CN113458384B - Modified stainless steel powder injection molding feed and preparation method thereof - Google Patents
Modified stainless steel powder injection molding feed and preparation method thereof Download PDFInfo
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Abstract
The invention provides a modified stainless steel powder injection molding feed and a preparation method thereof, wherein the injection molding feed comprises 92-95 parts of modified stainless steel powder, 3-4.5 parts of graft polymer and 2-3.5 parts of paraffin by mass. The synthesized polyacrylate type hyperdispersant with carboxyl is used for modifying the stainless steel powder, the carboxyl of the anchoring group of the hyperdispersant can generate interaction with the hydroxyl on the surface of the stainless steel powder to form tight connection, and the solvation chain of the hyperdispersant can generate steric hindrance effect between the powders, improve the agglomeration of the powders and ensure that the powders can be uniformly mixed when being fed and mixed. Meanwhile, the acrylate solvation chain interacts with a graft polymer side chain during mixing, so that the compatibility of the feeding component is improved.
Description
Technical Field
The invention belongs to the technical field of metal powder injection molding, and particularly relates to a modified stainless steel powder injection molding feed and a preparation method thereof.
Background
Metal Powder Injection Molding (MIM for short) is a net Molding technique for rapidly manufacturing parts with complex geometric shapes by using Metal Powder, has the characteristics of high precision, uniform tissue, excellent performance, low production cost and the like compared with the traditional process, and products of the Metal Powder Injection Molding are widely applied to the industrial fields of electronic information engineering, biomedical instruments, office equipment, automobiles, machinery, weapons, aerospace and the like.
Metal powder injection molding has developed a variety of binder systems, but the differences in properties are large. Wax-based systems are often used as the main component of thermoplastic systems due to their low melting point and viscosity, good wettability and short molecular chain; the water-soluble binder uses water as a solvent, is an environment-friendly binder, but has low powder loading capacity and is easy to deform a blank; the gel binder system has high degreasing rate, but has poor mechanical strength and shape retention of green bodies. Thermoplastic binders have been widely used because of their better flowability and moldability.
Because the compatibility between the high molecular components in the binder and the powder is poor, and the problem of powder agglomeration in the mixing process of the feeding materials has influence on the shape retention of the final product. Therefore, the problems of improving powder agglomeration, increasing the fluidity and feeding density of feeding components, reducing the defect of inner hole of a green body and simultaneously improving the strength of the green body are urgently needed to be solved.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention provides a modified stainless steel powder injection molding feedstock and a method for preparing the same, wherein a polyacrylate type hyperdispersant is used to perform a surface modification treatment on stainless steel powder, and then the stainless steel powder subjected to the surface modification treatment is combined with a graft polymer binder, so as to improve the agglomeration problem of the stainless steel powder and increase the compatibility and fluidity between the powder and the binder.
In order to achieve the above objects and other objects, the present invention provides a modified stainless steel powder injection molding feed material, comprising, by mass, 92 to 95 parts of modified stainless steel powder, 3 to 4.5 parts of a graft polymer, and 2 to 3.5 parts of paraffin.
Preferably, the modified stainless steel powder is a modified stainless steel powder modified with a hyperdispersant comprising a carboxyl anchoring group and a polyacrylate solvating chain.
Preferably, the hyperdispersant is prepared by reacting an acrylate monomer, a functional monomer containing carboxyl, N-dimethylformamide, an initiator of azobisisobutyronitrile and a chain transfer agent of dodecanethiol.
Preferably, the graft polymer is one of polyethylene grafted glycidyl methacrylate, polyethylene grafted maleic anhydride, polypropylene grafted glycidyl methacrylate and polypropylene grafted maleic anhydride.
In addition, the invention also provides a preparation method of the modified stainless steel powder injection molding feed, which comprises the following steps:
s1, mixing and copolymerizing an acrylate monomer, a functional monomer containing carboxyl and N, N-dimethylformamide to obtain a hyperdispersant;
s2, treating the surface of the stainless steel powder by using a hyper-dispersant to obtain modified stainless steel powder;
s3, placing the graft polymer, the paraffin and the modified stainless steel powder into an internal mixer for mixing to obtain the modified stainless steel powder injection molding feed. Preferably, the dispersant is an anionic polymer compound.
Preferably, step S1 comprises:
s11, fully mixing an acrylate monomer, a functional monomer containing carboxyl and N, N-dimethylformamide to obtain a mixture;
s12, dividing the mixture into two parts, adding one part of the mixture into a three-neck flask, introducing nitrogen to discharge air, adding an initiator azobisisobutyronitrile and a chain transfer agent dodecanethiol into the other part of the mixture, slowly dropping the mixture into the three-neck flask through a constant pressure funnel, and reacting at the constant temperature of 70-80 ℃ for 7-8 hours to obtain a reaction product;
s13, adding the reaction product into methanol and deionized water, precipitating a polymer, washing the polymer by the methanol and the deionized water, and drying to obtain the hyperdispersant.
Preferably, step S2 comprises:
s21, adding 100 parts by mass of stainless steel powder into a high-speed mixer;
s22, adding 0.3-1.0 part by mass of hyperdispersant into acetone for dissolving to obtain a solution of polyacrylate type hyperdispersant;
s23, when the temperature of the stainless steel powder reaches 110-120 ℃, uniformly adding the solution of the polyacrylate type hyper-dispersant into a high-speed mixer for three times to be mixed with the stainless steel powder, and taking out the stainless steel powder after mixing for 30-60 min to obtain the hyper-dispersant modified stainless steel powder.
Preferably, the rotating speed of the internal mixer is 50 to 100rmp in the mixing process.
Preferably, the mixing temperature is 160 to 190 ℃.
Preferably, the mixing time is 15 to 30min.
As mentioned above, the modified stainless steel powder injection molding feed of the invention has the following beneficial effects:
firstly, the stainless steel powder modified by the hyper-dispersant and the graft polymer binder are used as raw materials to prepare the feed for the injection molding of the stainless steel powder, in the process of modifying the stainless steel powder by the hyper-dispersant, the anchoring group carboxyl of the hyper-dispersant interacts with the hydroxyl on the stainless steel powder to be tightly connected, and the hyper-dispersant is coated on the surface of the powder, so that the agglomeration phenomenon among the powder can be effectively improved, and the dispersion uniformity of the powder in the binder is improved.
In the injection molding feeding process of the stainless steel powder modified by the hyperdispersant and the graft polymer for preparing the modified stainless steel powder, the solvating chain of the hyperdispersant has steric hindrance in the binder, the powder is dispersed more uniformly during mixing, and the solvating chain can interact with the side chain of the graft polymer, so that the interface binding force between the two phases is improved, the compatibility of the feeding components is improved, and the mechanical property of a blank is improved.
Thirdly, the loading volume ratio of the feed prepared by the invention for injection molding of the modified stainless steel powder is 63-65%, the melt index is 33.6-36.8 g/10min (150 ℃,5 kg), the bending modulus of a green body prepared by the feed reaches 1911-2136 MPa, and the density of the green body reaches 4.30-4.41 g/cm < 3 >. The components of the invention are mutually matched, and the purpose of improving the green body performance is achieved on the premise of ensuring good fluidity of the feeding material.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1: the invention relates to a flow chart of a preparation method of modified stainless steel powder injection molding feed.
FIG. 2 is a schematic diagram: the invention discloses a structural schematic diagram of modified stainless steel powder injection molding feed.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs and the description of the present invention, and any methods, apparatuses, and materials similar or equivalent to those described in the examples of the present invention may be used to practice the present invention.
Note that "%" and "part(s)" shown in the description herein mean "% by mass" and "part(s) by mass", respectively, unless otherwise specified.
The invention provides a modified stainless steel powder injection molding feed, which comprises 92-95 parts by mass of modified stainless steel powder, 3-4.5 parts by mass of graft polymer and 2-3.5 parts by mass of paraffin.
In a particular embodiment, the stainless steel powder may be modified with a hyperdispersant, such as, more specifically, a polyacrylate type hyperdispersant including a carboxyl anchoring group and a polyacrylate solvating chain, to provide a modified stainless steel powder. When the hyper-dispersant is used for treating the surface of the stainless steel powder, the carboxyl anchoring group of the hyper-dispersant interacts with the hydroxyl on the stainless steel powder to be tightly connected, and the hyper-dispersant is coated on the surface of the stainless steel powder, so that the agglomeration phenomenon among the stainless steel powder can be effectively improved, and the dispersion uniformity of the stainless steel powder in the binder is improved. Meanwhile, in the reaction process with the graft polymer, the solvating chain of the hyperdispersant has steric hindrance in the binder, so that the powder is dispersed more uniformly during mixing; the solvated chains can also interact with the side chains of the graft polymer, and the interfacial bonding force between two phases is improved, so that the compatibility of the feeding components is improved, and the mechanical property of a blank body is improved.
In a specific embodiment, the graft polymer is one of polyethylene grafted glycidyl methacrylate, polyethylene grafted maleic anhydride, polypropylene grafted glycidyl methacrylate, and polypropylene grafted maleic anhydride. For example, polyethylene grafted glycidyl methacrylate may be used, and polypropylene grafted glycidyl methacrylate may be used.
The modified stainless steel powder injection molding feed of the invention can be prepared by the following steps:
s1, mixing and copolymerizing an acrylate monomer, a functional monomer containing carboxyl and N, N-dimethylformamide to obtain the hyperdispersant.
And S2, treating the surface of the stainless steel powder by using a hyper-dispersant to obtain the modified stainless steel powder.
S3, placing the graft polymer, the paraffin and the modified stainless steel powder into an internal mixer for mixing to obtain the modified stainless steel powder injection molding feed.
In a specific embodiment, in step S1, the process of obtaining the hyperdispersant may specifically include the following steps, for example.
S11, fully mixing an acrylate monomer, a functional monomer containing carboxyl and N, N-dimethylformamide to obtain a mixture.
S12, dividing the mixture into two parts, adding one part of the mixture into a three-neck flask, introducing nitrogen to discharge air, adding an initiator azobisisobutyronitrile and a chain transfer agent dodecanethiol into the other part of the mixture, slowly dropping the mixture into the three-neck flask through a constant pressure funnel, and reacting at the constant temperature of 70-80 ℃ for 7-8 hours to obtain a reaction product.
S13, adding the reaction product into methanol and deionized water, precipitating a polymer, washing the polymer by the methanol and the deionized water, and drying to obtain the hyperdispersant. The reaction product may be added to the methanol and deionized water by, for example, dropwise adding sufficient methanol and deionized water to ensure complete precipitation of the reaction product. The polymer washing process with methanol and deionized water can be repeated in multiple washes. The polymer may be dried, for example, in a vacuum oven at a temperature of, for example, 60 to 80 ℃ and, specifically, 60 ℃/70 ℃/80 ℃ or the like for a time of, for example, 6 to 24 hours and, specifically, 6h/12h/18h/24h or the like.
In a specific embodiment, in the step S2, the process of obtaining the modified stainless steel powder may specifically include the following steps, for example.
S21, adding 100 parts by mass of stainless steel powder into a high-speed mixer.
S22, adding 0.3-1.0 part by mass of the hyper-dispersant into acetone for dissolving to obtain a solution of the polyacrylate type hyper-dispersant.
S23, when the temperature of the stainless steel powder reaches 110-120 ℃, uniformly adding the solution of the polyacrylate type hyper-dispersant into a high-speed mixer for three times to be mixed with the stainless steel powder, and taking out the stainless steel powder after mixing for 30-60 min to obtain the hyper-dispersant modified stainless steel powder.
In a specific embodiment, in step S3, the rotational speed of the mixer during mixing may be 50 to 100rmp, such as 50rmp/60rmp/70rmp/80rmp/90rmp/100 rmp. The kneading temperature may be 160 to 190 ℃ such as 160 ℃/170 ℃/180 ℃/190 ℃. The kneading time may be 15 to 30min, for example, 15min/20min/25min/30 min.
The invention will now be described by way of the following examples.
The sources of materials used in the following examples are illustrated below: the raw materials of the present invention other than the hyperdispersant used are commercially available, for example, the 17-4PH stainless steel powder used in the present invention is manufactured by Sandvik Osprey, UK, and the high density polyethylene grafted glycidyl methacrylate is manufactured by DuPont, dow, USA. The other raw materials are common materials which are known and used, and can be produced by manufacturers and purchased in various ways.
Example 1
A modified stainless steel powder injection molding feed is prepared by the following steps:
(1) Preparation of the Hyperdispersant
After 7.2g (7.7 wt%) of Acrylic Acid (AA), 30g (32.1 wt%) of Methyl Methacrylate (MMA), 6.4g (6.8 wt%) of Butyl Acrylate (BA) and 50g (53.4 wt%) of N, N-Dimethylformamide (DMF) solvent were weighed out by an electronic balance and mixed uniformly, two portions were prepared for use, one portion of the mixture was put into a three-necked flask equipped with a stirrer and a condenser, and nitrogen was introduced for 20 minutes to discharge air, and 0.872g of azobisisobutyronitrile (AIBN, 2% by mass of the monomer used and 0.436g of dodecanethiol as a chain transfer agent (TDDM, 1% by mass of the monomer used) were added to the other portion of the mixture, and then slowly dropped into the three-necked flask through a constant pressure funnel and reacted in an oil bath at a constant temperature of 80 ℃ for 7 hours to obtain a reaction product. After the reaction is finished, methanol and deionized water are used as precipitating agents, and the reaction product is dropwise added into sufficient methanol and deionized water to precipitate a polymer. And washing the polymer for multiple times by using methanol and deionized water, and then carrying out vacuum drying for 12 hours in a vacuum drying oven at 70 ℃ to obtain the polyacrylate type hyperdispersant.
(2) Preparation of modified stainless Steel powder
Adding 100 parts by mass of stainless steel powder into a high-speed mixer, adding 0.4 part by mass of hyperdispersant into a certain amount of acetone for dissolving to obtain an acetone solution of polyacrylate type hyperdispersant, uniformly adding the acetone solution of polyacrylate type hyperdispersant into the high-speed mixer for three times when the temperature of the stainless steel powder reaches 110 ℃, mixing with the stainless steel powder, taking out the stainless steel powder after mixing for 30min, and obtaining the modified stainless steel powder modified by the hyperdispersant.
(3) Preparing modified stainless steel powder injection molding feed
241.721g of modified stainless steel powder, 8.841g of high-density polyethylene grafted glycidyl methacrylate and 5.367g of paraffin are added into an internal mixer, the set rotating speed is 50rpm, and the mixture is mixed for 15min at 160 ℃, so as to obtain the injection molding feed consisting of the hyper-dispersant modified stainless steel powder and the adhesive containing the grafted polymer.
Example 2
A modified stainless steel powder injection molding feed is prepared by the following steps:
(1) Preparation of the Hyperdispersant
10.8g (11.7 wt%) of Acrylic Acid (AA), 25g (27.1 wt%) of Methyl Methacrylate (MMA), 6.4g (7.0 wt%) of Butyl Acrylate (BA) and 50g (54.2 wt%) of N, N-Dimethylformamide (DMF) solvent were weighed using an electronic balance, mixed uniformly and divided into two portions for use, one portion of the mixture was put into a three-necked flask equipped with a stirrer and a condenser, and nitrogen was introduced for 20 minutes to discharge air, and 0.844g of azobisisobutyronitrile (AIBN, 2% by mass of the monomer used and 0.422g of a chain transfer agent dodecanethiol (TDDM, 1% by mass of the monomer used) were added to the other portion of the reaction, and then slowly dropped into the three-necked flask through a constant pressure funnel, and reacted in an oil bath at 80 ℃ for 7 hours to obtain a reaction product. After the reaction is finished, methanol and deionized water are used as precipitating agents, and the reaction product is dropwise added into sufficient methanol and deionized water to precipitate a polymer. And washing the polymer for multiple times by using methanol and deionized water, and then carrying out vacuum drying for 12 hours in a vacuum drying oven at 70 ℃ to obtain the polyacrylate type hyperdispersant.
(2) Preparation of modified stainless Steel powder
Adding 100 parts by mass of stainless steel powder into a high-speed mixer, adding 0.6 part by mass of hyper-dispersant into a certain amount of acetone for dissolving to obtain an acetone solution of polyacrylate type hyper-dispersant, uniformly adding the acetone solution of polyacrylate type hyper-dispersant into the high-speed mixer for three times when the temperature of the stainless steel powder reaches 110 ℃, mixing with the stainless steel powder for 45min, taking out the stainless steel powder, and obtaining the hyper-dispersant modified stainless steel powder.
(3) Preparing modified stainless steel powder injection molding feed
240.574g of modified stainless steel powder, 9.341g of high-density polyethylene grafted glycidyl methacrylate and 5.649g of paraffin are added into an internal mixer, the set rotating speed is 50rpm, and the mixture is mixed for 20min at 170 ℃, so that the modified stainless steel powder injection molding feed consisting of the hyperdispersant modified stainless steel powder and the adhesive containing the grafted polymer is obtained.
Example 3
A modified stainless steel powder injection molding feed is prepared by the following steps:
(1) Preparation of the Hyperdispersant
14.4g (15.9 wt%) of Acrylic Acid (AA), 20g (22.0 wt%) of Methyl Methacrylate (MMA), 6.4g (7.0 wt%) of Butyl Acrylate (BA) and 50g (55.1 wt%) of N, N-Dimethylformamide (DMF) solvent were weighed out using an electronic balance, mixed uniformly and divided into two portions for use, one portion of the mixture was put into a three-necked flask equipped with a stirrer and a condenser, and nitrogen was introduced for 20 minutes to discharge air, and 0.816g of azobisisobutyronitrile (AIBN, 2% by mass of the monomer used and 0.408g of dodecylmercaptan (TDDM, 1% by mass of the monomer used) as an initiator were added to the other portion of the reaction mixture, and then slowly dropped into the three-necked flask through a constant pressure funnel, and reacted in an oil bath at 80 ℃ for 7 hours to obtain a reaction product. After the reaction is finished, methanol and deionized water are used as precipitating agents, and the reaction product is dropwise added into sufficient methanol and deionized water to precipitate a polymer. And washing the polymer for multiple times by using methanol and deionized water, and then carrying out vacuum drying for 12 hours in a vacuum drying oven at 70 ℃ to obtain the polyacrylate type hyperdispersant.
(2) Preparation of modified stainless Steel powder
Adding 100 parts by mass of stainless steel powder into a high-speed mixer, adding 0.8 part by mass of hyperdispersant into a certain amount of acetone for dissolving to obtain an acetone solution of polyacrylate type hyperdispersant, uniformly adding the acetone solution of polyacrylate type hyperdispersant into the high-speed mixer for three times when the temperature of the stainless steel powder reaches 120 ℃, mixing with the stainless steel powder, taking out the stainless steel powder after mixing for 60min, and obtaining the modified stainless steel powder modified by the hyperdispersant.
(3) Preparing modified stainless steel powder injection molding feed
239.616g of modified stainless steel powder, 9.830g of high-density polyethylene grafted glycidyl methacrylate and 5.944g of paraffin are added into an internal mixer, the set rotating speed is 50rpm, and the mixture is mixed for 25min at 180 ℃ to obtain the modified stainless steel powder injection molding feed consisting of the hyper-dispersant modified stainless steel powder and the adhesive containing the graft polymer.
In order to compare the fluidity of the feed and the improvement degree of the green body performance and the density of the modified stainless steel powder and the binder, the invention also adopts the unmodified stainless steel powder and the binder containing the high-density polyethylene grafted glycidyl methacrylate to prepare the injection molding feed consisting of the unmodified stainless steel powder and the binder in the comparative example, and compares the melt index of the feed prepared by the two preparation methods and the green body performance and the density.
Comparative example
239.616g of unmodified stainless steel powder, 9.830g of high-density polyethylene grafted glycidyl methacrylate and 5.944g of paraffin are added into an internal mixer, the rotating speed is set to be 50rpm, and the mixture is mixed for 25min at 180 ℃ to obtain the stainless steel powder injection molding feed consisting of the unmodified stainless steel powder and the grafted polymer binder.
Performance testing
The melt index (150 ℃,5 kg) and green performance parameters for the modified stainless steel powder injection molding feedstock of hyperdispersant modified stainless steel powder and grafted polymer containing binder of examples 1-3 versus the unmodified stainless steel powder injection molding feedstock of comparative example and grafted polymer binder are shown in table 1.
TABLE 1 feed melt index for injection molding and green body Performance Table for examples 1-3 and comparative examples
| Example 1 | Example 2 | Example 3 | Comparative example | |
| Melt index (g/10 min) | 33.6 | 35.6 | 36.8 | 31.8 |
| Green density (g/cm) 3 ) | 4.30 | 4.36 | 4.41 | 3.91 |
| Flexural modulus (MPa) | 1911 | 2021 | 2136 | 1386 |
As can be seen from the above table, the injection molding feedstock of the hyperdispersant modified stainless steel powder of the present invention with a graft polymer binder improves flowability and improves the properties of the green article compared to the injection molding feedstock of the unmodified stainless steel powder of the comparative example with a graft polymer-containing binder.
The above examples are intended to illustrate the disclosed embodiments of the present invention and are not to be construed as limiting the invention. In addition, various modifications of the methods and compositions of the present invention as set forth herein will be apparent to those skilled in the art without departing from the scope and spirit of the invention. While the invention has been specifically described in connection with various specific preferred embodiments thereof, it should be understood that the invention is not limited to those specific embodiments. Indeed, various modifications of the above-described embodiments which are obvious to those skilled in the art to which the invention pertains are intended to be covered by the scope of the present invention.
Claims (5)
1. A preparation method of a modified stainless steel powder injection molding feed is characterized by comprising the following steps:
fully mixing an acrylate monomer, a functional monomer containing carboxyl and N, N-dimethylformamide to obtain a mixture;
dividing the mixture into two parts, adding one part into a three-neck flask, introducing nitrogen to discharge air, adding an initiator azodiisobutyronitrile and a chain transfer agent dodecanethiol into the other part, slowly dropping the mixture into the three-neck flask through a constant-pressure funnel, and reacting at the constant temperature of 70-80 ℃ for 7-8h to obtain a reaction product;
adding the reaction product into methanol and deionized water, precipitating a polymer, washing the polymer by the methanol and the deionized water, and drying to obtain a hyper-dispersant;
treating the surface of the stainless steel powder with a hyperdispersant to obtain modified stainless steel powder, wherein the hyperdispersant comprises a carboxyl anchoring group and a polyacrylate solvation chain;
placing the graft polymer, the paraffin and the modified stainless steel powder into an internal mixer for mixing to obtain a modified stainless steel powder injection molding feed;
the material comprises, by mass, 92 to 95 parts of modified stainless steel powder, 3 to 4.5 parts of a graft polymer and 2 to 3.5 parts of paraffin.
2. The method for preparing a modified stainless steel powder injection molding feedstock according to claim 1, wherein the step of obtaining the modified stainless steel powder comprises:
adding 100 parts by mass of stainless steel powder into a high-speed mixer;
adding 0.3 to 1.0 part by mass of a hyper-dispersant into acetone for dissolving to obtain a solution of a polyacrylate type hyper-dispersant;
and when the temperature of the stainless steel powder reaches 110-120 ℃, uniformly adding the solution of the polyacrylate type hyper-dispersant into a high-speed mixer for three times to mix with the stainless steel powder, and taking out the stainless steel powder after mixing for 30-60min to obtain the hyper-dispersant modified stainless steel powder.
3. The method for preparing a modified stainless steel powder injection molding feed as claimed in claim 1, wherein the rotation speed of an internal mixer in the mixing process is 50 to 100rmp.
4. The method for preparing the modified stainless steel powder injection molding feed according to claim 1, wherein the mixing temperature is 160 to 190 ℃.
5. A method for preparing a modified stainless steel powder injection molding feed according to claim 1, wherein the mixing time is 15 to 30min.
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