CN107935556B - Preparation method of nano ceramic binder - Google Patents

Preparation method of nano ceramic binder Download PDF

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Publication number
CN107935556B
CN107935556B CN201711415293.XA CN201711415293A CN107935556B CN 107935556 B CN107935556 B CN 107935556B CN 201711415293 A CN201711415293 A CN 201711415293A CN 107935556 B CN107935556 B CN 107935556B
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grinding
temperature
sintering
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bonding agent
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CN107935556A (en
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赵志伟
杨宝震
王顺
赵小苗
任瑛
陈利霞
毛淑芳
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Linying Decat New Material Co ltd
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Henan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C04B33/16—Lean materials, e.g. grog, quartz
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
    • B24D3/14—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/04—Clay; Kaolin
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B33/00—Clay-wares
    • C04B33/02—Preparing or treating the raw materials individually or as batches
    • C04B33/13—Compounding ingredients
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
    • C04B2235/3886—Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
    • C04B2235/445—Fluoride containing anions, e.g. fluosilicate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Abstract

The invention belongs to the field of preparation of bonding agents, and relates to a preparation method of a nano ceramic bonding agent. The preparation method comprises the following steps: a. taking 30-50% of talc, 10-20% of kaolin, 15-20% of boron glass, 8-10% of fluorite and 20-25% of quartz powder by mass percent, grinding, and sieving with a 200-300-mesh sieve to prepare a mixture; b. and c, pressing, smelting and water quenching the mixture prepared in the step a. c. Drying the product obtained in the step b, adding a nano vanadium nitride/chromium nitride modifier, grinding and sieving to obtain a basic ceramic bonding agent; d. and c, pressing the basic ceramic bond prepared in the step c into a blank by using a press, and sintering by using a microwave sintering furnace to prepare the ceramic bond. The method has the characteristics of low reaction temperature, short reaction time, low production cost, energy conservation and the like, and is easy for industrial production.

Description

Preparation method of nano ceramic binder
Technical Field
The invention belongs to the technical field of preparation of bonding agents, and particularly provides a method for preparing a nano ceramic bonding agent.
Background
The CBN grinding wheel has good chip-containing, heat-dissipating and self-sharpening performances and stable chemical performance, can well meet the requirements of grinding and high-efficiency grinding of materials difficult to process, and has very wide application prospect. The performance of the ceramic bonding agent is directly related to whether the excellent performance of the CBN abrasive particles can be fully exerted, so that the grinding effect of the CBN abrasive wheel is finally influenced. Therefore, the ceramic bond is one of the key factors for researching the ceramic bond CBN grinding tool.
The strength of the vitrified bond is an important factor affecting the use of CBN grinding tools. The strength of the binder mainly includes two aspects: the strength of the binder itself and the holding ability between the binder and the abrasive grains. The CBN grinding tool requires that the ceramic bond used must form a firm bond bridge and has good holding capacity for abrasive particles, otherwise, the high hardness of the CBN grinding tool is not reflected.
The refractoriness of the ceramic bond is one of the main performance indexes of the bond, for example, the refractoriness of the bond is too high, the sintering degree is poor during sintering, and the bond between the ceramic bond and abrasive particles is not firm, so that the hardness of the abrasive tool is unstable; on the contrary, if the fire resistance of the binder is too low, the viscosity of the liquid phase is small during firing, which causes the deformation and foaming of the grinding tool. The main factors affecting the refractoriness of the binder are the chemical composition and the particle size of the raw materials. The finer the particle size of the binder, the greater the degree of dispersion, the stronger the reactivity, and the lower the refractoriness.
The traditional normal pressure sintering method for preparing the ceramic bond needs high sintering temperature, the prepared ceramic bond has low strength and poor impact resistance and fatigue resistance, and in order to improve the performance and avoid the damage of high temperature sintering to CBN grinding materials, at present, low temperature high strength ceramic bonds are researched in a lot so as to realize the low temperature sintering of grinding tools. Compared with normal pressure sintering, the microwave sintering can rapidly and uniformly heat the material without causing cracking of the bonding agent or forming thermal stress in the bonding agent, so that a uniform fine crystal structure is formed inside the bonding agent, the performance of the ceramic bonding agent is improved, the strength of the CBN grinding tool is enhanced, the use and processing performance of the grinding tool are improved, and the purpose of preparing the ceramic bonding agent of the low-temperature high-strength CBN grinding tool is achieved. In addition, the microwave sintering can reduce the sintering temperature and shorten the sintering time, and the prepared ceramic has uniform and compact structure.
Vanadium nitride has good thermal conductivity, thermal shock resistance, electrical conductivity, chemical and thermal stability, and has been widely used in the field of machining. Chromium nitride has extremely high hardness and mechanical strength, excellent corrosion resistance and high temperature stability. The nano vanadium nitride/chromium nitride composite powder is prepared by compounding and nanocrystallizing the two. The composite powder has the comprehensive properties of high hardness, high strength, high conductivity, corrosion resistance and the like. The nano modifier is added into the bonding agent as a nano modifier, so that the comprehensive performance of the bonding agent can be obviously improved, and the bending strength and the fluidity of the bonding agent can be greatly improved.
Therefore, in order to better improve the comprehensive performance of the ceramic bond CBN grinding tool and obtain the low-temperature high-strength ceramic bond CBN grinding tool, a method for quickly preparing the ceramic bond added with the nano vanadium nitride/chromium nitride composite modifier at low temperature needs to be explored.
Disclosure of Invention
The invention aims to provide a novel method for quickly preparing a nano ceramic bonding agent with excellent performance for a CBN grinding tool. The ceramic bond prepared by the method can better meet the requirement of manufacturing a high-performance CBN grinding tool, so that the manufactured low-temperature high-strength ceramic bond CBN grinding tool can more easily achieve the conditions of high-speed, high-efficiency and high-precision grinding. The method has the characteristics of high economic benefit, cleanness, energy conservation, simple process and the like.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the nano ceramic bonding agent comprises the following steps:
a. taking 30-50% of talc, 10-20% of kaolin, 15-20% of boron glass, 8-10% of fluorite and 20-25% of quartz powder by mass percent, grinding, and sieving with a 200-300-mesh sieve to prepare a mixture;
b. b, briquetting the mixture prepared in the step a by using a die, smelting by using a program control heating mode, heating at the speed of 5-10 ℃/min at the temperature of 0-400 ℃, heating to 1200-1400 ℃ at the speed of 2-5 ℃/min after reaching 400 ℃, preserving heat for 4-8 h, and performing water quenching on the molten flowing-down glass material;
c. drying the product obtained in the step b at the temperature of 80-120 ℃ for 10-16 h, adding 0.5-1.5 mass percent of nano vanadium nitride/chromium nitride composite powder, grinding, and sieving with a 200-300-mesh sieve to obtain a basic ceramic bonding agent;
d. and c, pressing the basic ceramic bond prepared in the step c into a blank by using a press, and sintering by using a microwave sintering furnace to prepare the ceramic bond.
Preferably, the mass ratio of vanadium nitride to chromium nitride in the nano vanadium nitride/chromium nitride composite powder is 1: 1.
Preferably, the sintering temperature of the microwave oven is 550-700 ℃, and the sintering time is 10 min-1 h.
The mixing and grinding are carried out in one of a high-energy ball mill, a rolling ball mill and a grinding mill.
And c, drying equipment in the step c is any one of an air-blast drying box and a vacuum drying box.
Preferably, the average grain diameter of the nano vanadium nitride/chromium nitride composite powder is less than 100 nm.
The nano vanadium nitride/chromium nitride composite powder used in the invention can be synthesized by adopting a conventional technical method in the field, such as methods disclosed in Chinese patents, namely ' a method for synthesizing nano vanadium nitride/chromium nitride composite powder by using a carbothermic nitridation method ' (patent number 201310672946.8) ' a method for preparing nano vanadium nitride/chromium nitride composite powder ' (patent number 201310698867.4) ', and the like.
Compared with the existing method for preparing the ceramic bond for the CBN grinding tool, the method has the following beneficial effects:
(1) the sintering temperature is uniform, the microwave sintering method has the effect of synchronous heating inside and outside, and the microwave sintering can rapidly and uniformly heat the material without causing cracking of the binder or forming thermal stress in the binder;
(2) the reaction temperature is low, the reaction time is short, the energy consumption is reduced, and compared with the traditional method for sintering the ceramic bonding agent under normal pressure, the preparation method can greatly reduce the reaction temperature, shorten the reaction time and effectively reduce the energy consumption;
(3) excellent performance and wide application prospect: the ceramic bond for the CBN grinding tool generated by the reaction has high bending strength and good fluidity. In addition, the ceramic bond prepared by the method has uniform pores and large holding force with the abrasive particles, and the prepared grinding tool has good grinding performance and wide application prospect.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
A preparation method of a nano ceramic bonding agent comprises the following steps:
a. respectively weighing 44g of talc, 11g of kaolin, 22g of boron glass, 8.8g of fluorite and 24.2g of quartz powder, grinding, and sieving with a 200-mesh sieve to obtain a mixture;
b. b, briquetting the mixture prepared in the step a by using a die, raising the temperature to 400 ℃ at a heating rate of 10 ℃/min, raising the temperature to 1400 ℃ at a heating rate of 5 ℃/min, preserving heat for 8 hours, and performing water quenching on the melted and flowed-down glass material;
c. drying the product prepared in the step b at 80 ℃ for 16h, adding 1.1g of nano vanadium nitride/chromium nitride composite powder (the mass ratio of vanadium nitride to chromium nitride is 1: 1), grinding, and sieving with a 200-mesh sieve to prepare a basic ceramic bonding agent;
d. and c, pressing the basic ceramic bond prepared in the step c into a blank by using a press, and sintering by using a microwave sintering furnace (the sintering temperature is 600 ℃, and the sintering time is 30 min) to prepare the ceramic bond.
The fluidity and the flexural strength of the ceramic bond were measured separately. The results show that: the fluidity of the bonding agent is 210 percent, and the flexural strength is 110 MPa.
Example 2
A preparation method of a nano ceramic bonding agent comprises the following steps:
a. respectively weighing 36.5g of talc, 18.5g of kaolin, 15.4g of boron glass, 8.4g of fluorite and 21.2g of quartz powder, grinding, and sieving with a 200-mesh sieve to obtain a mixture;
b. b, briquetting the mixture prepared in the step a by using a die, raising the temperature to 400 ℃ at a heating rate of 5 ℃/min, raising the temperature to 1200 ℃ at a heating rate of 2 ℃/min, preserving heat for 4 hours, and performing water quenching on the melted and flowed-down glass material;
c. drying the product obtained in the step b at 120 ℃ for 10 hours, adding 1.5g of nano vanadium nitride/chromium nitride composite powder (the mass ratio of vanadium nitride to chromium nitride is 1: 1), grinding, and sieving by using a 300-mesh sieve to obtain a basic ceramic bonding agent;
d. and c, pressing the basic ceramic bond prepared in the step c into a blank by using a press, and sintering by using a microwave sintering furnace (the sintering temperature is 700 ℃, and the sintering time is 10 min) to prepare the ceramic bond.
The fluidity and the flexural strength of the ceramic bond were measured separately. The results show that: the fluidity of the bonding agent is 160 percent, and the breaking strength is 86 MPa.
Example 3
A preparation method of a nano ceramic bonding agent comprises the following steps:
a. respectively weighing 66.5g of talc, 26.25g of kaolin, 29.75g of boron glass, 14g of fluorite and 38.5g of quartz powder, grinding, and sieving with a 200-mesh sieve to obtain a mixture;
b. b, briquetting the mixture prepared in the step a by using a die, raising the temperature to 400 ℃ at the heating rate of 8 ℃/min, raising the temperature to 1350 ℃ at the heating rate of 4 ℃/min, preserving heat for 6 hours, and performing water quenching on the melted and flowed-down glass material;
c. drying the product prepared in the step b at 100 ℃ for 12 hours, then adding 1.25g of nano vanadium nitride/chromium nitride composite powder (the mass ratio of vanadium nitride to chromium nitride is 1: 1), grinding, and sieving with a 200-mesh sieve to prepare a basic ceramic bonding agent;
d. and c, pressing the basic ceramic bond prepared in the step c into a blank by using a press, and sintering by using a microwave sintering furnace (the sintering temperature is 550 ℃, and the sintering time is 1 hour) to prepare the ceramic bond.
The fluidity and the flexural strength of the ceramic bond were measured separately. The results show that: the fluidity of the bonding agent is 182 percent, and the breaking strength is 93 MPa.
Example 4
A preparation method of a nano ceramic bonding agent comprises the following steps:
a. respectively weighing 14g of talc, 4.2g of kaolin, 6.3g of boron glass, 3.15g of fluorite and 7.35g of quartz powder, grinding, and sieving with a 200-mesh sieve to obtain a mixture;
b. b, briquetting the mixture prepared in the step a by using a die, raising the temperature to 400 ℃ at the heating rate of 6 ℃/min, raising the temperature to 1250 ℃ at the heating rate of 3 ℃/min, preserving the heat for 7 hours, and performing water quenching on the melted and flowed-down glass material;
c. drying the product prepared in the step b at 90 ℃ for 14h, adding 0.32g of nano vanadium nitride/chromium nitride composite powder (the mass ratio of vanadium nitride to chromium nitride is 1: 1), grinding, and sieving with a 300-mesh sieve to prepare a basic ceramic bonding agent;
d. and c, pressing the basic ceramic bond prepared in the step c into a blank by using a press, and sintering by using a microwave sintering furnace (the sintering temperature is 600 ℃, and the sintering time is 20 min) to prepare the ceramic bond.
The fluidity and the flexural strength of the ceramic bond were measured separately. The results show that: the fluidity of the bonding agent is 202 percent, and the flexural strength is 104 MPa.
Comparative example 1: by taking example 1 as a comparison, under the condition that other conditions are not changed, when the mass ratio of vanadium nitride to chromium nitride in the added nano vanadium nitride/chromium nitride composite powder is 1:2, the flowability of the bonding agent is 185%, and the flexural strength is 96 MPa.
Comparative example 2: by taking example 1 as a comparison, under the condition that other conditions are not changed, when the mass ratio of vanadium nitride to chromium nitride in the added nano vanadium nitride/chromium nitride composite powder is 2:1, the flowability of the bonding agent is 172%, and the flexural strength is 87 MPa.
Comparative example 3: by taking the example 1 as a comparison, when the nano vanadium nitride/chromium nitride composite powder is changed into nano vanadium nitride under the condition of keeping other conditions unchanged, the flowability of the bonding agent is 157 percent, and the flexural strength is 75 MPa.
Comparative example 4: by taking example 1 as a comparison, when the nano vanadium nitride/chromium nitride composite powder is changed into nano chromium nitride under the condition that other conditions are not changed, the flowability of the bonding agent is 162%, and the flexural strength is 79 MPa.
By comparison, the effect of modifying the bonding agent by using the nano vanadium nitride/chromium nitride composite powder is obviously superior to the modification effect of using the nano vanadium nitride or the chromium nitride alone, and the modification effect is optimal when the mass ratio of the nano vanadium nitride to the chromium nitride is 1: 1. The product prepared according to the invention is excellent in fluidity and breaking strength.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.

Claims (5)

1. A preparation method of a nano ceramic bonding agent is characterized by comprising the following steps: the preparation method comprises the following steps:
a. taking 30-50% of talc, 10-20% of kaolin, 15-20% of boron glass, 8-10% of fluorite and 20-25% of quartz powder by mass percent, grinding, and sieving with a 200-300-mesh sieve to prepare a mixture;
b. b, briquetting the mixture prepared in the step a by using a die, raising the temperature to 400 ℃ at a rate of 5-10 ℃/min, raising the temperature to 1200-1400 ℃ at a rate of 2-5 ℃/min, and keeping the temperature for 4-8 hours, and performing water quenching on the obtained glass material;
c. drying the product obtained in the step b at the temperature of 80-120 ℃ for 10-16 h, adding 0.5-1.5 mass percent of nano vanadium nitride/chromium nitride composite powder, grinding, and sieving with a 200-300-mesh sieve to obtain a basic ceramic bonding agent;
d. and c, pressing the basic ceramic bond prepared in the step c into a blank, and sintering the blank by using a microwave sintering furnace to prepare the nano ceramic bond.
2. The method of claim 1, wherein: the mass ratio of vanadium nitride to chromium nitride in the nano vanadium nitride/chromium nitride composite powder is 1: 1.
3. The method of claim 1, wherein: the mixing and grinding are carried out in one of a high-energy ball mill, a rolling ball mill and a grinding mill.
4. The method of claim 1, wherein: the drying equipment is any one of an air blowing drying box and a vacuum drying box.
5. The method of claim 1, wherein: the sintering temperature of the microwave oven is 550-700 ℃, and the sintering time is 10 min-1 h.
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