CN104802104B - A kind of preparation method of nano-grade ceramic binding agent extra hard material grinding wheel - Google Patents

A kind of preparation method of nano-grade ceramic binding agent extra hard material grinding wheel Download PDF

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CN104802104B
CN104802104B CN201510234075.0A CN201510234075A CN104802104B CN 104802104 B CN104802104 B CN 104802104B CN 201510234075 A CN201510234075 A CN 201510234075A CN 104802104 B CN104802104 B CN 104802104B
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agent
nano
binding agent
grinding wheel
preparation
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CN104802104A (en
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刘瑞平
贺鹏
苏伟明
邓福铭
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China University of Mining and Technology Beijing CUMTB
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China University of Mining and Technology Beijing CUMTB
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D18/00Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
    • B24D18/0009Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using moulds or presses

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  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
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Abstract

The present invention prepares the extra hard material grinding wheel of nano-grade ceramic binding agent using one-step method, the raw material used is the corresponding water-soluble nitrate of ceramic powder or chlorate of required preparation, superhard abrading agent and pore creating material, by raw material, monomer and crosslinking agent are soluble in water, initiator is added and catalyst aggregates into nanoscale three-dimensional space network under the conditions of constant temperature (20-80 DEG C) and form gel later, these water-soluble nitrates or chlorination salt out during gel drying, and it is limited to form nanocrystal by this three-dimensional space network, it is evenly distributed in superhard abrading agent in vitrified bond matrix simultaneously, it is added that one or more water solubilitys are preferable and lower melting-point organic matter simultaneously, it is substantially reduced contraction when wet gel low temperature drying, and it melts or decomposes earlier in xerogel calcination process, gradually it is sustained Stress is concentrated, and is solved the problems, such as nano-grade ceramic binding agent abnormal growth in the subsequent sintering process using Fast Sintering technology, is prepared the nano-grade ceramic binding agent extra hard material grinding wheel of function admirable.

Description

A kind of preparation method of nano-grade ceramic binding agent extra hard material grinding wheel
Technical field
The present invention relates to superhard material and abrasive grinding field, provides and a kind of prepare nano-grade ceramic binding agent superhard material sand The new method of wheel.
Background technique
Since superhard material (such as diamond, cubic boron nitride) to have that hardness is high, wearability is good, thermal stability is good etc. excellent Point is widely applied in all kinds of grinding tools.In all kinds of ultrahard material grinding wheel bonds, metallic bond is from sharp Property is poor, easily adheres when processing metal material, and resinoid bond thermal stability is poor, and vitrified bond is between metal knot Between mixture and resinoid bond, heat resisting temperature is higher, self-sharpening is preferable, intensity is high, wearability is good.Ceramic bond super-hard Material grinding wheel not only has that cutting is sharp, grinding force is small, high production efficiency, long service life, to be easy to shaping and dressing, grinding smart Workpiece temperature is low when spending the advantages that high, but also having grinding, can eliminate residual tension and generate residual compressive stress, make workpiece The characteristics of durability improves 30~50%.Therefore, the conduct of ceramic bond super-hard material grinding wheel is a kind of at a high speed, efficient, high-precision, low The high-performance grinding tool product of cost, low pollution, becomes the research and development emphasis of world's grinding tool in recent years.
High-performance ceramic bonding agent is the key that prepare high-performance ceramic bonding agent extra hard material grinding wheel.With surpassing in recent years The development of high speed extra hard material grinding wheel, to the performance of vitrified bond, more stringent requirements are proposed, that is, bonding agent is required to have height Intensity, low refractoriness, good gas porosity, wellability, craftsmanship, chemical stability, and thermally expanded with superhard abrading agent and be Number matching, however the defects such as the generally existing sintering temperature of traditional vitrified bond is high, intensity is low.Nano-grade ceramic binding agent due to The advantages that its granularity is small, large specific surface area, sintering temperature is low, intensity is high, good toughness is expected to solve current traditional ceramics bonding agent Contradictory problems between sintering temperature and low and high intensity improve the performance of ceramic bond super-hard material grinding wheel, further widen The application range of extra hard material grinding wheel.
Recent domestic has carried out exploratory development to nano-grade ceramic binding agent.Compared with traditional vitrified bond, to the greatest extent Pipe nano-grade ceramic binding agent has the advantages that intensity height, good toughness, sintering temperature are low etc., but since its granularity is smaller, specific surface area Greatly, there are still some problems in the preparation process of extra hard material grinding wheel, is in particular in the following aspects: (1) due to receiving The fine granularity and large surface area of rice vitrified bond, appearance is bulk, and density is lower, this may bring centainly the molding of grinding tool Difficulty, green density and sintering strength are lower, shrink it is larger.(2) appearance is compared in nano-grade ceramic binding agent one pack system powder preparation Easily, how to guarantee its favorable dispersibility during subsequent ball milling mixes and be uniformly distributed.(3) due to the activity of nano particle It is higher, easily occur the abnormal growth of crystal grain in sintering process and be difficult to the disadvantages of densifying, therefore, to obtain truly Nano ceramics structural material is not easy to.(4) compared with traditional ceramics bonding agent, to the structure of stomata in nano-grade ceramic binding agent Relationship between (such as shape, content and size) and its performance lacks system in-depth study.
Based on the above analysis, if direct in-situ can generate nano-ceramic particle during preparation and be allowed to and superhard material Material is built into the nano-grade ceramic binding agent extra hard material grinding wheel with ideal structure and performance, it would be possible to solve current nanometer pottery The problem of porcelain bonding agent extra hard material grinding wheel preparation and application.
Summary of the invention
The object of the present invention is to provide a kind of methods that one-step method prepares nano-grade ceramic binding agent extra hard material grinding wheel.This hair Bright preparation process is simple, and the requirement to equipment and process conditions is low, is conducive to promote and apply.
A kind of preparation method of nano-grade ceramic binding agent extra hard material grinding wheel, it is characterised in that preparation process includes following step It is rapid:
(1) 2h is mixed in deionized water, monomer and crosslinking agent first, in accordance with following mass ratio, be configured to clear pre- Mixed liquid, deionized water: monomer: crosslinking agent=60~90:9.5~30:0.5~10, wherein the monomer is acrylamide, institute Stating crosslinking agent is N, N '-methylene-bisacrylamide;
(2) organic slow-release agent is added in above-mentioned premixed liquid, stirs 2h, the additional amount of organic slow-release agent is premixed liquid quality 0.5-20%;
(3) the starting material inorganic salt of superhard abrading agent, pore creating material and vitrified bond is continuously added, 2-6h is stirred, until Obtain finely dispersed slurry, wherein the gross mass of the superhard abrading agent of addition, pore creating material and inorganic salts is premixed liquid quality 20~60%, the mass ratio of superhard abrading agent, pore creating material and inorganic salts is 45~60:5~20:20~50, described superhard Material abrasive material is one or both of diamond or cubic boron nitride, and the pore creating material is carbon ball, PMMA microsphere or PS microballoon One of or it is a variety of, the inorganic salts be aluminum nitrate, zirconium oxychloride, zinc chloride, sodium chloride or potassium chloride in it is two or more;
(4) catalyst and initiator are sequentially added in the slurry that step (3) obtains, injects mold after mixing evenly, Polymerization reaction occurs for single body and crosslinking agent when 20 DEG C~80 DEG C of temperature, forms gel green body;
(5) green body for obtaining step (4) demoulds, dry 1 under the conditions of 40 DEG C~80 DEG C, humidity are greater than 50%rh~ 5d obtains xerogel, or is completely dried in -40 DEG C~-50 DEG C, vacuum freeze drier of the vacuum degree less than 0.1Pa, obtains To xerogel;
(6) xerogel that step (5) obtains is put into Muffle furnace, in air atmosphere or nitrogen, argon gas protect gas Under atmosphere, rise to 200 DEG C~300 DEG C with the heating rate of 0.2~5 DEG C/min, keep the temperature 0.5~3 hour, then with 0.2~5 DEG C/ The heating rate of min rises to 400~650 DEG C, keeps the temperature 1~6 hour, finally rises to 700 with the heating rate of 0.5~10 DEG C/min DEG C~1000 DEG C between, soaking time is 0.5~3 hour, finally obtained nano-grade ceramic binding agent extra hard material grinding wheel.
The organic slow-release agent is one of sucrose, fructose, urea or glucose or a variety of.,
The catalyst is N, N, N ', the aqueous solution of N '-tetramethylethylenediamine, concentration of polymer solution is 10~50%, Additional amount is the 1~10% of premixed liquid quality.
The initiator is the aqueous solution of ammonium persulfate or potassium peroxydisulfate, and concentration of polymer solution is 10~50%, is added Amount is the 5~20% of premixed liquid quality.
Compared with prior art, the present invention its significant advantage is:
(1) extra hard material grinding wheel of nano-grade ceramic binding agent is prepared using one-step method, the raw material used is required preparation The corresponding water-soluble nitrate of ceramic powder or chlorate, superhard abrading agent and pore creating material etc., by raw material (nitrate Or chlorate etc.), monomer (acrylamide) and crosslinking agent (N, N '-methylene-bisacrylamide) it is soluble in water, be added initiator (ammonium persulfate) aggregates into nanoscale three-dimensional space network under the conditions of constant temperature (20-80 DEG C) later and forms gel, gel These water-soluble nitrates or chlorination salt out in dry process, and limited by this three-dimensional space network to be formed it is nanocrystalline Grain, while it is evenly distributed in superhard abrading agent in vitrified bond matrix.
(2) one or more water solubilitys are preferable and lower melting-point organic matter by being added in gel, which can It with the contraction being substantially reduced when wet gel low temperature drying, and melts or decomposes earlier in xerogel calcination process, gradually delay Stress concentration is released, solves the problems, such as to crack in nano-grade ceramic binding agent cBN grinding wheel sintering process.
(3) it is asked simultaneously using the nano-grade ceramic binding agent abnormal growth that Fast Sintering technology solves in the subsequent sintering process Topic, is successfully introduced into the technique preparation field of nano-grade ceramic binding agent extra hard material grinding wheel, the nano ceramics knot prepared The flexural strength of mixture extra hard material grinding wheel is 100~120MPa, and the porosity is 0~30%.The technique have simple process, at This lower advantage.
Specific embodiment
The present invention is further illustrated using embodiment below.
Embodiment 1: at room temperature, by acrylamide monomer, N, N'- methylene-bisacrylamide and deionized water are pressed It is configured to the clear solution of 200ml according to the mass ratio of 30:10:60,1g sucrose, stirring is added according to the 0.5% of premixed liquid quality 1h obtains premixed liquid.3g zirconium oxychloride, 0.72g aluminum nitrate, 4.4g sodium chloride, 24g cubes of nitridation are added into above-mentioned premixed liquid Boron, 8g PMMA microsphere, stirring 4h obtain finely dispersed solution.The 20wt% tetramethyl of 0.05ml is sequentially added into solution The 40wt% ammonium persulfate aqueous solution of ethylenediamine solution and 0.4ml, injects mold after mixing evenly, is formed under 40 DEG C of constant temperature solidifying Glue.Then by wet gel 40 DEG C, humidity be 60%rh under conditions of it is 3 days dry, obtain xerogel.Gained xerogel is in Muffle 600 DEG C of heat preservation 4h are risen to the heating rate of 0.3 DEG C/min in furnace, then rise to 1000 DEG C with the heating rate of 1 DEG C/min, are protected Warm 2h.Finally obtain the nano-grade ceramic binding agent cubic boron nitride abrasive wheel that the porosity is about 28%.
Embodiment 2: at room temperature, by acrylamide monomer, N, N'- methylene-bisacrylamide and deionized water are pressed It is configured to the clear solution of 200ml according to the mass ratio of 9.5:0.5:90,40g fructose is added according to the 20% of premixed liquid quality, stirs It mixes 2h and obtains premixed liquid.4g sodium chloride, 10g aluminum nitrate, 3g zirconium oxychloride, 18g diamond, 2g carbon are added into above-mentioned premixed liquid Ball, stirring 3h obtain finely dispersed solution.Sequentially added into solution 0.04ml 20wt% tetramethylethylenediamine solution and The 40wt% ammonium persulfate aqueous solution of 0.6ml, injects mold after mixing evenly, forms gel under 60 DEG C of constant temperature.It then will be wet Gel, to dry 5 days under conditions of 90%rh, obtains xerogel in 80 DEG C, humidity.Gained xerogel in Muffle furnace with 2 DEG C/ The heating rate of min rises to 300 DEG C of heat preservation 0.5h, continues to rise to 550 DEG C of heat preservation 4h, then with the heating rate liter of 2 DEG C/min To 800 DEG C, 3h is kept the temperature.Finally obtain the nano-grade ceramic binding agent skive that the porosity is about 2~3%.
Embodiment 3: at room temperature, by acrylamide monomer, N, N'- methylene-bisacrylamide and deionized water are pressed It is configured to the clear solution of 200ml according to the mass ratio of 15:0.6:84.4,20g glucose is added according to the 10% of premixed liquid quality, Stirring 1h obtains premixed liquid.3g zirconium oxychloride, 0.72g aluminum nitrate, 4.4g potassium chloride, 10g cubes are added into above-mentioned premixed liquid Boron nitride, 14g diamond, 8g PS microballoon, stirring 4h obtain finely dispersed solution.Sequentially add 0.1ml's into solution The 40wt% ammonium persulfate aqueous solution of 20wt% tetramethylethylenediamine aqueous solution and 0.2ml, injects mold, 40 after mixing evenly Form gel under DEG C constant temperature, later by wet gel under conditions of 50 DEG C, humidity are greater than 60%rh 5 days dry, gained xerogel 200 DEG C of heat preservation 3h are risen to the heating rate of 0.5 DEG C/min in Muffle furnace, then rise to 750 with the heating rate of 5 DEG C/min DEG C, keep the temperature 4h.Finally obtain nano-grade ceramic binding agent diamond-cubic boron nitride complex sand that the porosity is about 25~28% Wheel.

Claims (4)

1. a kind of preparation method of nano-grade ceramic binding agent extra hard material grinding wheel, it is characterised in that preparation process includes following step It is rapid:
(1) 2h is mixed in deionized water, monomer and crosslinking agent first, in accordance with following mass ratio, is configured to clear premix Liquid, deionized water: monomer: crosslinking agent=60~90:9.5~30:0.5~10, wherein the monomer is acrylamide, described Crosslinking agent is N, N '-methylene-bisacrylamide;
(2) organic slow-release agent is added in above-mentioned premixed liquid, stirs 2h, the additional amount of organic slow-release agent is premixed liquid quality 0.5-20%;
(3) inorganic salts of superhard abrading agent, pore creating material and vitrified bond raw material are continuously added, 2-6h is stirred, until obtaining Finely dispersed slurry, wherein the gross mass of the superhard abrading agent of addition, pore creating material and inorganic salts is the 20 of premixed liquid quality ~60%, the mass ratio of superhard abrading agent, pore creating material and inorganic salts is 45~60:5~20:20~50, the superhard material Abrasive material is one or both of diamond or cubic boron nitride, and the pore creating material is in carbon ball, PMMA microsphere or PS microballoon One or more, the inorganic salts are two or more in aluminum nitrate, zirconium oxychloride, zinc chloride, sodium chloride or potassium chloride;
(4) catalyst and initiator are sequentially added in the slurry that step (3) obtains, injects mold after mixing evenly, at 20 DEG C Polymerization reaction occurs for single body and crosslinking agent when~80 DEG C of temperature, forms gel green body;
(5) the gel green body that step (4) obtains is demoulded, dry 1 under the conditions of 40 DEG C~80 DEG C, humidity are greater than 50%rh ~5d obtains xerogel, or is completely dried in -40 DEG C~-50 DEG C, vacuum freeze drier of the vacuum degree less than 0.1Pa, Obtain xerogel;
(6) xerogel that step (5) obtains is put into Muffle furnace, in air atmosphere or under nitrogen, argon atmosphere, 200 DEG C~300 DEG C are risen to the heating rate of 0.2~5 DEG C/min, 0.5~3 hour is kept the temperature, then with 0.2~5 DEG C/min's Heating rate rises to 400~650 DEG C, keeps the temperature 1~6 hour, finally with the heating rate of 0.5~10 DEG C/min rise to 700 DEG C~ Between 1000 DEG C, soaking time is 0.5~3 hour, finally obtained nano-grade ceramic binding agent extra hard material grinding wheel.
2. preparation method according to claim 1, it is characterised in that: the organic slow-release agent be sucrose, fructose, urea or One of glucose is a variety of.
3. preparation method according to claim 1, it is characterised in that: the catalyst is N, N, N ', N '-tetramethyl second two The aqueous solution of amine, concentration of polymer solution are 10~50%, and additional amount is the 1~10% of premixed liquid quality.
4. preparation method according to claim 1, it is characterised in that: the initiator is ammonium persulfate or potassium peroxydisulfate Aqueous solution, concentration of polymer solution are 10~50%, and additional amount is the 5~20% of premixed liquid quality.
CN201510234075.0A 2015-05-11 2015-05-11 A kind of preparation method of nano-grade ceramic binding agent extra hard material grinding wheel Expired - Fee Related CN104802104B (en)

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