CN100551879C - Cubic boron nitride surface sol-gal process plating TiO 2/ Al 2O 3Laminated film technology - Google Patents
Cubic boron nitride surface sol-gal process plating TiO 2/ Al 2O 3Laminated film technology Download PDFInfo
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- CN100551879C CN100551879C CNB2006101368410A CN200610136841A CN100551879C CN 100551879 C CN100551879 C CN 100551879C CN B2006101368410 A CNB2006101368410 A CN B2006101368410A CN 200610136841 A CN200610136841 A CN 200610136841A CN 100551879 C CN100551879 C CN 100551879C
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- boron nitride
- cubic boron
- tio
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Abstract
A kind of cubic boron nitride surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology the steps include: cubic boron nitride abrasive materials immersed and carried out surface activation process in the certain density hot nitric acid about 1 hour, is neutral with clear water flushing abrasive surface to cleaning fluid again; In medium-acetone, cleaned abrasive surface about 1 hour with the certain frequency ultrasonic wave; Use TiO
2About 3 minutes of the cubic boron nitride abrasive materials of the above-mentioned processing of sol impregnation process; Pull out, after the oven dry, about 550 ℃ of roastings 1 hour; Cool off with stove; Use again Al
2O
3Sol impregnation is pulled out, and oven dry repeats this step 3 twice; After the abrasive material oven dry, about 1 hour of about 800 ℃ of roastings; With the stove cooling, obtain the final cubic boron nitride abrasive materials that is coated with described laminated film.When preparing vitrified bonded grinding wheel with the cubic boron nitride abrasive materials behind the plated film, abrasive material and vitrified bond have good wetability, can significantly increase the service life of ceramic abrasive tool.
Description
Technical field
The present invention relates to a kind of cubic boron nitride abrasive materials process for modifying surface, especially can be at the firmly uniform plating one deck TiO in cubic boron nitride surface
2/ Al
2O
3Ceramic composite film.
Background technology
At present, commercial cubic boron nitride abrasive materials process for modifying surface is to utilize electrochemical plating at abrasive surface plating layer of metal simple substance, modal metal plating has Ti, Ni, Cr etc., but when using cubic boron nitride and preparing ceramic abrasive tool with metal plating, metal plating and ceramic bond wettability are bad, and the grinding tool durability is poor.Therefore can be for the wettability of improving cubic boron nitride abrasive materials and ceramic bond at abrasive surface plating ceramic coating, existing film coating method has the steam plated film, collosol and gel plated film and physical vapor deposition.Wherein the sol-gal process filming process is the simplest, existing the successful plating individual layer Al in cubic boron nitride surface
2O
3Film.Although Al
2O
3Film can protect cubic boron nitride abrasive materials not to be subjected to the erosion of alkali metal oxide in the vitrified bond in sintering process, and the cubic boron nitride abrasive materials behind the plated film and the wetability of vitrified bond have had very big improvement simultaneously, but Al
2O
3Film and cubic boron nitride basal body interface adhesion a little less than, the in use inefficacy of CBN shows as coming off of cubic boron nitride abrasive grain.
Summary of the invention
The technical problem to be solved in the present invention is for the deficiency that prior art exists, to propose a kind of cubic boron nitride surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology, this technology adopt earlier sol-gal process at cubic boron nitride abrasive grain coating surface TiO
2Film, and then be coated with TiO
2The cubic boron nitride surface of film utilizes sol-gal process plating one deck Al
2O
3Film, when preparing vitrified bonded grinding wheel with the cubic boron nitride abrasive materials behind the plated film, abrasive material and vitrified bond have good wetability, can significantly increase the service life of ceramic abrasive tool.
Technical solution of the present invention is described cubic boron nitride surface sol-gal process plating TiO
2/ Al
2O
3The step of laminated film technology is:
(1) cubic boron nitride abrasive materials being immersed temperature is that 75 ℃-85 ℃, concentration are in the hot nitric acid of 85%-88%, and activation treatment is carried out on the surface, and the treatment time is 0.8-1.2 hour, uses the flushing with clean water abrasive surface then, is neutral until scavenging solution; Be the ultrasonic wave of 70KHz-90KHz with frequency again, in medium-acetone, cleaned abrasive surface 0.8-1.2 hour;
(2) use TiO
2Sol impregnation is through above-mentioned surface-treated cubic boron nitride abrasive materials, and dipping time is 2.5-3.5 minute; Then with abrasive material from TiO
2Pull out in the colloidal sol, at 95 ℃-105 ℃ down after the oven dry, 530 ℃-570 ℃ roasting 0.8-1.2 hour; Furnace cooling, obtaining coated with uniform has TiO
2The cubic boron nitride abrasive materials of film;
(3) use Al
2O
3The described surface of sol impregnation is coated with TiO
2Cubic boron nitride abrasive materials, dip time is 2.5-3.5 minute, then with abrasive material from Al
2O
3Pull out in the colloidal sol, 95 ℃-105 ℃ lower oven dry;
(4) repeat above-mentioned steps 3 twice;
(5) with abrasive material after 95 ℃ of-105 ℃ of oven dry, 780 ℃-820 ℃ roasting 0.8-1.2 hour; With the stove cooling, obtain the final Al that is coated with
2O
3-TiO
2The cubic boron nitride abrasive materials of laminated film.
The used TiO of the present invention
2The preparation method of colloidal sol can be, adopt butyl (tetra) titanate as organic precursor, butyl (tetra) titanate and ethanol are pressed 4: 1 mixed of mass ratio, high-speed stirring (1000 rev/mins) 3 hours, drip the ratio adding distilled water of 1 ml water then in per 50 milliliters of mixed solutions, high-speed stirring is 1 hour again, utilizes the hydrolysis of butyl (tetra) titanate to prepare stable TiO
2Colloidal sol is with TiO
2Colloidal sol was at room temperature placed 24 hours, came into operation.
The used Al of the present invention
2O
3The preparation method of colloidal sol can be, with aluminium isopropoxide as organic precursor, with aluminium isopropoxide and ethanol in mass ratio 1: 1 ratio mixed high-speed stirred 3 hours, dripping hydrochloric acid in the mixed liquor then, concentration of hydrochloric acid is the 1mol/ liter, when the pH value of solution stops dripping hydrochloric acid less than 3 the time, high-speed stirred is 1 hour again, utilizes the hydrolysis of aluminium isopropoxide to prepare Al
2O
3Colloidal sol is with Al
2O
3Colloidal sol was at room temperature placed 72 hours, came into operation.
The present invention adopts sol-gal process, and elder generation is at the TiO of cubic boron nitride abrasive materials coating surface one deck densification
2Film has TiO at plating again
2Cubic boron nitride abrasive materials coating surface one deck Al of film
2O
3Film.Utilize the Al on abrasive particle surface
2O
3Film is protected time outer field TiO
2Film and cubic boron nitride abrasive grain are not subjected to the erosion of vitrified bond in sintering process, with improving the hold of bond to abrasive material.Utilize TiO
2Film serves as Al
2O
3Transition zone between film and the cubic boron nitride matrix increases substantially Al
2O
3The bond strength of film and cubic boron nitride.As known from the above, the present invention is cubic boron nitride surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology, it can be implemented in the Al that cubic boron nitride abrasive materials coats one deck densification
2O
3-TiO
2Laminated film (referring to Fig. 1); When preparing vitrified bonded grinding wheel with the cubic boron nitride abrasive materials behind the plated film, abrasive material and vitrified bond have good wetability, as shown in Figure 2, can significantly increase the service life of ceramic abrasive tool.
Description of drawings
Fig. 1 is the configuration of surface photo of the cubic boron nitride abrasive materials behind the plated film;
Fig. 2 is the microstructure photograph of the vitrified bonded grinding wheel of the cubic boron nitride abrasive materials preparation behind the plated film.
Embodiment
Cubic boron nitride of the present invention surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology, its process is:
Earlier cubic boron nitride abrasive materials being immersed temperature is 80 ℃, concentration is in 85% the hot nitric acid, effects on surface carries out activation process, processing time is 1 hour, wash abrasive surface with clear water again, until cleaning fluid is neutral, use at last the ultrasonic wave of frequency 80KHz, in medium-acetone, cleaned abrasive surface 1 hour;
Adopt butyl (tetra) titanate as organic precursor, butyl (tetra) titanate and ethanol are pressed 4: 1 mixed of mass ratio, high-speed stirring (1000 rev/mins) 3 hours, drip the ratio adding distilled water of 1 ml water then in per 50 milliliters of mixed solutions, high-speed stirring is 1 hour again, utilizes the hydrolysis of butyl (tetra) titanate to prepare stable TiO
2Colloidal sol is with TiO
2Colloidal sol is at room temperature placed 24 hours, and is standby;
Dipping carried out the cubic boron nitride abrasive materials of above-mentioned surface activation process then, and dipping time is 3 minutes, again with abrasive material from TiO
2Pull out in the colloidal sol, dry the back down 550 ℃ of roastings 1 hour at 100 ℃, furnace cooling, obtaining coated with uniform has TiO
2The cubic boron nitride abrasive materials of film;
With aluminium isopropoxide as organic precursor, with aluminium isopropoxide and ethanol in mass ratio 1: 1 ratio mixed high-speed stirred 3 hours, dripping hydrochloric acid in the mixed liquor then, concentration of hydrochloric acid is the 1mol/ liter, when the pH value of solution stops dripping hydrochloric acid less than 3 the time, high-speed stirred is 1 hour again, utilizes the hydrolysis of aluminium isopropoxide to prepare Al
2O
3Colloidal sol is with Al
2O
3Colloidal sol is at room temperature placed 72 hours, and is for subsequent use;
Use Al
2O
3The sol impregnation surface is coated with TiO
2Cubic boron nitride abrasive materials, dip time is 3 minutes, then with abrasive material from Al
2O
3Pull out in the colloidal sol, 100 ℃ of lower oven dry;
Again according to above-mentioned dipping Al
2O
3The step of colloidal sol repeats 2 times;
With abrasive material after 100 ℃ of oven dry 800 ℃ of roastings, the time is 1 hour, obtains the final Al that is coated with stove cooling
2O
3-TiO
2The cubic boron nitride abrasive materials of laminated film.
Claims (3)
1, a kind of cubic boron nitride surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology is characterized in that, its step is:
(1) cubic boron nitride abrasive materials being immersed temperature is that 75 ℃-85 ℃, concentration are in the hot nitric acid of 85%-88%, and activation treatment is carried out on the surface, and the treatment time is 0.8-1.2 hour, uses the flushing with clean water abrasive surface then, is neutral until scavenging solution; Be the ultrasonic wave of 70KHz-90KHz with frequency again, in medium-acetone, cleaned abrasive surface 0.8-1.2 hour;
(2) use TiO
2Sol impregnation is through above-mentioned surface-treated cubic boron nitride abrasive materials, and dipping time is 2.5-3.5 minute; Then with abrasive material from TiO
2Pull out in the colloidal sol, at 95 ℃-105 ℃ down after the oven dry, 530 ℃-570 ℃ roasting 0.8-1.2 hour; Furnace cooling, obtaining coated with uniform has TiO
2The cubic boron nitride abrasive materials of film;
(3) use Al
2O
3The described surface of sol impregnation is coated with TiO
2Cubic boron nitride abrasive materials, dip time is 2.5-3.5 minute, then with abrasive material from Al
2O
3Pull out in the colloidal sol, 95 ℃-105 ℃ lower oven dry;
(4) repeat above-mentioned steps (3) twice;
(5) with abrasive material after 95 ℃ of-105 ℃ of oven dry, 780 ℃-820 ℃ roasting 0.8-1.2 hour; With the stove cooling, obtain the final Al that is coated with
2O
3-TiO
2The cubic boron nitride abrasive materials of laminated film.
2, according to the described cubic boron nitride of claim 1 surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology is characterized in that, described TiO
2The preparation method of colloidal sol is, adopt butyl titanate as organic precursor, with butyl titanate and in mass ratio 4: 1 ratio mixing of ethanol, with 100 rev/mins speed high-speed stirred 3 hours, drip then the ratio adding distilled water of 1 ml water in per 50 milliliters of mixed liquors, high-speed stirred is 1 hour again, utilizes the hydrolysis of butyl titanate to prepare stable TiO
2Colloidal sol is with TiO
2Colloidal sol is at room temperature placed 24 hours, and get final product.
3, according to the described cubic boron nitride of claim 1 surface sol-gal process plating TiO
2/ Al
2O
3Laminated film technology is characterized in that, described Al
2O
3The preparation method of colloidal sol is, with aluminium isopropoxide as organic precursor, with aluminium isopropoxide and ethanol in mass ratio 1: 1 ratio mixed high-speed stirred 3 hours, dripping hydrochloric acid in the mixed liquor then, concentration of hydrochloric acid is the 1mol/ liter, when the pH value of solution stops dripping hydrochloric acid less than 3 the time, high-speed stirred is 1 hour again, utilizes the hydrolysis of aluminium isopropoxide to prepare Al
2O
3Colloidal sol is with Al
2O
3Colloidal sol is at room temperature placed 72 hours, and get final product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101368410A CN100551879C (en) | 2006-12-11 | 2006-12-11 | Cubic boron nitride surface sol-gal process plating TiO 2/ Al 2O 3Laminated film technology |
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|---|---|---|---|
| CNB2006101368410A CN100551879C (en) | 2006-12-11 | 2006-12-11 | Cubic boron nitride surface sol-gal process plating TiO 2/ Al 2O 3Laminated film technology |
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| CN100551879C true CN100551879C (en) | 2009-10-21 |
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| CN103273434B (en) * | 2013-05-31 | 2015-05-27 | 湖南大学 | Ultrafine diamond and ceramic binding agent stacked abrasive materials and preparation method thereof |
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| JP6964821B2 (en) * | 2019-08-06 | 2021-11-10 | 住友電気工業株式会社 | Super-abrasive grain and super-abrasive wheel |
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| CN111485155A (en) * | 2020-06-09 | 2020-08-04 | 齐鲁工业大学 | (Ti, W) C-based metal ceramic cutting tool material added with alumina coated cubic boron nitride composite powder and preparation method thereof |
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| CN113149661A (en) * | 2021-04-27 | 2021-07-23 | 中国科学院兰州化学物理研究所 | Preparation method of high-density boron nitride self-lubricating composite ceramic |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Changsha IWADA Coating Technology Co Ltd Assignor: Hunan University Contract fulfillment period: 2009.11.18 to 2015.11.17 contract change Contract record no.: 2009430000214 Denomination of invention: Process of TiO#-[2]/Al#-[2]O#-[3] composite film deposited by sol-gel process on cubic boron nitride surface Granted publication date: 20091021 License type: Exclusive license Record date: 2009.12.1 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.11.18 TO 2015.11.17; CHANGE OF CONTRACT Name of requester: CHANGSHA YANTIAN COATING TECHNOLOGY CO., LTD. Effective date: 20091201 |
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Granted publication date: 20091021 Termination date: 20111211 |