CN105271180B - A kind of preparation method of Jubilee - Google Patents
A kind of preparation method of Jubilee Download PDFInfo
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- CN105271180B CN105271180B CN201510811362.3A CN201510811362A CN105271180B CN 105271180 B CN105271180 B CN 105271180B CN 201510811362 A CN201510811362 A CN 201510811362A CN 105271180 B CN105271180 B CN 105271180B
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Abstract
The invention provides a kind of preparation method of Jubilee, it is related to diamond manufacture technology field.The purity that the preparation method of the Jubilee includes the carbon extracted in crushing, further pickling, purification, the several steps of diamond cultivation, the preparation method for the Jubilee that the present invention is provided is very high, and additional carbon source is fewer during making diamond, economizes on resources.Present invention also offers a kind of carbon containing detection method of diamond made from above method.The carbon containing detection method can be using marking carbon to track the carbon in sample tissue, if being mixed into mark carbon in powder, and mark carbon can track whole purification process, more comprehensively proves the use of the carbon in sample tissue, relatively reliable；If being mixed into mark carbon in carbon crude product, it can quantify to identify the ratio of the carbon of the sample tissue retained in Jubilee by calculating.
Description
Technical field
The present invention relates to diamond manufacture technology field, in particular to a kind of preparation method of Jubilee.
Background technology
The deceased can be cremated, and the bone ash after cremate, into its unique voucher, is also that its family members kith and kin recalls the deceased's
Spiritual ballast.The consideration of the deceased is missed based on relatives, in the prior art, just has the carbon in the deceased's bone ash that will be obtained after cremate to carry
Take out and the operation of diamond be made, so that its relatives wears, and then recall the deceased, realize on spirit level, the deceased with its with
Hope.But of the prior art extract operates, the carbon that diamond cultivates purity requirement is met in order to extract, is to put the deceased mostly
It is placed in low-temperature space to be cremated, cremates incomplete, for its relatives, such a operation is a kind of operation for being contrary to ethics, very
There is a complete state to can not all allow the deceased.Also certain operations are exactly that gaseous state is constantly injected in diamond cultivating process
Carbon source is flowed, 5 ~ 50kg carbon source is typically necessary, and all there was only 1 ~ 2kg carbon sources in the bone ash of adult, in order to meet diamond
The purity requirement of the carbon of cultivation, so needing additional substantial amounts of carbon source.
In addition, being extracted to the carbon contained in life entity there is also very big difficulty, because mostly in existing industry is pin
The plurality of heavy metal salt and silicate contained in oil or mineral is extracted, and the material contained in life entity is mainly
Sclerotin, carbohydrate, protein etc., so existing extracting mode is extracted also and do not applied to for the carbon in life entity.Moreover, to life
Carbon in life body is extracted, and the purity of wherein keratin also can only achieve 30 ~ 50%（Such as patent US20080145299A1）, head
The purity of hair also can only achieve 98 ~ 99%（Such as patent WO2009091285A1）, cultivated to be applied to diamond, it is such
The purity of carbon is low-down, even if the biological carbon of purity 99% is cultivated for diamond, all also needs to high-purity work of 40 times of addition
Industry graphite, could obtain the carbon that purity is 99.975%.
Therefore, the technology of existing carbon purification is still not mature enough, for how to extract high-purity from life entity
Carbon is even more to require study.
The content of the invention
In view of this, the invention provides a kind of preparation method of Jubilee and the carbon containing detection side of obtained diamond
Method is existing low from purity of the life entity containing the carbon extracted in bone tissue to improve, it is difficult to meet diamond and make asking for requirement
Topic.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of Jubilee, comprises the following steps：
A. sample tissue is crushed, powder is obtained；
B. the powder is added into percentage by weight to be dissolved in 5 ~ 75% acid solution, after 20 ~ 120min of mixing, adjusted
The pH value for saving the carbon crude product is 6 ~ 7, obtains carbon crude product；
C. the carbon crude product is further purified using the one or more in high temperature graphitization purification, chloridising roasting
Removal of impurities；
D. HTHP gradient method is passed through（HPHT）Cultivate diamond.
Relative to prior art, the present invention includes following beneficial effect：The present invention is first carried to the carbon in sample tissue
It is pure, then crystal seed cultivation is carried out to the carbon of purification, cultivated into Jubilee.In step a, powder first is carried out to sample tissue
Broken, because the small purification for being more beneficial for later stage carbon of its particle diameter, in stepb, pickling can remove the alkali that may contain in powder
Property element, alkaline impurities are removed, while also avoiding the possibility that these alkaline impurities and carbon react.In abundant pickling
Afterwards, solution is adjusted to neutrality, effectively can avoided in end processing sequences, powder participates in other reactions.And in step c,
High temperature graphitization purification, chloridising roasting is recycled further to purify carbon crude product, the impurity that will can be remained in carbon crude product
Thoroughly removed.Extract after the higher carbon of purity, just utilize HTHP gradient method（HPHT）To cultivate diamond.
In the preparation method for the Jubilee that the present invention is provided, purification of the sample tissue Jing Guo several steps is extracted
The purity of carbon is very high, if so being applied to the extraction of human body carbon source, with regard to carrying out fire without the deceased is positioned over into low-temperature space
Change, so as to avoid the incomplete phenomenon of cremate.And this method can be made using without bone tissue and containing bone tissue, institute
Whole bone ashes after being cremated with the deceased may be incorporated for making culture diamond.And due to this method, can to extract purity very high
Carbon, so without additional too many carbon source, additional 40 times of carbon source is needed in the prior art, and extracted using this method
Carbon carry out diamond culture when, only need to add 5 ~ 10 times of carbon source, greatly reduce the addition of carbon source, saved resource, be
A kind of Optimal improvements.
Preferably, in the preparation method of above-mentioned Jubilee, if the sample tissue is without bone tissue, the method crushed
For：It will first be dried without bone tissue isolation air to its water content below 30%, and then be crushed to particle diameter below 20 μm；
If the sample tissue is containing bone tissue, the method crushed is：The grinding particle diameter containing bone tissue to 6.5 ~
25μm.For without bone tissue, having completely cut off the processing that air is dried again, effectively can having avoided in drying course, air
In impurity or other elements material contacted with without bone tissue so that the impurity avoided in air falls into no bone tissue
In, it also avoid under drying temperature, the other elements material in air is produced more miscellaneous with being reacted without bone tissue
Matter, or aoxidize without the carbon in bone tissue.For containing bone tissue, grinding advantageously in the purification of carbon.
Preferably, in the preparation method of above-mentioned Jubilee, if the sample tissue is without bone tissue, in the step
Include before the step b after a and also：The powder is put into container, completely cuts off air, and be passed through protective gas and go back
The air remained in the container is drained in former agent, and the powder then is heated into 600 ~ 1200 DEG C, and carbon is carried out at this temperature
Change reaction, then removal of impurities, obtain carbon crude product；
The reducing agent is reducibility gas or reducing metal, and the volume of the reducibility gas accounts for volume of gas
5 ~ 10%, the quality of the reducing metal accounts for the 2 ~ 8% of solid gross mass.It is main if sample tissue is without bone tissue, such a operation
Syllabus is exactly to occur carburizing reagent, generates simple substance carbon, while by the impurity elements such as hydrogen, oxygen, nitrogen phosphate and sulfur and excessive water
Divide and remove.In addition, the step is also the processing for completely cut off air, while protective gas and reducing agent have also been passed through, one
Aspect, eliminates the air remained in container, on the other hand, and the addition of reducing agent can be prevented effectively from high operating temperatures, powder
Carbon in material is oxidized, and the amount of reducing agent is controlled in less scope, so can also avoid the carbon in powder and reduction
Agent is reacted.The fusing point of the impurity elements such as hydrogen, oxygen, the nitrogen phosphate and sulfur that may contain in powder is very small, is completely cutting off the 600 of air
Under ~ 1200 DEG C of the condition of high temperature, these impurity elements are easily carbonized, and can be decomposed because heated, from the exhaust outlet of container gradually
It is discharged, in this way, these impurity elements can be just removed by high-temperature heating, and due to being to be organized as raw material with bone free, institute
May wherein contain, moisture is more, and at high temperature heat, moisture therein can also be evaporated.Certainly, slowly arranged in exhaust outlet
During gas, air inlet also slowly continues to be passed through protective gas, it is to avoid introduced contaminants gas enters from exhaust outlet, no
Cross, the foreign gas amount decomposited due to heated is very small, and discharge is slow, even if so be not passed through protective gas,
The entrance of introduced contaminants gas is not had substantially yet.
Preferably, in the preparation method of above-mentioned Jubilee, the step d high temperatures geopressure gradient method（HPHT）It is specific
Operate and be：Graphite is made in the obtained carbon pressures of step c, diamond is cultivated using superhigh-pressure high-temp method.Bored using such a method
Stone is cultivated, and cultivate effect is preferable.
Preferably, in the preparation method of above-mentioned Jubilee, also include after the step d：, will at 20 ~ 90 DEG C
Obtained diamond is placed in the concentrated nitric acid that percentage by weight is 40 ~ 60% or the concentrated sulfuric acid that percentage by weight is 70 ~ 90% and cleaned
Removal of impurities, until no longer produce bubble in solution, and the diamond surface without black attachment.Handled using concentrated acid, can
It is effective to remove the metal impurities for being attached to diamond surface, dissolve it in solution.
Preferably, in the preparation method of above-mentioned Jubilee, in the HTHP gradient method（HPHT）In cultivating process,
Also include processing of changing colour.By processing of changing colour, the diamond of different colours can be made, the market demand is met, is provided for consumer
More selections.
Preferably, in the preparation method of above-mentioned Jubilee, described change colour is processed as：To make white diamond, then exist
Denitrifier is added in cultivating process；To make diamond, then retain nickel element in cultivating process, and add lithium nitride or
Magnesium nitride；To make red colour system diamond, then after cultivation, using electron beam irradiation diamond, then the high temperature anneal is carried out；If
Blueness or Black Diamond are made, then retains boron element in cultivating process, and add denitrifier.Pass through different places of changing colour
Reason, can obtain the diamond of different colours, processing procedure of changing colour is simultaneously uncomplicated, it is easy to operate.
Preferably, in the preparation method of above-mentioned Jubilee, the cultivation of the diamond is extracted from 100% sample tissue
The carbon gone out.That is, diamond cultivates the carbon that carbon used can be extracted all from sample tissue, without external carbon
Source.
Preferably, addition supplement carbon is also needed in the preparation method of above-mentioned Jubilee, in the cultivating process.Supplement carbon energy
Enough carbon sources that abundance is provided in diamond cultivating process for seeded growth, it is ensured that the good generation of diamond.
Present invention also offers a kind of carbon containing detection method of diamond made from utilization above method, isotope marks are utilized
Method is detected that the isotope-labelling method concrete operations are：The 1% of sample tissue weight is added in the step a powder
~ 10% mark carbon, is well mixed, or adds the 1% ~ 10% of sample tissue weight in the carbon crude product after step c purification removal of impurities
Mark carbon, be well mixed, then by aoxidizing the powder of supplement carbon and the obtained diamond of oxidation, test and analyze respectively wherein
The content of carbon 13, if the content of carbon 13 is more than the content of carbon 13 in supplement carbon, obtained diamond in the powder of obtained diamond
In contain the carbon in sample tissue.
In diamond cultivating process, supplement carbon with the addition of（What it is generally as supplement carbon is all native graphite）, finally it is made
During diamond, also just containing supplement carbon in diamond, and supplement carbon and contain carbon 13 in itself, for the cultivation result of general diamond, addition
In the diamond that supplement carbon is cultivated, the content of carbon 13 is less than or equal to the content of carbon 13 in supplement carbon itself, so diamond
Carbon 13 in powder not can determine that it is from sample tissue, that is to say, that the carbon in diamond powder not can determine that it is to come from
Sample tissue.And the present invention has been sufficiently mixed mark carbon in powder or carbon crude product, mark the content of carbon 13 in carbon very high, institute
Will be more much higher than supplementing the content of carbon 13 of carbon with the content of carbon 13 that with the addition of in the diamond powder that mark carbon is obtained, mark carbon is again
The carbon in sample tissue is tracked, if so the content of carbon 13 illustrates more than the content for supplementing carbon 13 in carbon in diamond powder
Contain the carbon in sample tissue in diamond powder.Carbon 13 is the tracer element in the isotope-labelling method, by following the trail of spike
Element, you can whether detect in obtained Jubilee containing the carbon in sample tissue, verify the carbon source of Jubilee.If
Mark carbon is mixed into powder, then marks carbon to track whole purification process, more comprehensively can prove in sample tissue
Carbon use, if being mixed into mark carbon in carbon crude product, can by calculate, the guarantor for accurately drawing the carbon in sample tissue
Stay ratio.
In the present invention, if sample tissue is without bone tissue, when being completely cut off air drying, it may also be necessary to be passed through nitrogen
Gas or inert gas, to exclude oxygen.And in the carbonisation of the powder without bone tissue, the quality of powder and carburizing reagent
Time relationship is that the quality of powder is then incubated 0.5 ~ 1h in below 500g；The quality of powder is often incremented by 1 ~ 500g, soaking time
Then it is incremented by 0.01 ~ 1h on the basis of 1h.The protective gas that carbonisation is passed through is nitrogen or inert gas.
After the step a and before step b, in addition to dehydrated alcohol clean powder, filtering.The weight hundred of dehydrated alcohol
Divide ratio preferably 95 ~ 100%, the concrete operations washed with alcohol are：Powder is poured into the container equipped with dehydrated alcohol, repeats to dissolve
And be stirred continuously, then filter out solid matter.
After step a and before step b, in addition to elementary analysis is carried out to powder, when carrying out elementary analysis, Ke Yili
Analyzed with elemental analyser.
In stepb, the method for regulation pH value is：The strong basicity that percentage by weight is 5 ~ 35% is added in an acidic solution
Solution, regulation pH value is 6 ~ 7, then filters, the solid matter being filtrated to get is cleaned with distilled water.In acid cleaning process, if carbon
Crude product is less than 50g, then can extract carbon by filtering after regulation pH value, can be if carbon crude product is in more than 50g
Adjust after pH value, carbon crude product is dehydrated under 800 ~ 1500rpm using centrifuge, obtained solid matter is then put into perseverance
In warm drying oven, 20 ~ 90min is dried at 105 ~ 150 DEG C.And when adjusting the pH value of carbon crude product, it is possible to use distilled water is carried out
Regulation, can also utilize alkaline solution regulation.When using in alkaline solution with acid solution, the preferred potassium hydroxide of alkaline solution
Solution or sodium hydroxide solution because potassium ion, sodium ion are soluble in water, can in distilled water cleaning process the row of being rinsed
Go out, so as to avoid in N-process, other impurities element is introduced into carbon crude product.If sample tissue is bone or tooth
Tooth, then preferably handled for 30 ~ 85% phosphoric acid with percentage by weight, can generate calcium dihydrogen phosphate, be dissolved in water and divided
From.
High temperature graphitization purification method be：Carbon crude product is placed in graphitizing furnace, purified at 1800 ~ 3300 DEG C.It is high
Warm graphitization purification graphitizing furnace used can be acheson furnace, or inner string graphitization stove, preferably acheson furnace.And
Relation is between purification time of the carbon crude product in graphitizing furnace and the quality without bone tissue, the quality of carbon crude product 500g with
Under, then purify 0.5 ~ 1h；The quality of carbon crude product is often incremented by 1 ~ 500g, and the purification time is then incremented by 0.01 ~ 1h on the basis of 1h.
The method of chloridising roasting is：Carbon crude product is put into container, completely cuts off air, and be passed through chlorine or fluorine gas or hydrogen fluoride
Gas, excludes the air remained in container, is calcined at 1500 ~ 2800 DEG C.During chloridising roasting, chlorine is preferably pressed into, because
It is minimum to the pollution of environment for chlorine.And the mode being calcined can also be from the mode for vacuumizing roasting, i.e., in vacuum environment
Roasting is without bone tissue, and the pressure of vacuum environment is small, helps speed up the evaporation of metal chloride or metal fluoride.Carbon crude product
Relation is between roasting time and the quality of carbon crude product, and the quality of carbon crude product is then calcined 0.5 ~ 1h in below 500g；Carbon crude product
Quality is often incremented by 1 ~ 500g, and roasting time is then incremented by 0.01 ~ 1h on the basis of 1h.All it is first to rise to temperature during roasting
1500 ~ 2800 DEG C, then start to calculate roasting time.
When carrying out step c operation, in order to obtain the carbon that purity is more increased, carbon crude product can be subjected to high fire stons successively
Inkization is purified and chloridising roasting.
Utilizing HTHP gradient method（HPHT）When being cultivated, be under 1200 ~ 2500 DEG C, 1200 ~ 8000MPa,
The carbon extracted is all positioned over and is close to metal solvent, the side of diamond crystal seed, metal solvent can be urged from Ni-Mn-Co
Agent combination, Fe-Ni-Co catalyst combinations etc..And in diamond cultivating process, it is possible to use carbon is supplemented to mend carbon source
Fill, supplement carbon can be the carbon source that extracts of hair of the alive relatives of the deceased, can carry in the article that the deceased likes before death
The carbon source that plant extract in the Nature of the carbon source of taking-up, such as letter, down toy or symbol life goes out.Mend
When filling carbon and being supplemented, it can be in two layers of state with the carbon extracted in manufacturing process, overlay on the top of the carbon extracted,
The carbon extracted can be surrounded, in inverted " recessed " word state, the carbon extracted is fastened on inside.Certainly, if making
The carbon source of the carbon extracted in journey is enriched, then without supplementing again carbon, would not also use supplement carbon.HTHP ladder
Degree method（HPHT）During cultivation, it can be cultivated using the method for big crystal seed or many crystal seeds, cultivate the device used preferably Russian
BARS systems, U.S.'s Belt systems, belt type press, cubic hinge press.Because the grade of diamond is extremely important, manufacturing
During requirement to " matter " be more than requirement to " amount ", it is possible to cultivation situation is controlled by following main points：
（1）The speed of growth：The cultivation speed of general recommendations per hour, can obtain more excellent jewel close to 0.5 ~ 2 milligram
The rhinestone of level Ib types；In the case where denitrogenating agent use condition（The IIa type rhinestones of blueness, white）, it is high-quality to obtain
The diamond of high-grade cleanliness, speed of growth control needs more strictly, more slowly, to reach 0.05 ~ 0.5 milligram per hour；And
When need to cultivate more than 1 carat of diamond, the stage of crystallization is just started in diamond, above speed control, also need to slow down 30% ~ 60% with
On, to ensure the laboratory culture diamond of higher level.
（2）Thermograde is controlled：General thermograde control is at 5 ~ 45 DEG C, it is proposed that as far as possible below 20 DEG C, to obtain more
Plus stable growing environment, and reduce crystalline rate.
（3）Control accuracy：The relation control precision of pressure should reach 0.5%, and temperature relation control precision should reach 0.3%.
（4）Seed crystal is chosen：Using X-ray crystal orientation device, petrographic microscope examines seed crystal.To obtain high-grade diamond,
Crystal seed selection with（111）Aufwuchsplate is better than（100）Aufwuchsplate.Big crystal seed is better than small crystal seed, preferably more than 0.6mm import Gao Pin
Level hexakisooctahedron monocrystalline, but need to be cultivated under higher, longer stability and compared with narrow temperature gradient environment.
For the color of diamond, diamond can be obtained by processing of changing colour white, orange, yellow, green, blueness, black,
Peony, pink, brown etc..Using HTHP gradient method（HPHT）Diamond after cultivation, due to wherein there is nitrogen,
So generally can all show the color between the pale yellow section to orange red tone；By adding the reducing metals such as titanium, aluminium
Simple substance（Denitrifier）, white diamond can be obtained；By combining the nickel element retained in carbon source, lithium nitride or nitridation are added
Magnesium, can obtain diamond；Pass through the high-energy of electron beam（50~90keV）Treatment with irradiation, and later stage high annealing, can
It is different according to parameters such as irradiation time and energy to obtain N-V nitrogen void geometry colour centers, pink-dark red-rufous can be obtained
Diamond；By combining the boron element retained in carbon source, the denitrifiers such as reducing metal are added, blueness-Black Diamond can be obtained,
The number of boron content determines the different colours from light blue to dark blue to black.
In the present invention, as mark spike mark carbon do not require that absolute purity, as long as the content of its carbon 13 95% with
It is upper, so in the present invention, simple substance of the content of carbon 13 more than 95% can be ordered as mark carbon.Mark carbon be mixed into powder or
When in carbon crude product, the percetage by weight requirement of total carbon 13 reaches 1.2 ~ 95% in powder or carbon crude product.When mark carbon is added
Afterwards, it is possible to use mass spectrograph carries out initial analysis to powder or carbon crude product.Completed for cultivating, the diamond not yet polished,
Retain its powder in bruting process, the powder of acquisition is placed in a reservoir, be passed through pure oxygen and drain air, heating container to 800
DEG C, diamond powder is reacted with pure oxygen, the carbon dioxide for reacting generation is passed through into mass spectrograph is analyzed, and obtains carbon 13 in diamond
Content Atom%5, because existing supplement carbon typically uses the native graphite of native graphite, even different regions, wherein carbon
13 content difference is also and little, so determining the content Atom%4 of carbon 13 in supplement carbon, if Atom%5 is more than Atom%4, says
Contain the carbon in sample tissue in bright diamond.In addition, the existing mark carbon bought on the market is actually also not absolute purity,
It is sufficiently mixed so can name in mark carbon in the content Atom%1 of carbon 13, powder in the content Atom%2 of carbon 13, powder
Mark after carbon, the wherein content Atom%3 of carbon 13；The weight of carbon is that the weight of carbon in w1, sample tissue is in name mark carbon
w2；The ratio for naming carbon in sample tissue in diamond powder is p, can carry out verification and target data meter according to below equation
Calculate：
Atom%1*w1+Atom%2*w2=Atom%3*（w1+w2）；
Atom%4*（1-p）+Atom%3*p=Atom%5；
P=(Atom%5-Atom%4)/(Atom%3-Atom%4)；
Atom% data in above-mentioned formula can be determined individually, can also extrapolate some by after other data determinations
Data, w1, w2 data can also be extrapolated.
Due to typically with the addition of in the diamond that supplement carbon is cultivated, the content of carbon 13 is both less than or equal to supplement carbon itself
The content of middle carbon 13, it is possible to by marking carbon to determine in diamond containing the carbon in sample tissue.Even if some with the addition of benefit
Fill in the diamond that carbon is cultivated, the content of carbon 13 is higher than the content of carbon 13 in supplement carbon itself, gap therebetween also very little,
And add mark carbon after, the content of carbon 13 is very high in obtained diamond powder, with supplement carbon itself in carbon 13 content difference away from
It is very big, so still can be measured by such a method.
In the present invention, after the diamond is cleaned, can also polish diamond.The processing of polishing enables to diamond more to have light
Pool, more glitters brilliant.
After diamond polishing is good, to increase radium on the identifiability and commemoration meaning of diamond, diamond that can also be after dicing
Diamond numbering is penetrated, or scribes some personalized language, numeral, patterns.
In the present invention, if using bone free setup action sample tissue, can be after step b be carried out with regard to without being walked
Rapid c operation, directly can also carry out step c operation and omit step b operation.
Compared with prior art, beneficial effects of the present invention are：
（1）If being extracted using the dead ash obtained after cremate, obtained whole bone ashes are taken, it is ensured that life entity
The integrality of carbon, while also also avoiding the secondary burial to remaining bone ash certainly without remaining bone ash；
（2）Refining effect is good, and the purity of the carbon of extraction is very high, can reach 99.90% ~ 99.99%, applied to diamond training
Educate, its purity requirement can be reached；
（3）If the carbon extracted in obtained dead ash is cultivated into diamond, carried with for relatives, neither lose the deceased's body
Part it is honorable, the emotional connection between relatives can be strengthened again.Moreover, diamond is also likened as nature most firm material
The emotional connection such as diamond of people is firm, does not go out not bad, eternal beauty；
（4）If the carbon extracted in obtained dead ash is cultivated into diamond, funeral and interment land used can be also reduced, nature is saved
Resource, may advantageously facilitate environment sustainable development.
Brief description of the drawings
, below will be to embodiment or existing for the clearer explanation embodiment of the present invention or technical scheme of the prior art
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the preparation method process chart for the Jubilee that the embodiment of the present invention one is provided；
Fig. 2 is the view without diamond cultivation when supplementing carbon that the embodiment of the present invention one is provided；
Fig. 3 is the preparation method process chart for the Jubilee that the embodiment of the present invention two is provided；
Fig. 4 is the schematic diagram that the step b that the embodiment of the present invention two is provided carries out device used in anaerobic high-temperature roasting；
Fig. 5 is the schematic diagram for the acheson furnace that the embodiment of the present invention two is provided；
Fig. 6 is the structural representation for the firing chamber that the embodiment of the present invention two is provided；
Fig. 7 is the view that diamond is cultivated when the addition that the embodiment of the present invention two is provided supplements carbon；
Fig. 8 is the preparation method process chart for the Jubilee that the embodiment of the present invention three is provided；
Fig. 9 is the view that diamond is cultivated when the addition that the embodiment of the present invention three is provided supplements carbon；
Figure 10 is the schematic diagram for the cremator that the embodiment of the present invention three is provided.
Wherein, reference is summarized as follows：
Waste gas outlet 101；Temperature controller 102；Protective gas air inlet 103；Case lid 104；Casing 105；Graphite crucible 106；
Electric heater 107；
Electrode 201；Waste gas outlet 202；Waste liquid outlet 203；Bell 204；Body of heater 205；Ceramic foam oozes out layer 206；Sample
This 207；
Vacuum pump interface 301；Insulation crust 302；Electric induction coil 303；Reload window 304；Graphite crucible 305；Electric arc
Heater 306；Chlorine inlet 307；Region of no pressure 308；Insulate inner casing 309；Sample 310；
Air intlet 401；Gas outlet 402；Temperature sensor 403；Cremate bed 404；Furnace wall 405；Cremate room 406；It is close
Closure door 407；Convey roll shaft 408；Support 409；Oxidizing solids 410；
Supplement carbon 501；The carbon 502 that sample tissue is extracted；Metal solvent 503；Crystal seed 504；Brilliant bed 505.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
After being cremated due to the deceased's remains, cremation furnaceman is typically all to scan out a part from whole bone ashes to be put into cinerary casket,
So the whole bone ashes being previously mentioned in the present invention each mean the bone ash in the cinerary casket obtained by the deceased family members.As for what is be previously mentioned
In the prior art, the bone ash used in diamond is cultivated, this part bone ash also referred to, the part bone ash taken in the prior art refers to
The part bone ash taken from obtained bone ash, whole bone ash also refers to the whole bone ashes obtained in cinerary casket.
Bone ash in following examples is obtained by legal means.
Embodiment one
The preparation method that Fig. 1 shows the Jubilee that the embodiment of the present invention one is provided, sample tissue is whole from adult
Bone ash, comprise the following steps：
A. grinding bone ash to particle diameter is 10 μm, obtains 505g powders；
B. powder is added in 50% sulfuric acid solution, 30% salpeter solution, the mixed solution of 38% hydrochloric acid solution and dissolved, sulfuric acid
Solution, salpeter solution, the volume ratio of hydrochloric acid solution are 2:1:1,30min is reacted with rotating speed 100rpm in mixer after dissolving,
Then filter, carbon crude product is cleaned with distilled water, the pH value of regulation carbon crude product is 6；
C. carbon crude product is placed in inner string graphitization stove, 1.2h is purified at 1800 DEG C；
D. under 1200 DEG C, 1200MPa, the carbon extracted is all positioned over and is close to Ni-Mn-Co catalyst, diamond crystalline substance
The side planted, is cultivated.
Cultivate and complete to obtain orange diamond.
In the present embodiment, it is the carbon that sample tissue is extracted to cultivate the carbon 100% used in diamond, i.e., all from sample
The carbon that tissue extraction goes out, without additional carbon, view during cultivation is referring to Fig. 2.
Embodiment two
The preparation method that Fig. 3 shows the Jubilee that the embodiment of the present invention two is provided, sample tissue selects animal body skin
Skin, comprises the following steps：
A. animal body skin is put into dryer, the air of residual in nitrogen, discharge dryer is passed through, at 200 DEG C
Drying is 25% without bone tissue to its water content, is then crushed to particle diameter for 20 μm, obtains 500g powders, mixed in powder
Enter to mark carbon, powder is poured into the dehydrated alcohol that percentage by weight is 95%, be stirred continuously, then filter out powder, recycled
Organic element analyzer carries out elementary analysis to powder, and analysis is learnt in powder containing 0.09% metal ion；
B. powder is put into baking oven, completely cuts off air, and be passed through nitrogen and hydrogen drains the air remained in baking oven, hydrogen
Volume account for the 8% of volume of gas, powder is then heated to 800 DEG C, carburizing reagent 1h is carried out at this temperature, then removal of impurities,
Obtain carbon crude product；
C. toward sodium citrate is added in carbon crude product, the mass ratio of sodium citrate and carbon crude product is 1:10, then use distilled water
Cleaning, carbon crude product after cleaning added and dissolved in the mixed solution of 50% dilute sulfuric acid and 30% dust technology, dilute sulfuric acid and dust technology
Volume ratio is 1:1,20min is reacted with rotating speed 180rpm in mixer after dissolving, then filters, carbon crude product is cleaned with distilled water
It is 5 to its pH value, then carbon crude product is added to percentage by weight to occur neutralization reaction in 5% potassium hydroxide solution, adjusts pH
It is worth for 6, filtering, the solid matter for recycling distilled water cleaning to be filtrated to get, filtering；
Obtained carbon crude product is placed in acheson furnace, 1h is purified at 2500 DEG C；
Carbon crude product after purification is put into firing chamber, completely cuts off air, and is passed through chlorine, the sky remained in container is excluded
Gas, 2500 DEG C are warming up to by firing chamber, are calcined 1h；
D. under 2500 DEG C, 8000MPa, the carbon extracted is all positioned over and is close to Fe-Ni-Co catalyst, diamond crystalline substance
The side planted, is cultivated, carbon source is supplemented in cultivating process, the quality of supplement carbon and the carbon of the obtained purifications of step c
Than for 8.5:1, the carbon that supplement carbon is also gone out from animal body skin extraction, in supplement, supplement carbon surrounds what step c was extracted
Carbon, in inverted " recessed " word state, referring to Fig. 7, adds Titanium, cultivation obtains diamond in cultivating process；
E. at room temperature, obtained diamond is placed in the concentrated nitric acid that percentage by weight is 45% and cleans removal of impurities, until solution
In no longer produce bubble, and diamond surface without black attachment；
F. polish diamond, obtain white diamond, and collect the powder after polishing, the powder of acquisition is placed in a reservoir,
It is passed through pure oxygen and drains air, heating container makes diamond powder be reacted with pure oxygen, the carbon dioxide for reacting generation is led to 800 DEG C
Enter mass spectrograph to be analyzed, obtain the content Atom%5 of carbon 13 in diamond, determine the content Atom%4 of carbon 13 in supplement carbon,
Atom%5 is more than in Atom%4, diamond and contains the carbon in sample tissue.
In the present embodiment, the structure chart of the baking oven used in step b is referring to Fig. 4, and certainly, other embodiment is carrying out step b
Anaerobic high-temperature roasting when, the device can also be selected.
In the present embodiment, the structure chart of the acheson furnace used in step c referring to Fig. 5, the structure chart of firing chamber referring to Fig. 6,
Certainly, other embodiment can also select the graphitizing furnace and the calciner.
Embodiment three
The preparation method that Fig. 8 shows the Jubilee that the embodiment of the present invention three is provided, sample tissue is whole from children
Bone ash, comprise the following steps：
A. grinding bone ash to particle diameter is 18 μm, obtains 350g powders；
B. powder is added into percentage by weight to be dissolved in 50% phosphoric acid solution, gained mixture is then poured into stirring
In machine, 60min is handled under 100rpm rotating speed, then mixture is poured out, with the sodium hydroxide solution that percentage by weight is 5%
Generation neutralization reaction, regulation pH value is 6, filtering, then cleans the solid matter that is filtrated to get using distilled water, then by solids
Matter is placed in freeze-day with constant temperature stove, and 30min is dried at 130 DEG C, obtains carbon crude product；
C. obtained carbon crude product is placed in acheson furnace, 1h is purified at 2500 DEG C；
Carbon crude product after purification is put into firing chamber, completely cuts off air, vacuumizes, and is passed through chlorine, is excluded residual in container
The air stayed, 2500 DEG C are warming up to by firing chamber, are calcined 1h；
D. mark carbon is mixed into the carbon extracted, under 2000 DEG C, 2300MPa, extracting for mark carbon will be mixed with
Carbon be all positioned over and be close to Ni-Mn-Co catalyst, the side of diamond crystal seed, cultivated, carbon source carried out in cultivating process
The mass ratio of supplement, supplement carbon and the carbon of the obtained purifications of step c is 5:1, hair of the supplement carbon from the alive relatives of the deceased
The carbon extracted, in supplement, supplement carbon and the state that the carbon that step c is extracted is in two layers, referring to Fig. 9, after cultivating process
Electron beam irradiation processing is carried out to the diamond that cultivation is obtained, then by high annealing, obtains blue diamonds；
E. at room temperature, obtained diamond is placed in the concentrated sulfuric acid that percentage by weight is 75% and cleans removal of impurities, until solution
In no longer produce bubble, and diamond surface without black attachment；
F. polish diamond, and collect the powder after polishing, the powder of acquisition is placed in a reservoir, pure oxygen is passed through and drains sky
Gas, heating container makes diamond powder be reacted with pure oxygen to 800 DEG C, and the carbon dioxide for reacting generation is passed through into mass spectrograph is divided
Analysis, obtains the content Atom%5 of carbon 13 in diamond, and the content Atom%4, Atom%5 for determining carbon 13 in supplement carbon are more than Atom%4,
Contain the carbon in sample tissue in diamond.
In the present embodiment, the structure of cremator of bone ash is obtained referring to Figure 10, certainly, such a cremator is also not intended as limit
System, can also be from other cremators, and other embodiment cremate bone ash can also select the cremator.
In addition, in the prior art, carbon is purified using hair, the present embodiment is as contrast experiment：
Quality, i.e. the 500g hair such as take as sample, by it in the environment of isolation air, be heated to 500 DEG C, carbon
Obtain, containing the carbon that 2.5g purity is 98.8% in carbonized product, carbonized product, the carbon being used in into diamond and cultivated, also after change
Spectroscopically pure graphite powder need to be mixed into, and the ratio of spectroscopically pure graphite powder and the carbon of purification is 40:1.
The purity for the carbon that method of purification of the life entity without the carbon in bone tissue that the present embodiment is provided is extracted is 99.98%,
Purity is very high, can be directly used for diamond cultivation, and supplement carbon also need to only supplement the amount of the carbon of 5 times of extractions, and the method for purification is real
High with property, after production, its productive value is also very high.
The method of purification of the present invention is applied to all carbon-based life entities（Using carbohydrate as life basis）It is dynamic
Thing, plant, and animal, any of plant body can be used as purification body without bone tissue, containing bone tissue.
The purity for the carbon that the present invention is extracted can reach 99.8% and more than, can also realize what sample tissue was extracted
Carbon 100% is cultivated for diamond, and technically without artificially adding again, mixing high-purity commercial graphites to improve purity（Existing tradition
Method）.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (4)
1. a kind of preparation method of Jubilee, it is characterised in that comprise the following steps：
A. sample tissue is crushed, powder is obtained；The sample tissue is that the method for crushing is the grinding group containing bone containing bone tissue
The particle diameter knitted is to 6.5 ~ 25 μm；
B. the powder is added into percentage by weight to be dissolved in 5 ~ 75% acid solution, after 20 ~ 120 min of mixing, adjusts pH
It is worth for 6 ~ 7, obtains carbon crude product；
C. further purification is carried out to the carbon crude product using the one or more in high temperature graphitization purification, chloridising roasting to remove
It is miscellaneous；
D. under 1200 ~ 2500 DEG C, 1200 ~ 8000MPa, the carbon extracted is all positioned over and is close to metal solvent, diamond crystalline substance
The side planted, passes through HTHP gradient method（HPHT）Cultivate diamond；
E. at 20 ~ 90 DEG C, obtained diamond is placed in into concentrated nitric acid or percentage by weight that percentage by weight is 40 ~ 60% is
Removal of impurities is cleaned in 70 ~ 90% concentrated sulfuric acid, until bubble is no longer produced in solution, and the surface of the diamond is adhered to without black
Thing.
2. the preparation method of Jubilee according to claim 1, it is characterised in that in the HTHP gradient method
（HPHT）In cultivating process, in addition to processing of changing colour.
3. the preparation method of Jubilee according to claim 2, it is characterised in that described change colour is processed as：To system
Make white diamond, then denitrifier is added in cultivating process；To make diamond, then retain nickel member in cultivating process
Element, and add lithium nitride or magnesium nitride；To make red colour system diamond, then after cultivation, using electron beam irradiation diamond, then enter
Row the high temperature anneal；To make blueness or Black Diamond, then retain boron element in cultivating process, and add denitrifier.
4. the preparation method of Jubilee according to claim 1, it is characterised in that also need addition to supplement in cultivating process
Carbon.
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| CN113247892A (en) * | 2021-06-07 | 2021-08-13 | 杭州宝照晶体技术有限公司 | Method for preparing artificial diamond and crystal from mineral, bone ash and recycled material |
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| US20060261512A1 (en) * | 2003-02-25 | 2006-11-23 | Moti Weisbrot | Method of encapsulating material from humans or animals in a natural gemstone and its product |
| CN101124158A (en) * | 2005-02-21 | 2008-02-13 | 单晶研究有限公司 | Personalised synthetic diamond of different colours, obtained from (living or dead) human or animal keratin and production method thereof |
| CN102070136A (en) * | 2010-11-30 | 2011-05-25 | 李立华 | Extraction process of organism diamond raw material carbon |
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| US20060261512A1 (en) * | 2003-02-25 | 2006-11-23 | Moti Weisbrot | Method of encapsulating material from humans or animals in a natural gemstone and its product |
| CN101124158A (en) * | 2005-02-21 | 2008-02-13 | 单晶研究有限公司 | Personalised synthetic diamond of different colours, obtained from (living or dead) human or animal keratin and production method thereof |
| CN102070136A (en) * | 2010-11-30 | 2011-05-25 | 李立华 | Extraction process of organism diamond raw material carbon |
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