阅读说明：本技术 一种陶瓷模具材料的制备方法 (Preparation method of ceramic mold material ) 是由 不公告发明人 于 2020-06-16 设计创作，主要内容包括：本发明公开了一种陶瓷模具材料的制备方法,属于陶瓷模具材料领域,其制备方法为：将陶瓷模具材料用粉体与去离子水混合均匀,制得混合浆料,将混合浆料置于模具中,静置与干燥,脱模,得到陶瓷模具材料生坯,再经过高温烧结,得到陶瓷模具材料。上述陶瓷模具材料用粉体的制备方法包括：将α-氧化铝粉体、硼酸铝晶须、氧化锡粉体、氧化锆珠粉体、聚氨酯/石棉纳米复合材料粉体在机械研磨作用下研磨均匀,得到陶瓷模具材料用粉体。本发明制备方法所用陶瓷模具材料用粉体分散性好、颗粒均匀,可得到断裂韧性与耐磨性好,高强度与高硬度的陶瓷模具材料。(The invention discloses a preparation method of a ceramic mold material, belonging to the field of ceramic mold materials, and the preparation method comprises the following steps: uniformly mixing the ceramic mold material powder with deionized water to prepare mixed slurry, placing the mixed slurry in a mold, standing, drying and demolding to obtain a ceramic mold material green body, and sintering at high temperature to obtain the ceramic mold material. The preparation method of the powder for the ceramic die material comprises the following steps: and uniformly grinding the alpha-alumina powder, the aluminum borate whisker, the tin oxide powder, the zirconia bead powder and the polyurethane/asbestos nano composite material powder under the mechanical grinding action to obtain the powder for the ceramic mold material. The ceramic die material used by the preparation method has good powder dispersibility and uniform particles, and can obtain the ceramic die material with good fracture toughness and wear resistance, high strength and high hardness.)

1. A preparation method of powder for a ceramic mold material comprises the following steps: and uniformly grinding the alpha-alumina powder, the aluminum borate whisker, the tin oxide powder, the zirconia bead powder and the polyurethane/asbestos nano composite material powder under the mechanical grinding action to obtain the powder for the ceramic mold material.

2. The method for preparing a powder for a ceramic mold material according to claim 1, wherein: the composite material comprises, by weight, 50-70 parts of alpha-alumina powder, 5-10 parts of aluminum borate whisker, 2-7 parts of tin oxide powder, 1-5 parts of zirconia bead powder and 6-10 parts of polyurethane/asbestos nanocomposite powder.

3. The method for preparing a powder for a ceramic mold material according to claim 1, wherein: the particle size of the alpha-alumina powder is 20-50 nm, the particle size of the aluminum borate whisker is 30-90 nm, the particle size of the tin oxide powder is 50-100 nm, the particle size of the zirconia bead powder is 50-90 nm, and the particle size of the polyurethane/asbestos nanocomposite powder is 40-100 nm.

4. The method for preparing a powder for a ceramic mold material according to claim 1, wherein: the mechanical grinding time is 4-6 h.

5. The powder for a ceramic mold material produced by the production method according to any one of claims 1 to 4.

6. A preparation method of a ceramic die material is characterized by comprising the following steps: uniformly mixing the powder for the ceramic mold material of claim 5 with deionized water under the mechanical action to obtain mixed slurry; and placing the mixed slurry into a mold, standing in a closed environment, then placing the mold into an oven for drying and demolding to obtain a ceramic mold material green body, placing the ceramic mold material green body into a high-temperature furnace for sintering, preserving heat, cooling to room temperature, and taking out to obtain the ceramic mold material.

7. The method for preparing a ceramic mold material according to claim 6, wherein: the mass ratio of the powder for the ceramic die material to the deionized water is 1: 4-5.

8. The method for preparing a ceramic mold material according to claim 6, wherein: the mechanical stirring speed is 500-700 r/min, and the stirring time is 0.5-1 h.

9. The method for preparing a ceramic mold material according to claim 6, wherein: the standing time is 1-3 days, the drying temperature is 50-60 ℃, and the time is 9-10 hours.

10. The method for preparing a ceramic mold material according to claim 6, wherein: the heat treatment curve of the ceramic die material green body in a high-temperature furnace is as follows: heating to 1100-1250 ℃ at a heating rate of 7-9 ℃/min, preserving heat for 2.5-3.5 h, cooling to room temperature, and taking out to obtain the ceramic mold material.

Technical Field

The invention belongs to the field of ceramic mold materials, and particularly relates to a preparation method of a ceramic mold material.

Background

At present, the materials applied to the hot working die are mainly divided into die steel and hard alloy. Although the die steel has high strength, the lower hardness and the poorer wear resistance shorten the service life of the die steel. The hard alloy die material developed later is superior to die steel in comprehensive mechanical property and high wear resistance, the service life is greatly prolonged, and the hard alloy die material is widely used in the field of dies. But the development of productivity requires that the die has better high-temperature strength and wear resistance, and the hard alloy material is difficult to adapt to the requirement of actual production. Compared with hard alloy, the cermet material has higher high-temperature strength, wear resistance, corrosion resistance and oxidation resistance, and has wide development prospect in the mold industry. The ceramic material is expensive and inexperienced for production, but with the development of science and technology, the improvement of manufacturing process and the increase of dosage, the cost is necessarily reduced, and the application is becoming more and more extensive, so from a long-term viewpoint, the research of advanced ceramic die material should be undertaken.

The application research of ceramic materials in various moulds is mostly limited to micron-sized composite ceramic materials. In the research aspect of oxide ceramic mould materials, the research of the university of the fertilizer industry shows that: ZrO (ZrO)₂Toughening A1₂O₃The base composite ceramic ZTA can be used for manufacturing wire-drawing dies. As a novel die material, the material is superior to high-speed steel and hard alloy in certain performance, and the fracture toughness and the bending strength respectively reach about 7.2 MPa.m^1/2And 740 MPa. In the prior art, for example, the publication number CN106116618A discloses a preparation method of a low-expansibility composite ceramic mold material, which comprises the steps of crushing straw stalks, extracting fibers by alkaline leaching, mixing and grinding for filling, forming a microporous structure by fermentation, and calcining to prepare a microporous carbon fiber material, wherein when the microporous carbon fiber material is used, the internal microporous carbon fiber is elastically changed, so that the internal stress of the material is improved, the thermal expansion coefficient of the composite ceramic mold material prepared by the invention is obviously reduced, the composite ceramic mold material is reduced by 10-15% compared with the similar ceramic mold material at the same temperature, and the fracture toughness can reach 7.8-9.0 MPa.m^1/2(ii) a And the preparation process is simple, green and environment-friendly, and has no pollution to the environment. Application publication No. CN106747433A discloses a zirconia-based nano ceramic tool and die material and a preparation method thereof, the component comprises yttrium-stabilized nano zirconia as a matrix, micron alumina as a reinforcing phase, micron molybdenum, micron nickel carbonyl and graphene oxide as sintering aids, and the zirconia-based nano ceramic tool and die material is prepared by hot-pressing and sintering; the preparation method comprises the steps of respectively dispersing the nano-zirconia and the micron alumina powder, performing ball milling and drying to obtain powder, and sintering by adopting a hot pressing method. The ceramic tool and die has better comprehensive mechanical property and very high comprehensive mechanical propertyThe material has hardness, wear resistance and heat conductivity, and can be used for manufacturing ceramic tools and dies such as extrusion dies, drawing dies, cutting tools and the like and other wear-resistant and corrosion-resistant parts.

Due to the large performance difference, the die materials of different ceramic systems are limited by the use environment, and the traditional ceramic die materials have poor bending strength and fracture toughness, so that the comprehensive performance is poor, and the use limitation is caused.

Disclosure of Invention

The invention aims to provide a preparation method of a ceramic die material of powder for the ceramic die material, which has good dispersibility and uniform particles, and the ceramic die material has excellent fracture toughness and wear resistance, high strength and high hardness.

The technical scheme adopted by the invention for realizing the purpose is as follows:

a preparation method of powder for a ceramic mold material comprises the following steps: and uniformly grinding the alpha-alumina powder, the aluminum borate whisker, the tin oxide powder, the zirconia bead powder and the polyurethane/asbestos nano composite material powder under the mechanical grinding action to obtain the powder for the ceramic mold material.

Preferably, the weight portion of the composite material is 50-70 portions of alpha-alumina powder, 5-10 portions of sodium borate powder, 2-7 portions of tin oxide powder, 1-5 portions of zirconia bead powder and 6-10 portions of polyurethane/asbestos nano composite material powder.

Preferably, the particle size of the alpha-alumina powder is 20-50 nm, the particle size of the aluminum borate whisker is 30-90 nm, the particle size of the tin oxide powder is 50-100 nm, the particle size of the zirconia bead powder is 50-90 nm, and the particle size of the polyurethane/asbestos nanocomposite powder is 40-100 nm.

Preferably, the preparation method of the polyurethane/asbestos nano composite material powder comprises the following steps:

dissolving 0.02-0.05 part of asbestos nano powder in 95% ethanol solution by weight, performing ultrasonic dispersion for 0.5-1 h to form slurry, then adding 1-3 parts of aqueous polyurethane dispersion, stirring for 1-2 h in a water bath at 50-60 ℃, filtering, drying for 5-8 h in an oven at 65-75 ℃, and grinding to obtain polyurethane/asbestos nano composite material powder; the aqueous polyurethane dispersion (the content is more than or equal to 54-56%) can be obtained commercially.

Preferably, the mechanical grinding time is 5-6 h.

The invention adopts alpha-alumina powder as a base material, and the alpha-alumina powder interacts with aluminum borate whisker, tin oxide powder, zirconia bead powder and polyurethane/asbestos nano composite material powder under the mechanical grinding action to form nano powder with good dispersibility and uniform particles, the mixture of the zirconia bead powder and the polyurethane/asbestos nano composite material powder is added, on one hand, the mixture is easy to dissociate and charge, the surface potential between particles can be improved by being adsorbed on the surface of the powder, the electrostatic repulsion force is increased, meanwhile, the mixture has a macromolecular branched chain structure, the agglomeration is not easy to occur between nano particles, better uniform dispersity is achieved, on the other hand, the abrasion on the surface of the particles can not be caused in the grinding process, the grinding efficiency of the mixed powder is greatly improved, and the powder for the ceramic mold material with good dispersibility and uniform particles is obtained, so as to obtain the ceramic die material with excellent wear resistance and fracture toughness, high strength and high hardness; in addition, the aluminum borate whisker and the tin oxide powder are added, and the two substances have a synergistic effect, so that the effect of refining the grain size of the ceramic die can be better achieved, the toughening and reinforcing effects are achieved, and the fracture toughness, the wear resistance, the strength and the hardness of the ceramic die material are further improved.

The invention also aims to provide a ceramic die material which has good internal particle dispersibility and uniform size, excellent fracture toughness and wear resistance, high strength and high hardness, and is used for the ceramic die material.

The preparation method of the ceramic mold material comprises the steps of uniformly mixing the prepared powder for the ceramic mold material with deionized water under the mechanical action to obtain mixed slurry; and placing the mixed slurry into a mold, standing in a closed environment, then placing the mold into an oven for drying and demolding to obtain a ceramic mold material green body, placing the ceramic mold material green body into a high-temperature furnace for sintering, preserving heat, cooling to room temperature, and taking out to obtain the ceramic mold material.

Preferably, the mass ratio of the powder for the ceramic mold material to the deionized water is 1: 4-5.

Preferably, the mechanical stirring speed is 500-700 r/min, and the stirring time is 0.5-1 h.

Preferably, the standing time is 1-3 days, the drying temperature is 50-60 ℃, and the time is 9-10 hours.

Preferably, the heat treatment profile of the green ceramic mold material in the high temperature furnace is: heating to 1100-1250 ℃ at a heating rate of 7-9 ℃/min, preserving heat for 2.5-3.5 h, cooling to room temperature, and taking out to obtain the ceramic mold material.

In order to further improve the wear resistance and the strength of the ceramic die material, the preferable measures further comprise:

in the process of preparing the mixed slurry, a mixture of palladium chloride and calcium chloride is added, the addition amount of the mixture accounts for 0.5-1% of the total weight of the mixed powder for the ceramic mold material, the weight percentage of the palladium chloride to the calcium chloride is 1: 0.2-0.5, the strength and the hardness of the ceramic mold material are further improved by adding the mixture of the palladium chloride and the calcium chloride, and a layer of palladium oxide film is formed on the surface of the ceramic mold material in the green sintering process of the ceramic mold material, so that the wear resistance of the ceramic mold material is improved.

The obtained ceramic mold material powder and deionized water are stirred and uniformly mixed to obtain mixed slurry, the obtained slurry has good fluidity, internal particles are uniformly dispersed, the slurry can be uniformly attached to a mold after being placed in the mold, a ceramic mold material green compact with a compact structure is formed after standing and drying, and the ceramic mold material with fine grain size, excellent fracture toughness, wear resistance and high strength is obtained through high-temperature sintering.

Compared with the prior art, the powder for the ceramic mould material is prepared from alpha-alumina powder, aluminum borate crystal whisker, tin oxide powder, zirconia bead powder and polyurethane/asbestos nano composite material powder, so that the powder has the following beneficial effects: the invention adopts alpha-alumina powder as a base material, and can obtain nano powder with good dispersibility and uniform particles with aluminum borate whisker, tin oxide powder, zirconia bead powder and polyurethane/asbestos nano composite material powder, the obtained ceramic mold material is uniformly stirred and mixed by powder deionized water to obtain mixed slurry, the mixed slurry is placed in a mold, the mixed slurry is stood and dried to form a ceramic mold material green compact with a compact structure, the ceramic mold material green compact is demolded, sintered at high temperature and cooled to room temperature, and the ceramic mold material is taken out to obtain the ceramic mold material with excellent fracture toughness and wear resistance, high strength and high hardness. Accordingly, an object of the present invention is to provide a method for preparing a ceramic mold material of powder for a ceramic mold material having excellent fracture toughness and wear resistance, as well as high strength and high hardness, with good dispersibility and uniform particle size.

Drawings

FIG. 1 shows the density of a suspension prepared from a powder for a ceramic mold material;

FIG. 2 is a graph of the bending strength of the ceramic mold material;

FIG. 3 is a graph of hardness of a ceramic mold material;

FIG. 4 is a schematic view showing the indentation of the test piece in test example 1;

FIG. 5 is a graph of fracture toughness of a ceramic mold material;

fig. 6 shows the amount of wear of the ceramic mold material.

Detailed Description

The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings: