CN109502582A - A kind of method of diamond perfectly roundization processing - Google Patents
A kind of method of diamond perfectly roundization processing Download PDFInfo
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- CN109502582A CN109502582A CN201811576171.3A CN201811576171A CN109502582A CN 109502582 A CN109502582 A CN 109502582A CN 201811576171 A CN201811576171 A CN 201811576171A CN 109502582 A CN109502582 A CN 109502582A
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention discloses a kind of methods of diamond perfectly roundization processing, belong to diamond shaping process field.It is main that anisotropic etching realization is carried out to the diamond after surface treatment using vanadium oxide, it can specifically be divided into diamond surface processing, etching agent and diamond blending, heat treatment, purification four steps of diamond.The present invention can carry out perfectly roundization processing to diamond without using modes such as mechanical ball mills, with high-efficient, it is at low cost, the advantage being easy without expensive device technology innovation, unexpectedly also in the hole by this method treated diamond surface discovery triangle, the hole facilitates holding of the bonding agent to diamond, improves life tools.
Description
Technical field
The invention patent relates to diamond shaping processing technology field, especially a kind of diamond perfectly roundization processing technique.
Background technique
Perfectly roundization diamond is that a kind of round and smooth spherical shape in surface handled by diamond surface perfectly roundization is high-intensitive
Diamond, especially suitable for tools such as geological drill bit, disc type trimmer, contact roller for dressing.In boring tool, perfectly round diamond can
To extend the service life of tool well；In dressing tool, the finishing effect of higher precision is may be implemented in perfectly round diamond.
The perfectly round chemical industry sequence of diamond is that the key link of diamond, the perfectly roundization place being widely used at present are pre-processed during manufacturing drill bit
Reason method mainly mechanically makes diamond particles, and mill is hit mutually under the promotion of external force, so that its corner angle be made to become round
It is sliding.
However diamond have high hardness and wearability, mechanically carry out perfectly roundization handle it is time-consuming and laborious and
It is serious to equipment loss, thus need to provide a kind of method of efficient diamond perfectly roundization processing.
Summary of the invention
It is time-consuming and laborious at high cost to diamond progress perfectly roundization processing based on the mode of mechanical lapping and tight to equipment loss
The disadvantage of weight, it is an object of the invention to: to diamond progress perfectly roundization processing, raising processing by way of specificity etching
Efficiency reduces processing cost, reduces the loss in diamond treatment process to equipment, it is even more important that the quarter of diamond
Erosion generally believes that needs are carried out in starvation or under being passed through protective atmosphere, and the technical program without starvation or is passed through
Protective atmosphere；The technical program is without the processing equipment for using the valuableness such as plasma etching machine.
The inventive concept of the technical solution carries out anisotropic etching to diamond using etching agent, using etching agent to gold
Hard rock difference crystal face etch rate difference carries out perfectly roundization processing to achieve the purpose that eliminate diamond corner angle to diamond.Hair
Bright people chances on during the experiment, vanadic anhydride can to the modified diamond in surface realize anisotropic etching from
And realize diamond perfectly roundization, the detailed process of the program can be divided into four steps, step 1: diamond surface processing；Step
Rapid two, diamond and etching agent are blended；Step 3: heat treatment；Step 4: purification diamond.
In order to realize that the purpose of the present invention, the particular technique feature of each step are as follows.
Step 1, diamond surface processing, it is characterised in that treated diamond surface is without greasy dirt, no solid or liquid
Impurity residual, and the Raman spectrum of treated diamond has peak near 1418cm-1.
Step 2, etching agent and diamond are blended, and major way is to be placed in diamond in vanadium-containing compound to stir
It is even, drying and processing is carried out later.
Step 3, heat treatment, the material of mixed drying is placed in heatproof container, is heated, and heating final temperature exists
Between 660 DEG C to 795 DEG C.
Step 4, purification of diamond, will treated diamond and etching agent separation, preferably with sodium hydroxide solution or
Oxalic acid solution is purified.
It is to be noted that following " part " is to be defined as 1 part with the weight of diamond, it is only used for expressing between each material
Weight ratio, be not used in limit its specific quality.
Preferably, the detailed process of step 1 are as follows: surface treatment can be divided into purification and two stages of hydrogenation, purification process
Be by a diamond as mass fraction be 8% ~ 19% sodium hydroxide solution in boil 20 to 80 minutes after be washed till neutrality, should
Purifying step, which also can be used after acetone cleans diamond, dries；Hydrogenation process is that purified diamond is placed in strong acid
Property solution in boil 7 to 99 minutes, clean later, the strongly acidic solution be preferably mass fraction be 20% to 38% nitric acid
With 2% to 5% mixed solution of hydrogen peroxide, the mixed acid solution of acid of hydrochloric acid and nitric acid volume ratio 1:0.2 ~ 3 also can be used, need to illustrate
It is the purpose of hydrogenation can also to be realized using other kinds of acid, but effect is slightly poor, of the invention is not limited to using above two molten
Liquid, the acid solution that diamond Raman spectrum 1418cm-1 can be made nearby peak occur after other processing should all fall within guarantor of the invention
Within the scope of shield.
Preferably, the detailed process of step 2 is weight to be remembered to 1 part of step 1 treated diamond and 2 parts to 8 parts contain
The direct mechanical mixture of vfanadium compound is uniform, and mixed material in baking oven at a temperature of 80 DEG C to 220 DEG C as drying.More into one
The preferred embodiment of step is that will remember to be aged after 4 parts to 10 parts oxalic acid and 2 parts to 8 parts vanadium-containing compounds are configured to solution with weight
30min to 150min, until 1 part of step 1 of addition is made solution to dark blue-green, then into the solution after ageing in navy blue
Diamond, be uniformly mixed, mixed material in baking oven at a temperature of 80 DEG C to 220 DEG C as drying.Further
Ground can also be added 0.02 part to 0.2 part calcirm-fluoride as additive and improve perfectly roundization effect.
It should be pointed out that the vanadium-containing compound refers to the substance that can form vanadic anhydride after the heating, it is unlimited
It is set to pure substance, can be the mixture of many kinds of substance, preferably contains vanadyl oxalate acid ammonium, vanadyl oxalate, vanadium oxide, vanadium
One of sour ammonium is a variety of.It should be pointed out that solution described in leading portion is only to help this hair in navy blue to dark blue-green
Bright implementation personnel judge the foundation that ageing is completed, and the present invention are not defined.
Preferably, the heating process of step 3 uses two-stage method, specifically keeps the temperature under the conditions of 280 DEG C to 450 DEG C first
30min to 150min is continuously heating to 660 DEG C to 795 DEG C later, keeps the temperature 45min to 330min.It can make to contain in heating process
There is the container rotation of material to reach better perfectly roundization effect.
Preferably, if step 2 joined calcirm-fluoride, the second stage temperature of step 3 should 660 DEG C to 755 DEG C it
Between.
It is further preferred that step 4, which carries out purification to diamond using oxalic acid solution, may be implemented the recycling benefit of etching agent
With detailed process is to be placed in the material after the reaction configured according to aforementioned ratio in the solution that 4 parts configure to 10 parts of oxalic acid, is fitted
Work as stirring, filtered after only remaining diamond precipitating, filtrate can be when handling diamond next time as vanadium-containing compound, gold
Hard rock is dried after being washed till neutrality with clear water, and perfectly roundization diamond can be obtained.
Unexpectedly, by this method carry out perfectly roundization treated diamond surface can hole, these holes generally in
Triangle arrives triangular pyramid, these holes can make to form anchoring combination between diamond and bonding agent, helps to improve knot
Mixture improves the service life of tool to the holding power of diamond.
The beneficial effects of the present invention are:
1. improving efficiency without carrying out perfectly roundization processing to diamond by mechanical systems such as ball millings, reducing equipment loss, reduce
Cost；
2. technology innovation is at low cost without using expensive device；
3. reducing potential security risk without being passed through hydrogen, it is not necessarily to atmosphere protection, reduces cost；
4. the diamond surface that unexpectedly, the present invention obtains has also appeared hole, which is conducive to bonding agent to diamond
It holds, improves tool life.
Detailed description of the invention
Fig. 1 is the whole shape appearance figure for the perfectly roundization diamond that embodiment 1 obtains.
Fig. 2 is the partial enlarged view for the perfectly roundization diamond surface hole that embodiment 1 obtains.
Fig. 3 is original diamond surface Raman spectrogram in embodiment 1.
Fig. 4 is step 1 treated diamond surface hand-pulled noodles spectrogram in embodiment 1.
Specific embodiment
The invention is described further below in conjunction with specific embodiment:
Embodiment 1:
It cleans, adds after twenty minutes Step 1: diamond 0.2g is put into boil in the sodium hydroxide that 50ml mass fraction is 30%
It is to be cleaned after being boiled 30 minutes in 30% nitric acid and 2% mixed solution of hydrogen peroxide to 50ml mass fraction, diamond in the embodiment
Before and after the processing both Raman spectrum has apparent peak as shown in Fig. 3 and Fig. 4 in Figure of description at 1331cm-1, and Fig. 4 is aobvious
Show, by this process treated diamond than untreated diamond the more one more wide scattered peak near 1418cm-1；
Step 2: stirring and dissolving in 10ml water is added in 1g ammonium metavanadate and 1.6g oxalic acid, stands 55min and obtain solution；To institute
Solution is added by step 1 treated diamond, stir evenly and be put into baking oven in 120 DEG C of heat preservation 120min drying；
Step 3: step 2 resulting material is placed in corundum crucible, it is heated with Muffle furnace, with 5 DEG C/min's
Rate keeps the temperature 60min after being warming up to 450 DEG C, be warming up to 710 DEG C of heat preservation 100min again after the completion of heat preservation with the rate of 5 DEG C/min,
Furnace cooling after heat preservation.
It is filtered Step 4: the resulting product of step 3 is added in the oxalic acid solution that mass fraction is 20% after heating stirring,
Filtrate retains, and the diamond filtered is cleaned with clear water, dries, and can obtain the diamond of perfectly roundization processing, diamond
Pattern is as shown in Figure 1, it can be seen that the corner angle of diamond script have disappeared, and shape becomes almost spherical, and can be in { 111 }
It is observed on face by triangle hole, diamond is overturn, as shown in Fig. 2, can see after being amplified to one of hole
There is apparent hole configurations by the diamond that this method obtains out.
Embodiment 2:
Step 1: by diamond 0.2g be put into 50ml mass fraction be 25% sodium hydroxide in boil 28 minutes after clean, add
It is to boil to clean after forty minutes in 28% nitric acid and 3% mixed solution of hydrogen peroxide to 40ml mass fraction；
Step 2: stirring and dissolving in 25ml water is added in 1g ammonium metavanadate, 1.7g oxalic acid and 0.04g calcirm-fluoride, stands 30min and obtain
To solution；It is added to acquired solution by step 1 treated diamond, stirs evenly to be put into baking oven and kept the temperature at 110 DEG C
90min drying；
Step 3: step 2 resulting material is placed in corundum crucible, it is heated with Muffle furnace, and in heating process
Rotate crucible automatically, revolving speed is about 35 r/min, keeps the temperature 45min after being warming up to 390 DEG C with the rate of 4 DEG C/min, has kept the temperature
Cheng Houzai is warming up to 695 DEG C of heat preservation 100min, furnace cooling after heat preservation with the rate of 5 DEG C/min.
It is filtered Step 4: the resulting product of step 3 is added in the oxalic acid solution that mass fraction is 15% after heating stirring,
Filtrate retains, and the diamond filtered is cleaned with clear water, dries, and can obtain the diamond of perfectly roundization processing.
Embodiment 3:
Step 1: by diamond 0.2g be put into 50ml mass fraction be 20% sodium hydroxide in boil 35 minutes after clean, add
It is to boil to clean after forty minutes in 30% nitric acid and 2% mixed solution of hydrogen peroxide to 50ml mass fraction；
Step 2: stirring and dissolving in 20ml water is added in 0.9g ammonium metavanadate, 2g oxalic acid and 0.05g calcirm-fluoride, stands 40min and obtain
To solution；It is added to acquired solution by step 1 treated diamond, stirs evenly to be put into baking oven and kept the temperature at 80 DEG C
120min drying；
Step 3: step 2 resulting material is placed in corundum crucible, it is heated with Muffle furnace, with 4 DEG C/min's
Rate keeps the temperature 60min after being warming up to 400 DEG C, be warming up to 690 DEG C of heat preservation 120min again after the completion of heat preservation with the rate of 7 DEG C/min,
Furnace cooling after heat preservation.
Step 4: the resulting product of step 3 is added in the sodium hydroxide solution that mass fraction is 20% after heating stirring
Filtering, the diamond filtered is cleaned with clear water, is dried, and the diamond of perfectly roundization processing can be obtained.
Claims (10)
1. a kind of method of diamond perfectly roundization processing, it is characterised in that realized by following steps:
Step 1: diamond surface is handled, the Raman spectrum of diamond is near 1331cm-1 and 1418cm-1 after the completion of processing
There is peak；Step 2: etching agent and diamond are blended, step 1 treated diamond is stirred evenly with vanadium-containing compound, it
After carry out drying and processing, the vanadium-containing compound refers to the substance that vanadium oxide can be formed after heating；Step 3: heat treatment, it will
The mixed material of step 2 is heated to 660 DEG C to 795 DEG C；Step 4: purification of diamond, diamond and etching agent are separated and cleaned
It can be obtained perfectly roundization treated diamond.
2. the method for diamond perfectly roundization processing according to claim 1, it is characterised in that: it is net that the step one, which is divided,
Change and two processes of hydrogenation, purification process are that diamond is boiled 20 minutes extremely by the sodium hydroxide solution for being 8% ~ 19% with mass fraction
Diamond is cleaned after 80 minutes, hydrogenation process is that purified diamond is placed in strongly acidic solution to boil 7 minutes to 99 points
It is cleaned after clock.
3. the method for diamond perfectly roundization processing according to claim 2, it is characterised in that: make in the hydrogenation process
Strongly acidic solution is the nitric acid that mass fraction is 20% to 38% and 2% to 5% mixed solution of hydrogen peroxide or acid of hydrochloric acid and nitric acid body
Mixed acid solution of the product than 1:0.2 ~ 3.
4. the method for diamond perfectly roundization according to claim 1 processing, it is characterised in that: the step two is specially
One treated diamond of the step of weight is remembered 1 part and 2 parts to the 8 parts direct mechanical mixtures of vanadium-containing compound are uniform, after mixing
Material as being dried at a temperature of 80 DEG C to 220 DEG C in baking oven；Or the step of weight remembered 1 part one, treated that diamond adds
Solution after entering the ageing that 4 parts to 10 parts oxalic acid and 2 parts to 8 parts vanadium-containing compounds are configured to, is uniformly mixed, mixed
Material in baking oven at a temperature of 80 DEG C to 220 DEG C as drying.
5. the method for diamond perfectly roundization according to claim 4 processing, it is characterised in that: the vanadium-containing compound is
One of vanadyl oxalate acid ammonium, vanadyl oxalate, vanadium oxide, ammonium vanadate are a variety of.
6. the method for diamond perfectly roundization processing according to claim 1, it is characterised in that: the step four uses hydrogen
Sodium hydroxide solution or oxalic acid solution purify diamond, and the resulting mixed material of step 3 is specifically added to the hydrogen of heat
In sodium oxide molybdena or oxalic acid solution, stirring is filtered to after only remaining diamond solid, is cleaned followed by with water to gained diamond.
7. the method for diamond perfectly roundization processing according to claim 1, it is characterised in that: first at 280 DEG C to 450 DEG C
Under the conditions of keep the temperature 30min to 150min, be continuously heating to 660 DEG C to 795 DEG C later, keep the temperature 45min to 330min.
8. according to the method for the diamond perfectly roundization processing any in claim 7, it is characterised in that: the step three
Material is rotated in heating in the process.
9. according to claim 1 to the method for any diamond perfectly roundization processing in 8, it is characterised in that: with diamond
Weight be denoted as 1 part, 0.02 part to 0.2 part of calcirm-fluoride is also added into the step two.
10. the method for diamond perfectly roundization processing according to claim 9, it is characterised in that: the final temperature temperature of step 3
At 660 DEG C to 755 DEG C.
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| CN201811576171.3A CN109502582A (en) | 2018-12-22 | 2018-12-22 | A kind of method of diamond perfectly roundization processing |
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| CN201811576171.3A CN109502582A (en) | 2018-12-22 | 2018-12-22 | A kind of method of diamond perfectly roundization processing |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113308745A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of perforated diamond |
| CN115322747A (en) * | 2022-07-18 | 2022-11-11 | 上海昌润极锐超硬材料有限公司 | Rounded diamond and preparation method and application thereof |
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| US20100213175A1 (en) * | 2009-02-22 | 2010-08-26 | General Electric Company | Diamond etching method and articles produced thereby |
| CN106925775A (en) * | 2017-04-17 | 2017-07-07 | 河南工业大学 | A kind of method of diadust plated surface chromium carbide |
Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113308745A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | Preparation method of perforated diamond |
| CN115322747A (en) * | 2022-07-18 | 2022-11-11 | 上海昌润极锐超硬材料有限公司 | Rounded diamond and preparation method and application thereof |
| CN115322747B (en) * | 2022-07-18 | 2024-06-28 | 上海昌润极锐超硬材料有限公司 | Round diamond and preparation method and application thereof |
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