CN109852871B - Nitrogen-containing steel bonded hard alloy prepared from titanium nitride carbide - Google Patents
Nitrogen-containing steel bonded hard alloy prepared from titanium nitride carbide Download PDFInfo
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Abstract
The nitrogen-containing steel bonded hard alloy is prepared by titanium nitride carbide, wherein a bonding phase in the nitrogen-containing steel bonded hard alloy is steel powder, and a hard phase is titanium nitride carbide powder; the nitrogen-containing steel bonded hard alloy is prepared by uniformly mixing titanium nitride carbide powder and steel powder and then synthesizing the nitrogen-containing steel bonded hard alloy in situ by adopting a powder metallurgy method. The titanium nitride carbide powder is titanium carbonitride powder, or titanium nitride carbide powder and titanium carbide powder are mixed to form titanium nitride carbide powder, or titanium nitride powder, titanium nitride powder and titanium carbide powder are mixed to form titanium nitride carbide powder. The weight ratio of titanium nitride carbide powder to steel powder is as follows: 30-70% of titanium nitride carbide, 68-28% of steel powder and the balance of nitrogen fixation phase. The invention can form steel bonded hard alloy with more compact combination of hard phase and bonding; can produce the steel bonded hard alloy with higher microhardness, lubricity and wear resistance than the traditional steel bonded hard alloy.
Description
Technical Field
The invention relates to a steel bonded hard alloy and a manufacturing method thereof, in particular to a steel bonded hard alloy manufactured by titanium nitride carbide and a manufacturing method thereof. The nitrogen-containing steel-bonded hard alloy prepared from the titanium nitride carbide and the preparation method thereof can obtain the steel-bonded hard alloy which is more compact in combination of hard phase and bonding and has higher microhardness, lubricity and wear resistance. Belongs to the technical field of hard alloy manufacture.
Background
With the increasing investment of infrastructure construction in the world, the demand for steel, cement, gravel and other building materials is also increasing. Because steel bond hard alloy (hereinafter referred to as steel bond alloy) is an excellent material for manufacturing steel wire guide wheels and crusher hammers, people especially have deepened understanding on the steel bond alloy, and the market demand on the steel bond alloy is increased in a blowout mode in recent years.
The steel bonded alloy is a novel wear-resistant material which is mainly prepared by using chromium steel or manganese steel as a bonding phase and titanium carbide or tungsten carbide as a hard phase and adopting a powder metallurgy method. Because tungsten belongs to scarce materials, is expensive and has high density, the tungsten is rarely used in practice, and the steel-bonded alloy on the market generally adopts titanium carbide as a hard phase.
With respect to the binder phase: since titanium carbide has a significant amount of free carbon (typically between 0.2% and 0.6%), the free carbon in titanium carbide changes the properties of the steel if steel powder is used directly as a binder phase. In addition, the components of the steel powder are fixed, the components are not easy to adjust, and the price is high, so the steel powder is not directly used in the actual production, but iron powder, molybdenum powder, nickel powder, ferromanganese powder, ferrochrome powder, ferrovanadium powder, carbon black and the like are in-situ synthesized with the titanium carbide powder, and the existing steel bond alloy production process directly mixes titanium carbide, the iron powder, the nickel powder, the ferromanganese powder, the ferrochrome powder, the molybdenum powder, the carbon black and the like together, and then the mixture is put into a sintering furnace to be in-situ sintered into the steel bond hard alloy after being subjected to glue mixing and press molding.
With respect to the hard phase: titanium carbide has high microhardness, low density and low price, and is an ideal hard phase material for steel bonded alloy. However, titanium carbonitride is known to have higher microhardness, lubricity and wear resistance and to be more wettable by steel substrates as a binder phase. However, one of the main reasons why titanium carbonitride has not been selected as the hard phase material of steel-bonded alloys is that nitrogen has considerable "evasion" during the alloy manufacturing process, which causes the alloy to form large porosity or pores, thereby greatly reducing the service performance of the alloy. Therefore, the problem that titanium carbonitride is used as steel bonding alloy without generating large gaps can be solved, and the steel bonding alloy can be used for overcoming the high quality of steel bonding alloy.
Through searching, the same patent literature reports as the present invention are not found, but some related patent literatures are searched, and the following patents mainly exist:
1. the patent number is CN201710074648, which is named as 'a preparation method of TiC matrix steel-based steel bonded hard alloy', and the applicant is: the invention patent of Danyang huida die material science and technology limited company discloses a preparation method of TiC matrix steel-based steel bonded hard alloy, which comprises the following steps: weighing titanium carbide powder and matrix steel matrix powder according to a ratio, putting the alloy powder into a ball mill for mixing and crushing, adding absolute ethyl alcohol as a process control agent, putting wet mixed powder into a vacuum drying oven for drying after ball milling, and drying for later use. Adding an organic monomer and an initiator into a solvent to prepare a premixed solution; adding an additive for improving the fluidity and the dispersibility of the slurry; adding a catalyst and a pH regulator, and uniformly stirring to obtain slurry; and injecting the slurry into a gel casting mould, vacuumizing or vibrating to remove gas, curing and molding the slurry, then putting the blank into a vacuum drying box for drying, and carrying out integrated degumming and sintering on the dried blank in a vacuum sintering furnace to prepare the steel bond hard alloy.
2. The patent number is CN201711296675, entitled "steel bond hard alloy material and preparation method thereof", filed by: the invention patent of Yangzhou Huixiang precision impact member limited company discloses a steel bond hard alloy material and a preparation method thereof; the components of the composition are as follows: titanium carbide, stearic acid, iron, manganese, vanadium 0.25, chromium, molybdenum, zirconium, nickel, and aluminum; according to the invention, molybdenum, chromium, vanadium and titanium carbide are uniformly mixed and then pressed into a blank, stearic acid is doped into the blank as a filler, metals in the sintered blank are fused together, the blank forms a capillary pipeline in the blank after the stearic acid is evaporated, and molten liquid of manganese, aluminum and nickel enters the blank during infiltration, wherein the manganese and the vanadium are matched for use, so that the defect that the manganese promotes the growth of crystal grains can be overcome by using the vanadium, thereby better embodying the high hardness and the high strength of the alloy, the oxidation resistance and the corrosion resistance of the alloy can be obviously improved by matching the chromium, the zirconium and the aluminum, the service life of the alloy is prolonged, the transverse impact toughness of the alloy can be improved, and the durability of a mold is improved.
3. The patent number is CN201110164167, entitled "preparation method of titanium carbide-based steel bonded hard alloy material", applicant is: the invention patent of Wuxin new material science and technology company limited discloses a titanium carbide-based steel bonded hard alloy material, which takes hard alloy titanium carbide as a hard base, alloy tool steel is used as a binding phase, the mass percent of the titanium carbide is 35-45%, the alloy tool steel comprises 55-65% by mass, the sum of the titanium carbide and the alloy tool steel is 100%, the alloy tool steel comprises chromium, molybdenum, aluminum, nickel, titanium and iron, wherein, the mass percent of chromium is 3.1-18%, the mass percent of molybdenum is 0.5-4.5%, the mass percent of aluminum is 0.6-1%, the mass percent of nickel is 0.6-11%, the mass percent of titanium is 0.5-1%, and the balance is iron and carbon, and the sum of the mass percent of all the components is 100.
Through careful analysis of the above patents, although the patents relate to steel bonded cemented carbide and a manufacturing method thereof, some improved technical solutions have been proposed, through careful analysis, the proposed steel bonded cemented carbide is still an improvement on the existing steel bonded cemented carbide manufactured by titanium carbide, only in the material formulation or process, and no method for manufacturing the steel bonded cemented carbide by nitrogen-containing cemented carbide has been proposed, so that the problems described above still exist, and further research and improvement are still needed.
Disclosure of Invention
The purpose of the invention is: how to solve the problem that titanium nitride carbide is used as steel bond alloy without generating large gaps, provides a steel bond hard alloy which contains sufficient nitrogen, and the formed steel bond hard alloy is nitrogen-containing steel bond hard alloy.
Aiming at the problems, the technical scheme provided by the invention is as follows: a steel bonded hard alloy made of titanium nitride-nitrogen bonded hard alloy. The bonding phase in the nitrogen-containing steel bonded hard alloy is steel, and the hard phase is titanium nitride carbide. The steel bonded hard alloy formed by uniformly mixing titanium nitride carbide powder and steel powder and then carrying out in-situ synthesis together is nitrogen-containing steel bonded hard alloy.
Further, nitrogen of the nitrogen-containing steel-bonded hard alloy exists in the nitrogen-containing steel-bonded hard alloy in a mode of titanium carbonitride, titanium nitride plus titanium carbide, titanium carbonitride plus titanium carbide, titanium nitride plus titanium carbonitride plus titanium carbide and the like.
Further, the titanium nitride carbide is titanium nitride carbide with free carbon less than 0.15% and oxygen content less than 0.6%; the nitrogen-carbon ratio and the content of each in the alloy are adjusted according to the actual application of the product.
Further, the titanium carbonitride powder includes titanium carbonitride powder, or titanium carbonitride powder formed by mixing titanium nitride powder with titanium carbide powder, or titanium carbonitride powder formed by mixing titanium carbonitride powder with titanium carbide powder, or titanium carbonitride powder formed by mixing titanium nitride powder with titanium carbonitride powder with titanium carbide powder.
Further, the weight ratio of the hard phase titanium nitride carbide to the binding phase steel is as follows: the hard phase content interval is 30-70%, the binding phase content interval is 68-28%, and the rest is nitrogen-fixing phase.
Furthermore, the nitrogen fixation phase is niobium powder, and nitrogen is fixed by adding the niobium powder.
Further, the specific adding amount of the niobium powder is determined according to the actual free carbon content of the titanium nitride carbide; after the addition of the niobium powder is determined, the addition of the binder phase is determined.
Furthermore, the adding amount of the niobium powder is 0.5-2% of the weight of the titanium nitride carbide.
Further, the titanium carbide nitride powder and the steel powder are mixed by wet grinding according to the weight ratio of the titanium carbide nitride to the steel powder.
Further, the steel powder is pretreated steel powder as a binding phase; the pretreated steel powder is obtained by dissolving the steel powder in water to fully reduce free carbon in the steel powder.
The invention has the advantages that:
1. the formed nitrogen-containing steel bonded hard alloy contains a proper amount of nitrogen, and after the nitrogen element is added, beta (N) crystal grains are finer than the nitrogen-free beta crystal grains and are distributed in a spherical shape, so that the steel bonded hard alloy has higher strength and toughness compared with the nitrogen-free steel bonded hard alloy.
2. The nitrogen-containing steel bonded hard alloy has a refined structure, so that the oxidation resistance is better than that of the common steel bonded hard alloy. The binder phase is first solutionized to reduce the free carbon content in the steel powder.
3. The nitrogen-containing steel bonded hard alloy is added with a proper amount of niobium powder, the niobium powder can be carbonized by free carbon before the alloy appears in a liquid phase, and simultaneously, the niobium can also react with nitrogen to generate niobium nitride. In this way, the escape of nitrogen is prevented both directly and indirectly.
Detailed Description
The invention is described in one step with reference to the following examples:
examples 1 to 3
The GT type (main mark) steel bonded alloy produced according to the principle of the invention adopts chromium steel powder as a binding phase, titanium carbonitride (or titanium nitride plus titanium carbide, or titanium carbonitride plus titanium carbide, or a mixture of titanium nitride plus titanium carbide, the same later) as a hard phase, titanium carbonitride and chromium steel powder are mixed, and a proper amount of niobium powder is added into the mixture; the weight percentage ratio of the titanium carbonitride to the chromium steel powder to the niobium powder is as follows:
titanium nitride carbide chromium steel powder (self-made) niobium powder
GT30 30 68-69.5 0.5-2
GT35 35 63-64.5 0.5-2
GT40 40 58-59.5 0.5-2
The amount of the niobium powder to be added is determined depending on the actual free carbon content of the hard phase. After the addition of the niobium powder is determined, the addition of the binder phase is determined.
The content of free carbon in the titanium carbonitride should be controlled to be less than 0.15%, and the content of oxygen should be controlled to be less than 0.6%.
When producing the steel bonded hard alloy, the chromium steel powder needs to be subjected to solid solution treatment.
When in production, the binding phase chromium steel powder is firstly dissolved, and the free carbon in the steel powder is fully reduced. Then, titanium carbonitride, chromium steel powder and niobium powder are mixed, wet grinding and pressing are carried out according to the traditional steel bonded alloy technology, and nitrogen-filled atmosphere sintering is adopted to prepare the nitrogen-containing steel bonded hard alloy.
The nitrogen-containing steel bonded hard alloy produced by the method has finer crystal grains and is distributed in a spherical shape, so that the nitrogen-containing steel bonded hard alloy has higher strength and toughness compared with the nitrogen-free steel bonded hard alloy. In addition, the oxidation resistance of the nitrogen-containing steel bonded hard alloy is better than that of the common steel bonded hard alloy.
Examples 4 to 6
The TM (main mark) steel bonded alloy produced according to the principle of the invention adopts manganese steel powder (self-made) as a binding phase, titanium carbonitride as a hard phase, the titanium carbonitride and the manganese steel powder are mixed, and a proper amount of niobium powder is added into the mixture; the weight percentage ratio of the titanium carbonitride to the chromium steel powder to the niobium powder is as follows:
titanium nitride manganese steel powder (self-made) niobium powder
TM30 70 28-29.5 0.5-2
TM52 48 50-51.5 0.5-2
TM60 40 58-59.5 0.5-2
The amount of the niobium powder to be added is determined depending on the actual free carbon content of the hard phase. After the addition of the niobium powder is determined, the addition of the binder phase is determined.
The content of free carbon in the titanium carbonitride should be controlled to be less than 0.15% and less than 0.6% of oxygen.
When producing the steel bond hard alloy, manganese steel powder needs to be subjected to solid solution treatment.
When in production, the binding phase chromium steel powder is firstly dissolved, and the free carbon in the steel powder is fully reduced. Then, titanium carbonitride, chromium steel powder and niobium powder are mixed, wet grinding and pressing are carried out according to the traditional steel bonded alloy technology, and nitrogen-filled atmosphere sintering is adopted to prepare the nitrogen-containing steel bonded hard alloy.
The nitrogen-containing steel bonded hard alloy produced by the method has finer crystal grains, is distributed in a spherical shape, and has higher strength and toughness compared with the nitrogen-free steel bonded hard alloy. In addition, the oxidation resistance of the nitrogen-containing steel bonded hard alloy is better than that of the common steel bonded hard alloy.
The technical standard of the conventional steel bonded alloy (titanium carbide base) grade is compared with the technical index of the steel bonded alloy produced by adopting the titanium carbonitride base (test measured value) as shown in the following table:
it will be apparent that modifications and variations are possible without departing from the principles of the invention as set forth herein.
From the above examples, it can be seen that the present invention relates to a steel-bonded cemented carbide made of titanium carbonitride, in which the binder phase is steel and the hard phase is titanium carbonitride. The steel bonded hard alloy formed by uniformly mixing titanium nitride carbide powder and steel powder and then carrying out in-situ synthesis together is nitrogen-containing steel bonded hard alloy.
Further, nitrogen of the nitrogen-containing steel-bonded hard alloy exists in the nitrogen-containing steel-bonded hard alloy in a mode of titanium carbonitride, titanium nitride plus titanium carbide, titanium carbonitride plus titanium carbide, titanium nitride plus titanium carbonitride plus titanium carbide and the like.
Further, the titanium nitride carbide is titanium nitride carbide with free carbon less than 0.15% and oxygen content less than 0.6%. The nitrogen-carbon ratio and the content of each in the alloy are adjusted according to the actual application of the product.
Further, the titanium carbonitride powder comprises titanium carbonitride powder, or titanium carbonitride powder formed by mixing titanium nitride powder and titanium carbide powder, or titanium carbonitride powder formed by mixing titanium carbonitride powder and titanium carbide powder, or titanium carbonitride powder formed by mixing titanium nitride powder, titanium carbonitride powder and titanium carbide powder.
Further, the weight ratio of the hard phase titanium nitride carbide to the binding phase steel is as follows: the hard phase content interval is 30-70%, the binding phase content interval is 68-28%, and the rest is nitrogen-fixing phase.
Furthermore, the nitrogen fixation phase is niobium powder, and nitrogen is fixed by adding the niobium powder.
Further, the specific addition amount of the niobium powder is determined according to the actual free carbon content of the titanium nitride carbide. After the addition of the niobium powder is determined, the addition of the binder phase is determined.
Furthermore, the adding amount of the niobium powder is 0.5-2% of the weight of the titanium nitride carbide.
Further, the titanium carbide nitride powder and the steel powder are mixed by wet grinding according to the weight ratio of the titanium carbide nitride to the steel powder.
Further, the steel powder is pretreated steel powder as a binding phase. The pretreated steel powder is obtained by dissolving the steel powder in water to fully reduce free carbon in the steel powder. .
The inventor finds that titanium is a hexagonal-face-centered lattice structure through analytical research, and can form intermittent solid solution with hydrogen, carbon, nitrogen, oxygen, boron and the like. Because a certain amount of carbon black (part of carbon black is carried in by a hard phase) needs to be added in the process of in-situ synthesizing the steel, under the thermodynamic driving, high-concentration carbon continuously occupies the position of nitrogen to enable the combined nitrogen to form nitrogen to escape, and thus nitrogen escape is formed (of course, under the thermodynamic driving, the combined carbon can also convert part of the combined nitrogen into nitrogen, which is only very weak and can be ignored).
For this reason, the invention reduces the nitrogen slip to a negligible extent by taking three measures.
1. Firstly, the binding phase is dissolved to fully reduce the free carbon in the steel powder
The liquidus temperature of steel is generally about 1400 degrees (liquidus at eutectic temperature), and if the liquidus temperature occurs, the steel is difficult to break. Therefore, the sintering of the mixed steel powder raw material must be controlled at a temperature at which the raw material is sufficiently tempered but not liquefied. Through a large number of experiments, this temperature control is optimal between 1250 and 1280 degrees.
2. Hard phase selected material
Because the interstitial phase of the titanium carbide only contains carbon, and the process of producing the titanium carbide by using the titanium dioxide has certain reversibility, the control of free carbon is difficult. Titanium carbonitride is not so good, because the interstitial phase is carbon and nitrogen, if the proportion of carbon black and titanium dioxide is well adjusted and the sintering temperature and the nitrogen flow are well controlled during the production of titanium carbonitride, the titanium carbonitride with low oxygen content and low free carbon (less than 0.15%) can be prepared.
3. Adding appropriate amount of niobium powder
Despite the two previous measures, nitrogen escape cannot be completely avoided because a significant portion of the free carbon is still present in the hard and binder phases. Therefore, measures of adding proper niobium powder are taken to fix nitrogen. Because the niobium powder can be carbonized by free carbon before the alloy appears in liquid phase, and niobium can also react with nitrogen to form niobium nitride. In this way, the escape of nitrogen is prevented both directly and indirectly.
4. Nitrogen-filled sintering
Under the multi-atmosphere sintering, the novel method adopts a method of replacing argon with nitrogen for sintering. Therefore, the nitrogen in the alloy body is prevented from escaping due to the high concentration of the nitrogen outside the alloy body, and the surface of the alloy can be fully nitrided.
The invention has the advantages that:
1. the formed nitrogen-containing steel bonded hard alloy contains a proper amount of nitrogen, and after the nitrogen element is added, beta (N) crystal grains are finer than the nitrogen-free beta crystal grains and are distributed in a spherical shape, so that the steel bonded hard alloy has higher strength and toughness compared with the nitrogen-free steel bonded hard alloy.
2. The structure of the nitrogenous steel bonded hard alloy is refined, so that the oxidation resistance is better than that of the common steel bonded hard alloy in that the bonding phase is dissolved in a solid solution, and the free carbon in the steel powder is fully reduced.
The nitrogen-containing steel bonded hard alloy is added with a proper amount of niobium powder, the niobium powder can be carbonized by free carbon before the alloy appears in a liquid phase, and simultaneously, the niobium can also react with nitrogen to generate niobium nitride. In this way, the escape of nitrogen is prevented both directly and indirectly.
Claims (10)
1. The nitrogen-containing steel bonded hard alloy is characterized in that a binding phase in the nitrogen-containing steel bonded hard alloy is steel powder, and a hard phase is titanium nitride powder; after titanium nitride carbide powder and steel powder are uniformly mixed, in-situ synthesis is carried out on the nitrogen-containing steel bonded hard alloy by adopting a powder metallurgy production method; the specific mode is as follows:
1) firstly, the binding phase is dissolved to fully reduce the free carbon in the steel powder
Sintering the mixed steel powder raw material at a temperature at which the raw material is fully toughened but not liquefied; through a large number of experiments, the temperature is controlled to be 1250-1280 ℃;
2) hard phase selected material
When the titanium carbonitride is produced, the proportion of the carbon black and the titanium dioxide is adjusted, the sintering temperature and the nitrogen flow are controlled, and the titanium carbonitride with the oxygen content of less than 0.6 percent and the free carbon of less than 0.15 percent is produced;
3) adding appropriate amount of niobium powder
Adding appropriate niobium powder to fix nitrogen; niobium powder can be carbonized by free carbon before the alloy appears in a liquid phase, and simultaneously, niobium can also react with nitrogen to generate niobium nitride, so that the escape of nitrogen is directly and indirectly prevented;
4) nitrogen-filled sintering
Sintering by adopting a method of replacing argon with nitrogen under multi-atmosphere sintering; the nitrogen in the alloy body is prevented from escaping due to the high concentration of the nitrogen outside the alloy body, and the surface of the alloy can be fully nitrided.
2. The cemented carbide of claim 1, wherein the nitrogen in the cemented carbide is titanium carbonitride, titanium nitride plus titanium carbide, titanium carbide plus titanium carbide, titanium nitride plus titanium carbide, or the like.
3. The cemented carbide made of nitrogen-containing steel bonded with titanium nitride according to claim 2, wherein the titanium nitride is titanium nitride having free carbon of less than 0.15% and oxygen content of less than 0.6%; the nitrogen-carbon ratio and the content of each in the alloy are adjusted according to the actual application of the product.
4. The cemented carbide made of titanium nitride according to claim 2, wherein the titanium nitride powder comprises titanium nitride carbide powder, or titanium nitride carbide powder mixed with titanium carbide powder, or titanium nitride powder mixed with titanium nitride powder, or titanium nitride powder mixed with titanium carbide powder.
5. The cemented carbide with nitrogen-containing steel structure made of titanium carbonitride according to claim 1, wherein the weight ratio of the cemented carbide with titanium carbonitride to the binder phase steel is as follows: the hard phase content interval is 30-70%, the binding phase content interval is 68-28&, and the rest is nitrogen fixing phase.
6. The nitrogen-containing steel-bonded cemented carbide made of titanium carbonitride according to claim 5, wherein the nitrogen fixation phase is niobium powder, and nitrogen is fixed by adding niobium powder.
7. The cemented carbide with a nitrogen-containing steel structure made of titanium carbonitride as claimed in claim 6, wherein the specific addition amount of the niobium powder is determined according to the actual free carbon content of titanium carbonitride; after the addition of the niobium powder is determined, the addition of the binder phase is determined.
8. The cemented carbide with a nitrogen-containing steel structure made of titanium carbonitride as claimed in claim 7, characterized in that the niobium powder is added in an amount of 0.5-2% by weight of titanium carbonitride.
9. The cemented carbide made of titanium nitride according to claim 1, wherein the titanium nitride powder and the steel powder are wet-milled and mixed according to the weight ratio of the titanium nitride to the steel powder.
10. The cemented carbide made of titanium carbonitride containing nitrogen according to claim 1, characterized in that the steel powder is pretreated steel powder as a binder phase. The pretreated steel powder is obtained by dissolving the steel powder in water to fully reduce free carbon in the steel powder.
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