CN109293393A - A kind of preparation method of plating boron carbide diamond abrasive grain - Google Patents

A kind of preparation method of plating boron carbide diamond abrasive grain Download PDF

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Publication number
CN109293393A
CN109293393A CN201811269336.2A CN201811269336A CN109293393A CN 109293393 A CN109293393 A CN 109293393A CN 201811269336 A CN201811269336 A CN 201811269336A CN 109293393 A CN109293393 A CN 109293393A
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China
Prior art keywords
diamond
boron carbide
preparation
plating
abrasive grain
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CN201811269336.2A
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Chinese (zh)
Inventor
穆云超
王志新
马明星
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Zhongyuan University of Technology
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Zhongyuan University of Technology
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Priority to CN201811269336.2A priority Critical patent/CN109293393A/en
Publication of CN109293393A publication Critical patent/CN109293393A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81Coating or impregnation
    • C04B41/85Coating or impregnation with inorganic materials
    • C04B41/87Ceramics
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5053Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
    • C04B41/5057Carbides
    • C04B41/5058Boron carbide
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1436Composite particles, e.g. coated particles

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention discloses a kind of preparation methods of plating boron carbide diamond abrasive grain.Diamond surface is cleaned first, diamond and boron powder are placed in after evenly mixing in mold later, and mold is placed in discharge plasma sintering furnace and is sintered;Sintering condition is that vacuum degree is less than 100pa, and 1200 ~ 1400 DEG C of sintering temperature, constant temperature keeps the temperature 10 ~ 15min, and sintering terminates furnace cooling;Cooling terminates that sintered mixture is ground up, sieved and is cleaned, the last vacuum dried diamond for obtaining surface plating boron carbide.Preparation process of the invention is simple, coating is uniform, low in cost, and surface is prepared being coated between the diamond of boron carbide and metal or vitrified bond can be well bonded, falling off too early for diamond can be effectively reduced, the service life and processing efficiency of product are improved.

Description

A kind of preparation method of plating boron carbide diamond abrasive grain
Technical field
The invention belongs to diamond preparation technical fields, and in particular to the preparation side of plating boron carbide diamond abrasive grain Method.
Background technique
Diamond has a series of excellent performances such as high rigidity, high-wearing feature, high-termal conductivity and electrical insulating property, by Buddha's warrior attendant The particle studded diamond tool prepared into carcass of stone becomes the various essential tools of stiff materials of processing, such as sand Wheel, drill bit and cutting tool etc., these tools obtain in fields such as processing of stone, building decoration, national defence, optical glass producings It is widely applied.
In diamond tool, play main shear action is the diamond being embedded in carcass material, the property of tool Energy and service life depend on the adhesion strength between diamond particles and carcass material.Diamond is made of carbon, is constituted The chemical bond of diamond is covalent bond, this structure determines to be difficult between diamond and the metal or ceramics that constitute tool base Preferable binding force, diamond is difficult to the metal after being melted or ceramics are infiltrated, and in use, diamond can be too early It falls off, largely reduces the service performance and service life of diamond tool.Currently, solving the problems, such as this method There are two main classes, and one kind is to add the elements such as the titanium chromium manganese tungsten that chemical combination is easy with diamond in the base, and such method needs Higher sintering temperature is used when preparing tool, it is clear that is injured to diamond larger;Another kind of is special in diamond surface plating Fixed coating, to solve the problems, such as the combination between diamond and matrix.
Currently, the method in diamond surface plated coating is broadly divided into wet process and two kinds of dry method, wet process coating and Buddha's warrior attendant Without chemical bonding between stone, binding force is weaker, it is difficult to significantly improve the binding force between diamond and matrix, be only applicable to intensity Lower matrix;There is chemical bonding in dry method coating, binding force is stronger, can improve diamond and matrix generally between diamond Between binding force, but the generally existing complex process of plating technic of dry method coating, diamond is in high temperature in preparation process State for time is long, and diamond is impaired than more serious.In addition, the coats of metal such as titanium chromium manganese tungsten of dry method coating institute plating are to ceramic junction Binding force raising in mixture tool between diamond and matrix has no remarkable effect.
Therefore, find a kind of coating suitable for ceramics and metallic bond matrix, and plating technic is simple, cost compared with Low, the higher plating technic of efficiency, it appears particularly important.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides the preparation of plating boron carbide diamond abrasive grain Method, for existing diamond coating complex process, it is at high cost, coating effect is poor the disadvantages of, provide plating boron carbide gold The preparation method of hard rock abrasive grain, plated layer compact is uniform, low in cost, is simple and efficient
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of preparation method of plating boron carbide diamond abrasive grain, the specific steps of which are as follows:
(1) it is uniformly mixed with boron powder according to volume ratio 4:0.5 ~ 1.5 after being cleaned diamond surface and is placed on graphite jig In cavity, and graphite jig is placed in discharge plasma sintering furnace.
(2) by discharge plasma sintering stove evacuation to vacuum degree less than 100 Pa, 10 are pressurized to graphite jig cavity Temperature is risen to 1200 ~ 1400 DEG C of 10 ~ 15 min of heat preservation by MPa, and cool down furnace cooling later.
(3) sintered mixture is ground up, sieved and is cleaned, obtained to surface and be coated with the diamond of boron carbide.
Diamond grit is 30 ~ 60 mesh in the step (1), and boron Powder Particle Size is 300 ~ 1000 mesh.
The process that diamond surface is cleaned in the step (1) are as follows: diamond is placed in nitric acid, in hydrochloric acid mixed solution 30min is boiled under magnetic agitation, then rinses diamond taking-up with deionized water.This process purpose is to remove diamond surface Grease, oil removal process is stirred using magnetic stirring apparatus.
In the step (2), control heating speed is not less than 80 DEG C/min.
In the step (2), after system vacuum degree is less than 100 pa, 10 MPa are pressurized to graphite jig cavity, and Constant pressure keeps to sintering terminating.
Mixture cleaning step after sintering in the step (3) are as follows: the mixture after being ground up, sieved is placed in dust technology Cleaning is boiled under magnetic agitation, is then cleaned by ultrasonic diamond taking-up in deionized water.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) the method for the present invention, which can make to react between diamond surface and boron powder, generates boron carbide coating.Boron carbide and diamond it Between have stable chemical bonds, also, in metallic matrix, boron carbide coating can generate metal diboride with metal reaction Object, the binding force between diamond and metal matrix is obviously improved, and in ceramic matrix, boride can enter ceramic structure Among, good bonding is formed, the binding force between diamond and ceramic matrix is significantly improved.
(2) the method for the present invention carries out plating using discharge plasma sintering technique, during plating, what pulse current generated Plasma and sintering pressure advantageously reduce the reaction temperature of diamond Yu boron powder, and can effectively shorten the reaction time, Improve plating rate, save the cost.
(3) discharge plasma sintering technique that the method for the present invention uses has the characteristics that temperature rate is exceedingly fast, both can be with The time of diamond holding at high temperature is effectively reduced, damage of the high temperature to diamond is substantially reduced, and plating week can be shortened Phase improves production efficiency.
Detailed description of the invention
Fig. 1 is the SEM pattern for not plating the diamond of boron carbide;
Fig. 2 is the SEM pattern for plating the diamond of boron carbide;
Fig. 3 is the diamond body stereomicroscope figure for not plating boron carbide;
Fig. 4 is the diamond body stereomicroscope figure for plating boron carbide;
Fig. 5 is the diamond XRD analysis for plating boron carbide.
Specific embodiment
With reference to the accompanying drawings and detailed description, the present invention will be further described.
Embodiment 1
Steps are as follows for a kind of preparation method of plating boron carbide diamond abrasive grain:
(1) after 3.98 g diamond surfaces being cleaned first with 0.33 g boron powder (i.e. volume ratio diamond: boron powder=4: 0.5) it is uniformly mixed and is placed in graphite jig cavity, and graphite jig is placed in discharge plasma sintering furnace;Wherein diamond Granularity is 30 mesh, and boron Powder Particle Size is 300 mesh;Diamond surface carries out cleaning process are as follows: diamond is placed in nitric acid, mixed in hydrochloric acid 30min is boiled in liquid under magnetic agitation, then rinses diamond taking-up deionized water 2 times, this process purpose is to remove gold The grease on hard rock surface, oil removal process are stirred using magnetic stirring apparatus;
(2) by discharge plasma sintering stove evacuation to vacuum degree less than 100 Pa, 10 MPa are pressurized to graphite jig cavity, Temperature is risen into 1200 DEG C of 15 min of heat preservation, furnace cooling.Wherein control heating speed is 100 DEG C/min;Wherein to graphite Cavity body of mould is pressurized to 10 MPa, pressurizes after being 100 Pa from vacuum degree, and constant pressure keeps to sintering terminating;Wherein mixture is clear Wash step are as follows: the mixture after being ground up, sieved is placed in dust technology under magnetic agitation and boils 5 min of cleaning, then by diamond Taking-up is cleaned by ultrasonic 10 min in deionized water.
Embodiment 2
Steps are as follows for a kind of preparation method of plating boron carbide diamond abrasive grain:
(1) after 3.98 g diamond surfaces being cleaned first with 0.99 g boron powder (i.e. volume ratio diamond: boron powder=4: 1.5) it is uniformly mixed and is placed in graphite jig cavity, and graphite jig is placed in discharge plasma sintering furnace;Wherein diamond Granularity is 60 mesh, and boron Powder Particle Size is 1200 mesh;Diamond surface carries out cleaning process are as follows: diamond is placed in nitric acid, salt acid-mixed It closes in liquid and boils 30min under magnetic agitation, then rinse diamond taking-up deionized water 2 times, this process purpose is to remove The grease of diamond surface, oil removal process are stirred using magnetic stirring apparatus;
(2) by discharge plasma sintering stove evacuation to vacuum degree less than 100 Pa, 10 MPa are pressurized to graphite jig cavity, Temperature is risen into 1400 DEG C of 10 min of heat preservation, furnace cooling.Wherein control heating speed is 120 DEG C/min;Wherein to graphite Cavity body of mould is pressurized to 10 MPa, pressurizes after being 100 pa from vacuum degree, and constant pressure keeps to sintering terminating;Wherein mixture is clear Wash step are as follows: the mixture after being ground up, sieved is placed in dust technology under magnetic agitation and boils 5 min of cleaning, then by diamond Taking-up is cleaned by ultrasonic 10 min in deionized water.
The SEM pattern that the method for the present invention does not plate the diamond of boron carbide is as shown in Figure 1;The gold of the method for the present invention plating boron carbide The SEM pattern of hard rock is as shown in Fig. 2, the diamond surface for the plating boron carbide that as can be seen from the figure the method for the present invention is prepared plates Layer is uniform, fine and close, and coating is complete;The method of the present invention does not plate the diamond of boron carbide using the pattern such as figure of stereomicroscope observation Shown in 3, for the diamond of non-plating boron carbide rich in gloss, surface is smooth, and color is yellow;The gold of the method for the present invention plating boron carbide Hard rock uses the pattern observed under stereomicroscope as shown in figure 4, after plating boron carbide, and diamond integrally becomes black, color Uniformly, and diamond shapes are regular, without obvious carbonization phenomenon;Diamond XRD analysis such as Fig. 5 institute of the method for the present invention plating boron carbide Show, by analysis by, hence it is evident that have diamond, boron carbide, three kinds of object phases of boron characteristic peak, illustrate between diamond and carbon dust Interfacial reaction is good, there is boron carbide generation, and gained coating performance is preferable.
Embodiment 3
Steps are as follows for a kind of preparation method of plating boron carbide diamond abrasive grain:
(1) postposition is uniformly mixed according to volume ratio 4: 1 with 0.66 g boron powder after first being cleaned 3.98 g diamond surfaces Discharge plasma sintering furnace is placed in graphite jig cavity, and by graphite jig;Wherein diamond grit is 50 mesh, boron powder Degree is 500 mesh;Diamond surface carries out cleaning process are as follows: diamond is placed in nitric acid, is boiled in hydrochloric acid mixed solution under magnetic agitation 30min is boiled, then rinses diamond taking-up deionized water 2 times, this process purpose is the grease for removing diamond surface, is removed Oily process is stirred using magnetic stirring apparatus;
(2) by discharge plasma sintering stove evacuation to vacuum degree less than 100 Pa, 10 MPa are pressurized to graphite jig cavity, Temperature is risen into 1300 DEG C of 12 min of heat preservation, furnace cooling.Wherein control heating speed is 100 DEG C/min;Wherein to graphite Cavity body of mould is pressurized to 10 MPa, pressurizes after being 100 Pa from vacuum degree, and constant pressure keeps to sintering terminating;Wherein mixture is clear Wash step are as follows: the mixture after being ground up, sieved is placed in dust technology under magnetic agitation and boils 5 min of cleaning, then by diamond Taking-up is cleaned by ultrasonic 10 min in deionized water.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept Put that various changes can be made.

Claims (6)

1. a kind of preparation method of plating boron carbide diamond abrasive grain, it is characterised in that steps are as follows:
(1) with boron powder according to volume ratio 4:(0.5 ~ 1.5 after diamond surface being cleaned) it is uniformly mixed and is placed on graphite mo(u)ld Have in cavity, and graphite jig is placed in discharge plasma sintering furnace;
(2) it will be evacuated to vacuum degree in discharge plasma sintering furnace less than 100 Pa, 10 are pressurized to graphite jig cavity Temperature is risen to 1200 ~ 1400 DEG C of 10 ~ 15min of heat preservation by MPa, and cool down furnace cooling later;
(3) sintered mixture is ground up, sieved and is cleaned, the Buddha's warrior attendant for being coated with boron carbide to surface is obtained after vacuum drying Stone.
2. the preparation method of plating boron carbide diamond abrasive grain according to claim 1, it is characterised in that: the step (1) diamond grit is 30 ~ 60 mesh in, and boron Powder Particle Size is 300 ~ 1000 mesh.
3. the preparation method of plating boron carbide diamond abrasive grain according to claim 1, it is characterised in that: the step (1) process that diamond surface is cleaned in are as follows: diamond is placed in nitric acid, is boiled under magnetic agitation in hydrochloric acid mixed solution Then 30min rinses diamond taking-up with deionized water.
4. the preparation method of plating boron carbide diamond abrasive grain according to claim 1, it is characterised in that: the step (2) In, control heating speed is not less than 80 DEG C/min.
5. the preparation method of plating boron carbide diamond abrasive grain according to claim 1, it is characterised in that: the step (2) In, pressure applying mode are as follows: after system vacuum is less than 100 Pa, 10 MPa are pressurized to graphite jig cavity, and constant pressure is protected Holding to sintering terminates.
6. the preparation method of plating boron carbide diamond abrasive grain according to claim 1, it is characterised in that: the step (3) Mixture cleaning step after middle sintering are as follows: the mixture after being ground up, sieved is placed in dust technology and boils cleaning under magnetic agitation, Then diamond taking-up is cleaned by ultrasonic in deionized water.
CN201811269336.2A 2018-10-29 2018-10-29 A kind of preparation method of plating boron carbide diamond abrasive grain Pending CN109293393A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110643327A (en) * 2019-10-17 2020-01-03 江苏吉星新材料有限公司 Preparation method of sapphire wafer grinding fluid

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EP0313323A1 (en) * 1987-10-21 1989-04-26 Takeo Oki Coated abrasive grains and a manufacturing method therefor
EP0360305A2 (en) * 1985-12-24 1990-03-28 Sumitomo Electric Industries, Ltd. Process for producing particles of a composite material, and their use
CN1836057A (en) * 2003-08-15 2006-09-20 元素六(私人)有限公司 Boron coated abrasives
JP2009062607A (en) * 2007-09-10 2009-03-26 Sumitomo Electric Ind Ltd Coated body
CN102046564A (en) * 2008-05-16 2011-05-04 六号元素(产品)(控股)公司 Boron carbide composite materials
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EP0360305A2 (en) * 1985-12-24 1990-03-28 Sumitomo Electric Industries, Ltd. Process for producing particles of a composite material, and their use
EP0313323A1 (en) * 1987-10-21 1989-04-26 Takeo Oki Coated abrasive grains and a manufacturing method therefor
CN1836057A (en) * 2003-08-15 2006-09-20 元素六(私人)有限公司 Boron coated abrasives
JP2009062607A (en) * 2007-09-10 2009-03-26 Sumitomo Electric Ind Ltd Coated body
CN102046564A (en) * 2008-05-16 2011-05-04 六号元素(产品)(控股)公司 Boron carbide composite materials
CN104591783A (en) * 2015-01-29 2015-05-06 吉林大学 Method for plating boron carbide on diamond surface
CN106032555A (en) * 2015-03-18 2016-10-19 中国科学院宁波材料技术与工程研究所 Granular material and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110643327A (en) * 2019-10-17 2020-01-03 江苏吉星新材料有限公司 Preparation method of sapphire wafer grinding fluid

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