3) into a sintering furnace for vacuum sintering, and cooling to obtain a sintered blank; the temperature of vacuum sintering is 1180-1260 ℃;
(5) thermal treatment
And (4) preheating the sintered blank obtained in the step (4), then carrying out high-temperature quenching, carrying out deep cooling treatment after quenching and cleaning, carrying out multiple tempering treatments after the deep cooling product naturally returns to the room temperature, and obtaining a finished product after the heat treatment is finished.
In a preferable scheme, in the step (1), the wet ball milling medium is absolute ethyl alcohol, ball milling is protected by inert gas atmosphere, the adopted milling balls can be hard alloy or steel balls, the ball-material ratio is (4-8): 1, and the ball milling time is 24-36 hours. By ball milling Cr, La and Y element powder in advance, the Cr, La and Y element powder is fully mixed and uniformly distributed, so that La and Y rare earth elements are favorable for adsorbing oxygen elements in Cr elements in the subsequent sintering process, and the sintering activity is ensured.
Preferably, in the step (1), the drying is performed in a protective atmosphere, the drying temperature is 50-60 ℃, the protective atmosphere is a mixed gas of nitrogen and oxygen, the content of oxygen is 1-3 vol.%, and the drying time is 4-8 h. Through the controllable oxidation of the low oxygen partial pressure, a thin oxidation film is generated on the surface of the Cr, La and Y element powder, and the Cr, La and Y elements are protected in the subsequent mixing, drying and storing processes.
In a preferred embodiment, in the step (2), the carbon black is additionally added in an amount of 0.3 to 0.9 wt.%. The purpose of adding carbon black is to remove the surface oxidation of raw materials in preparation through carbon-oxygen reaction in the sintering process and promote the sintering densification of the materials.
Preferably, in the step (2), the forming agent can be a forming agent commonly used in the industry, and is preferably paraffin, and the addition amount is 4-6 wt.%.
In a preferable scheme, in the step (2), the wet ball milling medium is absolute ethyl alcohol, ball milling is protected by inert gas atmosphere, the adopted milling balls can be hard alloy or steel balls, roller ball milling is preferably adopted in consideration of batch production, and the rotating speed is 60-100 rpm. The mass ratio of the primary ball-milling ball material is (4-8) to 1, and the ball-milling time is 36-64 h. After the pretreated Cr powder, La powder and Y powder are added, the mass ratio of the secondary ball-milling ball material is (1-3) to 1, and the ball-milling time is 12-24 hours.
Preferably, in the step (2), the drying can be performed in a vacuum drying oven, and the drying pressure is 10000-20000 Pa.
Preferably, in the step (3), the pressing pressure is 100-250 MPa, and the pressing mode can be conventional die pressing and cold isostatic pressing. When producing the hollow cylindrical product, the pressing mode is preferably cold isostatic pressing, which helps to ensure the density uniformity of each part of the compact.
Preferably, in the step (4), a vacuum sintering mode is adopted, and the pressure in the sintering process is 10-210Pa, 1180 to 1250 ℃ of the highest sintering temperature and 2 to 4 hours of heat preservation time.
In the preferable scheme, in the step (5), the quenching temperature is 1170-1220 ℃, the quenching heat preservation time is 30-120 min according to the size of the product, the quenching is carried out in salt bath or atmosphere protection, and the medium is selected as quenching oil; the deep cooling temperature is-180 ℃ to-60 ℃, and the deep cooling time is 60-240 min; the tempering temperature is 540-570 ℃, the tempering process is to temper for three times, each time for 1h, and naturally cool to the room temperature after each tempering.
Preferably, the preparation method only comprises the preparation flow of the material, and a rough processing step is required to be added after sintering in the production process of the knife roller, and final finishing is carried out after heat treatment is finished.
Because the traditional high-speed steel preparation process gas atomization-hot isostatic pressing process needs to atomize alloy elements, the high-speed steel with high alloy content has high melting point, so that the high-speed steel is limited by a gas atomization technology, and under the condition of a large amount of existing alloy elements, the high chromium content is difficult to add, and the gas atomized powder with high chromium and high alloy content is obtained. The high-speed steel material prepared by the traditional powder metallurgy method has the problems of low density, poor bonding force among particles and poor mechanical property, and the high-content Cr element is easy to oxidize in the preparation process, so that the densification difficulty is further increased.
The invention adopts the traditional powder metallurgy method, and realizes the preparation of high-density and high-performance powder metallurgy stainless high-speed steel with high carbon and high chromium content under the innovation of component design and solid-phase sintering by premixing Cr and rare earth elements, controllable oxidation pretreatment of easily-oxidized elements, carbon-oxygen reaction activation sintering and the adsorption and enhanced sintering of impurity elements of the rare earth elements in the preparation process, thereby breaking through the technical limitations and the technical self limitations of the traditional powder metallurgy high-speed steel gas atomization-hot isostatic pressing process route.
In the technical scheme of the invention, the addition amount of the alloy element determines the key mechanical property, wear resistance and corrosion resistance of the material. Wherein, Cr element is a key element of the stainless powder metallurgy high-speed steel, and the addition amount of the Cr element determines the corrosion resistance and the mechanical property of the material. The excessively low content of the Cr element cannot provide enough oxidation resistance for the material, the higher content of the Cr element causes the material to have low hardness, the Cr element is easily oxidized in the preparation process, and an oxide which cannot be reduced by adding carbon black is introduced, so that serious defects are brought to the material, and the strength and the toughness of the material are remarkably reduced. And the additionally added carbon black and rare earth elements are used for reducing an oxide layer on the surface of the particles in the sintering process, the carbon black can remove oxygen elements on the surface of the powder through carbon-oxygen reaction, and the generated CO can form a reducing atmosphere to further reduce the material, so that the material is endowed with higher sintering activity. The addition of the La and Y rare earth elements is an oxygen element which can absorb materials and is not removed in the sintering process, so that the material per se obtains high sintering activity, and strong binding force among particles and excellent mechanical properties of the material are endowed.
The oxygen content control in the preparation process is an important influence factor of the density, the hard phase binding force and the mechanical property of the sintered material. In order to avoid the Cr, La and Y elements which are easy to oxidize from being seriously oxidized in the ball milling process and the drying process, the controllable oxidation treatment of low oxygen partial pressure is adopted, a thin oxidation film can be pre-generated on the surface of the elements which are easy to oxidize, and the elements which are easy to oxidize can be protected in the subsequent mixing, slurry drying and storing processes.
In addition to the mechanical properties, wear resistance and corrosion resistance of the material itself, the material also needs to have a high sharpness to ensure that the flexible material is completely cut off in the high-speed rotation process for rotary die cutting applications. The sharpness of the powder metallurgy high-speed steel is determined by the size of the carbide, and the carbide with too coarse grain diameter in the tissue cannot ensure the sharpness of the cutting edge, so that the cutting edge is cracked or passivated. The grain size of the carbide in the stainless powder metallurgy high-speed steel material structure provided by the invention is controlled by the raw material grain size, the sintering process and the heat treatment process, so that fine and uniformly distributed carbide is obtained, and the sharpness of the product is ensured.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
(1) by adopting the wet die-cutting stainless powder metallurgy high-speed steel and the preparation method provided by the invention, the high-performance preparation of the stainless powder metallurgy high-speed steel with high chromium and high alloy content is realized by adjusting the content of alloy elements and activating and sintering modes and combining the control of the particle size of raw materials and the heat treatment process. The prepared stainless powder metallurgy high-speed steel material is compact, has uniform and fine carbides in the structure, has high compactness, high sharpness, high hardness and high wear resistance, and has excellent corrosion resistance.
(2) When the stainless powder metallurgy high-speed steel provided by the invention is applied to a wet type rotary die cutting knife roller, the corrosivity of an additive in liquid can be effectively resisted in the high-speed die cutting process, the service life is long, the cost consumption is low, and the material blank among imported powder metallurgy high-speed steel, hard alloy and stainless steel in the wet type rotary die cutting application is made up;
(3) besides the use performance, compared with the imported knife roll material, the stainless powder metallurgy high-speed steel provided by the invention has obvious cost advantage. Compared with the characteristics of long process and expensive equipment of the traditional powder metallurgy high-speed steel, the preparation method has the advantages of short process, economy, convenience and capability of achieving near-net-shape preparation, preparing the hollow cylinder of the sintered cutter roller, avoiding raw material loss caused by processing the solid cylinder, improving the production efficiency and reducing the production cost.
Drawings
FIG. 1 microstructure morphology of stainless powder metallurgy high speed steel prepared in example 3
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Examples and comparative examples
The stainless powder metallurgy high-speed steel material for the wet type rotary die-cutting knife roller is prepared in the examples 1 to 5, and the non-metallurgical high-speed steel material which is not in the preferable range of patent components and processes is prepared in the comparative examples 1 to 3:
raw materials
The raw material tables (in weight percent) prepared in examples and comparative examples are shown in the following table 1.
TABLE 1 raw material tables (in mass percent) of examples and comparative examples
The preparation method comprises the following steps:
example 1
(1) Pretreatment of raw materials
Carrying out wet ball milling on Cr powder, La powder and Y powder serving as raw materials in absolute ethyl alcohol under the protection atmosphere of nitrogen, wherein the grinding balls are made of hard alloy, the ball-material mass ratio is 5:1, and the ball milling time is 36 hours. Drying in mixed gas of nitrogen and oxygen after ball milling, wherein the content of oxygen is 2 vol.%, the drying time is 8h, and the drying temperature is 50 ℃;
(2) ball milling and mixing of raw materials
Weighing raw material powder in corresponding mass percentage except Cr powder, La powder and Y powder according to the formula, adding additionally added 0.5% of carbon black and 5% of paraffin, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 5:1, the ball milling time is 72h, and the ball milling rotating speed is 60 rpm. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the obtained slurry, continuously performing ball milling and mixing, wherein a ball milling medium is alcohol, a protective atmosphere is nitrogen, a milling ball is hard alloy, the ball-material ratio is 2:1, and the ball milling time is 12 hours. Drying the ball-milled mixture by using a vacuum oven at the drying temperature of 75 ℃ for 8 h;
(3) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 150MPa to obtain a hollow cylindrical pressed blank;
(3) sintering of
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1200 ℃, the heat preservation time is 3h, and cooling to obtain a sintered blank;
(4) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and insulating for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1180 ℃, the insulating time is 60min, and the quenching medium is quenching oil. Cooling to room temperature, cleaning, and deep cooling in a deep cooling tank at-90 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
Example 2
(1) Pretreatment of raw materials
Carrying out wet ball milling on Cr powder, La powder and Y powder serving as raw materials in absolute ethyl alcohol under the protection atmosphere of nitrogen, wherein the grinding balls are made of hard alloy, the ball-material mass ratio is 4:1, and the ball milling time is 24 hours. Drying in mixed gas of nitrogen and oxygen after ball milling, wherein the content of oxygen is 3 vol.%, the drying time is 6h, and the drying temperature is 55 ℃;
(2) ball milling and mixing of raw materials
Weighing raw material powder in corresponding mass percentage except Cr powder, La powder and Y powder according to the formula, adding additionally added 0.4% of carbon black and 4% of paraffin, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 6:1, the ball milling time is 48h, and the ball milling rotating speed is 80 rpm. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the obtained slurry, continuously performing ball milling and mixing, wherein a ball milling medium is alcohol, a protective atmosphere is nitrogen, a milling ball is hard alloy, the ball-material ratio is 1:1, and the ball milling time is 18 hours. Drying the ball-milled mixture by using a vacuum oven at the drying temperature of 85 ℃ for 8 h;
(3) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 160MPa to obtain a hollow cylindrical pressed blank;
(4) sintering of
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1190 ℃, the heat preservation time is 2 hours, and cooling to obtain a sintered blank;
(5) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and insulating for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1190 ℃, the insulating time is 40min, and the quenching medium is quenching oil. Cooling to room temperature, washing, and deep cooling in a deep cooling tank at-90 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
Example 3
(1) Pretreatment of raw materials
Carrying out wet ball milling on Cr powder, La powder and Y powder serving as raw materials in absolute ethyl alcohol under the protection atmosphere of nitrogen, wherein the grinding balls are made of hard alloy, the ball-material mass ratio is 5:1, and the ball milling time is 24 hours. Drying in mixed gas of nitrogen and oxygen after ball milling, wherein the content of oxygen is 2 vol.%, the drying time is 6h, and the drying temperature is 60 ℃;
(2) ball milling and mixing of raw materials
Weighing raw material powder in corresponding mass percentage except Cr powder, La powder and Y powder according to the formula, adding 0.4% of carbon black and 5% of paraffin which are additionally added, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 4:1, the ball milling time is 72h, and the ball milling rotating speed is 100 rpm. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the obtained slurry, and continuously performing ball milling and mixing, wherein a ball milling medium is alcohol, a protective atmosphere is nitrogen, a milling ball is hard alloy, the ball-material ratio is 1:1, and the ball milling time is 24 hours. Drying the ball-milled mixture by using a vacuum oven at the drying temperature of 80 ℃ for 6 h;
(3) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 200MPa to obtain a hollow cylindrical pressed blank;
(4) sintering of
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1200 ℃, the heat preservation time is 3h, and cooling to obtain a sintered blank;
(5) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and insulating for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1190 ℃, the insulating time is 60min, and the quenching medium is quenching oil. Cooling to room temperature, cleaning, and deep cooling in a deep cooling tank at-90 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
Example 4
(1) Pretreatment of raw materials
Carrying out wet ball milling on Cr powder, La powder and Y powder serving as raw materials in absolute ethyl alcohol under the protection atmosphere of nitrogen, wherein the grinding balls are made of hard alloy, the ball-material mass ratio is 5:1, and the ball milling time is 36 hours. Drying in mixed gas of nitrogen and oxygen after ball milling, wherein the content of oxygen is 1 vol.%, the drying time is 8h, and the drying temperature is 60 ℃;
(2) ball milling and mixing of raw materials
Weighing raw material powder in corresponding mass percentage except Cr powder, La powder and Y powder according to the formula, adding additionally added 0.3% of carbon black and 6% of paraffin, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 5:1, the ball milling time is 60 hours, and the ball milling rotating speed is 80 rpm. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the obtained slurry, continuously performing ball milling and mixing, wherein a ball milling medium is alcohol, a protective atmosphere is nitrogen, a milling ball is hard alloy, the ball-material ratio is 2:1, and the ball milling time is 12 hours. The drying temperature is 80 ℃, and the drying time is 8 hours;
(3) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 140MPa to obtain a hollow cylindrical pressed blank;
(4) sintering
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1190 ℃, the heat preservation time is 4 hours, and cooling to obtain a sintered blank;
(5) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and insulating for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1200 ℃, the insulating time is 60min, and the quenching medium is quenching oil. Cooling to room temperature, cleaning, and deep cooling in a deep cooling tank at-180 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
Example 5
(1) Pretreatment of raw materials
Carrying out wet ball milling on Cr powder, La powder and Y powder serving as raw materials in absolute ethyl alcohol under the protection atmosphere of nitrogen, wherein the grinding balls are made of hard alloy, the ball-material mass ratio is 5:1, and the ball milling time is 36 hours. Drying in mixed gas of nitrogen and oxygen after ball milling, wherein the content of oxygen is 1 vol.%, the drying time is 8h, and the drying temperature is 55 ℃;
(2) ball milling and mixing of raw materials
Weighing raw material powder in corresponding mass percentage except Cr powder, La powder and Y powder according to the formula, adding additionally added 0.4% of carbon black and 5% of paraffin, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 6:1, the ball milling time is 66h, and the ball milling rotating speed is 100 rpm. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the obtained slurry, continuously performing ball milling and mixing, wherein a ball milling medium is alcohol, the protective atmosphere is nitrogen, a milling ball is hard alloy, the ball-material ratio is 2:1, the ball milling time is 12 hours, drying is performed by adopting a vacuum oven after ball milling, the drying temperature is 80 ℃, and the drying time is 8 hours;
(3) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 180MPa to obtain a hollow cylindrical pressing blank;
(4) sintering
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1180 ℃, the heat preservation time is 3 hours, and cooling to obtain a sintered blank;
(5) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and preserving heat for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1200 ℃, the heat preservation time is 60min, and the quenching medium is quenching oil. Cooling to room temperature, cleaning, and deep cooling in a deep cooling tank at-90 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
Comparative examples 1, 2 and 3 were prepared by the same procedure as in example 3.
Comparative example 4
(1) Pretreatment of raw materials
Carrying out wet ball milling on Cr powder, La powder and Y powder serving as raw materials in absolute ethyl alcohol under the protection atmosphere of nitrogen, wherein the grinding balls are made of hard alloy, the ball-material mass ratio is 5:1, and the ball milling time is 36 hours. Drying in mixed gas of nitrogen and oxygen after ball milling, wherein the content of oxygen is 2 vol.%, the drying time is 8h, and the drying temperature is 50 ℃;
(2) ball milling and mixing of raw materials
Weighing raw material powder in corresponding mass percentage except Cr powder, La powder and Y powder according to the formula, adding additionally added 0.4% of carbon black and 5% of paraffin, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 5:1, the ball milling time is 72h, and the ball milling rotating speed is 150 rpm. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the obtained slurry, continuously performing ball milling and mixing, wherein a ball milling medium is alcohol, a protective atmosphere is nitrogen, a milling ball is hard alloy, the ball-material ratio is 2:1, and the ball milling time is 12 hours. Drying the ball-milled mixture by using a vacuum oven at the drying temperature of 75 ℃ for 8 h;
(3) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 150MPa to obtain a hollow cylindrical pressing blank;
(4) sintering
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1150 ℃, the heat preservation time is 3 hours, and cooling to obtain a sintered blank;
(5) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and insulating for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1190 ℃, the insulating time is 60min, and the quenching medium is quenching oil. Cooling to room temperature, cleaning, and deep cooling in a deep cooling tank at-90 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
Comparative example 5
(1) Ball milling and mixing of raw materials
Weighing raw material powder according to the corresponding mass percentage, adding 0.4 percent of carbon black and 5 percent of paraffin which are additionally added, and putting the mixture into a ball milling tank for roller ball milling. In the ball milling process, the ball milling medium is alcohol, the protective atmosphere is nitrogen, the milling balls are hard alloy, the ball-material ratio is 4:1, the ball milling time is 72h, and the ball milling rotating speed is 100 rpm. Drying the ball-milled mixture by using a vacuum oven at the drying temperature of 80 ℃ for 6 h;
(2) press forming
Placing the ball-milling mixture obtained in the step (1) in a cold isostatic pressing mould, and performing cold isostatic pressing at 200MPa to obtain a hollow cylindrical pressing blank;
(3) sintering
Putting the cold isostatic pressing blank obtained in the step (2) into a sintering furnace, and vacuumizing until the air pressure is lower than 10-2After Pa, starting sintering, wherein the maximum sintering temperature is 1200 ℃, the heat preservation time is 3h, and cooling to obtain a sintered blank;
(4) thermal treatment
And (4) carrying out heat treatment on the sintered blank obtained in the step (3) under the protection of nitrogen, preheating and insulating for 30min at the temperature of 600 ℃ and 800 ℃, wherein the quenching temperature is 1190 ℃, the insulating time is 60min, and the quenching medium is quenching oil. Cooling to room temperature, cleaning, and deep cooling in a deep cooling tank at-90 deg.C for 120 min. And taking out the sample after the deep cooling is finished, tempering the product for three times after the temperature is returned to the room temperature, wherein the tempering temperature is 250 ℃, and obtaining a finished product after the heat treatment is finished.
And (3) performance detection:
the sampling pins prepared in the examples and the comparative examples are subjected to performance detection. Table 2 shows hardness, flexural strength, impact toughness, wear resistance and corrosion resistance data of the materials prepared in the examples and comparative examples. The specific wear resistance of the wear resistance is characterized by the wear amount in reciprocating type friction wear, a pairing part is a YG8 hard alloy ball, the load is 80N, the reciprocating rate is 3600mm/min, and the test time is 10 min; the corrosion resistance is characterized by the self-corrosion current density in a 3.5 wt% NaCl solution.
TABLE 2 results of performance test of examples and comparative examples
From table 2, it can be seen that the stainless powder metallurgy high-speed steel for wet rotary die cutter roll prepared by the technical route of the present invention has excellent corrosion resistance and excellent toughness and wear resistance through comparison of the performances of the examples and the comparative examples. Components which are not in the component range of the invention may cause the reduction of material compactness and mechanical property due to improper content of alloy elements, insufficient sintering activity and other factors.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention.
From the microstructure morphology of the stainless high-speed steel prepared in example 3 of fig. 1, it can be observed that carbides are uniformly distributed in the material matrix, and the size of the carbides is less than 5 μm.
Claims (10)
1. The utility model provides a high-speed steel of wet-type rotary die cutter roller stainless powder metallurgy which characterized in that:
when the high-speed steel is prepared, the used raw materials comprise the following components in percentage by mass: mo22-5% of C, 3-5% of VC, 2-5% of Co, 18-25% of Cr, 1-2% of NbC, 1-2% of WC, 0.05-0.5% of La and Y, and the balance of Fe, wherein the sum of the mass percentages of the raw materials is 100%; the Cr powder, the La powder and the yttrium powder are subjected to wet ball milling and are dried under the condition of containing oxygen, and finally are introduced into the high-speed steel through mixing and sintering; said oxygen-containing conditions refer to conditions wherein the oxygen content is greater than 0 and less than 4 vol.%;
the carbide size in high speed steel is less than 5 μm.
2. The stainless powder metallurgy high speed steel for wet rotary die cutter roll according to claim 1, wherein: the powder is synthesized by a powder metallurgy method to achieve the near-net forming effect, the purity of the prepared raw materials is more than 99.8 percent, and the average grain diameter of each raw material powder is less than 5 mu m.
3. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 1 to 2, characterized in that: the method comprises the following steps:
(1) pretreatment of raw materials
Carrying out wet ball milling on raw materials Cr powder, La powder and Y powder for a certain time, and drying in an atmosphere A to obtain pretreated Cr powder, La powder and Y powder; said atmosphere a contains 1-3.5 vol.% oxygen;
(2) ball milling and mixing of raw materials
Weighing raw material powder with corresponding mass percentage except Cr powder, La powder and Y powder according to a formula, additionally adding carbon black and a forming agent according to a proportion, and performing ball milling and mixing for a certain time through wet ball milling to obtain mixed slurry. Adding the Cr powder, the La powder and the Y powder pretreated in the step (1) into the slurry, continuing to perform ball milling mixing under certain conditions, and drying the final mixed slurry in a vacuum oven to obtain a ball milling mixture;
(3) press forming
Placing the ball-milling mixture obtained in the step (2) into a die, and pressing to obtain a cold-pressed blank;
(4) sintering
Putting the cold-pressed blank obtained in the step (3) into a sintering furnace for vacuum sintering, and cooling to obtain a sintered blank; the temperature of vacuum sintering is 1180-1260 ℃;
(5) thermal treatment
And (4) preheating the sintered blank obtained in the step (4), then carrying out high-temperature quenching, carrying out deep cooling treatment after quenching and cleaning, carrying out multiple tempering treatments after the deep cooling product naturally returns to the room temperature, and obtaining a finished product after the heat treatment is finished.
4. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 3, wherein: in the step (1), the wet ball milling medium is absolute ethyl alcohol, ball milling is protected by inert gas atmosphere, the adopted milling balls can be hard alloy or steel balls, the ball-material ratio is (4-8): 1, and the ball milling time is 24-36 h.
5. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 3, characterized in that: in the step (1), drying is carried out in an atmosphere A, the drying temperature is 50-60 ℃, the atmosphere A is a mixed gas of nitrogen and oxygen, the content of the oxygen is 1-3 vol.%, and the drying time is 4-8 h.
6. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 3, characterized in that: in the step (2), the amount of the carbon black additionally added is 0.3-0.9 wt.%;
in the step (2), the addition amount of the forming agent is 4-6 wt.%.
7. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 3, wherein: in the step (2), the wet ball milling medium is absolute ethyl alcohol, ball milling is protected by inert gas atmosphere, the adopted milling balls can be hard alloy or steel balls, roller ball milling is preferably adopted in consideration of batch production, and the rotating speed is 60-100 rpm.
8. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 7, wherein: in the step (2), the mass ratio of the primary ball-milling ball material is (4-8) to 1, and the ball-milling time is 36-64 h; after the pretreated Cr powder, La powder and Y powder are added, the mass ratio of the secondary ball-milling ball material is adjusted to 1:1, and the ball-milling time is 12-24 h.
9. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 3, characterized in that:
in the step (2), drying is carried out in a vacuum drying oven, and the drying air pressure is 10000-20000 Pa.
In the step (3), the pressing pressure is 100-250 MPa;
in the step (4), a vacuum sintering mode is adopted, and the air pressure in the sintering process is 10-210Pa, 1180 to 1250 ℃ of the highest sintering temperature and 2 to 4 hours of heat preservation time.
10. The method for preparing stainless powder metallurgy high-speed steel for wet rotary die cutter roller according to claim 3, characterized in that: in the step (5), the quenching temperature is 1170-1220 ℃, the quenching heat preservation time is 30-120 min, the quenching is carried out in salt bath or under the protection of atmosphere, and the medium is selected as quenching oil; the deep cooling temperature is-180 ℃ to-60 ℃, and the deep cooling time is 60-240 min; the tempering temperature is 540-570 ℃, the tempering process is tempering for three times, each time is 50-90min, preferably 55-65min, and the tempering is naturally cooled to the room temperature after each time.
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